Science.gov

Sample records for active voltammetric microsensors

  1. Active voltammetric microsensors with neural signal processing.

    SciTech Connect

    Vogt, M. C.

    1998-12-11

    Many industrial and environmental processes, including bioremediation, would benefit from the feedback and control information provided by a local multi-analyte chemical sensor. For most processes, such a sensor would need to be rugged enough to be placed in situ for long-term remote monitoring, and inexpensive enough to be fielded in useful numbers. The multi-analyte capability is difficult to obtain from common passive sensors, but can be provided by an active device that produces a spectrum-type response. Such new active gas microsensor technology has been developed at Argonne National Laboratory. The technology couples an electrocatalytic ceramic-metallic (cermet) microsensor with a voltammetric measurement technique and advanced neural signal processing. It has been demonstrated to be flexible, rugged, and very economical to produce and deploy. Both narrow interest detectors and wide spectrum instruments have been developed around this technology. Much of this technology's strength lies in the active measurement technique employed. The technique involves applying voltammetry to a miniature electrocatalytic cell to produce unique chemical ''signatures'' from the analytes. These signatures are processed with neural pattern recognition algorithms to identify and quantify the components in the analyte. The neural signal processing allows for innovative sampling and analysis strategies to be employed with the microsensor. In most situations, the whole response signature from the voltammogram can be used to identify, classify, and quantify an analyte, without dissecting it into component parts. This allows an instrument to be calibrated once for a specific gas or mixture of gases by simple exposure to a multi-component standard rather than by a series of individual gases. The sampled unknown analytes can vary in composition or in concentration, the calibration, sensing, and processing methods of these active voltammetric microsensors can detect, recognize, and

  2. Molecular self-assembly of two-terminal, voltammetric microsensors with internal references.

    PubMed

    Hickman, J J; Ofer, D; Laibinis, P E; Whitesides, G M; Wrighton, M S

    1991-05-03

    Self-assembly of a ferrocenyl thiol and a quinone thiol onto Au microelectrodes forms the basis for a new microsensor concept: a two-terminal, voltammetric microsensor with reference and sensor functions on the same electrode. The detection is based on measurement of the potential difference of current peaks for oxidation and reduction of the reference (ferrocene) and indicator (quinone) in aqueous electrolyte in a two-terminal, linear sweep voltammogram in which a counterelectrode of relatively large surface area is used. The quinone has a half-wave potential, E((1/2)), that is pH-sensitive and can be used as a pH indicator; the ferrocene center has an E(1/2) that is a pH-insensitive reference. The key advantages are that such sensors require no separate reference electrode and function as long as current peaks can be located for reference and indicator molecules.

  3. Molecular Self-Assembly of Two-Terminal, Voltammetric Microsensors with Internal References

    NASA Astrophysics Data System (ADS)

    Hickman, James J.; Ofer, David; Laibinis, Paul E.; Whitesides, George M.; Wrighton, Mark S.

    1991-05-01

    Self-assembly of a ferrocenyl thiol and a quinone thiol onto Au microelectrodes forms the basis for a new microsensor concept: a two-terminal, voltammetric microsensor with reference and sensor functions on the same electrode. The detection is based on measurement of the potential difference of current peaks for oxidation and reduction of the reference (ferrocene) and indicator (quinone) in aqueous electrolyte in a two-terminal, linear sweep voltammogram in which a counterelectrode of relatively large surface area is used. The quinone has a half-wave potential, E1/2, that is pH-sensitive and can be used as a pH indicator; the ferrocene center has an E1/2 that is a pH-insensitive reference. The key advantages are that such sensors require no separate reference electrode and function as long as current peaks can be located for reference and indicator molecules.

  4. Microsensors as a tool to determine chemical microgradients and bacterial activity in wastewater biofilms and flocs.

    PubMed

    Santegoeds, C M; Schramm, A; de Beer, D

    1998-01-01

    Microsensors used in microbial ecology are reviewed with emphasis on new sensor developments (NO3-, NO2-, NH4+, CO2, H2, H2S and CH4 microsensors as well as fiberoptical microsensors for O2, temperature and pH). Examples of microsensor applications in biofilms and activated sludge flocs are presented, in which sulfate reduction and denitrification were studied.

  5. A method to determine photosynthetic activity from oxygen microsensor data in biofilms subjected to evaporation.

    PubMed

    Li, Tong; Podola, Björn; de Beer, Dirk; Melkonian, Michael

    2015-10-01

    Phototrophic biofilms are widely distributed in nature and their ecological importance is well recognized. More recently, there has been a growing interest in using artificial phototrophic biofilms in innovative photobioreactors for production of microalgal biomass in biotechnological applications. To study physiological processes within these biofilms, microsensors have been applied in several studies. Here, the 'light-dark shift method' relies on measurement of photosynthetic activity in terms of light-induced oxygen production. However, when applied to non-submerged biofilms that can be found in numerous locations in nature, as well as in some types of photobioreactors, limitations of this approach are obvious due to rapid removal of gaseous species at the biofilm surface. Here, we introduce a mathematical correction to recover the distribution of the actual photosynthetic activity along the depth gradient in the biofilm, based on a numerical solution of the inversed diffusion equation of oxygen. This method considers changes in mass transport during the measurement period as can found on biofilms possessing a thin flow/mass transfer boundary layer (e. g., non-submerged biofilms). Using both simulated and real microsensor data, the proposed method was shown to be much more accurate than the classical method, which leads to underestimations of rates near the biofilm surface. All test profiles could be recovered with a high fit. According to our simulated microsensor measurements, a depth resolution of ≤20 μm is recommended near the surface. We conclude that our method strongly improves the quality of data acquired from light-dark measurements of photosynthetic activity in biofilms.

  6. Advanced Microsensors

    NASA Technical Reports Server (NTRS)

    1991-01-01

    This video looks at a spinoff application of the technology from advanced microsensors -- those that monitor and determine conditions of spacecraft like the Space Shuttle. The application featured is concerned with the monitoring of the health of premature babies.

  7. Advanced Microsensors

    NASA Technical Reports Server (NTRS)

    1991-01-01

    This video looks at a spinoff application of the technology from advanced microsensors -- those that monitor and determine conditions of spacecraft like the Space Shuttle. The application featured is concerned with the monitoring of the health of premature babies.

  8. Overjet reduction in relation to wear time with the van Beek activator combined with a microsensor.

    PubMed

    Al-Kurwi, Ali S A; Bos, Annemieke; Kuitert, Reinder B

    2017-02-01

    The aim of this study was to use a microsensor to investigate the association among overjet reduction, treatment duration, and wear time of the van Beek activator. The study sample comprised patients (n = 28) with a mean age of 11.60 (±1.25) years at start of treatment treated with the van Beek activator. The prescribed wear time was 12 hours per day. The evaluation period was limited to the first 3 appointments. The wear times during the 3 intervals were assessed. Treatment periods with good compliance were characterized by a wear time of 8 hours or more per day. The medians of overjet were 9.00 mm at the start of treatment and 5.75 mm at the third appointment. The mean total wear time throughout the evaluation period was 7.75 (±3.66) hours per day. Significant correlations were found at the 3 intervals. Patients with a mean wear time of 8 hours or more per day achieved significantly greater overjet reductions. Patients with good compliance of at least 5 months showed significantly greater overjet reductions. Significant overjet reduction was achieved with a minimum daily wear time of 8 hours for at least 5 months. The level of compliance had a strong tendency to be maintained throughout the treatment period. No patient achieved the prescribed wear time of 12 hour per day. Copyright © 2017 American Association of Orthodontists. Published by Elsevier Inc. All rights reserved.

  9. Influence of uranium (VI) on the metabolic activity of stable multispecies biofilms studied by oxygen microsensors and fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Krawczyk-Bärsch, Evelyn; Grossmann, Kay; Arnold, Thuro; Hofmann, Susann; Wobus, Axel

    2008-11-01

    The effect of uranium added in ecologically relevant concentrations (1 × 10 -5 and 1 × 10 -6 M) to stable multispecies biofilms was studied by electrochemical oxygen microsensors with tip diameters of 10 μm and by confocal laser fluorescence microscopy (CLSM). The microsensor profile measurements in the stable multispecies biofilms exposed to uranium showed that the oxygen concentration decreased faster with increasing biofilm depth compared to the uranium free biofilms. In the uranium containing biofilms, the oxygen consumption, calculated from the steady-state microprofiles, showed high consumption rates of up to 61.7 nmol cm -3 s -1 in the top layer (0-70 μm) and much lower consumption rates in the lower zone of the biofilms. Staining experiments with 5-cyano-2,3-ditolyl tetrazolium chloride (CTC) and 4,6-diamidino-2-phenylindole (DAPI) confirmed the high respiratory activities of the bacteria in the upper layer. Analysis of the amplified 16S rRNA gene fragments showed that the addition of uranium in ecologically relevant concentrations did not change the bacterial diversity in the stable multispecies biofilms and is therefore not responsible for the different oxygen profiles in the biofilms. The fast decrease in the oxygen concentrations in the biofilm profiles showed that the bacteria in the top region of the biofilms, i.e., the metabolically most active biofilm zone, battle the toxic effects of aqueous uranium with an increased respiratory activity. This increased respiratory activity results in O 2 depleted zones closer to the biofilm/air interface which may trigger uranium redox processes, since suitable redox partners, e.g., extracellular polymeric substance (EPS) and other organics (e.g., metabolites), are sufficiently available in the biofilm porewaters. Such redox reactions may lead to precipitation of uranium (IV) solids and consequently to a removal of uranium from the aqueous phase.

  10. Acoustic, fiber optic, and silicon microelectronic microsensors research and development activities at Sandia National Laboratories

    SciTech Connect

    Wiczer, J.J.

    1993-08-01

    Sandia National Laboratories, an 8500+ person, multiprogram research and development facility operated for the US Department of Energy, has over 400 research, development and applications scientists and engineers working on sensor technologies. Sandia`s 20 person Microsensors Research and Development Department has invented, developed and fielded sensor systems based on acoustic, fiber optic, and silicon microelectronic technologies. These sensors have been used for diverse applications inducting the monitoring of cleaning chemical concentrations in industrial process effluent streams, detection of explosive gas concentrations in aging industrial equipment, real-time measurements of fluid viscosity in equipment lubricants, and monitoring of contaminant concentration levels in ultrapure process gases. Representative sensor technologies available for technology transfer will be described including bulk acoustic wave resonators, surface acoustic wave devices, fiber optic micromirror sensors, and silicon microelectronic sensors.

  11. Monitoring sulfide-oxidizing biofilm activity on cement surfaces using non-invasive self-referencing microsensors.

    PubMed

    Cheng, Liqiu; House, Mitch W; Weiss, W Jason; Banks, M Katherine

    2016-02-01

    Microbially influenced corrosion (MIC) in concrete results in significant cost for infrastructure maintenance. Prior studies have employed molecular techniques to identify microbial community species in corroded concrete, but failed to explore bacterial activity and functionality during deterioration. In this study, biofilms of different sulfur-oxidizing bacteria compositions were developed on the surface of cement paste samples to simulate the natural ecological succession of microbial communities during MIC processes. Noninvasive, self-referencing (SR) microsensors were used to quantify real time changes of oxygen, hydrogen ion and calcium ion flux for the biofilm to provide more information about bacterial behavior during deterioration. Results showed higher transport rates in oxygen consumption, and hydrogen ion at 4 weeks than 2 weeks, indicating increased bacterial activity over time. Samples with five species biofilm had the highest hydrogen ion and calcium ion transport rates, confirming attribution of acidophilic sulfur-oxidizing microorganisms (ASOM). Differences in transport rates between three species samples and two species samples confirmed the diversity between Thiomonas intermedia and Starkeya novella. The limitations of SR sensors in corrosion application could be improved in future studies when combined with molecular techniques to identify the roles of major bacterial species in the deterioration process.

  12. Comparative investigation of antioxidant activity of human serum blood by amperometric, voltammetric and chemiluminescent methods

    PubMed Central

    Korotkova, Elena; Voronova, Olesya; Sazhina, Natalia; Petrova, Ekatherina; Artamonov, Anton; Chernyavskaya, Ludmila; Dorozhko, Elena

    2015-01-01

    Introduction A blood test can provide important information about the functional state of the antioxidant system. Malfunction of this system increases the concentration of free radicals and can cause oxidative stress. A difficulty in assessing oxidative stress is the lack of a universal method for determining the antioxidant activity (AOA) of blood components, because of their different nature. Material and methods The objects of investigation were sera of 30 male patients with a diagnosis of alcohol dependence syndrome and healthy donors. Comparative investigation of total antioxidant activity (TAA) of human serum blood was carried out by voltammetric (VA), amperometric (AM) and chemiluminescent (HL) methods. Results All applied methods revealed that serum TAA of the patients with alcoholism is lower than TAA of healthy donors (control group); according to amperometric method the average value of serum TAA was 850 ±210 nA × s, and 660 ±150 nA × s for healthy donors and alcoholics respectively (p < 0.05). Similar trend was revealed by chemiluminescence and voltammetry methods. The results confirm that thiol compounds make a significant contribution to the antioxidant activity of serum. The average thiol concentrations were 0.94 ±0.34 mmol/l and 1.21 ±0.36 mmol/l (p < 0.05) for alcoholics and healthy donors respectively. Decreasing thiol concentration in blood of alcoholics leads to depletion of antioxidant systems of blood. However, the differences between the results of AM, VA and HL methods were significant, because they reflected different aspects of antioxidant activity. Conclusions For objective assessment of antioxidant activity of biological objects, we suggest using methods based on different model systems. PMID:27695499

  13. LLNL Microsensors Program

    SciTech Connect

    Lavietes, A

    2004-04-26

    The Microsensors Program was born out the need for enhanced sensor technology in support of the Weapons Program. In the interest of expanded diagnostic capabilities to provide true performance characteristics of weapon assemblies in flight and ground tests, a suite of sensor requirements was proposed. These potential new sensor technologies were envisioned to be completely unobtrusive and allow for the development of test vehicles (mock warheads and bomb assemblies) that were designed to mechanical and electrical specifications as close to the stockpile weapon design configuration as possible. The closeness of a test vehicle design to the respective stockpile weapon design is referred to as ''fidelity,'' with the term ''high-fidelity'' to mean all components are designed to emulate, very closely, the true system design. These efforts were in line with many activities associated with Stockpile Stewardship and were intended to enable better modeling and performance assessment without the need for underground testing. Several weapons are currently undergoing Life Extension Programs (LEP) to lengthen each weapon system's respective service life. The ability to assess the projected life of these complex assemblies is crucial to the success of the LEP activities.

  14. Microsensors for border patrol applications

    NASA Astrophysics Data System (ADS)

    Falkofske, Dwight; Krantz, Brian; Shimazu, Ron; Berglund, Victor

    2005-05-01

    A top concern in homeland security efforts is the lack of ability to monitor the thousands of miles of open border with our neighbors. It is not currently feasible to continually monitor the borders for illegal intrusions. The MicroSensor System (MSS) seeks to achieve a low-cost monitoring solution that can be efficiently deployed for border patrol applications. The modifications and issues regarding the unique requirements of this application will be discussed and presented. The MicroSensor System was developed by the Defense Microelectronics Activity (DMEA) for military applications, but border patrol applications, with their unique sensor requirements, demand careful adaptation and modification from the military application. Adaptation of the existing sensor design for border applications has been initiated. Coverage issues, communications needs, and other requirements need to be explored for the border patrol application. Currently, border patrol has a number of deficiencies that can be addressed with a microsensor network. First, a distributed networked sensor field could mitigate the porous border intruder detection problem. Second, a unified database needs to be available to identify aliens attempting to cross into the United States. This database needs to take unique characteristics (e.g. biometrics, fingerprints) recovered from a specialized field unit to reliably identify intruders. Finally, this sensor network needs to provide a communication ability to allow border patrol officers to have quick access to intrusion information as well as equipment tracking and voice communication. MSS already addresses the sensing portion of the solution, including detection of acoustic, infrared, magnetic, and seismic events. MSS also includes a low-power networking protocol to lengthen the battery life. In addition to current military requirements, MSS needs a solar panel solution to extend its battery life to 5 years, and an additional backbone communication link

  15. Catalase activity of cytochrome C oxidase assayed with hydrogen peroxide-sensitive electrode microsensor.

    PubMed

    Bolshakov, I A; Vygodina, T V; Gennis, R; Karyakin, A A; Konstantinov, A A

    2010-11-01

    An iron-hexacyanide-covered microelectrode sensor has been used to continuously monitor the kinetics of hydrogen peroxide decomposition catalyzed by oxidized cytochrome oxidase. At cytochrome oxidase concentration ~1 µM, the catalase activity behaves as a first order process with respect to peroxide at concentrations up to ~300-400 µM and is fully blocked by heat inactivation of the enzyme. The catalase (or, rather, pseudocatalase) activity of bovine cytochrome oxidase is characterized by a second order rate constant of ~2·10(2) M(-1)·sec(-1) at pH 7.0 and room temperature, which, when divided by the number of H2O2 molecules disappearing in one catalytic turnover (between 2 and 3), agrees reasonably well with the second order rate constant for H2O2-dependent conversion of the oxidase intermediate F(I)-607 to F(II)-580. Accordingly, the catalase activity of bovine oxidase may be explained by H2O2 procession in the oxygen-reducing center of the enzyme yielding superoxide radicals. Much higher specific rates of H2O2 decomposition are observed with preparations of the bacterial cytochrome c oxidase from Rhodobacter sphaeroides. The observed second order rate constants (up to ~3000 M(-1)·sec(-1)) exceed the rate constant of peroxide binding with the oxygen-reducing center of the oxidized enzyme (~500 M(-1)·sec(-1)) several-fold and therefore cannot be explained by catalytic reaction in the a(3)/Cu(B) site of the enzyme. It is proposed that in the bacterial oxidase, H2O2 can be decomposed by reacting with the adventitious transition metal ions bound by the polyhistidine-tag present in the enzyme, or by virtue of reaction with the tightly-bound Mn2+, which in the bacterial enzyme substitutes for Mg2+ present in the mitochondrial oxidase.

  16. Integrated Microsensors for Autonomous Microrobots

    SciTech Connect

    ADKINS, DOUGLAS R.; BYRNE, RAYMOND H.; HELLER, EDWIN J.; WOLF, JIMMIE V.

    2003-02-01

    This report describes the development of a miniature mobile microrobot device and several microsystems needed to create a miniature microsensor delivery platform. This work was funded under LDRD No.10785, entitled, ''Integrated Microsensors for Autonomous Microrobots''. The approach adopted in this project was to develop a mobile platform, to which would be attached wireless RF remote control and data acquisition in addition to various microsensors. A modular approach was used to produce a versatile microrobot platform and reduce power consumption and physical size.

  17. Encapsulated microsensors for reservoir interrogation

    SciTech Connect

    Scott, Eddie Elmer; Aines, Roger D.; Spadaccini, Christopher M.

    2016-03-08

    In one general embodiment, a system includes at least one microsensor configured to detect one or more conditions of a fluidic medium of a reservoir; and a receptacle, wherein the receptacle encapsulates the at least one microsensor. In another general embodiment, a method include injecting the encapsulated at least one microsensor as recited above into a fluidic medium of a reservoir; and detecting one or more conditions of the fluidic medium of the reservoir.

  18. Development process of automotive microsensors

    NASA Astrophysics Data System (ADS)

    Tang, William C.

    1995-05-01

    The phased product development approach can be applied advantageously to develop and manufacture automotive microsensors. The phased approach involves a multifunctional team from innovation to development to eventual production and maintenance phases. The key advantage of this approach is the shortened development cycle and fast product introduction, while minimizing waste of resources and lowering risk of product failure. When applied to the product cycles of automotive sensors based on micromachining technology, this approach elucidates several critical considerations. In particular, since industrial application of micromachining technology is still at the infant stage, standards and design rules are not firmly established. Therefore, several important activities must be initiated simultaneously from the start of the innovation phase, which proves to be crucial to the prudent decision of technology alternatives and sensor system configuration. The use of a multifunctional team, as mandated in the phased approach, enables coherent development and optimization of the sense element, the fabrication technology, the packaging approach, the interface circuit configuration, and design features that allow efficient test and assembly flow. Also, with intermediate milestones within each phase, risk assessment and necessary midcourse adjustment to technology trade- offs can be both timely and accurate. Accelerometers, one of the most developed micromachined sensors, serve as representative examples that illustrate how the phased approach can benefits the commercialization of the newly established and rapidly expanding field of micromechanics.

  19. Voltammetric determination of ruthenium in the form of complexes with biologically active ligands

    SciTech Connect

    Medyantseva, E.P.; Budnikov, G.K.; Balakaeva, T.A.

    1992-02-10

    The interest in the analytical chemistry of ruthenium and its compounds has recently been increasing. Ruthenium compounds can be used an antitumor agents and in the treatment of tuberculosis and fungal infections. It has been suggested that there is a specific relationship between the reduction potentials of the compounds and their biological activity. Of greatest interest among the biologically active compounds are the compounds with nitrogen-containing heterocycles. In order to obtain information on the degree of oxidation of the central atom in the complexes and to select the optimum conditions for the determination of the mono- and bi-nuclear complexes of ruthenium compounds with biologically active ligands such as imidazole (Im), histidine (His), benzimidazole (BIm) and its methyl derivative [1,2(CH{sub 3}){sub 2} - BIm], benzohyroxamic acid (Bha), and 1-phenyl-2-methylamino-1-propanol or ephedrine (Eph) in the present work, the authors studied their electrochemical behavior at dropping mercury (dme) and a platinum electrodes. 6 refs., 1 fig., 2 tabs.

  20. Voltammetric determination of TBHQ at a glassy carbon electrode surface activated by in situ chemical oxidation.

    PubMed

    Wang, Zhen; Yang, Feng; Zheng, Hao; Qin, Xianjing; Luo, Jiaojiao; Li, Yue; Xiao, Dan

    2014-07-21

    In this article, a bare glassy carbon electrode (GCE) surface was directly activated by a simple in situ chemical method, which was characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Based on these results, it was found that oxygen-containing functional groups at the modified GCE surface were enhanced with a low damage to the surface state. Hence, the modified GCE exhibited an excellent performance, such as the negatively charged surface, good reproducibility and high selectivity. The resulting electrode was applied as a sensitive sensor for detection of antioxidant tertiary butyl hydroquinone (TBHQ), and a good linear relationship was obtained between the oxidation peak current and the concentration in a broad range of 1.0 μM-1.1 mM, with detection limits of 67 nM (S/N = 3) by DPV. Electrochemical parameters of TBHQ on the resulting GCE were also investigated, suggesting that the modified GCE could promote electron transfer kinetics towards the electrochemical reaction of TBHQ. Besides, the present method was used for determination of TBHQ in jatropha biodiesel with recovery ranging from 95.2% to 103.2%.

  1. Chemical Microsensor Development for Aerospace Applications

    NASA Technical Reports Server (NTRS)

    Xu, Jennifer C.; Hunter, Gary W.; Lukco, Dorothy; Chen, Liangyu; Biaggi-Labiosa, Azlin M.

    2013-01-01

    Numerous aerospace applications, including low-false-alarm fire detection, environmental monitoring, fuel leak detection, and engine emission monitoring, would benefit greatly from robust and low weight, cost, and power consumption chemical microsensors. NASA Glenn Research Center has been working to develop a variety of chemical microsensors with these attributes to address the aforementioned applications. Chemical microsensors using different material platforms and sensing mechanisms have been produced. Approaches using electrochemical cells, resistors, and Schottky diode platforms, combined with nano-based materials, high temperature solid electrolytes, and room temperature polymer electrolytes have been realized to enable different types of microsensors. By understanding the application needs and chemical gas species to be detected, sensing materials and unique microfabrication processes were selected and applied. The chemical microsensors were designed utilizing simple structures and the least number of microfabrication processes possible, while maintaining high yield and low cost. In this presentation, an overview of carbon dioxide (CO2), oxygen (O2), and hydrogen/hydrocarbons (H2/CxHy) microsensors and their fabrication, testing results, and applications will be described. Particular challenges associated with improving the H2/CxHy microsensor contact wire-bonding pad will be discussed. These microsensors represent our research approach and serve as major tools as we expand our sensor development toolbox. Our ultimate goal is to develop robust chemical microsensor systems for aerospace and commercial applications.

  2. The Use of Wearable Microsensors to Quantify Sport-Specific Movements.

    PubMed

    Chambers, Ryan; Gabbett, Tim J; Cole, Michael H; Beard, Adam

    2015-07-01

    Microtechnology has allowed sport scientists to understand the locomotor demands of various sports. While wearable global positioning technology has been used to quantify the locomotor demands of sporting activities, microsensors (i.e. accelerometers, gyroscopes and magnetometers) embedded within the units also have the capability to detect sport-specific movements. The objective of this study was to determine the extent to which microsensors (also referred to as inertial measurement units and microelectromechanical sensors) have been utilised in quantifying sport-specific movements. A systematic review of the use of microsensors and associated terms to evaluate sport-specific movements was conducted; permutations of the terms used included alternate names of the various technologies used, their applications and different applied environments. Studies for this review were published between 2008 and 2014 and were identified through a systematic search of six electronic databases: Academic Search Complete, CINAHL, PsycINFO, PubMed, SPORTDiscus, and Web of Science. Articles were required to have used athlete-mounted sensors to detect sport-specific movements (e.g. rugby union tackle) rather than sensors mounted to equipment and monitoring generic movement patterns. A total of 2395 studies were initially retrieved from the six databases and 737 results were removed as they were duplicates, review articles or conference abstracts. After screening titles and abstracts of the remaining papers, the full text of 47 papers was reviewed, resulting in the inclusion of 28 articles that met the set criteria around the application of microsensors for detecting sport-specific movements. Eight articles addressed the use of microsensors within individual sports, team sports provided seven results, water sports provided eight articles, and five articles addressed the use of microsensors in snow sports. All articles provided evidence of the ability of microsensors to detect sport

  3. Microsensors and microscale gradients in biofilms.

    PubMed

    Beyenal, Haluk; Babauta, Jerome

    2014-01-01

    Understanding the limiting factors and mechanisms of biofilm processes requires the direct measurement of microscale gradients using the appropriate tools. Microscale measurements can provide mechanistic information that cannot be obtained from bulk-scale measurements. Among the most used and trusted tools in microscale biofilm research are microsensors. The goal of this chapter is to introduce microsensor technology along with several examples to illustrate microscale processes in biofilms that are usually absent in bulk. We define a microsensor for biofilm research as a needle-type sensor with tip diameter of a few microns and a length up to several hundred microns. Microsensors can be used noninvasively to monitor in situ biofilm processes. Both optical and electrochemical microsensors can be used for biofilm applications. Because of newly discovered biofilm processes, the design and use of microsensors require customization and carefully designed experiments. In this chapter we present several examples describing the use of microsensors (1) in environmental biofilms, (2) in medical biofilms, and (3) in biofilms for energy and bioproducts. Microsensors can be the most useful if the measured profiles are integrated into the study of overall biofilm processes.

  4. Microsensor Technologies for Plant Growth System Monitoring

    NASA Technical Reports Server (NTRS)

    Kim, Chang-Soo

    2004-01-01

    This document covered the following: a) demonstration of feasibility of microsensor for tube and particulate growth systems; b) Dissolved oxygen; c)Wetness; d) Flexible microfluidic substrate with microfluidic channels and microsensor arrays; e)Dynamic root zone control/monitoring in microgravity; f)Rapid prototyping of phytoremediation; and g) A new tool for root physiology and pathology.

  5. Miniature optical fiber pressure microsensors for in vivo measurement of intramuscular pressure

    NASA Astrophysics Data System (ADS)

    Cottler, P. S.; Blevins, D.; Averett, J.; Wavering, T. A.; Morrow, D. A.; Shin, A. Y.; Kaufman, K. R.

    2007-02-01

    An innovative fiber optic pressure microsensor has been developed that is based upon on Luna Innovations' patented extrinsic Fabry-Perot interferometric (EFPI) technique. The basic physics governing the operation of these sensors makes them relatively tolerant or immune to the effects of high-temperature, high-EMI, and highly-corrosive environments. Luna's pressure microsensor is extremely small, with an outer diameter of only 200 microns and a length of less than 1mm. The pressure microsensor has a high sensitivity that allows for sub-mmHg resolution over a dynamic range of 0-300 mmHg. The combination of these features makes this pressure microsensor ideal for medical applications where small size, high sensitivity and accuracy, EMI immunity, biocompatibility, and survivability (e.g. sterilizable - steam, ethylene oxide) are important. One example medical application of the pressure microsensor has been to adapt the microsensor for measurement of intramuscular pressure in vivo during active and passive muscle activation. Clinically it is difficult to study the in vivo mechanical properties of individual skeletal muscles for a variety of reasons. Initial experiments have demonstrated a correlation between intramuscular pressure and force. Such measurements can be a useful diagnostic tool for clinicians assessing muscular deficits in patients.

  6. Chemical micro-sensor

    DOEpatents

    Ruggiero, Anthony J.

    2005-05-03

    An integrated optical capillary electrophoresis system for analyzing an analyte. A modulated optical pump beam impinges on an capillary containing the analyte/buffer solution which is separated by electrophoresis. The thermally-induced change in the index of refraction of light in said electrophoresis capillary is monitored using an integrated micro-interferometer. The interferometer includes a first interferometer arm intersecting the electrophoresis capillary proximate the excitation beam and a second, reference interferometer arm. Changes in index of refraction in the analyte measured by interrogating the interferometer state using white light interferometry and a phase-generated carrier demodulation technique. Background thermo-optical activity in the buffer solution is cancelled by splitting the pump beam and exciting pure buffer solution in a second section of capillary where it crosses the reference arm of the interferometer.

  7. Flexible Microsensor Array for the Monitoring and Control of Plant Growth System

    NASA Technical Reports Server (NTRS)

    Kim, Chang-Soo; Porterfield, D. Marshall; Nagle, H. Troy; Brown, Christopher S.

    2004-01-01

    Testing for plant experiments in space has begun to explore active nutrient delivery concepts in which water and nutrients are replenished on a continuous basis for long-term growth. The goal of this study is to develop a novel microsensor array to provide information on the dissolved oxygen environment in the plant root zone for the optimum control of hydroponics and solid substrate plant cultivation systems in the space environment. Miniaturized polarographic dissolved oxygen sensors have been designed and fabricated on a flexible Kapton (trademark) (polyimide) substrate. Two capabilities of the new microsensor array were explored. First, measurements of dissolved oxygen in the plant root zone in hydroponics and solid substrate culture systems were made. The microsensor array was fabricated on a flexible substrate, and then cut out into a mesh type to make a suspended array that could be placed either in a hydroponics system or in a solid substrate cultivation system to measure the oxygen environments. Second, the in situ self-diagnostic and self-calibration capability (two-point for oxygen) was adopted by dynamically controlling the microenvironment in close proximity to the microsensors. With a built-in generating electrode that surrounds the microsensor, two kinds of microenvironments (oxygen-saturated and oxygen-depleted phases) could be established by water electrolysis depending on the polarity of the generating electrode. The unique features of the new microsensor array (small size, multiple sensors, flexibility and self-diagnosis) can have exceptional benefits for the study and optimization of plant cultivation systems in both terrestrial and microgravity environments. The in situ self-diagnostic and self-calibration features of the microsensor array will also enable continuous verification of the operability during entire plant growth cycles. This concept of automated control of a novel chemical monitoring system will minimize crew time required for

  8. Flexible Microsensor Array for the Monitoring and Control of Plant Growth System

    NASA Technical Reports Server (NTRS)

    Kim, Chang-Soo; Porterfield, D. Marshall; Nagle, H. Troy; Brown, Christopher S.

    2004-01-01

    Testing for plant experiments in space has begun to explore active nutrient delivery concepts in which water and nutrients are replenished on a continuous basis for long-term growth. The goal of this study is to develop a novel microsensor array to provide information on the dissolved oxygen environment in the plant root zone for the optimum control of hydroponics and solid substrate plant cultivation systems in the space environment. Miniaturized polarographic dissolved oxygen sensors have been designed and fabricated on a flexible Kapton (trademark) (polyimide) substrate. Two capabilities of the new microsensor array were explored. First, measurements of dissolved oxygen in the plant root zone in hydroponics and solid substrate culture systems were made. The microsensor array was fabricated on a flexible substrate, and then cut out into a mesh type to make a suspended array that could be placed either in a hydroponics system or in a solid substrate cultivation system to measure the oxygen environments. Second, the in situ self-diagnostic and self-calibration capability (two-point for oxygen) was adopted by dynamically controlling the microenvironment in close proximity to the microsensors. With a built-in generating electrode that surrounds the microsensor, two kinds of microenvironments (oxygen-saturated and oxygen-depleted phases) could be established by water electrolysis depending on the polarity of the generating electrode. The unique features of the new microsensor array (small size, multiple sensors, flexibility and self-diagnosis) can have exceptional benefits for the study and optimization of plant cultivation systems in both terrestrial and microgravity environments. The in situ self-diagnostic and self-calibration features of the microsensor array will also enable continuous verification of the operability during entire plant growth cycles. This concept of automated control of a novel chemical monitoring system will minimize crew time required for

  9. Voltammetric characterization of the aerobic energy-dissipating nitrate reductase of Paracoccus pantotrophus: exploring the activity of a redox-balancing enzyme as a function of electrochemical potential.

    PubMed

    Gates, Andrew J; Richardson, David J; Butt, Julea N

    2008-01-01

    Paracoccus pantotrophus expresses two nitrate reductases associated with respiratory electron transport, termed NapABC and NarGHI. Both enzymes derive electrons from ubiquinol to reduce nitrate to nitrite. However, while NarGHI harnesses the energy of the quinol/nitrate couple to generate a transmembrane proton gradient, NapABC dissipates the energy associated with these reducing equivalents. In the present paper we explore the nitrate reductase activity of purified NapAB as a function of electrochemical potential, substrate concentration and pH using protein film voltammetry. Nitrate reduction by NapAB is shown to occur at potentials below approx. 0.1 V at pH 7. These are lower potentials than required for NarGH nitrate reduction. The potentials required for Nap nitrate reduction are also likely to require ubiquinol/ubiquinone ratios higher than are needed to activate the H(+)-pumping oxidases expressed during aerobic growth where Nap levels are maximal. Thus the operational potentials of P. pantotrophus NapAB are consistent with a productive role in redox balancing. A Michaelis constant (K(M)) of approx. 45 muM was determined for NapAB nitrate reduction at pH 7. This is in line with studies on intact cells where nitrate reduction by Nap was described by a Monod constant (K(S)) of less than 15 muM. The voltammetric studies also disclosed maximal NapAB activity in a narrow window of potential. This behaviour is resistant to change of pH, nitrate concentration and inhibitor concentration and its possible mechanistic origins are discussed.

  10. ISFET Based Microsensors for Environmental Monitoring

    PubMed Central

    Jimenez-Jorquera, Cecilia; Orozco, Jahir; Baldi, Antoni

    2010-01-01

    The use of microsensors for in-field monitoring of environmental parameters is gaining interest due to their advantages over conventional sensors. Among them microsensors based on semiconductor technology offer additional advantages such as small size, robustness, low output impedance and rapid response. Besides, the technology used allows integration of circuitry and multiple sensors in the same substrate and accordingly they can be implemented in compact probes for particular applications e.g., in situ monitoring and/or on-line measurements. In the field of microsensors for environmental applications, Ion Selective Field Effect Transistors (ISFETs) have a special interest. They are particularly helpful for measuring pH and other ions in small volumes and they can be integrated in compact flow cells for continuous measurements. In this paper the technologies used to fabricate ISFETs and a review of the role of ISFETs in the environmental field are presented. PMID:22315527

  11. Electrochemical microsensor system for cancer research on photodynamic therapy in vitro

    NASA Astrophysics Data System (ADS)

    Marzioch, J.; Kieninger, J.; Sandvik, J. A.; Pettersen, E. O.; Peng, Q.; Urban, G.

    2016-10-01

    An electrochemical microsensor system to investigate photodynamic therapy of cancer cells in vitro was developed and applied to monitor the cellular respiration during and after photodynamic therapy. The redox activity and therefore influence of the photodynamic drug on the sensor performance was investigated by electrochemical characterization. It was shown, that appropriate operation conditions avoid cross-sensitivity of the sensors to the drug itself. The presented system features a cell culture chamber equipped with microsensors and a laser source to photodynamically treat the cells while simultaneous monitoring of metabolic parameter in situ. Additionally, the optical setup allows to read back fluorescence signals from the photosensitizer itself or other marker molecules parallel to the microsensor readings.

  12. An Electrochemical Microsensor Based on a AuNPs-Modified Microband Array Electrode for Phosphate Determination in Fresh Water Samples †

    PubMed Central

    Wang, Fangfang; Tong, Jianhua; Li, Yang; Bian, Chao; Sun, Jizhou; Xia, Shanhong

    2014-01-01

    This work describes the fabrication, characterization, and application of a gold microband array electrode (MAE) for the determination of phosphate in fresh water samples. The working principle of this MAE is based on the reduction of a molybdophosphate complex using the linear sweep voltammetric (LSV) method. The calibration of this microsensor was performed with standard phosphate solutions prepared with KH2PO4 and pH adjusted to 1.0. The microsensor consists of a platinum counter electrode, a gold MAE as working electrode, and an Ag/AgCl electrode as reference electrode. The microelectrode chips were fabricated by the Micro Electro-Mechanical System (MEMS) technique. To improve the sensitivity, gold nanoparticles (AuNPs) were electrodeposited on the working electrode. With a linear range from 0.02 to 0.50 mg P/L, the sensitivity of the unmodified microsensor is 2.40 μA per (mg P/L) (R2 = 0.99) and that of the AuNPs-modified microsensor is 7.66 μA per (mg P/L) (R2 = 0.99). The experimental results showed that AuNPs-modified microelectrode had better sensitivity and a larger current response than the unmodified microelectrode. PMID:25536001

  13. MicroSensors Systems: detection of a dismounted threat

    NASA Astrophysics Data System (ADS)

    Shimazu, Ron N.; Berglund, Victor P.; Falkofske, Dwight M.; Krantz, Brian S.

    2004-11-01

    The MicroSensors Systems (MSS) Program is developing a layered sensor network to detect dismounted threats approaching high value assets. The MSS subsystem elements include sensitive receivers (capable of detecting<<1 Watt emissions in dense signal or degraded signal environments) and low power, miniature, disposable sensors (acoustic, magnetic, and infrared). A novel network protocol has been developed to reduce the network traffic resulting in conservation of system power and lower probability of detection and interception. The MSS program will provide unprecedented levels of real-time battlefield information, greatly enhancing combat situational awareness when integrated with the existing Command, Control, and Communications, Computers, Intelligence, Surveillance and Reconnaissance (C4ISR) infrastructure. This system will provide an important boost to realizing the information dominant, network-centric objective of Joint Vision 2020. The program has established two Centers of Excellence for Sensor Technology each of which is capable of designing and building next generation, networked microsensor systems. The Defense Microelectronics Activity has teamed with the Centers of Excellence and industry to preserve long-term Department of Defense access to key next generation manufacturing technologies.

  14. Surface acoustic wave microsensors and applications

    NASA Astrophysics Data System (ADS)

    Galipeau, David W.; Story, Patrick R.; Vetelino, Kevin A.; Mileham, Russell D.

    1997-12-01

    Surface acoustic wave (SAW) devices have been studied for the last twenty years as highly sensitive yet relatively inexpensive microsensors for applications ranging from temperature and stress to gas and biological sensing. This wide range of applications is due to the SAW microsensors' high sensitivity to several physical parameters including mass, temperature, stress, and conductivity. Their low cost results from the use of standard batch microelectronic fabrication techniques for their manufacture. In this paper several chemical sensing applications for SAW devices are described. These include: gas detection; thin-film polymer characterization; dew-point measurements; surface energy measurements; and as a method to measure surface cleanliness. Experimental results are presented along with comparisons to other measurement techniques.

  15. Surface acoustic wave microsensors and applications

    NASA Astrophysics Data System (ADS)

    Galipeau, David W.; Story, Patrick R.; Vetelino, Kevin A.; Mileham, R. D.

    1997-06-01

    Surface acoustic wave (SAW) devices have been studied for the last twenty years as highly sensitive yet relatively inexpensive microsensors for applications ranging from gas and biological sensing to thin film and surface characterization. This wide range of applications is due to SAW microsensors high sensitivity to several physical parameters including mass, conductivity, permittivity, stress, temperature and electric fields. Their low cost results from the use of standard batch microelectronic fabrication techniques for their manufacture. In this work several SAW sensing applications are described. These include: gas detection; thin film polymer characterization; dew-point measurements; surface energy measurements; and as a method to measure surface cleanliness. Experimental results are presented along with comparisons to other measurement techniques.

  16. Micro-sensor thin-film anemometer

    NASA Technical Reports Server (NTRS)

    Sheplak, Mark (Inventor); McGinley, Catherine B. (Inventor); Spina, Eric F. (Inventor); Stephens, Ralph M. (Inventor); Hopson, Jr., Purnell (Inventor); Cruz, Vincent B. (Inventor)

    1996-01-01

    A device for measuring turbulence in high-speed flows is provided which includes a micro-sensor thin-film probe. The probe is formed from a single crystal of aluminum oxide having a 14.degree. half-wedge shaped portion. The tip of the half-wedge is rounded and has a thin-film sensor attached along the stagnation line. The bottom surface of the half-wedge is tilted upward to relieve shock induced disturbances created by the curved tip of the half-wedge. The sensor is applied using a microphotolithography technique.

  17. Micro-sensor thin-film anemometer

    NASA Technical Reports Server (NTRS)

    Sheplak, Mark (Inventor); Mcginley, Catherine B. (Inventor); Spina, Eric F. (Inventor); Stephens, Ralph M. (Inventor); Hopson, Purnell, Jr. (Inventor); Cruz, Vincent B. (Inventor)

    1994-01-01

    A device for measuring turbulence in high-speed flows is provided which includes a micro-sensor thin-film probe. The probe is formed from a single crystal of aluminum oxide having a 14 deg half-wedge shaped portion. The tip of the half-wedge is rounded and has a thin-film sensor attached along the stagnation line. The bottom surface of the half-wedge is tilted upward to relieve shock induced disturbances created by the curved tip of the half-wedge. The sensor is applied using a microphotolithography technique.

  18. Voltammetric Methods in Metallothionein Research

    PubMed Central

    Navrátil, Tomáš

    2005-01-01

    The application of voltammetric methods using different rates of polarisation on HMDE reveal inert or labile behaviour of Cd- or Zn- complexes in the presence of excessive cadmium or zinc ions in solution. This phenomenon was demonstrated first on the simplest phytochelatin – complex of peptide (γ-Glu-Cys)2 Gly with cadmium, later on rabbit liver metallothioneins – Cd7 MT in the presence of cadmium and Cd5 Zn2 MT in the presence of zinc. Voltammetric methods can distinguish between labile and inert complexes present simultaneously and therefore could elucidate their role in reactions of metal ion transfer. Another method using different rates of polarisation – elimination voltammetry with linear scan – proved that S-tetracoordinated complexes of Cd(II) or Zn(II) in the above-mentioned metallothioneins on HMDE are reduced in the adsorbed state. This implies the possibility of increasing the sensitivity of identification or determination of the above complexes. On carbon composite electrode, similar behaviour of Cd-complexes as on HMDE was observed using differential pulse voltammetry. PMID:18365088

  19. A Nitrite Microsensor for Profiling Environmental Biofilms

    PubMed Central

    De Beer, D.; Schramm, A.; Santegoeds, C. M.; Kuhl, M.

    1997-01-01

    A highly selective liquid membrane nitrite microsensor based on the hydrophobic ion-carrier aquocyanocobalt(III)-hepta(2-phenylethyl)-cobrynate is described. The sensor has a tip diameter of 10 to 15 (mu)m. The response is log-linear in freshwater down to 1 (mu)M NO(inf2)(sup-) and in seawater to 10 (mu)M NO(inf2)(sup-). A method is described for preparation of relatively large polyvinyl chloride (PVC)-gelled liquid membrane microsensors with a tip diameter of 5 to 15 (mu)m, having a hydrophilic coating on the tip. The coating and increased tip diameter resulted in more sturdy sensors, with a lower detection limit and a more stable signal than uncoated nitrite sensors with a tip diameter of 1 to 3 (mu)m. The coating protects the sensor membrane from detrimental direct contact with biomass and can be used for all PVC-gelled liquid membrane sensors meant for profiling microbial mats, biofilms, and sediments. Thanks to these improvements, liquid membrane sensors can now be used in complex environmental samples and in situ, e.g., in operating bioreactors. Examples of measurements in denitrifying, nitrifying, and nitrifying/denitrifying biofilms from wastewater treatment plants are shown. In all of these biofilms high nitrite concentrations were found in narrow zones of less than 1 mm. PMID:16535560

  20. Highly sensitive methane catalytic combustion micro-sensor based on mesoporous structure and nano-catalyst.

    PubMed

    Su, Jiacan; Cao, Liehu; Li, Liang; Wei, Jie; Li, Gengnan; Yuan, Yinyin

    2013-10-21

    In order to get a methane catalytic combustion micro-sensor, two different catalytic systems used in traditional methane catalytic combustion sensors were fabricated into a mesoporous structure and their catalytic activities were investigated. In comparison, the Rh2O3-Al2O3 system can form more a uniform mesoporous structure and has a much higher specific surface area. Even more importantly, it has relatively higher catalytic activity and stability for the methane catalytic combustion reaction. After being coated on a microelectro-mechanical system (MEMS) micro-heater, a catalytic combustion type methane micro-sensor was fabricated. The meso-structured Rh2O3-Al2O3 hybrid based MEMS sensor demonstrated a short T90 response time, relatively high signal output, high enough signal/noise ratio for practical detecting and strong anti-poison properties.

  1. Real-time microsensor measurement of local metabolic activities in ex vivo dental biofilms exposed to sucrose and treated with chlorhexidine.

    PubMed

    von Ohle, Christiane; Gieseke, Armin; Nistico, Laura; Decker, Eva Maria; DeBeer, Dirk; Stoodley, Paul

    2010-04-01

    Dental biofilms are characterized by structural and functional heterogeneity. Due to bacterial metabolism, gradients develop and diverse ecological microniches exist. The aims of this study were (i) to determine the metabolic activity of microorganisms in naturally grown dental biofilms ex vivo by measuring dissolved oxygen (DO) and pH profiles with microelectrodes with high spatial resolution and (ii) to analyze the impact of an antimicrobial chlorhexidine (CHX) treatment on microbial physiology during stimulation by sucrose in real time. Biofilms were cultivated on standardized human enamel surfaces in vivo. DO and pH profiles were measured in a flow cell system in sterile human saliva, after sucrose addition (10%), again after alternative treatment of the sucrose exposed biofilms with CHX (0.2%) for 1 or 10 min or after being killed with paraformaldehyde (4%). Biofilm structure was visualized by vitality staining with confocal microscopy. With saliva as the sole nutrient source oxygen consumption was high within the superficial biofilm layers rendering deeper layers (>220 mum) anoxic. Sucrose addition induced the thickness of the anaerobic zone to increase with a concurrent decrease in pH (7.1 to 4.4). CHX exposure reduced metabolic activity and microbial viability at the biofilm surface and drove metabolic activity deeper into the biofilm. CHX treatment led to a reduced viability at the biofilm surface with minor influence on overall biofilm physiology after 1 min; even after 10 min there was measurable respiration and fermentation inside the biofilm. However, the local microenvironment was more aerated, less acidogenic, and presumably less pathogenic.

  2. Voltammetric assay for the aging of beer.

    PubMed

    Guido, Luís F; Fortunato, Nélia A; Rodrigues, José A; Barros, Aguiles A

    2003-07-02

    A new method for the evaluation of beer aging, based on a voltammetric analysis of beer distillates, is described. By measuring the current of both acetaldehyde and sulfite voltammetric peaks it is possible to distinguish between fresh, naturally aged, and artificially aged beers. The results obtained for the ratio of acetaldehyde and SO(2) currents correlate well with those given by an expert sensory panel. The kinetics of the combining reaction of sulfite with acetaldehyde was followed for different acetaldehyde/SO(2) molar ratios by using a programmed voltammetric procedure. The formation of an acetaldehyde-sulfite adduct is rapid, and the reaction equilibrium is reached after 30 min, which is in accordance with the results previously obtained by other methods. This voltammetric-based approach seems to be a new attractive tool for detecting chemical equilibria of the addition of sulfite to carbonyls in beer model systems.

  3. Non-invasive microsensors for studying cell/tissue physiology

    NASA Astrophysics Data System (ADS)

    Vanegas, D. C.; Taguchi, M.; Chaturvedi, P.; Burrs, S.; McLamore, E. S.

    2013-05-01

    Non-invasive tools that allow real-time quantification of molecules relevant to metabolism, homeostasis, and cell signaling in cells and tissue are of great importance for studying physiology. Several microsensor technologies have been developed to monitor concentration of molecules such as ions, oxygen, electroactive molecules (e.g., nitric oxide, hydrogen peroxide), and biomolecules (e.g., sugars, hormones). The major challenges for microsensors are overcoming relatively low sensitivity and low signal-to-noise ratio. Modern approaches for enhancing microsensor performance focus on the incorporation of catalytic nanomaterials to increase sensitivity, reduce response time, and increase operating range. To improve signal-to-noise ratio, a non-invasive microsensor modality called self-referencing (SR) is being applied. The SR technique allows measurement of temporal and spatial transport dynamics at the cell, tissue, organ, and organismal level.

  4. Amperometric Solid Electrolyte Oxygen Microsensors with Easy Batch Fabrication

    NASA Technical Reports Server (NTRS)

    Hunter, Gary W.; Xu, Jennifer C.; Liu, ChungChiun

    2011-01-01

    An amperometric solid electrolyte oxygen (O2) microsensor using a novel and robust structure has been developed with a detection range of 0.025 to 21 percent of O2 concentration. The microsensor has a simple structure with a sensing area of 1.10 0.99 mm(exp 2), and is operated by applying voltage across the electrodes and measuring the resulting current flow at a temperature of 600 C.

  5. Thin Magnetically Soft Wires for Magnetic Microsensors

    PubMed Central

    Zhukova, Valentina; Ipatov, Mihail; Zhukov, Arcady

    2009-01-01

    Recent advances in technology involving magnetic materials require development of novel advanced magnetic materials with improved magnetic and magneto-transport properties and with reduced dimensionality. Therefore magnetic materials with outstanding magnetic characteristics and reduced dimensionality have recently gained much attention. Among these magnetic materials a family of thin wires with reduced geometrical dimensions (of order of 1–30 μm in diameter) have gained importance within the last few years. These thin wires combine excellent soft magnetic properties (with coercivities up to 4 A/m) with attractive magneto-transport properties (Giant Magneto-impedance effect, GMI, Giant Magneto-resistance effect, GMR) and an unusual re-magnetization process in positive magnetostriction compositions exhibiting quite fast domain wall propagation. In this paper we overview the magnetic and magneto-transport properties of these microwires that make them suitable for microsensor applications. PMID:22291562

  6. Fully integrated low-noise readout circuit with automatic offset cancellation loop for capacitive microsensors.

    PubMed

    Song, Haryong; Park, Yunjong; Kim, Hyungseup; Cho, Dong-Il Dan; Ko, Hyoungho

    2015-10-14

    Capacitive sensing schemes are widely used for various microsensors; however, such microsensors suffer from severe parasitic capacitance problems. This paper presents a fully integrated low-noise readout circuit with automatic offset cancellation loop (AOCL) for capacitive microsensors. The output offsets of the capacitive sensing chain due to the parasitic capacitances and process variations are automatically removed using AOCL. The AOCL generates electrically equivalent offset capacitance and enables charge-domain fine calibration using a 10-bit R-2R digital-to-analog converter, charge-transfer switches, and a charge-storing capacitor. The AOCL cancels the unwanted offset by binary-search algorithm based on 10-bit successive approximation register (SAR) logic. The chip is implemented using 0.18 μm complementary metal-oxide-semiconductor (CMOS) process with an active area of 1.76 mm². The power consumption is 220 μW with 3.3 V supply. The input parasitic capacitances within the range of -250 fF to 250 fF can be cancelled out automatically, and the required calibration time is lower than 10 ms.

  7. Fully Integrated Low-Noise Readout Circuit with Automatic Offset Cancellation Loop for Capacitive Microsensors

    PubMed Central

    Song, Haryong; Park, Yunjong; Kim, Hyungseup; Cho, Dong-il Dan; Ko, Hyoungho

    2015-01-01

    Capacitive sensing schemes are widely used for various microsensors; however, such microsensors suffer from severe parasitic capacitance problems. This paper presents a fully integrated low-noise readout circuit with automatic offset cancellation loop (AOCL) for capacitive microsensors. The output offsets of the capacitive sensing chain due to the parasitic capacitances and process variations are automatically removed using AOCL. The AOCL generates electrically equivalent offset capacitance and enables charge-domain fine calibration using a 10-bit R-2R digital-to-analog converter, charge-transfer switches, and a charge-storing capacitor. The AOCL cancels the unwanted offset by binary-search algorithm based on 10-bit successive approximation register (SAR) logic. The chip is implemented using 0.18 μm complementary metal-oxide-semiconductor (CMOS) process with an active area of 1.76 mm2. The power consumption is 220 μW with 3.3 V supply. The input parasitic capacitances within the range of −250 fF to 250 fF can be cancelled out automatically, and the required calibration time is lower than 10 ms. PMID:26473877

  8. Nanoporous-carbon adsorbers for chemical microsensors.

    SciTech Connect

    Overmyer, Donald L.; Siegal, Michael P.; Staton, Alan W.; Provencio, Paula Polyak; Yelton, William Graham

    2004-11-01

    Chemical microsensors rely on partitioning of airborne chemicals into films to collect and measure trace quantities of hazardous vapors. Polymer sensor coatings used today are typically slow to respond and difficult to apply reproducibly. The objective of this project was to produce a durable sensor coating material based on graphitic nanoporous-carbon (NPC), a new material first studied at Sandia, for collection and detection of volatile organic compounds (VOC), toxic industrial chemicals (TIC), chemical warfare agents (CWA) and nuclear processing precursors (NPP). Preliminary studies using NPC films on exploratory surface-acoustic-wave (SAW) devices and as a {micro}ChemLab membrane preconcentrator suggested that NPC may outperform existing, irreproducible coatings for SAW sensor and {micro}ChemLab preconcentrator applications. Success of this project will provide a strategic advantage to the development of a robust, manufacturable, highly-sensitive chemical microsensor for public health, industrial, and national security needs. We use pulsed-laser deposition to grow NPC films at room-temperature with negligible residual stress, and hence, can be deposited onto nearly any substrate material to any thickness. Controlled deposition yields reproducible NPC density, morphology, and porosity, without any discernable variation in surface chemistry. NPC coatings > 20 {micro}m thick with density < 5% that of graphite have been demonstrated. NPC can be 'doped' with nearly any metal during growth to provide further enhancements in analyte detection and selectivity. Optimized NPC-coated SAW devices were compared directly to commonly-used polymer coated SAWs for sensitivity to a variety of VOC, TIC, CWA and NPP. In every analyte, NPC outperforms each polymer coating by multiple orders-of-magnitude in detection sensitivity, with improvements ranging from 103 to 108 times greater detection sensitivity! NPC-coated SAW sensors appear capable of detecting most analytes tested to

  9. Poly-Alizarin red S/multiwalled carbon nanotube modified glassy carbon electrode for the boost up of electrocatalytic activity towards the investigation of dopamine and simultaneous resolution in the presence of 5-HT: A voltammetric study.

    PubMed

    Reddaiah, K; Madhusudana Reddy, T; Venkata Ramana, D K; Subba Rao, Y

    2016-05-01

    Poly-Alizarin red S/multiwalled carbon nanotube film on the surface of glassy carbon electrode (poly-AzrS/MWCNT/GCE) was synthesized by electrochemical process and was used for the sensitive and selective determination of dopamine (DA) by employing voltammetric techniques. The electrocatalytic response of the modified electrode was found to exhibit admirable activity. The simultaneous determination of dopamine in the presence of serotonin (5-HT) was found to exhibit very good response at poly-AzrS/MWCNTs/GCE. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at the developed poly-AzrS/MWCNTs/GCE. The poly-AzrS/MWCNTs/GCE exhibited an efficient electron mediating behavior together with well resolved peaks for dopamine, in 0.1 mol/dm(3) phosphate buffer (PBS) solution of pH 7.0. The limit of detection (LOD) and limit of quantification (LOQ) were found to be as 1.89 × 10(-7) mol/dm(3) and 6.312 × 10(-7) mol/dm(3) respectively with a dynamic range from 1 × 10(-6) to 1.8 × 10(-5) mol/dm(3). The interfacial electron transfer behavior of DA was studied by electrochemical impedance spectroscopy (EIS); the studies showed that the charge transfer rate was enhanced at poly-AzrS/MWCNTs/GCE when compared with bare GCE and poly-AzrS/GCE.

  10. Micro-sensors for space applications

    SciTech Connect

    Butler, M.A.; Frye-Mason, G.C.; Osbourn, G.C.

    1999-12-08

    Important factors in the application of sensing technology to space applications are low mass, small size, and low power. All of these attributes are enabled by the application of MEMS and micro-fabrication technology to microsensors. Two types of sensors are utilized in space applications: remotes sensing from orbit around the earth or another planetary body, and point sensing in the spacecraft or external to it. Several Sandia projects that apply microfabrication technologies to the development of new sensing capabilities having the potential for space applications will be briefly described. The Micro-Navigator is a project to develop a MEMS-based device to measure acceleration and rotation in all three axes for local area navigation. The Polychromator project is a joint project with Honeywell and MIT to develop an electrically programmable diffraction grating that can be programmed to synthesize the spectra of molecules. This grating will be used as the reference cell in a gas correlation radiometer to enable remote chemical detection of most chemical species. Another area of research where microfabrication is having a large impact is the development of a lab on a chip. Sandia's efforts to develop the {mu}ChemLab{trademark} will be described including the development of microfabricated pre-concentrators, chromatographic columns, and detectors. Smart sensors that allow the spacecraft independent decision making capabilities depend on pattern recognition. Sandia's development of a new pattern recognition methodology that can be used to interpret sensor response as well as for target recognition applications will be described.

  11. Secondary resonances of electrically actuated resonant microsensors

    NASA Astrophysics Data System (ADS)

    Abdel-Rahman, Eihab M.; Nayfeh, Ali H.

    2003-05-01

    We investigate the response of a microbeam-based resonant sensor to superharmonic and subharmonic electric actuations using a model that incorporates the nonlinearities associated with moderately large displacements and electric forces. The method of multiple scales is used, in each case, to obtain two first-order nonlinear ordinary-differential equations that describe the modulation of the amplitude and phase of the response and its stability. We present typical frequency-response and force-response curves demonstrating, in both cases, the coexistence of multivalued solutions. The solution corresponding to a superharmonic excitation consists of three branches, which meet at two saddle-node bifurcation points. The solution corresponding to a subharmonic excitation consists of two branches meeting a branch of trivial solutions at two pitchfork bifurcation points. One of these bifurcation points is supercritical and the other is subcritical. The results provide an analytical tool to predict the microsensor response to superharmonic and subharmonic excitations, specifically the locations of sudden jumps and regions of hysteretic behavior, thereby enabling designers to safely use these frequencies as measurement signals. They also allow designers to examine the impact of various design parameters on the device behavior.

  12. Nanoporous carbon films for gas microsensors.

    PubMed

    Siegal, M P; Yelton, W G; Overmyer, D L; Provencio, P P

    2004-02-17

    We study nanoporous carbon (NPC) as an adsorbent coating on surface acoustic wave (SAW) chemical microsensors for a wide range of analyte gases. By use of pulsed-laser deposition in a controlled inert gas ambient, NPC grows at room temperature with negligible residual stress and, hence, can coat most surfaces to any desired thickness. Acetone adsorption isotherms for NPC-coated SAW devices with mass density ranging from 0.18 to 1.08 g/cm3 indicate that the device frequency response relates to NPC density. Data analysis suggests the possibility of detecting acetone below parts-per-billion concentrations. We find NPC to be highly sensitive to a variety of other volatile organic and toxic industrial compounds. Transmission electron microscopy reveals that lower-density NPC has both larger and greater numbers of nanopores than higher-density NPC and that decreasing NPC density also increases the interplanar spacing between graphene sheet fragments within the ultrathin carbon wall structures. These physical differences effectively increase the available surface area for analyte gas adsorption with decreasing NPC density, with only the structural integrity of the internal NPC wall structures a limiting factor in determining the lowest useful density NPC coating.

  13. Fabrication and Characterization of Polyaniline/PVA Humidity Microsensors

    PubMed Central

    Yang, Ming-Zhi; Dai, Ching-Liang; Lin, Wei-Yi

    2011-01-01

    This study presents the fabrication and characterization of a humidity microsensor that consists of interdigitated electrodes and a sensitive film. The area of the humidity microsensor is about 2 mm2. The sensitive film is polyaniline doping polyvinyl alcohol (PVA) that is prepared by the sol-gel method, and the film has nanofiber and porous structures that help increase the sensing reaction. The commercial 0.35 μm Complimentary Metal Oxide Semiconductor (CMOS) process is used to fabricate the humidity microsensor. The sensor needs a post-CMOS process to etch the sacrificial layer and to coat the sensitive film on the interdigitated electrodes. The sensor produces a change in resistance as the polyaniline/PVA film absorbs or desorbs vapor. Experimental results show that the sensitivity of the humidity sensor is about 12.6 kΩ/%RH at 25 °C. PMID:22164067

  14. Fabrication and characterization of polyaniline/PVA humidity microsensors.

    PubMed

    Yang, Ming-Zhi; Dai, Ching-Liang; Lin, Wei-Yi

    2011-01-01

    This study presents the fabrication and characterization of a humidity microsensor that consists of interdigitated electrodes and a sensitive film. The area of the humidity microsensor is about 2 mm(2). The sensitive film is polyaniline doping polyvinyl alcohol (PVA) that is prepared by the sol-gel method, and the film has nanofiber and porous structures that help increase the sensing reaction. The commercial 0.35 μm Complimentary Metal Oxide Semiconductor (CMOS) process is used to fabricate the humidity microsensor. The sensor needs a post-CMOS process to etch the sacrificial layer and to coat the sensitive film on the interdigitated electrodes. The sensor produces a change in resistance as the polyaniline/PVA film absorbs or desorbs vapor. Experimental results show that the sensitivity of the humidity sensor is about 12.6 kΩ/%RH at 25 °C.

  15. Amperometric Carbon Fiber Nitrite Microsensor for In Situ Biofilm Monitoring

    EPA Science Inventory

    A highly selective needle type solid state amperometric nitrite microsensor based on direct nitrite oxidation on carbon fiber was developed using a simplified fabrication method. The microsensor’s tip diameter was approximately 7 µm, providing a high spatial resolution of at lea...

  16. Conformal and embedded IDT microsensors for health monitoring of structures

    NASA Astrophysics Data System (ADS)

    Varadan, Vijay K.; Varadan, Vasundara V.

    2000-06-01

    MEMS are currently being applied to the structural health monitoring of critical aircraft components and composites. The approach integrates acoustic emission, strain gauges, MEMS accelerometers and vibration monitoring aircraft components with a known history of catastrophic failure due to fracture. Recently a combination of the need for safety in the air and the desire to control costs is encouraging the use of in-flight monitoring of aircraft components and systems using light-weight, wireless and cost effective microsensors and MEMS. An in-situ aircraft structural health monitoring system, with sensors embedded in the composite structure or surface-mounted on the structure, would permit the timely detection of damage in aircraft. Micromachining offers the potential for fabricating a range of microsensor and MEMS for structural applications including load, vibration and acoustics characterization and monitoring. Such microsensors are extremely small; they can be embedded into structural materials, can be mass-produced and are therefore potentially cheap. The smart sensors are being developed using the standard microelectronics and micromachining in conjunction with novel Penn State wireless communication systems suitable for condition monitoring of aircraft structures in-flight. The main application areas of this investigation include continuos monitoring of a) structural integrity of aging aircraft, b) fatigue cracking, c) corrosion, d) deflection and strain of aircraft structures, wings, and rotorblades, e) impact damage, f) delamination and g) location and propagation of cracks. In this paper we give an overview of wireless programmable microsensors and MEMS and their associated driving electronics for such applications.

  17. Amperometric Carbon Fiber Nitrite Microsensor for In Situ Biofilm Monitoring

    EPA Science Inventory

    A highly selective needle type solid state amperometric nitrite microsensor based on direct nitrite oxidation on carbon fiber was developed using a simplified fabrication method. The microsensor’s tip diameter was approximately 7 µm, providing a high spatial resolution of at lea...

  18. Development of a Self-calibrating Dissolved Oxygen Microsensor Array for the Monitoring and Control of Plant Growth in a Space Environment

    NASA Technical Reports Server (NTRS)

    Kim, Chang-Soo; Brown, Christopher S.; Nagle, H. Troy

    2004-01-01

    Plant experiments in space will require active nutrient delivery concepts in which water and nutrients are replenished on a continuous basis for long-term growth. The goal of this study is to develop a novel microsensor array to provide information on the dissolved oxygen environment in the plant root zone for the optimum control of plant cultivation systems in the space environment. Control of water and oxygen is limited by the current state-of-the-art in sensor technology. Two capabilities of the new microsensor array were tested. First, a novel in situ self-diagnosis/self-calibration capability for the microsensor was explored by dynamically controlling the oxygen microenvironment in close proximity to an amperometric dissolved oxygen microsensors. A pair of integrated electrochemical actuator electrodes provided the microenvironments based on water electrolysis. Miniaturized thin film dissolved oxygen microsensors on a flexible polyimide (Kapton(Registered Trademark)? substrate were fabricated and their performances were tested. Secondly, measurements of dissolved oxygen in two representative plant growth systems were made, which had not been performed previously due to lack of proper sensing technology. The responses of the oxygen microsensor array on a flexible polymer substrate properly reflected the oxygen contents on the surface of a porous tube nutrient delivery system and within a particulate substrate system. Additionally, we demonstrated the feasibility of using a 4-point thin film microprobe for water contents measurements for both plant growth systems. mechanical flexibility, and self-diagnosis. The proposed technology is anticipated to provide a reliable sensor feedback plant growth nutrient delivery systems in both terrestrial environment and the microgravity environment during long term space missions. The unique features of the sensor include small size and volume, multiple-point sensing,

  19. Miniaturized optoelectronic system for telemetry of in vivo voltammetric signals.

    PubMed

    De Simoni, M G; De Luigi, A; Imeri, L; Algeri, S

    1990-08-01

    In vivo voltammetry is an electrochemical technique that uses carbon fiber microelectrodes stereotaxically implanted in brain areas to monitor monoamine metabolism and release continuously, in freely moving animals. Electric wires connect the polarograph to the animal. A wire-less transmission system (optoelectronic transmission, OPT) of voltammetric signals is described here. It uses infrared diffused light, exploiting the diffusion of the transmitted light over walls and ceiling towards a receiver. The transmission system consists of a main unit and a satellite unit (40 x 30 x 5 mm) positioned on the animal's back. Voltammetric recordings obtained by the classical system (with wires) and by OPT are well defined and almost identical in shape. The power supply is provided by two thin lithium batteries (+/- 3V) that can record for up to 20 h. OPT permits detailed behavioral observations since the animal can be left free to move in a spacious environment. Voltammetry using OPT allows simultaneous recording of neuronal firing activity as well as electroencephalographic recordings (EEG) since there is no cross-talk between the circuits used. The results illustrate the reliability and usefulness of this wire-less transmission system for studying relationships between neurochemical, behavioral and electrophysiological activities.

  20. Dielectric properties modelling of cellular structures with PDMS for micro-sensor applications

    NASA Astrophysics Data System (ADS)

    Kachroudi, Achraf; Basrour, Skandar; Rufer, Libor; Sylvestre, Alain; Jomni, Fathi

    2015-12-01

    Electro-active polymers are emerging in the fields of actuators and micro-sensors because their good dielectric and mechanical properties makes them suitable for such applications. In this work, we focus on micro-structured (cellular) polymer materials (referred as piezoelectrets or ferroelectrets) that need prior charging to attain piezoelectric behaviour. The development of such applications requires an in-depth knowledge of the intrinsic dielectric properties of such structures and models to enable the accurate prediction of a given micro-structured material’s dielectric properties. Various polymers including polypropylene, polytetrafluoroethylene, fluoroethylenepropylene, cyclo-olefines and poly(ethylene terephthalate) in a cellular form have been studied by researchers over the last fifteen years. However, there is still a lack of information on the intrinsic dielectric properties of the most recently used dielectric polymer (polydimethylsiloxane, PDMS) over wide frequency and temperature ranges. In this work, we shall propose an exhaustive equivalent electrical circuit model and explain how it can be used to predict the micro-structured PDMS complex permittivity versus frequency and temperature. The results obtained from the model were found to be in good agreement with experimental data for various micro-structured PDMS materials. Typically, for micro-sensor applications, the dielectric constant and dielectric losses are key factors which need to be minimized. We have developed a configuration which enables both to be strongly reduced with a reduction of 16% in the dielectric constant of a micro-structured PDMS compared with the bulk material. In addition, the phenomena responsible for dielectric losses variations with frequency and temperature are discussed and correlated with the theoretical model. Our model is thus proved to be a powerful tool for the control of the dielectric properties of micro-structured PDMS material for micro-sensor applications.

  1. Voltammetric and electrochemical gravimetric selective detection of interactions between Tl(I) and guanine and the influence on activity of DNA drug-intercalators.

    PubMed

    Nowicka, Anna M; Mackiewicz, Marcin; Matysiak, Edyta; Krasnodebska-Ostrega, Beata; Stojek, Zbigniew

    2013-03-15

    The interactions of Tl(I), a well known toxic species, with selected oligonucleotides were examined. The oligonucleotide sequences selected for the investigation were taken from gene hOGG1 responsible for repairing of DNA damage. Cyclic voltammetry was particularly useful, since nitrogen N-7 in guanine can be electrooxidized while its binding with Tl(I) leads to the loss of electroactivity. So, this selected interaction could be quantitatively used in drawing Scatchard's plot and calculating the binding constants and the number of active sites in guanine molecules occupied by one metal ion. Further, we have shown that the presence of Tl(I) leads to a decrease in activity of doxorubicin (DOX), a popular anticancer drug, vs. DNA. The obtained circular dichroism (CD) spectra and the measurements with an electrochemical quartz crystal microbalance (EQCM) led to a conclusion that in the presence of monovalent thallium cations the DNA double helix was neither damaged/oxidized nor its conformation changed substantially. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. Synthesis, spectroscopic, thermal, voltammetric studies and biological activity of crystalline complexes of pyridine-2,6-dicarboxylic acid and 8-hydroxyquinoline

    NASA Astrophysics Data System (ADS)

    Çolak, Alper Tolga; Çolak, Ferdağ; Yeşilel, Okan Zafer; Büyükgüngör, Orhan

    2009-11-01

    Two new compounds (8-H 2Q) 2[M(dipic) 2]·6H 2O (M = Co ( 1) and Ni ( 2), 8-HQ = 8-hydroxyquinoline, dipic = dipicolinate) have been prepared and characterized by elemental analysis, spectral (IR and UV-vis), thermal analyses, magnetic measurements and single-crystal X-ray diffraction techniques. Both 1 and 2 consist two 8-hydroxyquinolinium cations, one bis(dipicolinate)M(II) anion [M = Co(II), Ni(II)] and six uncoordinated water molecules. Both 1 and 2 crystallize in the monoclinic space group C2/c. In the compounds anion, each dipic ligand simultaneously exhibits tridentate coordination modes through N atom of pyridine ring and oxygen atoms of the carboxylate groups. The crystal packing of 1 and 2 is a composite of intermolecular hydrogen bonding and C-O⋯π interactions. The in vitro antibacterial and antifungal activities of 1 and 2 were evaluated by the agar well diffusion method by MIC tests. Both new compounds showed the same antimicrobial activity against Gram-positive bacteria and yeast and fungi expect Gram-negative bacteria.

  3. Resolution capacity of Hall microsensors in MOS structures

    NASA Astrophysics Data System (ADS)

    Căruntu, George; Panait, Cornel; Căruntu, Irina

    2010-11-01

    An essential parameter in the setting up of the performance of the measurement systems that uses Hall microsensors is the detection limit of such devices. The paper presents the results of research work regarding the analysis and optimization of magnetic microsensor structures realized in bipolar and MOS integrated circuits technology. On the basis of adequate models these have been established the noise main characteristics for double collector vertical magnetotransistor and for double-drain MOSFET magnetotransistors. By using the numerical simulation the values of the signal-to-noise ratio and the detection limits for the two analysed structured are compared and it is also emphasized the way in which choosing the geometry and the material features allow getting high-performance sensors.

  4. Applications of polysilicon films in microsensors and microactuators

    SciTech Connect

    Howe, R.T.

    1988-08-01

    This paper reviews the applications of polysilicon in microsensor technology and in the emerging field of microfabricated actuators. Polysilicon is an attractive material for thin-film strain gauges, and is also used to fabricate micromechanical structures. The need for better understanding of the non-electrical properties of polysilicon, such as Young's modulus, residual strain, ultimate strength, friction, and wear, is emphasized. 45 refs., 11 figs.

  5. General Atomics Smart Microsensors - FY05 Laboratory Fire Test Results

    DTIC Science & Technology

    2005-10-31

    recognition; Cyclic voltammetry , Microsensor arrays; Sensor arrays This report describes the cermet sensors and system control software recently evaluated...high temperature operation and are used as electrodes to perform electrochemical cyclic voltammetry on gases. A natural extension of this is to...capability the cyclic voltammetry has over the simple ionization or photoelectric methods the EST detectors use. For three of the flaming fires

  6. Monolithic GaAs surface acoustic wave chemical microsensor array

    SciTech Connect

    HIETALA,VINCENT M.; CASALNUOVO,STEPHEN A.; HELLER,EDWIN J.; WENDT,JOEL R.; FRYE-MASON,GREGORY CHARLES; BACA,ALBERT G.

    2000-03-09

    A four-channel surface acoustic wave (SAW) chemical sensor array with associated RF electronics is monolithically integrated onto one GaAs IC. The sensor operates at 690 MHz from an on-chip SAW based oscillator and provides simple DC voltage outputs by using integrated phase detectors. This sensor array represents a significant advance in microsensor technology offering miniaturization, increased chemical selectivity, simplified system assembly, improved sensitivity, and inherent temperature compensation.

  7. General Atomics Smart Microsensors FY05 Shipboard Fire Test Results

    DTIC Science & Technology

    2005-12-12

    Smart Microsensors and instrumentation such as thermocouples (TCs), optical density meters ( ODMs ), and COTS spot- type smoke detectors were added to...the locations of the TCs, ODMs and detectors on the 3 ’d deck. The TC, ODM , and detector locations on the 2nd deck are detailed in Fig. 12. Table 9...EST SIGAPS individual alarms monitoredMulti deteo (via 24 panel output relays toMulti detector (Qty = 7) EST SIGA-IPHS masscomp. Laser ODM (Qty = 9

  8. Chemical Microsensors For Detection Of Explosives And Chemical Warfare Agents

    SciTech Connect

    Yang, Xiaoguang; Swanson, Basil I.

    2001-11-13

    An article of manufacture is provided including a substrate having an oxide surface layer and a layer of a cyclodextrin derivative chemically bonded to said substrate, said layer of a cyclodextrin derivative adapted for the inclusion of selected compounds, e.g., nitro-containing organic compounds, therewith. Such an article can be a chemical microsensor capable of detecting a resultant mass change from inclusion of the nitro-containing organic compound.

  9. Identification of soft drinks using MEMS-IDT microsensors

    NASA Astrophysics Data System (ADS)

    Abraham, Jose K.; Karjathkar, Sonal; Jacesko, Stefany; Varadan, Vijay K.; Gardner, Julian W.

    2005-05-01

    Development of a taste sensor with high sensitivity, stability and selectivity is highly desirable for the food and beverage industries. The main goal of a taste sensor is to reproduce five kinds of senses of humans, which is quite difficult. The importance of knowing quality of beverages and drinking water has been recognized as a result of increase in concern in environmental pollution issues. However, no accurate measuring system appropriate for quality evaluation of beverages is available. A highly sensitive microsensor using horizontally polarized Surface Acoustic Waves (SH-SAW) for the detection and identification of soft drinks is presented in this paper. Different soft drinks were tested using this sensor and the results which could distinguish between two popular soft drinks like Pepsi and Coca cola is presented in this paper. The SH-SAW microsensors are fabricated on 36°-rotated Y cut X propagating LiTaO3 (36YX.LT) substrate. This design consists of a dual delay line configuration in which one line is free and other one is metallized and shielded. Due to high electromechanical coupling of 36YX.LT, it could detect difference in electrical properties and hence to distinguish different soft drinks. Measured electrical characteristics of these soft drinks at X-band frequency using free space system show distinguishable results. It is clear from these results that the microsensor based on 36YX.LT is an effective liquid identification system for quantifying human sensory expressions.

  10. Acoustic Wave Chemical Microsensors in GaAs

    SciTech Connect

    Albert G. Baca; Edwin J. Heller; Gregory C. Frye-Mason; John L. Reno; Richard Kottenstette; Stephen A. Casalnuovo; Susan L. Hietala; Vincent M. Hietala

    1998-09-20

    High sensitivity acoustic wave chemical microsensors are being developed on GaAs substrates. These devices take advantage of the piezoelectric properties of GaAs as well as its mature microelectronics fabrication technology and nascent micromachining technology. The design, fabrication, and response of GaAs SAW chemical microsensors are reported. Functional integrated GaAs SAW oscillators, suitable for chemical sensing, have been produced. The integrated oscillator requires 20 mA at 3 VK, operates at frequencies up to 500 MHz, and occupies approximately 2 mmz. Discrete GaAs sensor components, including IC amplifiers, SAW delay lines, and IC phase comparators have been fabricated and tested. A temperature compensation scheme has been developed that overcomes the large temperature dependence of GaAs acoustic wave devices. Packaging issues related to bonding miniature flow channels directly to the GaAs substrates have been resolved. Micromachining techniques for fabricating FPW and TSM microsensors on thin GaAs membranes are presented and GaAs FPW delay line performance is described. These devices have potentially higher sensitivity than existing GaAs and quartz SAW sensors.

  11. Wireless microsensors for health monitoring of aircraft structures

    NASA Astrophysics Data System (ADS)

    Varadan, Vijay K.

    2003-01-01

    The integration of MEMS, IDTs (interdigital transducers) and required microelectronics and conformal antennas to realize programmable, robust and low cost passive microsensors suitable for many military structures and systems including aircraft, missiles and munitions is presented in this paper. The technology is currently being applied to the structural health monitoring of critical aircraft components. The approach integrates acoustic emission, strain gauges, MEMS accelerometers, gyroscopes and vibration monitoring devices with signal processing electronics to provide real-time indicators of incipient failure of aircraft components with a known history of catastrophic failure due to fracture. Recently a combination of the need for safety in the air and the desire to control costs is encouraging the use of in-flight monitoring of aircraft components and systems using light-weight, wireless and cost effective microsensors and MEMS. An in-situ Aircraft structural health monitoring (ASHM) system, with sensors embedded in the composite structure or surface-mounted on the structure, would permit the timely detection of damage in aircraft. Micromachining offers the potential for fabricating a range of microsensors and MEMS for structural applications including load, vibration and acoustics characterization and monitoring. Such microsensors are extremely small; they can be embedded into structural materials, can be mass-produced and are therefore potentially cheap. Additionally a range of sensor types can be integrated onto a single chip with built-in electronics and ASIC (Application Specific Integrated Circuit), providing a low power Microsystems. The smart sensors are being developed using the standard microelectronics and micromachining in conjunction with novel Penn State smart electronics or wireless communication systems suitable for condition monitoring of aircraft structures in-flight. A hybrid accelerometer and gyroscope in a single chip suitable for inertial

  12. Wireless microsensor network solutions for neurological implantable devices

    NASA Astrophysics Data System (ADS)

    Abraham, Jose K.; Whitchurch, Ashwin; Varadan, Vijay K.

    2005-05-01

    The design and development of wireless mocrosensor network systems for the treatment of many degenerative as well as traumatic neurological disorders is presented in this paper. Due to the advances in micro and nano sensors and wireless systems, the biomedical sensors have the potential to revolutionize many areas in healthcare systems. The integration of nanodevices with neurons that are in communication with smart microsensor systems has great potential in the treatment of many neurodegenerative brain disorders. It is well established that patients suffering from either Parkinson"s disease (PD) or Epilepsy have benefited from the advantages of implantable devices in the neural pathways of the brain to alter the undesired signals thus restoring proper function. In addition, implantable devices have successfully blocked pain signals and controlled various pelvic muscles in patients with urinary and fecal incontinence. Even though the existing technology has made a tremendous impact on controlling the deleterious effects of disease, it is still in its infancy. This paper presents solutions of many problems of today's implantable and neural-electronic interface devices by combining nanowires and microelectronics with BioMEMS and applying them at cellular level for the development of a total wireless feedback control system. The only device that will actually be implanted in this research is the electrodes. All necessary controllers will be housed in accessories that are outside the body that communicate with the implanted electrodes through tiny inductively-coupled antennas. A Parkinson disease patient can just wear a hat-system close to the implantable neural probe so that the patient is free to move around, while the sensors continually monitor, record, transmit all vital information to health care specialist. In the event of a problem, the system provides an early warning to the patient while they are still mobile thus providing them the opportunity to react and

  13. Fiber-based temperature microsensor by using three-dimensional photomask

    NASA Astrophysics Data System (ADS)

    Kim, Yeachan; Zhang, Yi; Hayase, Masanori

    2017-06-01

    In this paper we present a new three-dimensional (3D) photomask technology for the direct fabrication of temperature microsensors on tiny fiber substrates. The 3D photomask consists of an exposure module having two half-pipe substrates with the outer and inner diameters of 1.8 and 0.32 mm, respectively, which have fine patterns of thin Cr metal film. Using the 3D photomask, two resistive temperature microsensors of thin Pt metal film including wiring pads are successfully and directly fabricated on different sides of the same quartz capillary with the outer and inner diameters of 300 and 180 µm, respectively. The minimum pattern width of the temperature microsensors is about 10 µm. The as-prepared temperature microsensors have shown excellent linear response to the variations in of temperature from 25 to 80 °C. It indicates that the fiber based temperature microsensor could be expected in many applications in biomedical devices.

  14. Microsensor measurements of hydrogen gas dynamics in cyanobacterial microbial mats.

    PubMed

    Nielsen, Michael; Revsbech, Niels P; Kühl, Michael

    2015-01-01

    We used a novel amperometric microsensor for measuring hydrogen gas production and consumption at high spatio-temporal resolution in cyanobacterial biofilms and mats dominated by non-heterocystous filamentous cyanobacteria (Microcoleus chtonoplastes and Oscillatoria sp.). The new microsensor is based on the use of an organic electrolyte and a stable internal reference system and can be equipped with a chemical sulfide trap in the measuring tip; it exhibits very stable and sulfide-insensitive measuring signals and a high sensitivity (1.5-5 pA per μmol L(-1) H2). Hydrogen gas measurements were done in combination with microsensor measurements of scalar irradiance, O2, pH, and H2S and showed a pronounced H2 accumulation (of up to 8-10% H2 saturation) within the upper mm of cyanobacterial mats after onset of darkness and O2 depletion. The peak concentration of H2 increased with the irradiance level prior to darkening. After an initial build-up over the first 1-2 h in darkness, H2 was depleted over several hours due to efflux to the overlaying water, and due to biogeochemical processes in the uppermost oxic layers and the anoxic layers of the mats. Depletion could be prevented by addition of molybdate pointing to sulfate reduction as a major sink for H2. Immediately after onset of illumination, a short burst of presumably photo-produced H2 due to direct biophotolysis was observed in the illuminated but anoxic mat layers. As soon as O2 from photosynthesis started to accumulate, the H2 was consumed rapidly and production ceased. Our data give detailed insights into the microscale distribution and dynamics of H2 in cyanobacterial biofilms and mats, and further support that cyanobacterial H2 production can play a significant role in fueling anaerobic processes like e.g., sulfate reduction or anoxygenic photosynthesis in microbial mats.

  15. Microsensor measurements of hydrogen gas dynamics in cyanobacterial microbial mats

    PubMed Central

    Nielsen, Michael; Revsbech, Niels P.; Kühl, Michael

    2015-01-01

    We used a novel amperometric microsensor for measuring hydrogen gas production and consumption at high spatio-temporal resolution in cyanobacterial biofilms and mats dominated by non-heterocystous filamentous cyanobacteria (Microcoleus chtonoplastes and Oscillatoria sp.). The new microsensor is based on the use of an organic electrolyte and a stable internal reference system and can be equipped with a chemical sulfide trap in the measuring tip; it exhibits very stable and sulfide-insensitive measuring signals and a high sensitivity (1.5–5 pA per μmol L-1 H2). Hydrogen gas measurements were done in combination with microsensor measurements of scalar irradiance, O2, pH, and H2S and showed a pronounced H2 accumulation (of up to 8–10% H2 saturation) within the upper mm of cyanobacterial mats after onset of darkness and O2 depletion. The peak concentration of H2 increased with the irradiance level prior to darkening. After an initial build-up over the first 1–2 h in darkness, H2 was depleted over several hours due to efflux to the overlaying water, and due to biogeochemical processes in the uppermost oxic layers and the anoxic layers of the mats. Depletion could be prevented by addition of molybdate pointing to sulfate reduction as a major sink for H2. Immediately after onset of illumination, a short burst of presumably photo-produced H2 due to direct biophotolysis was observed in the illuminated but anoxic mat layers. As soon as O2 from photosynthesis started to accumulate, the H2 was consumed rapidly and production ceased. Our data give detailed insights into the microscale distribution and dynamics of H2 in cyanobacterial biofilms and mats, and further support that cyanobacterial H2 production can play a significant role in fueling anaerobic processes like e.g., sulfate reduction or anoxygenic photosynthesis in microbial mats. PMID:26257714

  16. The offset equivalent magnetic induction for Hall microsensors

    NASA Astrophysics Data System (ADS)

    Căruntu, George; Panait, Cornel

    2009-01-01

    An essential parameter in the setting up of the performance of the measurement systems that uses Hall microsensors is the magnetic offset of such devices. This paperwork presents the structure, the operating conditions, and the main characteristic for the Hall plates and for bipolar lateral magnetotransistor. By using numerical simulation, the values of the offset-equivalent magnetic induction for the two analysed devices are compared and it is also emphasised the way in which choosing the geometry and the material features allows getting high-performance sensors.

  17. Development of microsensor arrays using near infrared probes

    SciTech Connect

    Landis, D.A.; Isola, N.R.; Alarie, J.P.

    1995-12-31

    A novel microsensor array has been developed using near infrared fluorphores. These near infrared probes are attached to specific sequences of single stranded DNA which are then hybridized with the sample of interest. The presence of the near infrared fluorphore after the hybridization is an indication of the existence within the sample of the compliment to the single stranded DNA. The probe is excited using a near infrared diode laser, and the sample is imaged onto a cooled CCD detector using an array of graded index (GRIN) microlenses. Using a simple experimental setup, we have been able to achieve final detection limits, which rival those of more conventional DNA detection methods.

  18. Fabrication and Characterization of CMOS-MEMS Magnetic Microsensors

    PubMed Central

    Hsieh, Chen-Hsuan; Dai, Ching-Liang; Yang, Ming-Zhi

    2013-01-01

    This study investigates the design and fabrication of magnetic microsensors using the commercial 0.35 μm complementary metal oxide semiconductor (CMOS) process. The magnetic sensor is composed of springs and interdigitated electrodes, and it is actuated by the Lorentz force. The finite element method (FEM) software CoventorWare is adopted to simulate the displacement and capacitance of the magnetic sensor. A post-CMOS process is utilized to release the suspended structure. The post-process uses an anisotropic dry etching to etch the silicon dioxide layer and an isotropic dry etching to remove the silicon substrate. When a magnetic field is applied to the magnetic sensor, it generates a change in capacitance. A sensing circuit is employed to convert the capacitance variation of the sensor into the output voltage. The experimental results show that the output voltage of the magnetic microsensor varies from 0.05 to 1.94 V in the magnetic field range of 5–200 mT. PMID:24172287

  19. Microsensors to monitor missile storage and maintenance needs

    SciTech Connect

    Mee, D.K.; Thundat, T.G.; Oden, P.I.

    1997-10-30

    Accurate assessments of reliability and condition based maintenance can only be implemented where a good understanding of ammunition stockpile condition exists. Use of miniaturized intelligent sensors provides an inexpensive means of nondestructively gaining insight into stockpile condition while keeping costs low. In the past, evaluation of ammunition lifetimes has utilized humidity, temperature, pressure, shock, and corrosion. New technologies provide the possibility of obtaining these environmental parameters, as well as a number of other indicators of propellant degradation, including NOx by utilizing a microsensor with capability for remote wireless monitoring. Micro-electro-mechanical systems (MEMS) like microcantilevers promise to revolutionize the field of sensor design. In the automobile industry, micromachined acceleration sensors are now used for triggering airbags and pressure sensors adjust the air-fuel intake ratio in the engine. By applying coatings to the sensor`s surface the behavior of the microdevice can be measurably altered to respond to chemical species as demonstrated by ORNL using microcantilevers to detect mercury vapor and humidity. Ultimately, single-chip detectors with electronics and telemetry could be developed with conceivably hundreds of individual microsensors on each chip to simultaneously monitor identify, and quantify many important chemical species for ammunition as well as measure environmental parameters.

  20. A Resonant Pressure Microsensor Capable of Self-Temperature Compensation

    PubMed Central

    Li, Yinan; Wang, Junbo; Luo, Zhenyu; Chen, Deyong; Chen, Jian

    2015-01-01

    Resonant pressure microsensors are widely used in the fields of aerospace exploration and atmospheric pressure monitoring due to their advantages of quasi-digital output and long-term stability, which, however, requires the use of additional temperature sensors for temperature compensation. This paper presents a resonant pressure microsensor capable of self-temperature compensation without the need for additional temperature sensors. Two doubly-clamped “H” type resonant beams were arranged on the pressure diaphragm, which functions as a differential output in response to pressure changes. Based on calibration of a group of intrinsic resonant frequencies at different pressure and temperature values, the functions with inputs of two resonant frequencies and outputs of temperature and pressure under measurement were obtained and thus the disturbance of temperature variations on resonant frequency shifts was properly addressed. Before compensation, the maximal errors of the measured pressure values were over 1.5% while after compensation, the errors were less than 0.01% of the full pressure scale (temperature range of −40 °C to 70 °C and pressure range of 50 kPa to 110 kPa). PMID:25938197

  1. Microsensors and wireless system for monitoring epilepsy

    NASA Astrophysics Data System (ADS)

    Whitchurch, Ashwin K.; Ashok, B. H.; Kumaar, Raman V.; Sarukesi, K.; Jose, K. A.; Varadan, Vijay K.

    2003-07-01

    Epilepsy is a form of brain disorder caused by abnormal discharges of neurons. The most common manifestations of epilepsy are seizures which could affect visual, aural and motor abilities of a person. Absence epilepsy is a form of epilepsy common mostly in children. The most common manifestations of absence epilepsy are staring and transient loss of responsiveness. Also, subtle motor activities may occur. Due to the subtle nature of these symptoms, episodes of absence epilepsy may often go unrecognized for long periods of time or be mistakenly attributed to attention deficit disorder or daydreaming. Spells of absence epilepsy may last about 10 seconds and occur hundreds of times each day. Patients have no recollections of the events occurred during those seizures and will resume normal activity without any postictal symptoms. The EEG during such episodes of Absence epilepsy shows intermittent activity of 3 Hz generalized spike and wave complexes. As EEG is the only way of detecting such symptoms, it is required to monitor the EEG of the patient for a long time, usually the whole day. This requires that the patient be connected to the EEG recorder all the time and thus remain only in the bed. So, effectively the EEG is being monitored only when the patient is stationary. The wireless monitoring system described in this paper aims at eliminating this constraint and enables the physician to monitor the EEG when the patient resumes his normal activities. This approach could even help the doctor identify possible triggers of absence epilepsy.

  2. Novel needle-electrochemical microsensor for in-vitro and in-vivo measurements of oxygen

    NASA Astrophysics Data System (ADS)

    Xu, Weiya; Ma, Wentao; Li, Kaiyang; Hu, Jiming; Li, Hongyi; Cao, Lianxin; Song, Yu; Zhao, Lan

    2001-09-01

    Electrochemical microsensors have been applied in the field of biomedicine for many years. The aim of this work was to develop a novel oxygen sensor to monitor the partial pressure of oxygen in tissues and acupuncture points. The functions of microsensor were evaluated through in vitro experiments. In vivo in tissues and acupuncture points. The data from oxygen microsensor were compared with the data from blood gas analyzer. The measurements depend on the physiological changes of experimental animal. The further development of this new sensor is to be a tool for meridian research.

  3. Infrared microsensor payload for miniature unmanned aerial vehicles

    NASA Astrophysics Data System (ADS)

    Kostrzewa, Joseph; Meyer, William H.; Laband, Stan; Terre, William A.; Petrovich, Peter; Swanson, Kyle; Sundra, Carrie; Sener, Ward; Wilmott, Jay

    2003-09-01

    Miniature unmanned aerial vehicles (UAVs) are a category of aircraft small enough to be transported, launched, operated, and retrieved by a crew of one or two. The concept is not new, having been in limited use by the U.S. military over the past fifteen years, but interest in potential applications is growing as size and cost of the vehicles come down. An application that is particularly significant to the military and law-enforcement agencies is remote reconnaissance, with one or more onboard sensors transmitting data back to the operator(s) in real time. Typically, a miniature UAV is capable of flying a pre-programmed route autonomously, with manual override as an option. At the conclusion of the mission, the vehicle returns for landing, after which it can be quickly disassembled and stowed until its next use. Thermal imaging extends the utility of miniature UAVs to operations in complete darkness and limited visibility, but historically thermal imagers have been too large and heavy for this application. That changed in 1999 with the introduction of Indigo System's AlphaTM camera, which established a new class of thermal imaging product termed the infrared "microsensor". Substantially smaller and lighter than any other infrared imaging product available at the time, AlphaTMwas the first camera that could be readily packaged into the nose of a miniature UAV. Its low power consumption was also a key enabling feature. Building upon the success of AlphaTM, Indigo then took the microsensor class a step further with its OmegaTM camera, which broke all the records established by AlphaTM for small size, weight, and power. OmegaTM has been successfully integrated into several miniature UAVs, including AeroVironment's Pointer and Raven, as well as the Snake Eye UAV manufactured by BAI Aerosystems. Aspects of the OmegaTM design that have led to its utility on these and other platforms are described, and future prospects for even smaller microsensors are discussed.

  4. Integration of Nanostructures into Microsensor Devices on Whole Wafers

    NASA Technical Reports Server (NTRS)

    Biaggi-Labiosa, Azlin M.; Evans, Laura J.; Berger, Gordon M.; Hunter, Gary W.

    2015-01-01

    Chemical sensors are used in a wide variety of applications, such as environmental monitoring, fire detection, emission monitoring, and health monitoring. The fabrication of chemical sensors involving nanostructured materials holds the potential for the development of sensor systems with unique properties and improved performance. However, the fabrication and processing of nanostructures for sensor applications currently are limited in the ability to control their location on the sensor, which in turn hinders the progress for batch fabrication. This report discusses the advantages of using nanomaterials in sensor designs, some of the challenges encountered with the integration of nanostructures into microsensor / devices, and then briefly describes different methods attempted by other groups to address this issue. Finally, this report will describe how our approach for the controlled alignment of nanostructures onto a sensor platform was applied to demonstrate an approach for the mass production of sensors with nanostructures.

  5. A wireless portable system with microsensors for monitoring respiratory diseases.

    PubMed

    Cao, Zhe; Zhu, Rong; Que, Rui-Yi

    2012-11-01

    A wireless portable monitoring system for respiratory diseases using microsensors is proposed. The monitoring system consists of two sensor nodes integrating with Bluetooth transmitters that measure user's respiratory airflow, blood oxygen saturation, and body posture. The utility of micro-hot-film flow sensor makes the monitor can acquire comprehensive respiration parameters which are useful for diagnoses of obstructive sleep apnea, chronic obstructive pulmonary disease, and asthma. The system can serve as both sleep recorder and spirometer. Additionally, a mobile phone or a PC connected to the Internet serving as a monitoring and transfer terminal makes telemedicine achievable. Several experiments were conducted to verify the feasibility and effectiveness of the proposed system for monitoring and diagnosing OSA, COPD, and asthma.

  6. VCSEL-based microsensors for photonic proximity fuzing of munitions

    NASA Astrophysics Data System (ADS)

    Keeler, G. A.; Mar, A.; Geib, K. M.; Hsu, A. Y.; Serkland, D. K.; Peake, G. M.

    2008-08-01

    This paper describes technologies developed at Sandia National Laboratories to support a joint DoD/DoE initiative to create a compact, robust, and affordable photonic proximity sensor for munitions fuzing. The proximity fuze employs high-power vertical-cavity surface-emitting laser (VCSEL) arrays, resonant-cavity photodetectors (RCPDs), and refractive micro-optics that are integrated within a microsensor whose volume is approximately 0.01 cm3. Successful development and integration of these custom photonic components should enable a g-hard photonic proximity fuze that replaces costly assemblies of discrete lasers, photodetectors, and bulk optics. Additional applications of this technology include void sensing, ladar and short-range 3-D imaging.

  7. Wireless surface acoustic wave and MEMS-based microsensors

    NASA Astrophysics Data System (ADS)

    Varadan, Vijay K.; Varadan, Vasundara V.

    2001-04-01

    The integration of SAW (Surface Acoustic Wave), MEMS and required microelectronics and conformal antennas to realize programmable microsensors suitable for many engineering and biomedical applications will be presented in this talk. This unique combination of technologies results in novel conformal sensors that can be remotely sensed by a wireless communication system with the advantage of no power requirements at the sensor site (passive sensor). The required features in many of these applications are high precision, wide dynamic range and wide frequency range. MEMS-SAW based devices presented possess typical advantages of MEMS sensors including the additional benefits of robustness, excellent sensitivity, surface conformability and durability. After a brief overview of SAW sensors and MEMS, the paper is focused on the design and fabrication of MEMS devices for a few engineering applications such as accelerometer and gyroscopes for automobile, inertial navigation sensors and tire pressure sensor.

  8. Indium Tin Oxide Resistor-Based Nitric Oxide Microsensors

    NASA Technical Reports Server (NTRS)

    Xu, Jennifer C.; Hunter, Gary W.; Gonzalez, Jose M., III; Liu, Chung-Chiun

    2012-01-01

    A sensitive resistor-based NO microsensor, with a wide detection range and a low detection limit, has been developed. Semiconductor microfabrication techniques were used to create a sensor that has a simple, robust structure with a sensing area of 1.10 0.99 mm. A Pt interdigitated structure was used for the electrodes to maximize the sensor signal output. N-type semiconductor indium tin oxide (ITO) thin film was sputter-deposited as a sensing material on the electrode surface, and between the electrode fingers. Alumina substrate (250 m in thickness) was sequentially used for sensor fabrication. The resulting sensor was tested by applying a voltage across the two electrodes and measuring the resulting current. The sensor was tested at different concentrations of NO-containing gas at a range of temperatures. Preliminary results showed that the sensor had a relatively high sensitivity to NO at 450 C and 1 V. NO concentrations from ppm to ppb ranges were detected with the low limit of near 159 ppb. Lower NO concentrations are being tested. Two sensing mechanisms were involved in the NO gas detection at ppm level: adsorption and oxidation reactions, whereas at ppb level of NO, only one sensing mechanism of adsorption was involved. The NO microsensor has the advantages of high sensitivity, small size, simple batch fabrication, high sensor yield, low cost, and low power consumption due to its microsize. The resistor-based thin-film sensor is meant for detection of low concentrations of NO gas, mainly in the ppb or lower range, and is being developed concurrently with other sensor technology for multispecies detection. This development demonstrates that ITO is a sensitive sensing material for NO detection. It also provides crucial information for future selection of nanostructured and nanosized NO sensing materials, which are expected to be more sensitive and to consume less power.

  9. Manipulation of Microenvironment with a Built-in Electrochemical Actuator in Proximity of a Dissolved Oxygen Microsensor

    NASA Technical Reports Server (NTRS)

    Kim, Chang-Soo; Lee, Cae-Hyang; Fiering, Jason O.; Ufer, Stefan; Scarantino, Charles W.; Nagle, H. Troy; Fiering, Jason O.; Ufer, Stefan; Nagle, H. Troy; Scarantino, Charles W.

    2004-01-01

    Abstract - Biochemical sensors for continuous monitoring require dependable periodic self- diagnosis with acceptable simplicity to check its functionality during operation. An in situ self- diagnostic technique for a dissolved oxygen microsensor is proposed in an effort to devise an intelligent microsensor system with an integrated electrochemical actuation electrode. With a built- in platinum microelectrode that surrounds the microsensor, two kinds of microenvironments, called the oxygen-saturated or oxygen-depleted phases, can be created by water electrolysis depending on the polarity. The functionality of the microsensor can be checked during these microenvironment phases. The polarographic oxygen microsensor is fabricated on a flexible polyimide substrate (Kapton) and the feasibility of the proposed concept is demonstrated in a physiological solution. The sensor responds properly during the oxygen-generating and oxygen- depleting phases. The use of these microenvironments for in situ self-calibration is discussed to achieve functional integration as well as structural integration of the microsensor system.

  10. Voltammetric behaviour of antimalarial drug artesunate in solubilized systems.

    PubMed

    Jain, Rajeev; Vikas

    2011-12-01

    The voltammetric behaviour of artesunate is studied at glassy carbon electrode in different buffer systems using square wave, differential pulse and cyclic voltammetric techniques. The peak current is linear with the drug concentration in the range 4.0-40 μg mL(-1) for serum, plasma and urine. The mean percentage recoveries of the drug, urine, plasma and serum samples are 98.6-100.2%. No electroactive interferences from the excipients and endogenous substance could be observed in the pharmaceutical dosage forms and in biological samples.

  11. Distribution of Sulfate-Reducing and Methanogenic Bacteria in Anaerobic Aggregates Determined by Microsensor and Molecular Analyses

    PubMed Central

    Santegoeds, Cecilia M.; Damgaard, Lars Riis; Hesselink, Gijs; Zopfi, Jakob; Lens, Piet; Muyzer, Gerard; de Beer, Dirk

    1999-01-01

    Using molecular techniques and microsensors for H2S and CH4, we studied the population structure of and the activity distribution in anaerobic aggregates. The aggregates originated from three different types of reactors: a methanogenic reactor, a methanogenic-sulfidogenic reactor, and a sulfidogenic reactor. Microsensor measurements in methanogenic-sulfidogenic aggregates revealed that the activity of sulfate-reducing bacteria (2 to 3 mmol of S2− m−3 s−1 or 2 × 10−9 mmol s−1 per aggregate) was located in a surface layer of 50 to 100 μm thick. The sulfidogenic aggregates contained a wider sulfate-reducing zone (the first 200 to 300 μm from the aggregate surface) with a higher activity (1 to 6 mmol of S2− m−3 s−1 or 7 × 10−9 mol s−1 per aggregate). The methanogenic aggregates did not show significant sulfate-reducing activity. Methanogenic activity in the methanogenic-sulfidogenic aggregates (1 to 2 mmol of CH4 m−3 s−1 or 10−9 mmol s−1 per aggregate) and the methanogenic aggregates (2 to 4 mmol of CH4 m−3 s−1 or 5 × 10−9 mmol s−1 per aggregate) was located more inward, starting at ca. 100 μm from the aggregate surface. The methanogenic activity was not affected by 10 mM sulfate during a 1-day incubation. The sulfidogenic and methanogenic activities were independent of the type of electron donor (acetate, propionate, ethanol, or H2), but the substrates were metabolized in different zones. The localization of the populations corresponded to the microsensor data. A distinct layered structure was found in the methanogenic-sulfidogenic aggregates, with sulfate-reducing bacteria in the outer 50 to 100 μm, methanogens in the inner part, and Eubacteria spp. (partly syntrophic bacteria) filling the gap between sulfate-reducing and methanogenic bacteria. In methanogenic aggregates, few sulfate-reducing bacteria were detected, while methanogens were found in the core. In the sulfidogenic aggregates, sulfate-reducing bacteria were

  12. Impedance and Voltammetric Studies of Electrogenerated Polyaniline Conducting Films

    DTIC Science & Technology

    1992-12-14

    discovered, such as polypyrrole, polythiophene and polyaniline ( PANI ) [3] which will be an object of this paper. All important conducting polymers, with...December 191 Technical _____________ 4. TITLE AND SUBTITLE S. FUNDING NUMBERS Impedance and voltammetric studies of electrogenerated C polyaniline ...unlimited nl 13. ABSTRACT (Maximum 200 words) Polyaniline films were electrochemically synthesized from three acidic media; sulfuric, hydrochloric and

  13. In situ applications of a new diver-operated motorized microsensor profiler.

    PubMed

    Weber, Miriam; Faerber, Paul; Meyer, Volker; Lott, Christian; Eickert, Gabriele; Fabricius, Katharina E; De Beer, Dirk

    2007-09-01

    Microsensors are powerful tools for microenvironment studies, however their use has often been restricted to laboratory applications due to the lack of adequate equipment for in situ deployments. Here we report on new features, construction details, and examples of applications of an improved diver-operated motorized microsensor profiler for underwater field operation to a water depth of 25 m. The new motorized profiler has a final precision of 5 microm, and can accommodate amperometric Clark-type microsensors for oxygen and hydrogen sulfide, potentiometric microsensors (e.g., for pH, Ca2+), and fiber-optic irradiance microsensors. The profiler is interfaced by a logger with a signal display, and has pushbuttons for underwater operation. The system can be pre-programmed to autonomous operation or interactively operated by divers. Internal batteries supply power for up to 24 h of measurements and 36 h of data storage (max. 64 million data points). Two flexible stands were developed for deployment on uneven or fragile surfaces, such as coral reefs. Three experimental pilot studies are presented, where (1) the oxygen distribution in a sand ripple was 3-D-mapped, (2) the microenvironment of sediment accumulated on a stony coral was studied, and (3) oxygen dynamics during an experimental sedimentation were investigated. This system allows SCUBA divers to perform a wide array of in situ measurements, with deployment precision and duration similar to those possible in the laboratory.

  14. Intangible pointlike tracers for liquid-crystal-based microsensors

    SciTech Connect

    Brasselet, Etienne; Juodkazis, Saulius

    2010-12-15

    We propose an optical detection technique for liquid-crystal-based sensors that is based on polarization-resolved tracking of optical singularities and does not rely on standard observation of light-intensity changes caused by modifications of the liquid crystal orientational ordering. It uses a natural two-dimensional network of polarization singularities embedded in the transverse cross section of a probe beam that passes through a liquid crystal sample, in our case, a nematic droplet held in laser tweezers. The identification and spatial evolution of such a topological fingerprint is retrieved from subwavelength polarization-resolved imaging, and the mechanical constraint exerted on the molecular ordering by the trapping beam itself is chosen as the control parameter. By restricting our analysis to one type of point singularity, C points, which correspond to location in space where the polarization azimuth is undefined, we show that polarization singularities appear as intangible pointlike tracers for liquid-crystal-based three-dimensional microsensors. The method has a superresolution potential and can be used to visualize changes at the nanoscale.

  15. Direct microsensor measurement of nitric oxide production by the osteoclast.

    PubMed

    Silverton, S F; Adebanjo, O A; Moonga, B S; Awumey, E M; Malinski, T; Zaidi, M

    1999-05-27

    Nitric oxide (NO) triggers marked osteoclast retraction which closely resembles that due to Ca2+. The effect of Ca2+ has been attributed to a stimulated release of NO. Here, we show for the first time, by direct measurement with a microsensor, that osteoclasts do indeed produce NO and that this production is enhanced by a high Ca2+. We also show that the Ca2+ ionophore, A23187, mimics the latter. Furthermore, osteoclasts on dentine produce more NO than osteoclasts on glass and NO release from dentine-plated osteoclasts is much less sensitive to stimulation by Ca2+. Finally, the microsomal Ca2+ store-depleting agent, thapsigargin, attenuates NO release only from osteoclasts on glass, suggesting that stored Ca2+ has the dominant effect in modulating NO release from non-resorbing cells. NO is a powerful inhibitor of bone resorption: a direct demonstration of its production is therefore strong evidence for a role in modulating osteoclast function. Copyright 1999 Academic Press.

  16. A Lateral Differential Resonant Pressure Microsensor Based on SOI-Glass Wafer-Level Vacuum Packaging.

    PubMed

    Xie, Bo; Xing, Yonghao; Wang, Yanshuang; Chen, Jian; Chen, Deyong; Wang, Junbo

    2015-09-21

    This paper presents the fabrication and characterization of a resonant pressure microsensor based on SOI-glass wafer-level vacuum packaging. The SOI-based pressure microsensor consists of a pressure-sensitive diaphragm at the handle layer and two lateral resonators (electrostatic excitation and capacitive detection) on the device layer as a differential setup. The resonators were vacuum packaged with a glass cap using anodic bonding and the wire interconnection was realized using a mask-free electrochemical etching approach by selectively patterning an Au film on highly topographic surfaces. The fabricated resonant pressure microsensor with dual resonators was characterized in a systematic manner, producing a quality factor higher than 10,000 (~6 months), a sensitivity of about 166 Hz/kPa and a reduced nonlinear error of 0.033% F.S. Based on the differential output, the sensitivity was increased to two times and the temperature-caused frequency drift was decreased to 25%.

  17. A Lateral Differential Resonant Pressure Microsensor Based on SOI-Glass Wafer-Level Vacuum Packaging

    PubMed Central

    Xie, Bo; Xing, Yonghao; Wang, Yanshuang; Chen, Jian; Chen, Deyong; Wang, Junbo

    2015-01-01

    This paper presents the fabrication and characterization of a resonant pressure microsensor based on SOI-glass wafer-level vacuum packaging. The SOI-based pressure microsensor consists of a pressure-sensitive diaphragm at the handle layer and two lateral resonators (electrostatic excitation and capacitive detection) on the device layer as a differential setup. The resonators were vacuum packaged with a glass cap using anodic bonding and the wire interconnection was realized using a mask-free electrochemical etching approach by selectively patterning an Au film on highly topographic surfaces. The fabricated resonant pressure microsensor with dual resonators was characterized in a systematic manner, producing a quality factor higher than 10,000 (~6 months), a sensitivity of about 166 Hz/kPa and a reduced nonlinear error of 0.033% F.S. Based on the differential output, the sensitivity was increased to two times and the temperature-caused frequency drift was decreased to 25%. PMID:26402679

  18. Voltammetric oxidation and determination of cinnarizine at glassy carbon electrode modified with multi-walled carbon nanotubes.

    PubMed

    Hegde, Rajesh N; Hosamani, Ragunatharaddi R; Nandibewoor, Sharanappa T

    2009-09-01

    The voltammetric oxidation of cinnarizine was investigated. In pH 2.5 Britton-Robinson buffer, cinnarizine shows an irreversible oxidation peak at about 1.20 V at a multi-walled carbon nanotube (MWCNT)-modified glassy carbon electrode. The cyclic voltammetric results indicate that MWCNT-modified glassy carbon electrode can remarkably enhance electrocatalytic activity towards the oxidation of cinnarizine. The electrocatalytic behavior was further exploited as a sensitive detection scheme for the cinnarizine determination by differential-pulse voltammetry. Under optimized conditions, the concentration range and detection limit are 9.0x10(-8) to 6.0x10(-6) M and 2.58x10(-9) M, respectively for cinnarizine. The proposed method was successfully applied to cinnarizine determination in pharmaceutical samples. The analytical performance of this sensor has been evaluated for the detection of analyte in urine as a real sample.

  19. Humidity-Induced Charge Leakage and Field Attenuation in Electric Field Microsensors

    PubMed Central

    Zhang, Haiyan; Fang, Dongming; Yang, Pengfei; Peng, Chunrong; Wen, Xiaolong; Xia, Shanhong

    2012-01-01

    The steady-state zero output of static electric field measuring systems often fluctuates, which is caused mainly by the finite leakage resistance of the water film on the surface of the electric field microsensor package. The water adsorption has been calculated using the Boltzmann distribution equation at various relative humidities for borosilicate glass and polytetrafluoroethylene surfaces. At various humidities, water film thickness has been calculated, and the induced charge leakage and field attenuation have been theoretically investigated. Experiments have been performed with microsensors to verify the theoretical predictions and the results are in good agreement. PMID:22666077

  20. Electrodeposition of high-T{sub c} superconductor material for microsensor fabrication

    SciTech Connect

    Natarajan, A.; Wang, W.; Ma, E.; Bhattacharya, R.N.; Khann-Malek, C.; Paranthaman, M.; Martin, P.M.

    1996-12-31

    Thin films of YBa{sub 2}Cu{sub 3}O{sub 7} (YBCO) superconductor precursor were synthesized using electrodeposition. The YBCO precursor thin films were deposited on Ag foils using pulsed potential deposition conditions of 10 s at -4 V and 10 s at -1 V (vs Ag reference electrode). The post-annealed films showed zero electrical resistance at 60 K. The procedures for fabricating a high precision micro-sensor using YBCO superconductor, for measuring weak magnetic fields are outlined. The micro-sensor templates were patterned using x rays and precursor films were deposited into the features. 8 figs, 10 refs.

  1. Optical microsensor for continuous glucose measurements in interstitial fluid

    NASA Astrophysics Data System (ADS)

    Olesberg, Jonathon T.; Cao, Chuanshun; Yager, Jeffrey R.; Prineas, John P.; Coretsopoulos, Chris; Arnold, Mark A.; Olafsen, Linda J.; Santilli, Michael

    2006-02-01

    Tight control of blood glucose levels has been shown to dramatically reduce the long-term complications of diabetes. Current invasive technology for monitoring glucose levels is effective but underutilized by people with diabetes because of the pain of repeated finger-sticks, the inconvenience of handling samples of blood, and the cost of reagent strips. A continuous glucose sensor coupled with an insulin delivery system could provide closed-loop glucose control without the need for discrete sampling or user intervention. We describe an optical glucose microsensor based on absorption spectroscopy in interstitial fluid that can potentially be implanted to provide continuous glucose readings. Light from a GaInAsSb LED in the 2.2-2.4 μm wavelength range is passed through a sample of interstitial fluid and a linear variable filter before being detected by an uncooled, 32-element GaInAsSb detector array. Spectral resolution is provided by the linear variable filter, which has a 10 nm band pass and a center wavelength that varies from 2.18-2.38 μm (4600-4200 cm -1) over the length of the detector array. The sensor assembly is a monolithic design requiring no coupling optics. In the present system, the LED running with 100 mA of drive current delivers 20 nW of power to each of the detector pixels, which have a noise-equivalent-power of 3 pW/Hz 1/2. This is sufficient to provide a signal-to-noise ratio of 4500 Hz 1/2 under detector-noise limited conditions. This signal-to-noise ratio corresponds to a spectral noise level less than 10 μAU for a five minute integration, which should be sufficient for sub-millimolar glucose detection.

  2. Distributed optical microsensors for hydrogen leak detection and related applications

    NASA Astrophysics Data System (ADS)

    Hunter, Scott R.; Patton, James F.; Sepaniak, Michael J.; Datskos, Panos G.; Smith, D. Barton

    2010-04-01

    Significant advances have recently been made to develop optically interrogated microsensor based chemical sensors with specific application to hydrogen vapor sensing and leak detection in the hydrogen economy. We have developed functionalized polymer-film and palladium/silver alloy coated microcantilever arrays with nanomechanical sensing for this application. The uniqueness of this approach is in the use of independent component analysis (ICA) and the classification techniques of neural networks to analyze the signals produced by an array of microcantilever sensors. This analysis identifies and quantifies the amount of hydrogen and other trace gases physisorbed on the arrays. Selectivity is achieved by using arrays of functionalized sensors with a moderate distribution of specificity among the sensing elements. The device consists of an array of beam-shaped transducers with molecular recognition phases (MRPs) applied to one surface of the transducers. Bending moments on the individual transducers can be detected by illuminating them with a laser or an LED and then reading the reflected light with an optical position sensitive detector (PSD) such as a CCD. Judicious selection of MRPs for the array provides multiple isolated interaction surfaces for sensing the environment. When a particular chemical agent binds to a transducer, the effective surface stresses of its modified and uncoated sides change unequally and the transducer begins to bend. The extent of bending depends upon the specific interactions between the microcantilever's MRP and the analyte. Thus, the readout of a multi-MRP array is a complex multidimensional signal that can be analyzed to deconvolve a multicomponent gas mixture. The use of this sensing and analysis technique in unattended networked arrays of sensors for various monitoring and surveillance applications is discussed.

  3. Monitoring Volatile Organic Tank Waste Using Cermet Microsensors

    SciTech Connect

    Edward G. Gatliff, Ph.D.; Laura R. Skubal, Ph.D.; Michael C. Vogt, Ph.D.

    2006-03-13

    Presently, very few inexpensive technologies exist in the marketplace that can determine the contents of tank waste or monitor the chemistry of tank constituents in near-real time. The research addressed this problem by developing and assessing ceramic-metallic based microsensors for determining the constituents of a liquid organic storage tank by examining the gases in the headspace of the tank. Overall, the WBO and YSZ sensors responded well to the chemicals in this study. Responses to various concentrations were distinguishable visually. This is a clear indication that pattern recognition tools will be effective in resolving the constituents and concentrations. In tests, such as the test with acetophenone, one sensor, the WBO sensor is not extremely effective. However, the other sensor, the YSZ sensor, is effective in resolving the concentrations. This supports the need to use an array of sensors, as one sensor may be reactive to a compound while another may not. In the course of this research, several interesting phenomena surfaced. New sensors, that were fabricated but not used in a contaminant gas, seemed to function more effectively and predictably if a ?conditioning? step was imposed upon them prior to use in square wave voltammetry. A conditioning step consists of running cyclic voltammetry prior to running square wave voltammetry. This step tends to ?cleanse? the sensor surface by providing a full -1.0 V to +1.0V sweep and both oxidizing and reducing compounds on the sensor surface. [Note: squarewave voltammetry will simply oxidize or reduce compounds ? it will not induce both reactions.] This sweep is essential for recovery between samples.

  4. Distributed optical microsensors for hydrogen leak detection and related applications

    SciTech Connect

    Hunter, Scott Robert; Patton, James; Sepaniak, Michael; Datskos, Panos G; Smith, Barton

    2010-01-01

    Significant advances have recently been made to develop optically interrogated microsensor based chemical sensors with specific application to hydrogen vapor sensing and leak detection in the hydrogen economy. We have developed functionalized polymer-film and palladium/silver alloy coated microcantilever arrays with nanomechanical sensing for this application. The uniqueness of this approach is in the use of independent component analysis (ICA) and the classi cation techniques of neural networks to analyze the signals produced by an array of microcantilever sensors. This analysis identifies and quantifies the amount of hydrogen and other trace gases physisorbed on the arrays. Selectivity is achieved by using arrays of functionalized sensors with a moderate distribution of specificity among the sensing elements. The device consists of an array of beam-shaped transducers with molecular recognition phases (MRPs) applied to one surface of the transducers. Bending moments on the individual transducers can be detected by illuminating them with a laser or an LED and then reading the reflected light with an optical position sensitive detector (PSD) such as a CCD. Judicious selection of MRPs for the array provides multiple isolated interaction surfaces for sensing the environment. When a particular chemical agent binds to a transducer, the effective surface stresses of its modified and uncoated sides change unequally and the transducer begins to bend. The extent of bending depends upon the specific interactions between the microcantilever s MRP and the analyte. Thus, the readout of a multi-MRP array is a complex multi-dimensional signal that can be analyzed to deconvolve a multicomponent gas mixture. The use of this sensing and analysis technique in unattended networked arrays of sensors for various monitoring and surveillance applications is discussed.

  5. Micro-sensors for in-situ meteorological measurements

    NASA Technical Reports Server (NTRS)

    Crisp, David; Kaiser, William J.; Vanzandt, Thomas R.; Tillman, James E.

    1993-01-01

    Improved in-situ meteorological measurements are needed for monitoring the weather and climate of the terrestrial and Martian atmospheres. We have initiated a program to assess the feasibility and utility of micro-sensors for precise in-situ meteorological measurements in these environments. Sensors are being developed for measuring pressure, temperature, wind velocity, humidity, and aerosol amounts. Silicon micro-machining and large scale integration technologies are being used to make sensors that are small, rugged, lightweight, and require very little power. Our long-term goal is to develop very accurate miniaturized sensors that can be incorporated into complete instrument packages or 'micro weather stations,' and deployed on a variety of platforms. If conventional commercially available silicon production techniques can be used to fabricate these sensor packages, it will eventually be possible to mass-produce them at low cost. For studies of the Earth's troposphere and stratosphere, they could be deployed on aircraft, dropsondes, radiosondes, or autonomous surface stations at remote sites. Improved sensor accuracy and reduced sensor cost are the primary challenges for these applications. For studies of the Martian atmosphere, these sensor packages could be incorporated into the small entry probes and surface landers that are being planned for the Mars Environmental SURvey (MESUR) Mission. That decade-long program will deploy a global network of small stations on the Martian surface for monitoring meteorological and geological processes. Low mass, low power, durability, large dynamic range and calibration stability are the principal challenges for this application. Our progress on each of these sensor types is presented.

  6. Use of a dissolved oxygen microsensor for assessing the viability and thickness of microbial biofilm on root surfaces.

    PubMed

    Tomazinho, F S F; Sousa-Neto, M D; Pécora, J D; Lamon, A W; Gonzalez, B C; Silva-Sousa, Y T C

    2015-05-01

    To evaluate the use of a dissolved oxygen microsensor (DOMS) for assessing the viability and thickness of microbial biofilms on the apical external surface of contaminated human tooth roots. Apical biofilm formation was evaluated in 15 roots contaminated in vitro with a polymicrobial mixture of Staphylococcus aureus, Enterococcus faecalis, Pseudomonas aeruginosa and Candida albicans for 7, 21 and 60 days and in three freshly extracted roots with associated radiographically visible periapical lesions. In each root, the thickness and viability (measured by the amount of dissolved oxygen) of biofilm formed on the apical 2 mm were examined with the DOMS. Scanning electron microscopy (SEM) was used as an auxiliary analysis to confirm the existence of the biofilms detected by the DOMS. The DOMS detected dissolved oxygen on the biofilms formed on the three residual roots up to thickness of 375 μm, 480 μm and 1650 μm. In the 15 roots contaminated in vitro, the DOMS detected dissolved oxygen in six specimens up to thicknesses from 75 to 250 μm, and the intensity of the metabolic activity (biofilm thickness) was directly proportional to the contamination time. SEM confirmed the presence of biofilm in all roots. The dissolved oxygen microsensor allowed the measurement of the amount of dissolved oxygen in the biofilm, which is indicative of the intensity of the microbial metabolic activity (viability), correlating the results with biofilm thickness. The DOMS was effective in freshly extracted roots, but had limitations in roots contaminated in vitro after short periods (7 and 21 days) of contamination. © 2014 International Endodontic Journal. Published by John Wiley & Sons Ltd.

  7. Microsensor and transcriptomic signatures of oxygen depletion in biofilms associated with chronic wounds: Biofilms and oxygen

    SciTech Connect

    James, Garth A.; Ge Zhao, Alice; Usui, Marcia; Underwood, Robert A.; Nguyen, Hung; Beyenal, Haluk; deLancey Pulcini, Elinor; Agostinho Hunt, Alessandra; Bernstein, Hans C.; Fleckman, Philip; Olerud, John; Williamson, Kerry S.; Franklin, Michael J.; Stewart, Philip S.

    2016-02-16

    Polymicrobial biofilms have been implicated in delayed wound healing, although the mechanisms by which biofilms impair wound healing are poorly understood. Many species of bacteria produce exotoxins and exoenzymes that may inhibit healing. In addition, oxygen consumption by biofilms may impede wound healing. In this study, we used oxygen microsensors to measure oxygen transects through in vitro-cultured biofilms, biofilms formed in vivo in a diabetic (db/db) mouse model, and ex vivo human chronic wound specimens. The results show that oxygen levels within both euthanized and live mouse wounds had steep gradients that reached minima ranging from 19 to 61% oxygen partial pressure, compared to atmospheric oxygen levels. The oxygen gradients in the mouse wounds were similar to those observed for clinical isolates cultured in vitro and for human ex vivo scabs. No oxygen gradients were observed for heat-killed scabs, suggesting that active metabolism by the viable bacteria contributed to the reduced oxygen partial pressure of the wounds. To characterize the metabolic activities of the bacteria in the mouse wounds, we performed transcriptomics analyses of Pseudomonas aeruginosa biofilms associated with the db/db mice wounds using Affymetrix microarrays. The results demonstrated that the bacteria expressed genes for metabolic activities associated with cell growth. Interestingly, the transcriptome results indicated that the bacteria within the wounds also experienced oxygen-limitation stress. Among the bacterial genes that were expressed in vivo were genes associated with the Anr-mediated hypoxia-stress response. Other bacterial stress response genes highly expressed in vivo were genes associated with stationary-phase growth, osmotic stress, and RpoH-mediated heat shock stress. Overall, the results support the hypothesis that the metabolic activities of bacteria in biofilms act as oxygen sinks in chronic wounds and that the depletion of oxygen contributes to the

  8. Determination of L- Ascorbic Acid in Plasma by Voltammetric Method

    PubMed Central

    Behfar, Abdol Azim; Sadeghi, Nafiseh; Jannat, Behrooz; Oveisi, Mohammad Reza

    2010-01-01

    Voltammetric techniques have been considered as important methods among the analytical techniques used for the identification and determination of trace concentrations of many biological molecules such as L-ascorbic acid (AA). L-ascorbic acid is an electro-active molecule, though it is difficult to determine its value directly with a majority of electrodes made of carbon and transition metals, because of electrode surface problems. The present study is based on I-E curves for AA analysis at various pH. Furthermore, the effects of the presence of other electro-active substances; such as copper, as well as the effect of the sweep rate of potential will be studied. The present study is based on analysis of the current-voltage curves for L-ascorbic acid at varying pH and sweep rate scan values. An analysis was also carried out to measure the influence of the concentration of some electro active species. The peak height of the first oxidation wave is used for L-ascorbic acid assay. L-ascorbic acid was determined in aqueous media by linear-scan voltammetry on a gold electrode; ranging between (1-175 μg/mL). In biologic samples, for elimination of uric acid or some sugars and effects, a significant interference of copper ions whose presence reduces the height of the L-ascorbic acid oxidation peak was used. The optimum pH and sweep rate were 3.2 and 7500mV/s, respectively. Under these conditions, the detection limit of the method was 0.3 μg/mL. Repeatability of the method based on relative standard deviation (RSD) 50, 10 and 1 μg/mL concentrations was 0.83, 2.1 and 10.3%, respectively. The calibration curve was linear over the range 1-175μg/mL (r2 = 0.9977, p < 0.001). The advantage of this method lies in the fact that the use of copper eliminates the interference of different substances such as uric acid. PMID:24363717

  9. Microgravimetric and voltammetric study of Zn underpotential deposition on platinum in alkaline medium

    NASA Astrophysics Data System (ADS)

    Calegaro, M. L.; Santos, M. C.; Miwa, D. W.; Machado, S. A. S.

    2005-03-01

    The microgravimetric and voltammetric responses of a polycrystalline Pt electrode in 0.1 mol L -1 NaOH solution in the presence and the absence of 1.6 × 10 -4 Zn 2+, at 0.1 V s -1 were analyzed. During the positive potential sweep, the water molecules are progressively substituted by OH - ions, prior to PtO formation. The voltammetric charges obtained under the Zn ads dissolution peaks suggest that 0.7 monolayers are deposited, with each Zn ad-atom occupying one active site and transferring two electrons. The total loss of mass due to the dissolution of the Zn ad-layer was 136.6 ng cm -2 and the mass increase due to PtO formation was found to be only 12 ng cm -2 less than the theoretical ones, 157.5 and 37.4 ng cm -2, respectively, indicating that both processes are overlapped. In this way it is proposed that an adsorbed by-layer of Zn and OH - ions is formed.

  10. Microsensor and transcriptomic signatures of oxygen depletion in biofilms associated with chronic wounds.

    PubMed

    James, Garth A; Ge Zhao, Alice; Usui, Marcia; Underwood, Robert A; Nguyen, Hung; Beyenal, Haluk; deLancey Pulcini, Elinor; Agostinho Hunt, Alessandra; Bernstein, Hans C; Fleckman, Philip; Olerud, John; Williamson, Kerry S; Franklin, Michael J; Stewart, Philip S

    2016-03-01

    Biofilms have been implicated in delayed wound healing, although the mechanisms by which biofilms impair wound healing are poorly understood. Many species of bacteria produce exotoxins and exoenzymes that may inhibit healing. In addition, oxygen consumption by biofilms and by the responding leukocytes, may impede wound healing by depleting the oxygen that is required for healing. In this study, oxygen microsensors to measure oxygen transects through in vitro cultured biofilms, biofilms formed in vivo within scabs from a diabetic (db/db) mouse wound model, and ex vivo human chronic wound specimens was used. The results showed that oxygen levels within mouse scabs had steep gradients that reached minima ranging from 17 to 72 mmHg on live mice and from 6.4 to 1.1 mmHg on euthanized mice. The oxygen gradients in the mouse scabs were similar to those observed for clinical isolates cultured in vitro and for human ex vivo specimens. To characterize the metabolic activities of the bacteria in the mouse scabs, transcriptomics analyses of Pseudomonas aeruginosa biofilms associated with the db/db mice wounds was performed. The results demonstrated that the bacteria expressed genes for metabolic activities associated with cell growth. Interestingly, the transcriptome results also indicated that the bacteria within the wounds experienced oxygen-limitation stress. Among the bacterial genes that were expressed in vivo were genes associated with the Anr-mediated hypoxia-stress response. Other bacterial stress response genes highly expressed in vivo were genes associated with stationary-phase growth, osmotic stress, and RpoH-mediated heat shock stress. Overall, the results supported the hypothesis that bacterial biofilms in chronic wounds promote chronicity by contributing to the maintenance of localized low oxygen tensions, through their metabolic activities and through their recruitment of cells that consume oxygen for host defensive processes.

  11. Flexible Microsensor Array for the Root Zone Monitoring of Porous Tube Plant Growth System

    NASA Technical Reports Server (NTRS)

    Sathyan, Sandeep; Kim, Chang-Soo; Porterfield, D. Marshall; Nagle, H. Troy; Brown, Christopher S.

    2004-01-01

    Control of oxygen and water in the root zone is vital to support plant growth in the microgravity environment. The ability to control these sometimes opposing parameters in the root zone is dependent upon the availability of sensors to detect these elements and provide feedback for control systems. In the present study we demonstrate the feasibility of using microsensor arrays on a flexible substrate for dissolved oxygen detection, and a 4-point impedance microprobe for surface wetness detection on the surface of a porous tube (PT) nutrient delivery system. The oxygen microsensor reported surface oxygen concentrations that correlated with the oxygen concentrations of the solution inside the PT when operated at positive pressures. At negative pressures the microsensor shows convergence to zero saturation (2.2 micro mol/L) values due to inadequate water film formation on porous tube surface. The 4-point microprobe is useful as a wetness detector as it provides a clear differentiation between dry and wet surfaces. The unique features of the dissolved oxygen microsensor array and 4-point microprobe include small and simple design, flexibility and multipoint sensing. The demonstrated technology is anticipated to provide low cost, and highly reliable sensor feedback monitoring plant growth nutrient delivery system in both terrestrial and microgravity environments.

  12. Flexible microsensor technology for real-time navigation tracking in balloon sinus ostial dilation

    PubMed Central

    Lam, Kent; Bigcas, Jo-Lawrence; Luong, Amber; Yao, William

    2017-01-01

    Background: Microsensor navigation has the potential to aid balloon sinus ostial dilation by providing real-time tracking of balloon devices within the complex anatomy of the sinonasal cavities. Objective: This feasibility study evaluated the incorporation of a new microsensor technology into a flexible guidewire for use with current instruments in balloon sinus ostial dilation. Methods: A retrospective study was conducted to include seven men and one woman (age range, 33–68 years), who underwent balloon sinus ostial dilation with flexible microsensor navigation in the operating room setting. All the procedures were performed at target sinuses with the patient under general anesthesia, in conjunction with subsequent endoscopic sinus surgery. Results: Balloon dilation was attempted at the maxillary (n = 3), frontal (n = 14), and sphenoid (n = 1) sinuses. In all the cases, the surgical navigation system displayed the flexible wire tip as it was advanced to the target sinus ostia; this visual feedback for wire position guided the balloon placement. Successful balloon dilation with assistance of flexible microsensor navigation was performed on most sinuses, except a single frontal sinus with adjacent type 2 frontal cells. Conclusion: Flexible navigation technology may be combined with balloon sinus technology to facilitate localization of instruments in the sinus anatomy. Additional optimization of both the device and software technology is warranted. PMID:28381323

  13. The modelling of a capacitive microsensor for biosensing applications

    NASA Astrophysics Data System (ADS)

    Bezuidenhout, P. H.; Schoeman, J.; Joubert, T. H.

    2014-06-01

    Microsensing is a leading field in technology due to its wide application potential, not only in bio-engineering, but in other fields as well. Microsensors have potentially low-cost manufacturing processes, while a single device type can have various uses, and this consequently helps with the ever-growing need to provide better health conditions in rural parts of the world. Capacitive biosensors detect a change in permittivity (or dielectric constant) of a biological material, usually within a parallel plate capacitor structure which is often implemented with integrated electrodes of an inert metal such as gold or platinum on a microfluidic substrate typically with high dielectric constant. There exist parasitic capacitance components in these capacitive sensors, which have large influence on the capacitive measurement. Therefore, they should be considered for the development of sensitive and accurate sensing devices. An analytical model of a capacitive sensor device is discussed, which accounts for these parasitic factors. The model is validated with a laboratory device of fixed geometry, consisting of two parallel gold electrodes on an alumina (Al2O3) substrate mounted on a glass microscope slide, and with a windowed cover layer of poly-dimethyl-siloxane (PDMS). The thickness of the gold layer is 1μm and the electrode spacing is 300μm. The alumina substrate has a thickness of 200μm, and the high relative permittivity of 11.5 is expected to be a significantly contributing factor to the total device capacitance. The 155μm thick PDMS layer is also expected to contribute substantially to the total device capacitance since the relative permittivity for PDMS is 2.7. The wideband impedance analyser evaluation of the laboratory device gives a measurement result of 2pF, which coincides with the model results; while the handheld RLC meter readout of 4pF at a frequency of 10kHz is acceptable within the measurement accuracy of the instrument. This validated model will

  14. O2 microsensors for minimally invasive tissue monitoring.

    PubMed Central

    Wang, W.; Vadgama, P.

    2004-01-01

    Tissue oxygenation is a key factor ensuring normal tissue functions and viability. Continuous real-time monitoring of the partial pressure of oxygen, pO(2), in tissues gives insight into the dynamic fluctuations of O(2) supplies to tissues by blood circulation. Small oxygen sensors enable investigations of the spatial variation of pO(2) in tissues at different locations in relation to local microvessels. In this paper, pO(2) measurement using microelectrodes and biocompatible sensorsv is discussed and recent progress of their application in human skin is reviewed. Emphasis is given to working principles of a number of existing oxygen sensors and their potential application in vivo and in tissue engineering. Results on spatial and temporal variations of the pO(2) in human skin introduced by localized ischaemia-reperfusion are presented when the surface of the skin is covered by an oxygen-free paraffin oil layer and the range of the tissue pO(2) is deduced to be between 0 and 60 mmHg. In the study, pO(2) increases from 8.0 +/- 3.2 mmHg (n = 6) at the surface of the skin to 35.2 +/- 8.0 mmHg (n = 9) at a depth just above the subpapillary plexus. Temporal decay in pO(2) following tissue compression and rise in pO(2) following pressure release can be described using mono-exponential functions. The time constant for the exponential decay, tau = 8.44 +/- 1.53 s (n = 7) is consistently greater than that for the exponential rises, tau' = 4.75 +/- 0.82 s (n = 6). The difference in pO2 change with the time following tissue compression and pressure release reveals different dynamic mechanisms involved in the two transient phases. The elevated steady state pO(2) following reperfusion, which is approximately 20% higher than the pre-occlusion value, indicates localized reactive hyperaemia. Possible applications of O(2) microsensors in diseases, e.g. tumours, pressure ulcers, are also discussed. PMID:16849157

  15. Microelectrodes for in situ voltammetric determination of pollutants

    NASA Astrophysics Data System (ADS)

    Paux, T.; Billon, G.; Pieta, 1.; Ouddane, B.; Fischer, J. C.; Wartel, M.

    2003-05-01

    The toxicity of sediments is often closely bound to the labile toxic elements contents. In porewaters, metal concentrations are generally measured after separation from the solid material by means of pressure or centrifugation. The recent developments of in situ metal measurements by microsensors do not require any pretreatment of the sediment and hence avoid some possible artefacts like oxygen penetration in anoxic sediment and/or temperature modification. Our work describes firstly the preparation of microelectrodes based on a thin solid Silver (diameter: 30 μm) or Iridium (diameter: 75 μm) wire, covered at the tip with a fine layer of mercury. Secondly, an analytical procedure (based on cathodic voltammetry) is presented to measure Mn(II), Fe(II) and S(-II) concentrations, which play a relevant role in the metal pollutant cycle in sediments. By anodic stripping voltammetry, such microsensors are able to detect trace heavy metals such as Cd(II) or Pb(II) at relatively low concentration levels ( 1 μg.dm^{-3}) with 5 minutes accumulation time. Finally, the most important challenge is to install the microelectrodes in natural media and to follow up metal pollution over a long time period.

  16. Assessment of air quality microsensors versus reference methods: The EuNetAir joint exercise

    NASA Astrophysics Data System (ADS)

    Borrego, C.; Costa, A. M.; Ginja, J.; Amorim, M.; Coutinho, M.; Karatzas, K.; Sioumis, Th.; Katsifarakis, N.; Konstantinidis, K.; De Vito, S.; Esposito, E.; Smith, P.; André, N.; Gérard, P.; Francis, L. A.; Castell, N.; Schneider, P.; Viana, M.; Minguillón, M. C.; Reimringer, W.; Otjes, R. P.; von Sicard, O.; Pohle, R.; Elen, B.; Suriano, D.; Pfister, V.; Prato, M.; Dipinto, S.; Penza, M.

    2016-12-01

    The 1st EuNetAir Air Quality Joint Intercomparison Exercise organized in Aveiro (Portugal) from 13th-27th October 2014, focused on the evaluation and assessment of environmental gas, particulate matter (PM) and meteorological microsensors, versus standard air quality reference methods through an experimental urban air quality monitoring campaign. The IDAD-Institute of Environment and Development Air Quality Mobile Laboratory was placed at an urban traffic location in the city centre of Aveiro to conduct continuous measurements with standard equipment and reference analysers for CO, NOx, O3, SO2, PM10, PM2.5, temperature, humidity, wind speed and direction, solar radiation and precipitation. The comparison of the sensor data generated by different microsensor-systems installed side-by-side with reference analysers, contributes to the assessment of the performance and the accuracy of microsensor-systems in a real-world context, and supports their calibration and further development. The overall performance of the sensors in terms of their statistical metrics and measurement profile indicates significant differences in the results depending on the platform and on the sensors considered. In terms of pollutants, some promising results were observed for O3 (r2: 0.12-0.77), CO (r2: 0.53-0.87), and NO2 (r2: 0.02-0.89). For PM (r2: 0.07-0.36) and SO2 (r2: 0.09-0.20) the results show a poor performance with low correlation coefficients between the reference and microsensor measurements. These field observations under specific environmental conditions suggest that the relevant microsensor platforms, if supported by the proper post processing and data modelling tools, have enormous potential for new strategies in air quality control.

  17. Microscopic and voltammetric characterization of bioanalytical platforms based on lactate oxidase.

    PubMed

    Parra, A; Casero, E; Vázquez, L; Jin, J; Pariente, F; Lorenzo, E

    2006-06-06

    A microscopic and voltammetric characterization of lactate oxidase- (LOx-) based bioanalytical platforms for biosensor applications is presented. In this context, emphasis is placed on amperometric biosensors based on LOx that have been immobilized by direct absorption on carbon surfaces, in particular, glassy carbon (GC) and highly ordered pyrolytic graphite (HOPG). The immobilized LOx layers have been characterized using atomic force microscopy (AFM) under liquid conditions and cyclic voltammetry. In addition, spatially resolved mapping of enzymatic activity has been carried out using scanning electrochemical microscopy (SECM). In the presence of lactate with hydroxymethylferrocene (HMF) as a redox mediator in solution, biosensors obtained by direct adsorption of LOx onto GC electrodes exhibited a clear electrocatalytic activity, and lactate could be determined amperometrically at 300 mV versus SSCE. The proposed biosensor also exhibits good operating performance in terms of linearity, detection limit, and lifetime.

  18. Theoretical treatment of staircase voltammetric stripping from the thin film mercury electrode

    USGS Publications Warehouse

    Christie, J.H.; Osteryoung, R.A.

    1976-01-01

    Staircase voltammetric stripping is an attractive alternative to both differential pulse and linear scan voltammetric stripping. This paper presents a theoretical treatment of this new stripping mode applied to the thin-film mercury electrode. For equivalent scan rates the faradaic response is somewhat smaller than that obtained by linear scan stripping.

  19. Electrochemical Quartz Crystal Microbalance Monitoring of the Cyclic Voltammetric Deposition of Polyaniline

    ERIC Educational Resources Information Center

    Xie, Qingji; Li, Zhili; Deng, Chunyan; Liu, Meiling; Zhang, Youyu; Ma, Ming; Xia, Shaoxi; Xiao, Xiaoming; Yin, Dulin; Yao, Shouzhuo

    2007-01-01

    A real-time, labeled-free and nanogram-sensitive mass sensor, electrochemical quartz crystal microbalance (EQCM) is used to monitor a cyclic voltammetric deposition of polyaniline (PANI). The results determined that the efficiency for PANI deposition and the anion-doping ratio is calculated in one single cyclic voltammetric.

  20. Electrochemical Quartz Crystal Microbalance Monitoring of the Cyclic Voltammetric Deposition of Polyaniline

    ERIC Educational Resources Information Center

    Xie, Qingji; Li, Zhili; Deng, Chunyan; Liu, Meiling; Zhang, Youyu; Ma, Ming; Xia, Shaoxi; Xiao, Xiaoming; Yin, Dulin; Yao, Shouzhuo

    2007-01-01

    A real-time, labeled-free and nanogram-sensitive mass sensor, electrochemical quartz crystal microbalance (EQCM) is used to monitor a cyclic voltammetric deposition of polyaniline (PANI). The results determined that the efficiency for PANI deposition and the anion-doping ratio is calculated in one single cyclic voltammetric.

  1. The use of microsensors to study the role of the loading rate and surface velocity on the growth and the composition of nitrifying biofilms.

    PubMed

    Gonzalez, B C; Spinola, A L G; Lamon, A W; Araujo, J C; Campos, J R

    2011-01-01

    The good composition and activity of biofilms are very important for successful operation and control of fixed-film biological reactors employed in liquid effluents treatment. During the last decade, microsensors have been applied to study microbial ecology. These sensors could provide information regarding the microbial activity concerning nitrification and denitrification that occur inside biofilms. Other techniques of molecular biology, such as fluorescence in situ hybridization (FISH), have also contributed to this matter because their application aids in the identification of the bacterial populations that compose the biofilms. The focus of this paper was to study the loading rate and surface velocity to promote the development of nitrifying biofilms in three distinct flow cells that were employed in the post treatment of a synthetic wastewater simulating the effluent from a UASB (Upflow Anaerobic Sludge Blanket) reactor. Using the FISH technique, it was found that the population of ammonia-oxidizing-bacteria was greater than that of nitrite-oxidizing-bacteria; this was also supported by the lower production of nitrate determined by physicochemical and microsensor analyses. It was verified that the loading rate and surface velocity that promoted the greatest nitrogen removal were 0.25 g N-amon m(-2)biofilm day(-1) and 1 m h(-1), respectively.

  2. Resistance to oxidation of white wines assessed by voltammetric means.

    PubMed

    Rodrigues, Astride; Silva Ferreira, A C; Guedes de Pinho, Paula; Bento, Fátima; Geraldo, Dulce

    2007-12-26

    This work concerns the development of a methodology suited to measure the resistance to oxidation of white wines by cyclic voltammetry. The voltammetric responses of several white wines of different origin and age were analyzed in the oxidation potential range (0.2-1.2 V vs SCE). Currents measured at fixed potentials were correlated to the concentration of ascorbic acid, SO2, and total phenolics. A forced degradation study was monitored by cyclic voltammetry; from plots of current versus time, the consumption rates of oxidizable species in wine were estimated.

  3. Application of graphene for preconcentration and highly sensitive stripping voltammetric analysis of organophosphate pesticide.

    PubMed

    Wu, Shuo; Lan, Xiaoqin; Cui, Lijun; Zhang, Lihui; Tao, Shengyang; Wang, Hainan; Han, Mei; Liu, Zhiguang; Meng, Changgong

    2011-08-12

    Electrochemical reduced β-cyclodextrin dispersed graphene (β-CD-graphene) was developed as a sorbent for the preconcentration and electrochemical sensing of methyl parathion (MP), a representative nitroaromatic organophosphate pesticide with good redox activity. Benefited from the ultra-large surface area, large delocalized π-electron system and the superconductivity of β-CD-graphene, large amount of MP could be extracted on β-CD-graphene modified electrode via strong π-π interaction and exhibited fast accumulation and electron transfer rate. Combined with differential pulse voltammetric analysis, the sensor shows ultra-high sensitivity, good selectivity and fast response. The limit of detection of 0.05 ppb is more than 10 times lower than those obtained from other sorbent based sensors. The method may open up a new possibility for the widespread use of electrochemical sensors for monitoring of ultra-trace OPs.

  4. The NASA Smart Probe Project for real-time multiple microsensor tissue recognition

    NASA Technical Reports Server (NTRS)

    Andrews, Russell J.; Mah, Robert W.

    2003-01-01

    BACKGROUND: Remote surgery requires automated sensors, effectors and sensor-effector communication. The NASA Smart Probe Project has focused on the sensor aspect. METHODS: The NASA Smart Probe uses neural networks and data from multiple microsensors for a unique tissue signature in real time. Animal and human trials use several probe configurations: (1) 8-microsensor probe (2.5 mm in diameter) for rodent studies (normal and subcutaneous mammary tumor tissues), and (2) 21-gauge needle probe with 3 spectroscopic fibers and an impedance microelectrode for breast cancer diagnosis in humans. Multisensor data are collected in real time (update 100 times/s) using PCs. RESULTS: Human data (collected by NASA licensee BioLuminate) from 15 women undergoing breast biopsy distinguished normal tissue from both benign tumors and breast carcinoma. Tumor margins and necrosis are rapidly detected. CONCLUSION: Real-time tissue identification is achievable. Potential applications, including probes incorporating nanoelectrode arrays, are presented. Copyright 2003 S. Karger AG, Basel.

  5. Integration of P-CuO Thin Sputtered Layers onto Microsensor Platforms for Gas Sensing

    PubMed Central

    Presmanes, Lionel; Thimont, Yohann; el Younsi, Imane; Chapelle, Audrey; Blanc, Frédéric; Talhi, Chabane; Bonningue, Corine; Barnabé, Antoine; Menini, Philippe; Tailhades, Philippe

    2017-01-01

    P-type semiconducting copper oxide (CuO) thin films deposited by radio-frequency (RF) sputtering were integrated onto microsensors using classical photolithography technologies. The integration of the 50-nm-thick layer could be successfully carried out using the lift-off process. The microsensors were tested with variable thermal sequences under carbon monoxide (CO), ammonia (NH3), acetaldehyde (C2H4O), and nitrogen dioxide (NO2) which are among the main pollutant gases measured by metal-oxide (MOS) gas sensors for air quality control systems in automotive cabins. Because the microheaters were designed on a membrane, it was then possible to generate very rapid temperature variations (from room temperature to 550 °C in only 50 ms) and a rapid temperature cycling mode could be applied. This measurement mode allowed a significant improvement of the sensor response under 2 and 5 ppm of acetaldehyde. PMID:28621738

  6. The NASA Smart Probe Project for real-time multiple microsensor tissue recognition

    NASA Technical Reports Server (NTRS)

    Andrews, Russell J.; Mah, Robert W.

    2003-01-01

    BACKGROUND: Remote surgery requires automated sensors, effectors and sensor-effector communication. The NASA Smart Probe Project has focused on the sensor aspect. METHODS: The NASA Smart Probe uses neural networks and data from multiple microsensors for a unique tissue signature in real time. Animal and human trials use several probe configurations: (1) 8-microsensor probe (2.5 mm in diameter) for rodent studies (normal and subcutaneous mammary tumor tissues), and (2) 21-gauge needle probe with 3 spectroscopic fibers and an impedance microelectrode for breast cancer diagnosis in humans. Multisensor data are collected in real time (update 100 times/s) using PCs. RESULTS: Human data (collected by NASA licensee BioLuminate) from 15 women undergoing breast biopsy distinguished normal tissue from both benign tumors and breast carcinoma. Tumor margins and necrosis are rapidly detected. CONCLUSION: Real-time tissue identification is achievable. Potential applications, including probes incorporating nanoelectrode arrays, are presented. Copyright 2003 S. Karger AG, Basel.

  7. Measurement of Respiration and Internal Oxygen in Germinating Cicer arietinum L. Seeds Using Optic Microsensor.

    PubMed

    Pandey, Sonika; Kumari, Aprajita; Bharadwaj, Chellapilla; Gupta, Kapuganti Jagadis

    2017-01-01

    Internal oxygen concentrations vary in different tissues depending on tissue size, developmental stage, and their location. Respiratory rate of tissue also determines internal oxygen levels. For studying various signaling pathways it is essential to establish a correlation between respiration and internal oxygen. Seed germination is associated with increase in respiration which can dictate the internal oxygen and subsequent production of reactive oxygen species. Using optic oxygen microsensor we made an attempt to measure respiratory rate and internal oxygen. We found that microsensor is able to sense internal oxygen and it is also possible to measure oxygen levels in a close vial that contains seeds. Step-by-step protocol is described here along with illustration.

  8. The NASA Smart Probe Project for real-time multiple microsensor tissue recognition.

    PubMed

    Andrews, Russell J; Mah, Robert W

    2003-01-01

    Remote surgery requires automated sensors, effectors and sensor-effector communication. The NASA Smart Probe Project has focused on the sensor aspect. The NASA Smart Probe uses neural networks and data from multiple microsensors for a unique tissue signature in real time. Animal and human trials use several probe configurations: (1) 8-microsensor probe (2.5 mm in diameter) for rodent studies (normal and subcutaneous mammary tumor tissues), and (2) 21-gauge needle probe with 3 spectroscopic fibers and an impedance microelectrode for breast cancer diagnosis in humans. Multisensor data are collected in real time (update 100 times/s) using PCs. Human data (collected by NASA licensee BioLuminate) from 15 women undergoing breast biopsy distinguished normal tissue from both benign tumors and breast carcinoma. Tumor margins and necrosis are rapidly detected. Real-time tissue identification is achievable. Potential applications, including probes incorporating nanoelectrode arrays, are presented. Copyright 2003 S. Karger AG, Basel

  9. Integration of P-CuO Thin Sputtered Layers onto Microsensor Platforms for Gas Sensing.

    PubMed

    Presmanes, Lionel; Thimont, Yohann; El Younsi, Imane; Chapelle, Audrey; Blanc, Frédéric; Talhi, Chabane; Bonningue, Corine; Barnabé, Antoine; Menini, Philippe; Tailhades, Philippe

    2017-06-16

    P-type semiconducting copper oxide (CuO) thin films deposited by radio-frequency (RF) sputtering were integrated onto microsensors using classical photolithography technologies. The integration of the 50-nm-thick layer could be successfully carried out using the lift-off process. The microsensors were tested with variable thermal sequences under carbon monoxide (CO), ammonia (NH₃), acetaldehyde (C₂H₄O), and nitrogen dioxide (NO₂) which are among the main pollutant gases measured by metal-oxide (MOS) gas sensors for air quality control systems in automotive cabins. Because the microheaters were designed on a membrane, it was then possible to generate very rapid temperature variations (from room temperature to 550 °C in only 50 ms) and a rapid temperature cycling mode could be applied. This measurement mode allowed a significant improvement of the sensor response under 2 and 5 ppm of acetaldehyde.

  10. Carbon nanotubes on polymer-based pressure micro-sensor for manometric catheters

    NASA Astrophysics Data System (ADS)

    Teng, M. F.; Hariz, A.; Hsu, H. Y.; Omari, T.

    2008-12-01

    In this paper we investigate the fabrication process of a novel polymer based pressure micro-sensor for use in manometric measurements in medical diagnostics. Review and analysis of polymer materials properties and polymer based sensors has been carried out and has been reported by us elsewhere [1]. The interest in developing a novel polymer based flexible pressure micro-sensor was motivated by the numerous problems inherent in the currently available manometric catheters used in the hospitals. The most critical issue regarding existing catheters was the running and maintenance costs [2]. Thus expensive operation costs lead to reuse of the catheters, which increase the risk for disease transmission. The novel flexible polymer based pressure micro-sensor was build using SU-8, which is a special kind of negative photoresist. Single-walled carbon nanotubes (SWCNTs) and aluminum are used as the sensing material and contacting electrodes respectively. The pressure sensor diaphragm was first patterned on top of an oxidized silicon wafer using SU-8, followed by aluminum deposition to define the electrodes. The carbon nanotube is then deposited using dielectrophoresis (DEP) process. Once the carbon nanotubes are aligned in between these electrodes, the remaining of the sensor structure is formed using SU-8. Patterning of SU-8 and release from the substrate make the device ready for further testing of sensing ability. This research not only investigates the use of polymeric materials to build pressure sensors, but also explores the feasibility of full utilization of polymeric materials to replace conventional silicon materials in micro-sensors fabrication for use in medical environments. The completed sensor is expected to form an integral part of a large versatile sensing system. For example, the biocompatible artificial skin, is predicted to be capable of sensing force, pressure, temperature, and humidity, and may be used in such applications as medical and robotic system.

  11. Review of Specific Chemical Interactions for Hydrazine Analysis and Proposed Adaptation for Microsensor Chemical Detection

    DTIC Science & Technology

    1984-11-30

    basic hydrszine chemistry relevant to the analytical reactions presented in subsequent sections and to the coating requirements for chemical microsensors...Sections 2, 3, 4 and 5 discuss specific analytical hydrazine reactions which have been classified as alldehyde or ketone condensations, aromatfc...surface. It "is ideally designed to have a specific chemical receptivity to a "particular vapor whose interaction coincidentally produces a -I property

  12. Piezoelectric cellular micro-structured PDMS material for micro-sensors and energy harvesting

    NASA Astrophysics Data System (ADS)

    Kachroudi, A.; Basrour, S.; Rufer, L.; Jomni, F.

    2015-12-01

    This paper reports a novel low-cost fabrication process of a charged cellular microstructured polydimethylsiloxane (PDMS) material referred as piezo-electret or ferro-electret for micro-sensors applications. The dielectric spectra reached on these structures exhibit a high piezoelectric longitudinal coefficient d33 of 350pC/N. A mechanical characterization method proves the reliability of this material for low-frequencies applications around 100Hz.

  13. Electrochemistry of moexipril: experimental and computational approach and voltammetric determination.

    PubMed

    Taşdemir, Hüdai I; Kiliç, E

    2014-09-01

    The electrochemistry of moexipril (MOE) was studied by electrochemical methods with theoretical calculations performed at B3LYP/6-31 + G (d)//AM1. Cyclic voltammetric studies were carried out based on a reversible and adsorption-controlled reduction peak at -1.35 V on a hanging mercury drop electrode (HMDE). Concurrently irreversible diffusion-controlled oxidation peak at 1.15 V on glassy carbon electrode (GCE) was also employed. Potential values are according to Ag/AgCI, (3.0 M KCI) and measurements were performed in Britton-Robinson buffer of pH 5.5. Tentative electrode mechanisms were proposed according to experimental results and ab-initio calculations. Square-wave adsorptive stripping voltammetric methods have been developed and validated for quantification of MOE in pharmaceutical preparations. Linear working range was established as 0.03-1.35 microM for HMDE and 0.2-20.0 microM for GCE. Limit of quantification (LOQ) was calculated to be 0.032 and 0.47 microM for HMDE and GCE, respectively. Methods were successfully applied to assay the drug in tablets by calibration and standard addition methods with good recoveries between 97.1% and 106.2% having relative standard deviation less than 10%.

  14. Voltammetric detection of biological molecules using chopped carbon fiber.

    PubMed

    Sugawara, Kazuharu; Yugami, Asako; Kojima, Akira

    2010-01-01

    Voltammetric detection of biological molecules was carried out using chopped carbon fibers produced from carbon fiber reinforced plastics that are biocompatible and inexpensive. Because chopped carbon fibers normally are covered with a sizing agent, they are difficult to use as an electrode. However, when the surface of a chopped carbon fiber was treated with ethanol and hydrochloric acid, it became conductive. To evaluate the functioning of chopped carbon fibers, voltammetric measurements of [Fe(CN)(6)](3-) were carried out. Redoxes of FAD, ascorbic acid and NADH as biomolecules were recorded using cyclic voltammetry. The sizing agents used to bundle the fibers were epoxy, polyamide and polyurethane resins. The peak currents were the greatest when using the chopped carbon fibers that were created with epoxy resins. When the electrode response of the chopped carbon fibers was compared with that of a glassy carbon electrode, the peak currents and the reversibility of the electrode reaction were sufficient. Therefore, the chopped carbon fibers will be useful as disposable electrodes for the sensing of biomolecules.

  15. Integrated Inductors for RF Transmitters in CMOS/MEMS Smart Microsensor Systems

    PubMed Central

    Kim, Jong-Wan; Takao, Hidekuni; Sawada, Kazuaki; Ishida, Makoto

    2007-01-01

    This paper presents the integration of an inductor by complementary metal-oxide-semiconductor (CMOS) compatible processes for integrated smart microsensor systems that have been developed to monitor the motion and vital signs of humans in various environments. Integration of radio frequency transmitter (RF) technology with complementary metal-oxide-semiconductor/micro electro mechanical systems (CMOS/MEMS) microsensors is required to realize the wireless smart microsensors system. The essential RF components such as a voltage controlled RF-CMOS oscillator (VCO), spiral inductors for an LC resonator and an integrated antenna have been fabricated and evaluated experimentally. The fabricated RF transmitter and integrated antenna were packaged with subminiature series A (SMA) connectors, respectively. For the impedance (50 Ω) matching, a bonding wire type inductor was developed. In this paper, the design and fabrication of the bonding wire inductor for impedance matching is described. Integrated techniques for the RF transmitter by CMOS compatible processes have been successfully developed. After matching by inserting the bonding wire inductor between the on-chip integrated antenna and the VCO output, the measured emission power at distance of 5 m from RF transmitter was -37 dBm (0.2 μW).

  16. Performance Characteristics of a New Generation Pressure Microsensor for Physiologic Applications

    PubMed Central

    Cottler, Patrick S.; Karpen, Whitney R.; Morrow, Duane A.; Kaufman, Kenton R.

    2009-01-01

    A next generation fiber-optic microsensor based on the extrinsic Fabry–Perot interferometric (EFPI) technique has been developed for pressure measurements. The basic physics governing the operation of these sensors makes them relatively tolerant or immune to the effects of high-temperature, high-EMI, and highly-corrosive environments. This pressure microsensor represents a significant improvement in size and performance over previous generation sensors. To achieve the desired overall size and sensitivity, numerical modeling of diaphragm deflection was incorporated in the design, with the desired dimensions and calculated material properties. With an outer diameter of approximately 250 µm, a dynamic operating range of over 250 mmHg, and a sampling frequency of 960 Hz, this sensor is ideal for the minimally invasive measurement of physiologic pressures and incorporation in catheter-based instrumentation. Nine individual sensors were calibrated and characterized by comparing the output to a U.S. National Institute of Standards and Technology (NIST) Traceable reference pressure over the range of 0–250 mmHg. The microsensor performance demonstrated accuracy of better than 2% full-scale output, and repeatability, and hysteresis of better than 1% full-scale output. Additionally, fatigue effects on five additional sensors were 0.25% full-scale output after over 10,000 pressure cycles. PMID:19495983

  17. Performance characteristics of a new generation pressure microsensor for physiologic applications.

    PubMed

    Cottler, Patrick S; Karpen, Whitney R; Morrow, Duane A; Kaufman, Kenton R

    2009-08-01

    A next generation fiber-optic microsensor based on the extrinsic Fabry-Perot interferometric (EFPI) technique has been developed for pressure measurements. The basic physics governing the operation of these sensors makes them relatively tolerant or immune to the effects of high-temperature, high-EMI, and highly-corrosive environments. This pressure microsensor represents a significant improvement in size and performance over previous generation sensors. To achieve the desired overall size and sensitivity, numerical modeling of diaphragm deflection was incorporated in the design, with the desired dimensions and calculated material properties. With an outer diameter of approximately 250 microm, a dynamic operating range of over 250 mmHg, and a sampling frequency of 960 Hz, this sensor is ideal for the minimally invasive measurement of physiologic pressures and incorporation in catheter-based instrumentation. Nine individual sensors were calibrated and characterized by comparing the output to a U.S. National Institute of Standards and Technology (NIST) Traceable reference pressure over the range of 0-250 mmHg. The microsensor performance demonstrated accuracy of better than 2% full-scale output, and repeatability, and hysteresis of better than 1% full-scale output. Additionally, fatigue effects on five additional sensors were 0.25% full-scale output after over 10,000 pressure cycles.

  18. Identification of Cross-Country Skiing Movement Patterns Using Micro-Sensors

    PubMed Central

    Marsland, Finn; Lyons, Keith; Anson, Judith; Waddington, Gordon; Macintosh, Colin; Chapman, Dale

    2012-01-01

    This study investigated the potential of micro-sensors for use in the identification of the main movement patterns used in cross-country skiing. Data were collected from four elite international and four Australian athletes in Europe and in Australia using a MinimaxX™ unit containing accelerometer, gyroscope and GPS sensors. Athletes performed four skating techniques and three classical techniques on snow at moderate velocity. Data from a single micro-sensor unit positioned in the centre of the upper back was sufficient to visually identify cyclical movement patterns for each technique. The general patterns for each technique were identified clearly across all athletes while at the same time distinctive characteristics for individual athletes were observed. Differences in speed, snow condition and gradient of terrain were not controlled in this study and these factors could have an effect on the data patterns. Development of algorithms to process the micro-sensor data into kinematic measurements would provide coaches and scientists with a valuable performance analysis tool. Further research is needed to develop such algorithms and to determine whether the patterns are consistent across a range of different speeds, snow conditions and terrain, and for skiers of differing ability. PMID:22666075

  19. Utilizing Microsensor Technology to Quantify Match Demands in Collegiate Women's Volleyball.

    PubMed

    Vlantes, Travis G; Readdy, Tucker

    2017-08-26

    The purpose of this study was to quantify internal and external load demands of women's NCAA Division I collegiate volleyball competitions using microsensor technology and session rating of perceived exertion (S-RPE). Eleven collegiate volleyball players wore microsensor technology (Optimeye S5; Catapult Sports USA, Chicago, IL) during fifteen matches played throughout the 2016 season. Parameters examined include: Player load (PL), High impact load (HI PL), percentage of high impact load (% HI PL), Explosive efforts (EE) and jumps. S-RPE was collected twenty minutes post-match using a modified Borg scale. The relationship between internal and external load was explored, comparing S-RPE data with the microsensor metrics (PL, HI PL, % HI PL, EE, Jumps). The setter had the greatest mean PL and highest number of jumps of all positions in a 5-1 system, playing all six rotations. Playing four sets yielded a mean PL increase of 25.1% over three sets, while playing five sets showed a 31.0% increase in PL. A multivariate analysis of variance (MANOVA) revealed significant differences (p <.01) across all position groups when examining % HI PL and jumps. Cohen's d analysis revealed large (≥ 0.8) effect sizes for these differences. Defensive specialists recorded the greatest mean S-RPE values over all fifteen matches (886 ± 384.6). Establishing positional load demands allows coaches, trainers, and strength and conditioning professionals to implement training programs for position specific demands, creating consistent peak performance and reducing injury risk.

  20. Nitric oxide microsensor for high spatial resolution measurements in biofilms and sediments.

    PubMed

    Schreiber, Frank; Polerecky, Lubos; de Beer, Dirk

    2008-02-15

    Nitric oxide (NO) is a ubiquitous biomolecule that is known as a signaling compound in eukaryotes and prokaryotes. In addition, NO is involved in all conversions of the biogeochemical nitrogen cycle: denitrification, nitrification, and the anaerobic oxidation of ammonium (Anammox). Until now, NO has not been measured with high spatial resolution within microbial communities, such as biofilms, sediments, aggregates, or microbial mats, because the available sensors are not robust enough and their spatial resolution is insufficient. Here we describe the fabrication and application of a novel Clark-type NO microsensor with an internal reference electrode and a guard anode. The NO microsensor has a spatial resolution of 60-80 microm, a sensitivity of 2 pA microM-1, and a detection limit of approximately 30 nM. Hydrogen sulfide (H2S) was found to be a major interfering compound for the electrochemical detection of NO. The application of the novel NO microsensor to nitrifying biofilms and marine sediments revealed dynamic NO concentration profiles with peaks in the oxic parts of the samples. The local concentrations suggested that NO may be an important bioactive compound in natural environments. The consumption and production of NO occurs in separate regions of stratified microbial communities and indicates that it is linked to distinct biogeochemical cycles.

  1. Voltammetric detection of sequence-selective DNA hybridization related to Toxoplasma gondii in PCR amplicons.

    PubMed

    Gokce, Gultekin; Erdem, Arzum; Ceylan, Cagdas; Akgöz, Muslum

    2016-01-01

    This work describes the single-use electrochemical DNA biosensor technology developed for voltammetric detection of sequence selective DNA hybridization related to important human and veterinary pathogen; Toxoplasma gondii. In the principle of electrochemical label-free detection assay, the duplex of DNA hybrid formation was detected by measuring guanine oxidation signal occured in the presence of DNA hybridization. The biosensor design consisted of the immobilization of an inosine-modified (guanine-free) probe onto the surface of pencil graphite electrode (PGE), and the detection of the duplex formation in connection with the differential pulse voltammetry(DPV) by measuring the guanine signal. Toxoplasma gondii capture probe was firstly immobilized onto the surface of the activated PGE by wet adsorption. The extent of hybridization at PGE surface between the probe and the target was then determined by measuring the guanine signal observed at +1.0V. The electrochemical monitoring of optimum DNA hybridization has been performed in the target concentration of 40µg/mL in 50min of hybridization time. The specificity of the electrochemical biosensor was then tested using non-complementary, or mismatch short DNA sequences. Under the optimum conditions, the guanine oxidation signal indicating full hybridization was measured in various target concentration from 0.5 to 25µg/mL and a detection limit was found to be 1.78µg/mL. This single-use biosensor platform was successfully applied for the voltammetric detection of DNA hybridization related to Toxoplasma gondii in PCR amplicons.

  2. In General, the Total Voltammetric Current from a Mixture of Redox-Active Substances will Not be the Sum of the Currents that Each Substance would Produce Independently at the Same Concentration as in the Mixture

    NASA Technical Reports Server (NTRS)

    Leventis, Nicholas; Oh, Woon Su; Gao, Xue-Rong; Rawashdeh, Abdel Monem M.

    2003-01-01

    At the potential range where both decamethylferrocene (dMeFc) and ferrocene (Fc) are oxidized with rates controlled by linear diffusion, electrogenerated Fc(+) radicals diffusing outwards from the electrode react quantitatively (K23 C=5.8 x 10(exp 8) with dMeFc diffusing towards the electrode and produce Fc and dMeFc. That reaction replaces dMeFc with Fc, whose diffusion coefficient is higher than that of dMeFc(+), and the total mass-transfer limited current from the mixture is increased by approximately 10%. Analogous observations are made when mass-transfer is controlled by convective-diffusion as in RDE voltammetry. Similar results have been obtained with another, and for all practical purposes randomly selected pair of redox-active substances, [Co(bipy)3](2+) and N - methylphenothiazine (MePTZ); reaction of MePTZ(+) with [Co(bipy)3](2+) replaces the latter with MePTZ, which diffuses faster and the current increases by approximately 20%. The experimental voltammograms have been simulated numerically and the role of (a) the rate constant of the homogeneous reaction; (b) the relative concentrations; and, (c) the diffusion coefficients of all species involved have been studied in detail. Importantly, it was also identified that within any given redox system the dependence of the mass-transfer limited current on the bulk concentrations of the redox-active species is expected to be non-linear. These findings are discussed in terms of their electroanalytical implications.

  3. Continuous glucose monitoring microsensor with a nanoscale conducting matrix and redox mediator

    NASA Astrophysics Data System (ADS)

    Pesantez, Daniel

    The major limiting factor in kidney clinical transplantation is the shortage of transplantable organs. The current inability to distinguish viability from non-viability on a prospective basis represents a major obstacle in any attempt to expand organ donor criteria. Consequently, a way to measure and monitor a relevant analyte to assess kidney viability is needed. For the first time, the initial development and characterization of a metabolic microsensor to assess kidney viability is presented. The rate of glucose consumption appears to serve as an indicator of kidney metabolism that may distinguish reversible from irreversible kidney damage. The proposed MetaSense (Metabolic Sensor) microdevice would replace periodic laboratory diagnosis tests with a continuous monitor that provides real-time data on organ viability. Amperometry, a technique that correlates an electrical signal with analyte concentration, is used as a method to detect glucose concentrations. A novel two-electrode electrochemical sensing cell design is presented. It uses a modified metallic working electrode (WE) and a bare metallic reference electrode (RE) that acts as a pseudo-reference/counter electrode as well. The proposed microsensor has the potential to be used as a minimally invasive sensor for its reduced number of probes and very small dimensions achieved by micromachining and lithography. In order to improve selectivity of the microdevice, two electron transfer mechanisms or generations were explored. A first generation microsensor uses molecular oxygen as the electron acceptor in the enzymatic reaction and oxidizes hydrogen peroxide (H2O2) to get the electrical signal. The microsensor's modified WE with conductive polymer polypyrrole (PPy) and corresponding enzyme glucose oxidase (GOx) immobilized into its matrix, constitutes the electrochemical detection mechanism. Photoluminescence spectroscopic analysis confirmed and quantified enzyme immobilized concentrations within the matrix. In

  4. Multicomponent analysis of drinking water by a voltammetric electronic tongue.

    PubMed

    Winquist, Fredrik; Olsson, John; Eriksson, Mats

    2011-01-10

    A voltammetric electronic tongue is described that was used for multicomponent analysis of drinking water. Measurements were performed on drinking water from a tap and injections of the compounds NaCl, NaN(3), NaHSO(3), ascorbic acid, NaOCl and yeast suspensions could be identified by use of principal component analysis (PCA). A model based on partial least square (PLS) was developed for the simultaneously prediction of identification and concentration of the compounds NaCl, NaHSO(3) and NaOCl. By utilizing this type of non-selective sensor technique for water quality surveillance, it will be feasible to detect a plurality of events without the need of a specific sensor for each type of event.

  5. Voltammetric and spectroscopic investigations of 4-nitrophenylferrocene interacting with DNA

    NASA Astrophysics Data System (ADS)

    Shah, Afzal; Zaheer, Muhammad; Qureshi, Rumana; Akhter, Zareen; Faizan Nazar, Muhammad

    2010-03-01

    Cyclic voltammetry (CV) coupled with UV-vis and fluorescence spectroscopy were used to probe the interaction of potential anticancer drug, 4-nitrophenylferrocene (NFC) with DNA. The electrostatic interaction of the positively charged NFC with the anionic phosphate of DNA was evidenced by the findings like negative formal potential shift in CV, ionic strength effect, smaller bathochromic shift in UV-vis spectroscopy, incomplete quenching in the emission spectra and decrease in viscosity. The diffusion coefficients of the free and DNA bound forms of the drug were evaluated from Randles-Sevcik equation. The binding parameters like binding constant, ratio of binding constants ( Kred/ Kox), binding site size and binding free energy were determined from voltammetric data. The binding constant was also determined from UV-vis and fluorescence spectroscopy with a value quite close to that obtained from CV.

  6. Indirect voltammetric determination of trace hydroxylamine using magnetic microspheres.

    PubMed

    Yang, Ming; Zhu, Jun-Jie

    2003-02-01

    A new indirect voltammetric method for the determination of hydroxylamine is described. It is based on the reduction of an electroactive derivative of hydroxylamine on the surface of a magnetic electrode. The electroactive derivative produced by hydroxylamine reacted with magnetic polymer microspheres containing carbonyl groups on the surface. The experimental conditions are discussed. It was found that the peak potential (Ep) of the derivative was -0.46 V (vs. Ag/AgCl) under optimum conditions. Hydroxylamine could be determined in the range of 5-2,000 microg l(-1) with the detection limit of 2 microg l(-1) and relative standard deviation for the determination of 100 microg l(-1) hydroxylamine was 2.35%. Satisfactory results were obtained for the determination of hydroxylamine in aqueous medium.

  7. Recent Trends in Monitoring of European Water Framework Directive Priority Substances Using Micro-Sensors: A 2007–2009 Review

    PubMed Central

    Namour, Philippe; Lepot, Mathieu; Jaffrezic-Renault, Nicole

    2010-01-01

    This review discusses from a critical perspective the development of new sensors for the measurement of priority pollutants targeted in the E.U. Water Framework Directive. Significant advances are reported in the paper and their advantages and limitations are also discussed. Future perspectives in this area are also pointed out in the conclusions. This review covers publications appeared since December 2006 (the publication date of the Swift report). Among priority substances, sensors for monitoring the four WFD metals represent 81% of published papers. None of analyzed publications present a micro-sensor totally validated in laboratory, ready for tests under real conditions in the field. The researches are mainly focused on the sensing part of the micro-sensors. Nevertheless, the main factor limiting micro-sensor applications in the environment is the ruggedness of the receptor towards environmental conditions. This point constitutes the first technological obstacle to be overcome for any long-term field tests. PMID:22163635

  8. Electrochemical and Hydrodynamic Interferences on the Performances of an Oxygen Microsensor with Built-in Electrochemical Microactuator

    NASA Technical Reports Server (NTRS)

    Kim, Chang-Soo; Lee, Chae-Hyang

    2004-01-01

    A concept of novel electrochemical in situ self-calibration technique for an oxygen microsensor has been proposed to devise a convenient calibration method without an externally coupled apparatus. Systemic investigations on the influences of various electrochemical (pH) and hydrodynamic (solution stirring) conditions on the proposed microsensor performances are presented. The results suggest that: 1) The calibrating microenvironments can be manipulated with carefully engineered sensor designs and optimized generating signals; 2) The external oxygen permeable membrane is needed to minimize the electrochemical and hydrodynamic interferences.

  9. Microsensors based on GaN semiconductors covalently functionalized with luminescent Ru(II) complexes.

    PubMed

    López-Gejo, Juan; Arranz, Antonio; Navarro, Alvaro; Palacio, Carlos; Muñoz, Elías; Orellana, Guillermo

    2010-02-17

    Covalent tethering of a Ru(II) dye to gallium nitride surfaces has been accomplished as a key step in the development of innovative sensing devices in which the indicator support (semiconductor) plays the role of both support and excitation source. Luminescence emission decays and time-resolved emission spectra confirm the presence of the dye on the semiconductor surfaces, while X-ray photoelectron spectroscopy proves its covalent bonding. The O(2) sensitivity of the new device is comparable to those of other ruthenium-based sensor systems. This achievement paves the way to a new generation of integrable ultracompact microsensors that combine semiconductor emitter-probe assemblies.

  10. Amperometric microsensor for direct probing of ascorbic acid in human gastric juice.

    PubMed

    Hutton, Emily A; Pauliukaitė, Rasa; Hocevar, Samo B; Ogorevc, Božidar; Smyth, Malcolm R

    2010-09-30

    This article reports on a novel microsensor for amperometric measurement of ascorbic acid (AA) under acidic conditions (pH 2) based on a carbon fiber microelectrode (CFME) modified with nickel oxide and ruthenium hexacyanoferrate (NiO-RuHCF). This sensing layer was deposited electrochemically in a two-step procedure involving an initial galvanostatic NiO deposition followed by a potentiodynamic RuHCF deposition from solutions containing the precursor salts. Several important parameters were examined to characterize and optimize the NiO-RuHCF sensing layer with respect to its current response to AA by using cyclic voltammetry, and scanning electron microscopy-energy dispersive X-ray spectroscopy methods. With the NiO-RuHCF coated CFME, the AA oxidation potential under acidic conditions was shifted to a less positive value for about 0.2 V (E(p) of ca. 0.23 V vs. Ag/AgCl) as compared to a bare CFME, which greatly improves the electrochemical selectivity. Using the hydrodynamic amperometry mode, the current vs. AA concentration in 0.01 M HCl, at a selected operating potential of 0.30 V, was found to be linear over a wide range of 10-1610 μM (n=22, r=0.999) with a calculated limit of detection of 1.0 μM. The measurement repeatability was satisfactory with a relative standard deviation (r.s.d.) ranging from 4% to 5% (n=6), depending on the AA concentration, and with a sensor-to-sensor reproducibility (r.s.d.) of 6.9% at 100 μM AA. The long-term reproducibility, using the same microsensor for 112 consecutive measurements of 20 μM AA over 11 h of periodic probing sets over 4 days, was 16.1% r.s.d., thus showing very good stability at low AA levels and suitability for use over a prolonged period of time. Moreover, using the proposed microsensor, additionally coated with a protective cellulose acetate membrane, the calibration plot obtained in the extremely complex matrix of real undiluted gastric juice was linear from 10 to 520 μM (n=14, r=0.998). These results

  11. Voltammetric performance and application of a sensor for sodium ions constructed with layered birnessite-type manganese oxide.

    PubMed

    Martinez, Murilo T; Lima, Alex S; Bocchi, Nerilso; Teixeira, Marcos F S

    2009-12-15

    The preparation and electrochemical characterization of a carbon paste electrode modified with layered birnessite-type manganese oxide for use as a sodium sensor is described. The effects of powder synthesis process (sol-gel and redox precipitation) for birnessite on the electrochemical activity of the sensor was investigated by cyclic voltammetry. The carbon paste electrode modified with birnessite-type manganese oxide that was synthesized by the sol-gel method showed a best electrochemical for sodium ions. The detection is based on the measurement of anodic current generated by oxidation of Mn(III) to Mn(IV) at the surface of the electrode and consequently the sodium ions extraction into the birnessite structure. The best voltammetric response was obtained for an electrode composition of 15% (w/w) birnessite oxide in the paste, a TRIS buffer solution of pH 8.0 and a scan rate of 50 mV s(-1). A sensitive linear voltammetric response for sodium ions was obtained in the concentration range of 7.89x10(-5) to 3.49x10(-4) mol L(-1) with a slope of 37.5 microA L mmol(-1) and a detection limit (3sigma/slope) of 3.43x10(-5) mol L(-1) using cyclic voltammetry. Under the working conditions, the proposed method was successfully applied to determination of sodium ions in urine samples.

  12. Simultaneous voltammetric determination of ascorbic acid, dopamine and uric acid using polybromothymol blue film-modified glassy carbon electrode.

    PubMed

    Xu, Xiongwei; Lin, Qihuang; Liu, Ailin; Chen, Wei; Weng, Xiuhua; Wang, Changlian; Lin, Xinhua

    2010-06-01

    A sensitive and selective electrochemical method for simultaneous determination of ascorbic acid (AA), dopamine (DA), and uric acid (UA) using an electropolymerized bromothymol blue (BTB)-modified glassy carbon electrode (GCE) was developed. The electrochemically synthesized film was investigated using electrochemical impedance spectroscopy and voltammetric methods. The electrochemical behavior of the polymer-modified electrode depends on film thickness, i.e., the electropolymyerization time. The poly-BTB-modified GCE shows excellent electrocatalytic activity toward the oxidation of AA, DA, and UA in phosphate buffer solution (pH 5.0). The voltametric peak separations of AA/DA, DA/UA, and AA/UA on this modified electrode are 118 mV, 298 mV, and 455 mV, respectively. Therefore the voltammetric responses of these three compounds can be resolved well on the polymer-modified electrode, and simultaneous determination of these three compounds can be achieved. In addition, this modified electrode can be successfully applied to determine AA and DA in injection and UA in urine samples without interference.

  13. Novel Carbon Dioxide Microsensor Based on Tin Oxide Nanomaterial Doped With Copper Oxide

    NASA Technical Reports Server (NTRS)

    Xu, Jennifer C.; Hunter, Gary W.; Lukco, Dorothy; Liu, Chung-Chiun; Ward, Benjamin J.

    2008-01-01

    Carbon dioxide (CO2) is one of the major indicators of fire and therefore its measurement is very important for low-false-alarm fire detection and emissions monitoring. However, only a limited number of CO2 sensing materials exist due to the high chemical stability of CO2. In this work, a novel CO2 microsensor based on nanocrystalline tin oxide (SnO2) doped with copper oxide (CuO) has been successfully demonstrated. The CuO-SnO2 based CO2 microsensors are fabricated by means of microelectromechanical systems (MEMS) technology and sol-gel nanomaterial-synthesis processes. At a doping level of CuO: SnO2 = 1:8 (molar ratio), the resistance of the sensor has a linear response to CO2 concentrations for the range of 1 to 4 percent CO2 in air at 450 C. This approach has demonstrated the use of SnO2, typically used for the detection of reducing gases, in the detection of an oxidizing gas.

  14. In Situ Characterization of Oil-in-Water Emulsions Stabilized by Surfactant and Salt Using Microsensors.

    PubMed

    Church, Jared; Paynter, Danielle M; Lee, Woo Hyoung

    2017-09-26

    Chemically stabilized emulsions are difficult to break because of micelle stability. Many physical and chemical processes have been used for emulsion breaking/separation; however, most operational parameters are based on empirical data and bulk analysis. A multiscale understanding of emulsions is required before these processes can advance further. This study utilized needle-type microsensors and confocal laser scanning microscopy (CLSM) for characterizing simulated bilge water emulsions with different types of surfactants (Triton X-100 and sodium dodecyl sulfate [SDS]) under various NaCl concentrations at microscale. Using microsensors, a diffusion process was clearly visualized across the oil/water interface which appears to be related to emulsion formation kinetics and mass transfer. While emulsion stability decreased with NaCl concentrations, SDS (anionic surfactant) is more likely to form emulsion as salinity increases, requiring more salinity to coalesce SDS emulsions than Triton X-100 (nonionic surfactant) emulsions. Triton X-100 emulsions showed the potential to exhibit particle stabilized emulsions with NaCl concentration below 10(-2.5) M. The research demonstrated that the use of nonionic surfactant allows better oil-in-water separation than anionic surfactant. Significant pH changes of emulsions from unknown additives have implications when operating pH-sensitive emulsion breaking/separation processes (e.g., electrocoagulation).

  15. Hydrazine leak detection using poly (3-hexylthiophene) thin film micro-sensor

    NASA Astrophysics Data System (ADS)

    Yang, H.; Wan, J.; Shu, H.; Liu, X.; Lakshmanan, R. S.; Guntupalli, R.; Hu, J.; Howard, W.; Chin, B. A.

    2006-05-01

    Hydrazine is mostly used as a propellant in the control/propulsion system of missiles, spacecraft and satellites. However with its highly toxic and strong reducing nature, hydrazine is very dangerous to humans and the environment. In this research, a low cost, passive, and highly sensitive micro-sensor has been developed as an alarm device for real-time monitoring for the accidental release of hydrazine, and to insure the safety of personnel and the readiness of the system before lift-off. The micro-sensor is fabricated using standard microelectronic manufacturing techniques and is composed of interdigitated electrodes and a hydrazine-sensitive poly (3-hexylthiophene) (P3HT) thin film. When exposed to 1ppm of hydrazine gas, the compensation interaction between the reducing hydrazine gas and p-type doped P3HT leads to a five order magnitude increase in the resistance of the device. The sensor is capable of detecting hydrazine leaks from tens of ppb to tens of ppm concentration. The sensitivity of sensor increases with the increasing of hydrazine concentration and the decreasing of the polymer film thickness. A numerical simulation result based on the possible theoretical model is compared with the experimental data, which shows a good agreement.

  16. Improving the performance of glutamate microsensors by purification of ascorbate oxidase.

    PubMed

    Oldenziel, Weite H; de Jong, Lutea A A; Dijkstra, Gerrit; Cremers, Thomas I F H; Westerink, Ben H C

    2006-04-01

    Enzyme-based biosensors have the potential to directly detect extracellular concentrations of glutamate in brain tissue with a high spatial and temporal resolution. To optimize their analytical performance, much attention has been paid to the architectural construction of these biosensors. In particular, the coupling of enzymes to the electrode surface has received much interest, which has resulted in many (derivatives of) first-, second-, and third-generation type of biosensors. However, it is remarkable that in the literature little attention, if any, has been paid to the influence of the quality of the enzyme itself on the analytical performance of a biosensor. Previously we have reported that different batches of ascorbate oxidase significantly altered the performance of our glutamate microsensor.(1) In this note, it is shown that a simple enzyme purification procedure as buffer exchange leads to a more uniform enzyme quality and also significantly improves the reproducibility and performance of the microsensor. In our opinion, this is an important observation and of general interest for the construction of enzyme-based biosensors.

  17. Xanthine microsensor based on polypyrrole molecularly imprinted film modified carbon fiber microelectrodes.

    PubMed

    Liu, Bin; Wang, Xiao-Li; Lian, Hui-Ting; Sun, Xiang-Ying

    2013-09-15

    A molecularly imprinted polymers (MIPs) microsensor was presented as a carbon fiber microelectrode (CFME) coating for specifically recognizing xanthine (Xan). The polymeric film was obtained based on the imprinted procedure of electropolymerization of pyrrole in the presence of the template molecule Xan by cyclic voltammetry, and template was removed by magnetic stirring. Under the optimum conditions, a satisfactory molecularly binding selectivity of Xan was obtained from the MIPs microsensor with an imprinting factor (IF) of 6.63 and a linear response to concentration in certain ranges. The ranges are from 4.0 × 10⁻⁶ to 6.0 × 10⁻⁵ M and from 8.0 × 10⁻⁵ to 2.0 × 10⁻³ M with a detection limit of 2.5 × 10⁻⁷ M. Meanwhile, good stability (relative standard deviation [RSD] = 3.2%, n = 10) and reproducibility (RSD = 2.0%, n = 10) were observed, and recoveries ranging from 96.9 to 102.5% were calculated when applied to Xan determination in real blood serum samples.

  18. Differential pulse voltammetric assay of lercanidipine in tablets.

    PubMed

    Alvarez-Lueje, Alejandro; Pujol, Sara; Núñez-Vergara, Luis J; Squella, Juan A

    2002-01-01

    Lercanidipine in ethanol-0.04M Britton-Robinson buffer (20 + 80) gives an irreversible anodic response on a glassy carbon electrode in a broad pH range (2-12) that depends on pH. This signal can be attributed to oxidation of the 1,4-dihydropyridine ring to give the corresponding pyridine derivative. For analytical purposes, differential pulse voltammetry at pH 4 was selected. Under these conditions, good values of both within- and interday reproducibility were obtained, with coefficient of variation (CV) values of 1.56 and 1.70%, respectively, for 10 successive runs. For quantitation, the calibration curve method was used for lercanidipine concentrations ranging from 1 x 10(-5) to 1 x 10(-4) M. The detection and quantitation limits were 1.39 x 10(-5) and 1.49 x 10(-5), respectively. A liquid chromatographic method with electrochemical detection was used for comparison. The voltammetric method showed good selectivity with respect to both excipients and degradation products. The recovery study exhibited a CV of 0.94% and an average recovery of 98.3%, and it was not necessary to treat the sample before the analysis. The method was successfully applied to the individual tablet assay of lercanidipine in commercial tablets.

  19. Voltammetric Determination of Ni and Co in Water Samples

    NASA Astrophysics Data System (ADS)

    Herrera-Melian, Jose Alberto; Dona-Rodriguez, Jose Miguel; Hernandez-Brito, Joaquin; Perez Pena, Jesus

    1997-12-01

    Stripping voltammetry has attracted considerable attention for the determination of trace and ultratrace metals. This is mainly due to its high sensitivity and low cost of instrumentation. In adsorptive stripping voltammetry an organometallic complex is formed by the addition of a suitable ligand to the sample. The complex is adsorbed onto the Hg-drop by the application of the proper adsorption potential (more positive than E1/2) and solution stirring. After an adsorption period a cathodic (negative going) potential scan is applied and the metal concentration is calculated by the standard addition method. Nickel is found in natural waters at nM levels and is closely related with phosphates and silicates. Cobalt is a component of vitamin B12 and occurs in natural waters at concentration about 0.1 nM. We propose the voltammetric analysis of these elements by adsorptive stripping voltammetry as an introductory laboratory experiment for advanced chemistry or for chemical or environmental engineering students. The experiment has been proven to be very suitable for the laboratory part of the instrumental analysis course at the University of Las Palmas de Gran Canaria (Spain). In general, about 70% of the students have obtained good agreement (less than 10% of difference) between their results and the expected ones. Two hours is enough for the overall instrumental performance and the preparation of Ni and Co standards.

  20. Carbon nanotubes for voltammetric determination of sulphite in some beverages.

    PubMed

    Silva, Erika M; Takeuchi, Regina M; Santos, André L

    2015-04-15

    In this work, a square-wave voltammetric method based on sulphite electrochemical reduction was developed for quantification of this preservative in commercial beverages. A carbon-paste electrode chemically modified with multiwalled carbon nanotubes was used as the working electrode. Under the optimised experimental conditions, a linear response to sulphite concentrations from 1.6 to 32 mg SO2 L(-1) (25-500 μmol L(-1) of sulphite), with a limit of detection of 1.0 mg SO2 L(-1) (16 μmol L(-1) of sulphite), was obtained. This method does not suffer interference from other common beverage additives such as ascorbic acid, fructose, and sucrose, and it enables fast and reliable sulphite determination in beverages, with minimal sample pretreatment. Despite its selectivity, the method is not applicable to red grape juice or red wine samples, because some of their components produce a cathodic peak at almost the same potential as that of sulphite reduction.

  1. Needle-type environmental microsensors: design, construction and uses of microelectrodes and multi-analyte MEMS sensor arrays

    NASA Astrophysics Data System (ADS)

    Lee, Woo Hyoung; Lee, Jin-Hwan; Choi, Woo-Hyuck; Hosni, Ahmed A.; Papautsky, Ian; Bishop, Paul L.

    2011-04-01

    The development of environmental microsensor techniques is a revolutionary advance in the measurement of both absolute levels and changes in chemical species in the field of environmental engineered and natural systems. The tiny tip (5-15 µm diameter) of microsensors makes them very attractive experimental tools for direct measurements of the chemical species of interest inside biological samples (e.g., biofilm, flocs). Microelectrodes fabricated from pulled micropipettes (e.g., dissolved oxygen, oxidation-reduction potential, ion-selective microelectrode) have contributed to greater understanding of biological mechanisms for decades using microscopic monitoring, and currently microelectromechanical system (MEMS) microfabrication technologies are being successfully applied to fabricate multi-analyte sensor systems for in situ monitoring. This review focuses on needle-type environmental microsensor technology, including microelectrodes and multi-analyte MEMS sensor arrays. Design, construction and applications to biofilm research of these sensors are described. Practical methods for biofilm microprofile measurements are presented and several in situ applications for a biofilm study are highlighted. Ultimately, the developed needle-type microsensors combined with molecular biotechnology (such as microscopic observation with fluorescent probes) show the tremendous promise of micro-environmental sensor technology.

  2. Using micro-sensor data to quantify macro kinematics of classical cross-country skiing during on-snow training.

    PubMed

    Marsland, Finn; Mackintosh, Colin; Anson, Judith; Lyons, Keith; Waddington, Gordon; Chapman, Dale W

    2015-01-01

    Micro-sensors were used to quantify macro kinematics of classical cross-country skiing techniques and measure cycle rates and cycle lengths during on-snow training. Data were collected from seven national level participants skiing at two submaximal intensities while wearing a micro-sensor unit (MinimaxX™). Algorithms were developed identifying double poling (DP), diagonal striding (DS), kick-double poling (KDP), tucking (Tuck), and turning (Turn). Technique duration (T-time), cycle rates, and cycle counts were compared to video-derived data to assess system accuracy. There was good reliability between micro-sensor and video calculated cycle rates for DP, DS, and KDP, with small mean differences (Mdiff% = -0.2 ± 3.2, -1.5 ± 2.2 and -1.4 ± 6.2) and trivial to small effect sizes (ES = 0.20, 0.30 and 0.13). Very strong correlations were observed for DP, DS, and KDP for T-time (r = 0.87-0.99) and cycle count (r = 0.87-0.99), while mean values were under-reported by the micro-sensor. Incorrect Turn detection was a major factor in technique cycle misclassification. Data presented highlight the potential of automated ski technique classification in cross-country skiing research. With further refinement, this approach will allow many applied questions associated with pacing, fatigue, technique selection and power output during training and competition to be answered.

  3. Experimental study of PDMS mechanical properties for the optimization of polymer based flexible pressure micro-sensors

    NASA Astrophysics Data System (ADS)

    Dinh, T. H. N.; Martincic, E.; Dufour-Gergam, E.; Joubert, P.-Y.

    2016-10-01

    This paper reports on the optimization of flexible PDMS-based normal pressure capacitive micro-sensors dedicated to wearable applications. The deformation under a normal force of PDMS thin films of thicknesses ranging from 40 μm to 10 mm is firstly experimentally studied. This study points out that for capacitive micro-sensors using bulky PDMS thin films as deformable dielectric material, the sensitivity to an applied normal load can be optimized thanks to an adequate choice of the so-called form ratio of the involved PDMS thin film. Indeed, for capacitive micro-sensors exhibiting 9 mm2 electrodes, the capacitance change under a 6 N load can be adjusted from a few percent up to over 35% according to the choice of the load-free thickness of the used PDMS film. These results have been validated thanks to electromechanical characterizations carried out on two flexible PDMS based capacitive normal pressure micro-sensor samples fabricated with two different thicknesses. The obtained results open the way to the enhanced design of PDMS based pressure sensors dedicated to wearable and medical applications. Further works will extend this study to a wider range of sensor dimensions, and using numerical modelling.

  4. Effects of tianeptine, sertraline and clomipramine on brain serotonin metabolism: a voltammetric approach in the rat.

    PubMed

    Marinesco, S; Poncet, L; Debilly, G; Jouvet, M; Cespuglio, R

    1996-10-14

    Tianeptine is a substance enhancing the serotonir uptake while sertraline and clomipramine inhibit it. By means of 5-hydroxyin-doleacetic acid (5-HIAA) voltammetric measurements, this study investigated their influence on serotonin metabolism which depends mainly upon the activity of monoamine oxidase type A. After tianeptine injection the 5-HIAA signal increased by about 60%. This effect was maintained when the animals were pre-treated with MDL 72145 (an inhibitor of monoamine oxidase type B) but reduced when clorgyline (an inhibitor of monoamine oxidase type A) was administered after tianeptine. Administration of sertraline or clomipramine reduced the 5-HIAA signal by about 30-50%, whether the animals were pre-treated with MDL 72145 or not. It is to be concluded that tianeptine, sertraline and clomipramine can regulate the 5-HT fraction present in the synaptic cleft, not only by acting at the level of the serotoninergic neurons, but also by favoring or reducing the access of the amine to monoamine oxidase type A which is synthesized within non-serotoninergic neurons and glial cells.

  5. Development simple and sensitive voltammetric procedure for ultra-trace determination of U(VI).

    PubMed

    Tyszczuk-Rotko, Katarzyna; Domańska, Katarzyna; Czech, Bożena; Rotko, Marek

    2017-04-01

    A simple and sensitive adsorptive stripping voltammetric procedure for the determination of trace concentration of U(VI) in natural water samples was developed. In order to remove surface active compounds from water sample solutions, a TiO2/Al2O3 photocatalysis system was applied. The linear calibration graph of U(VI) in the simultaneous presence of 2mgL(-1) anionic, cationic and nonionic surfactants, in the range from 5×10(-10) to 2×10(-8)molL(-1) (180s) was achieved. The detection limit obtained in the solution after the use of UV-irradiation (10min) with TiO2/Al2O3 photocatalyst (0.9g) is equal to 2.3×10(-10)mol L(-1). The presented procedure was successfully applied to uranium determination in SLEW-3 certified reference material, and to river water samples. In addition, a very low detection limit (2.9×10(-11)molL(-1)) for accumulation time of 180s was achieved due to application of a reversible deposited mediator (Zn) in the step of lead film electrode preparation. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Mesoporous carbon-containing voltammetric biosensor for determination of tyramine in food products.

    PubMed

    Kochana, Jolanta; Wapiennik, Karolina; Knihnicki, Paweł; Pollap, Aleksandra; Janus, Paula; Oszajca, Marcin; Kuśtrowski, Piotr

    2016-07-01

    A voltammetric biosensor based on tyrosinase (TYR) was developed for determination of tyramine. Carbon material (multi-walled carbon nanotubes or mesoporous carbon CMK-3-type), polycationic polymer-i.e., poly(diallyldimethylammonium chloride) (PDDA), and Nafion were incorporated into titania dioxide sol (TiO2) to create an immobilization matrix. The features of the formed matrix were studied by scanning electron microscopy (SEM) and cyclic voltammetry (CV). The analytical performance of the developed biosensor was evaluated with respect to linear range, sensitivity, limit of detection, long-term stability, repeatability, and reproducibility. The biosensor exhibited electrocatalytic activity toward tyramine oxidation within a linear range from 6 to 130 μM, high sensitivity of 486 μA mM(-1) cm(-2), and limit of detection of 1.5 μM. The apparent Michaelis-Menten constant was calculated to be 66.0 μM indicating a high biological affinity of the developed biosensor for tyramine. Furthermore, its usefulness in determination of tyramine in food product samples was also verified. Graphical abstract Different food samples were analyzed to determine tyramine using biosensor based on tyrosinase.

  7. Maize tassel-modified carbon paste electrode for voltammetric determination of Cu(II).

    PubMed

    Moyo, Mambo; Okonkwo, Jonathan O; Agyei, Nana M

    2014-08-01

    The preparation and application of a practical electrochemical sensor for environmental monitoring and assessment of heavy metal ions in samples is a subject of considerable interest. In this paper, a carbon paste electrode modified with maize tassel for the determination of Cu(II) has been proposed. Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were used to study morphology and identify the functional groups on the modified electrode, respectively. First, Cu(II) was adsorbed on the carbon paste electrode surface at open circuit and voltammetric techniques were used to investigate the electrochemical performances of the sensor. The electrochemical sensor showed an excellent electrocatalytic activity towards Cu(II) at pH 5.0 and by increasing the amount of maize tassel biomass, a maximum response at 1:2.5 (maize tassel:carbon paste; w/w) was obtained. The electrocatalytic redox current of Cu(II) showed a linear response in the range (1.23 μM to 0.4 mM) with the correlation coefficient of 0.9980. The limit of detection and current-concentration sensitivity were calculated to be 0.13 (±0.01) μM and 0.012 (±0.001) μA/μM, respectively. The sensor gave good recovery of Cu(II) in the range from 96.0 to 98.0 % when applied to water samples.

  8. Study of poly (3-hexylthiophene) conducting polymer thin film micro-sensor for hydrazine vapor detection

    NASA Astrophysics Data System (ADS)

    Yang, Hong

    This dissertation discussed the construction and investigation of a poly (3-hexylthiophene) conducting polymer based thin film micro-sensor for a real-time detection of hydrazine vapor at ambient pressure. A type of low cost, small size, passive poly (3-hexylthiophene) thin film micro-sensor was designed and fabricated. The micro-sensor platform consisted of a rectangular shaped inert substrate and gold interdigited electrode pairs. A layer of poly (3-hexylthiophene) thin film was coated onto the sensor platform using a spin coating method, and nitrosonium hexafluorophosphate (NOPF6) was used to dope the poly (3-hexylthiophene) thin film to increase its electrical conductivity and form the finished sensor. The basic responses of the sensor to hydrazine vapor were experimentally investigated. The primary results showed that the sensor responded to hydrazine vapor in less than a few seconds; attained orders of magnitude change in normalized resistance during hydrazine exposure, and was not easily saturated. The interaction between the hydrazine gas molecules and doped poly (3-hexylthiophene) thin film was studied. The plausible mechanism was determined as: Charge carriers inside the doped poly (3-hexylthiophene) thin film were depleted during the oxidation-reduction chemical reaction between the hydrazine vapor and polymer film, resulting a reduction in the polymer film's electrical conductivity. Experiments were also conducted to find out the effects of hydrazine concentration, poly (3-hexylthiophene) thin film thickness, sensor storage time, environment temperature, and environment humidity on the sensor's performance. The response rate of the sensor under different sensing conditions was calculated and discussed. A diffusion-reaction model was applied to simulate the interaction between hydrazine molecules and doped poly (3-hexylthiophene) thin film. The profiles of hydrazine gas diffusion and positive charge carrier neutralization in the polymer film were

  9. Design considerations in the use of interdigitated microsensor electrode arrays (IMEs) for impedimetric characterization of biomimetic hydrogels.

    PubMed

    Yang, Liju; Guiseppi-Wilson, Adilah; Guiseppi-Elie, Anthony

    2011-04-01

    Microlithographically fabricated interdigitated microsensor electrodes (IMEs) were cleaned, surface activated, chemically functionalized (amine) and derivatized with an Acrloyl-PEG-NHS to receive a spun-applied monomer cocktail of UV polymerizable monomer. IMEs were 2050.5, 1550.5, 1050.5 and 0550.5 possessing lines and spaces that were 20, 15, 10, and 5 μm respectively; 5 mm line lengths and were 50 lines on each opposing bus. Bioactive hydrogels were synthesized from spun-applied and UV-crosslinked tetraethyleneglycol diacrylate (TEGDA) (crosslinker), 2-hydroxyethylmethacrylate (HEMA), polyethyleneglycol(200) monomethacrylate (PEGMA), N-[tris(hydroxymethyl)methyl]-acrylamide (HMMA) and poly(HEMA) (MW 60,000) (viscosity modifier) and 2,2-dimethoxy-2-phenylacetophenone (DMPA) (photoinitiator) to produce a 5 μm thick p(HEMA-co-PEGMA-co-HMMA) hydrogel membrane on the IMEs. Unmodified and hydrogel coated IMEs where characterized by AC electrical impedance spectroscopy using 50 mV p-t-p over the frequency range from 10 Hz to 100 kHz in aqueous PBS 7.4 buffer and in buffer containing 50 mM [Fe(CN)(6)](3-/4- ) solution at RT. Impedimetric responses were found to scale with the device geometric parameters. Equivalent circuit modeling revealed deviations from ideality at lower device dimensions suggesting an implication of the substrate surface charge on the double layer capacitance of the electrodes. Diffusion coefficients derived from the Warburg component are in accord with literature values.

  10. Voltammetric studies of sparfloxacin and application to its determination in pharmaceuticals.

    PubMed

    Girish Kumar, K; Augustine, P; Poduval, R; John, S

    2006-04-01

    A detailed study of the electrochemistry of sparfloxacin at a glassy carbon electrode was carried out in the pH range 2.0-10.0 in aqueous solution using cyclic and differential pulse voltammetry. Influence of different supporting electrolytes, pH, scan rate and concentrations were studied on the voltammetric response. The studies revealed the irreversible oxidation of sparfloxacin at basic pH in a diffusion controlled manner. In addition, a differential pulse voltammetric method was proposed for the determination of the drug in different pharmaceutical formulations.

  11. A Zinc Oxide Nanorod Ammonia Microsensor Integrated with a Readout Circuit on-a-Chip

    PubMed Central

    Yang, Ming-Zhi; Dai, Ching-Liang; Wu, Chyan-Chyi

    2011-01-01

    A zinc oxide nanorod ammonia microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.35 μm complementary metal oxide semiconductor (CMOS) process was investigated. The structure of the ammonia sensor is composed of a sensitive film and polysilicon electrodes. The ammonia sensor requires a post-process to etch the sacrificial layer, and to coat the sensitive film on the polysilicon electrodes. The sensitive film that is prepared by a hydrothermal method is made of zinc oxide. The sensor resistance changes when the sensitive film adsorbs or desorbs ammonia gas. The readout circuit is used to convert the sensor resistance into the voltage output. Experiments show that the ammonia sensor has a sensitivity of about 1.5 mV/ppm at room temperature. PMID:22247656

  12. A zinc oxide nanorod ammonia microsensor integrated with a readout circuit on-a-chip.

    PubMed

    Yang, Ming-Zhi; Dai, Ching-Liang; Wu, Chyan-Chyi

    2011-01-01

    A zinc oxide nanorod ammonia microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.35 μm complementary metal oxide semiconductor (CMOS) process was investigated. The structure of the ammonia sensor is composed of a sensitive film and polysilicon electrodes. The ammonia sensor requires a post-process to etch the sacrificial layer, and to coat the sensitive film on the polysilicon electrodes. The sensitive film that is prepared by a hydrothermal method is made of zinc oxide. The sensor resistance changes when the sensitive film adsorbs or desorbs ammonia gas. The readout circuit is used to convert the sensor resistance into the voltage output. Experiments show that the ammonia sensor has a sensitivity of about 1.5 mV/ppm at room temperature.

  13. Variable-pitch dispensing workstation and its application to the preparation of microsensor arrays.

    PubMed

    Aoki, Hiroshi; Ikeda, Takashi; Torimura, Masaki; Tao, Hiroaki

    2008-06-01

    We have developed an 8-ch capillary-based dispensing workstation with a variable capillary pitch mechanism. The capillary intervals can be varied from 1 to 9 mm to dispense different solutions simultaneously at an arbitrary dispensing pitch, allowing direct dispensing from microplates to integrated analytical systems. To evaluate the precision of its dispensing performance, droplets of Rhodamine G dye were dispensed onto glass slides and the values of the optical volume were analyzed. The error in the dispensed volume proved to be 0.54 nL when dispensing 20 nL. In dispensing small volumes, the volume error for this workstation was found to be about 100-fold less than that seen in conventional dispensers. Even highly viscous solutions containing 50% glycerol could be dispensed with precision. Rapid dispensing was also achieved. Moreover, the application of the workstation to preparing addressable 8 x 12 microsensor array chips was demonstrated, providing an independent and reproducible spot array.

  14. Titanium Dioxide Nanoparticle Humidity Microsensors Integrated with Circuitry on-a-Chip

    PubMed Central

    Hu, Yu-Chih; Dai, Ching-Liang; Hsu, Cheng-Chih

    2014-01-01

    A humidity microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.18 μm CMOS (complementary metal oxide semiconductor) process was presented. The integrated sensor chip consists of a humidity sensor and a readout circuit. The humidity sensor is composed of a sensitive film and interdigitated electrodes. The sensitive film is titanium dioxide prepared by the sol-gel method. The titanium dioxide is coated on the interdigitated electrodes. The humidity sensor requires a post-process to remove the sacrificial layer and to coat the titanium dioxide. The resistance of the sensor changes as the sensitive film absorbs or desorbs vapor. The readout circuit is employed to convert the resistance variation of the sensor into the output voltage. The experimental results show that the integrated humidity sensor has a sensitivity of 4.5 mV/RH% (relative humidity) at room temperature. PMID:24594612

  15. Ethanol Microsensors with a Readout Circuit Manufactured Using the CMOS-MEMS Technique

    PubMed Central

    Yang, Ming-Zhi; Dai, Ching-Liang

    2015-01-01

    The design and fabrication of an ethanol microsensor integrated with a readout circuit on-a-chip using the complementary metal oxide semiconductor (CMOS)-microelectro-mechanical system (MEMS) technique are investigated. The ethanol sensor is made up of a heater, a sensitive film and interdigitated electrodes. The sensitive film is tin dioxide that is prepared by the sol-gel method. The heater is located under the interdigitated electrodes, and the sensitive film is coated on the interdigitated electrodes. The sensitive film needs a working temperature of 220 °C. The heater is employed to provide the working temperature of sensitive film. The sensor generates a change in capacitance when the sensitive film senses ethanol gas. A readout circuit is used to convert the capacitance variation of the sensor into the output frequency. Experiments show that the sensitivity of the ethanol sensor is 0.9 MHz/ppm. PMID:25594598

  16. A multiplexing fiber optic microsensor system for monitoring oxygen concentration in plants

    NASA Astrophysics Data System (ADS)

    Chaturvedi, P.; Hauser, B. A.; Allen, L. H.; Boote, K. J.; Karplus, E.; McLamore, E. S.

    2013-05-01

    The accurate and rapid measurement of physiological O2 transport is vital for understanding spatially and temporally dynamic metabolism and stress signalling in plant cells and tissues. Single channel luminescent O2- quenched optrodes have been available for use in laboratory and field experiments since the early 2000's. However, to collect the large datasets needed to understand O2 transport in complex systems, many experiments require a multiple channel O2 sensor system. This research reports the development of a multiplexing fiber optic O2 microsensor system designed to conduct high temporal resolution experiments for field studies of plant physiology. The 10 channel system was demonstrated for measuring O2 concentration in developing soybean seeds (Glycine max L. Merr.) within a climate controlled greenhouse.

  17. Integrated luminescent chemical microsensors based on GaN LEDs for security applications using smartphones

    NASA Astrophysics Data System (ADS)

    Orellana, Guillermo; Muñoz, Elias; Gil-Herrera, Luz K.; Muñoz, Pablo; Lopez-Gejo, Juan; Palacio, Carlos

    2012-09-01

    Development of PCB-integrateable microsensors for monitoring chemical species is a goal in areas such as lab-on-a-chip analytical devices, diagnostics medicine and electronics for hand-held instruments where the device size is a major issue. Cellular phones have pervaded the world inhabitants and their usefulness has dramatically increased with the introduction of smartphones due to a combination of amazing processing power in a confined space, geolocalization and manifold telecommunication features. Therefore, a number of physical and chemical sensors that add value to the terminal for health monitoring, personal safety (at home, at work) and, eventually, national security have started to be developed, capitalizing also on the huge number of circulating cell phones. The chemical sensor-enabled "super" smartphone provides a unique (bio)sensing platform for monitoring airborne or waterborne hazardous chemicals or microorganisms for both single user and crowdsourcing security applications. Some of the latest ones are illustrated by a few examples. Moreover, we have recently achieved for the first time (covalent) functionalization of p- and n-GaN semiconductor surfaces with tuneable luminescent indicator dyes of the Ru-polypyridyl family, as a key step in the development of innovative microsensors for smartphone applications. Chemical "sensoring" of GaN-based blue LED chips with those indicators has also been achieved by plasma treatment of their surface, and the micrometer-sized devices have been tested to monitor O2 in the gas phase to show their full functionality. Novel strategies to enhance the sensor sensitivity such as changing the length and nature of the siloxane buffer layer are discussed in this paper.

  18. Quantifying the physical demands of collision sports: does microsensor technology measure what it claims to measure?

    PubMed

    Gabbett, Tim J

    2013-08-01

    The physical demands of rugby league, rugby union, and American football are significantly increased through the large number of collisions players are required to perform during match play. Because of the labor-intensive nature of coding collisions from video recordings, manufacturers of wearable microsensor (e.g., global positioning system [GPS]) units have refined the technology to automatically detect collisions, with several sport scientists attempting to use these microsensors to quantify the physical demands of collision sports. However, a question remains over the validity of these microtechnology units to quantify the contact demands of collision sports. Indeed, recent evidence has shown significant differences in the number of "impacts" recorded by microtechnology units (GPSports) and the actual number of collisions coded from video. However, a separate study investigated the validity of a different microtechnology unit (minimaxX; Catapult Sports) that included GPS and triaxial accelerometers, and also a gyroscope and magnetometer, to quantify collisions. Collisions detected by the minimaxX unit were compared with video-based coding of the actual events. No significant differences were detected in the number of mild, moderate, and heavy collisions detected via the minimaxX units and those coded from video recordings of the actual event. Furthermore, a strong correlation (r = 0.96, p < 0.01) was observed between collisions recorded via the minimaxX units and those coded from video recordings of the event. These findings demonstrate that only one commercially available and wearable microtechnology unit (minimaxX) can be considered capable of offering a valid method of quantifying the contact loads that typically occur in collision sports. Until such validation research is completed, sport scientists should be circumspect of the ability of other units to perform similar functions.

  19. Assessment of subsurface VOCs using a chemical microsensor array. Final report

    SciTech Connect

    Batterman, S.A.; Zellers, E.T.

    1993-06-01

    This report describes the results of laboratory investigations of several performance parameters relevant to surface-acoustic-wave (SAW) chemical sensor arrays for the measurement of volatile organic compounds (VOCs) in contaminated soil and groundwater. The small size, low cost, sensitivity and selectivity of such instruments promise improvements in the quality and quantity of data used to guide site assessment and restoration efforts. In this investigation, calibrations were performed for 15 different coated SAW sensors. Each sensor was exposed to six VOCs selected to represent three chemical classes of contaminants that are commonly found at waste sites (i.e., aliphatic, aromatic and chlorinated hydrocarbons). A new pattern recognition method was developed for determining which coated sensors would maximize the selectivity and accuracy of quantitation for a given set of vapor contaminants. Using this method, an optimal subwet of four coated sensors was selected for testing in a prototype microsensor instrument. Additional laboratory experiments were performed with this optimized array to assess the limits of detection and linear response ranges for the representative vapors, as well as the additivity of responses to vapors in binary mixtures, temperature and humidity effects, aging effects, and other performance parameters related to the application of this technology to soil and groundwater VOC monitoring. Results demonstrate that SAW microsensor arrays can identify and quantify specific VOCs at concentrations in the {mu}g/L to mg/L range when present alone or in simple (e.g., binary) mixtures. SAW sensor technology offers a potentially effective alternative to existing field instrumentation for headspace analysis, soil vapor monitoring, and vacuum extraction process monitoring of VOCs in subsurface media.

  20. Chemical microsensors

    SciTech Connect

    Li, DeQuan; Swanson, Basil I.

    1995-01-01

    An article of manufacture is provided including a substrate having an oxide surface layer and a selective thin film of a cyclodextrin derivative chemically bound upon said substrate, said film is adapted for the inclusion of a selected organic compound therewith. Such an article can be either a chemical sensor capable of detecting a resultant mass change from inclusion of the selected organic compound or a chemical separator capable of reversibly selectively separating a selected organic compound.

  1. Spectrometric and Voltammetric Analysis of Urease – Nickel Nanoelectrode as an Electrochemical Sensor

    PubMed Central

    Hubalek, Jaromir; Hradecky, Jan; Adam, Vojtech; Krystofova, Olga; Huska, Dalibor; Masarik, Michal; Trnkova, Libuse; Horna, Ales; Klosova, Katerina; Adamek, Martin; Zehnalek, Josef; Kizek, Rene

    2007-01-01

    Urease is the enzyme catalyzing the hydrolysis of urea into carbon dioxide and ammonia. This enzyme is substrate-specific, which means that the enzyme catalyzes the hydrolysis of urea only. This feature is a basic diagnostic criterion used in the determination of many bacteria species. Most of the methods utilized for detection of urease are based on analysis of its enzyme activity – the hydrolysis of urea. The aim of this work was to detect urease indirectly by spectrometric method and directly by voltammetric methods. As spectrometric method we used is called indophenol assay. The sensitivity of detection itself is not sufficient to analyse the samples without pre-concentration steps. Therefore we utilized adsorptive transfer stripping technique coupled with differential pulse voltammetry to detect urease. The influence of accumulation time, pH of supporting electrolyte and concentration of urease on the enzyme peak height was investigated. Under the optimized experimental conditions (0.2 M acetate buffer pH 4.6 and accumulation time of 120 s) the detection limit of urease evaluated as 3 S/N was 200 ng/ml. The activity of urease enzyme depends on the presence of nickel. Thus the influence of nickel(II) ions on electrochemical response of the enzyme was studied. Based on the results obtained the interaction of nickel(II) ions and urease can be determined using electrochemical methods. Therefore we prepared Ni nanoelectrodes to measure urease. The Ni nanoelectrodes was analysed after the template dissolution by scanning electron microscopy. The results shown vertically aligned Ni nanopillars almost covered the electrode surface, whereas the defect places are minor and insignificant in comparison with total electrode surface. We were able to not only detect urease itself but also to distinguish its native and denatured form.

  2. Development of a rapid and simple voltammetric method to determine total antioxidative capacity of edible oils.

    PubMed

    Gulaboski, Rubin; Mirčeski, Valentin; Mitrev, Saša

    2013-05-01

    In this work we report on a new, rapid and simple voltammetric method to determine the total antioxidant capacity (TAC) of the edible oils. The method explores the ABTS radical (2,2'-azinobis(3-ethylbenzothiazoline-6-sulphonic acid)) assay as a redox probe and it relays on measuring catalytic voltammetric currents. The electrocatalysis comprises redox regeneration of the electrochemically created ABTS(+) radical either by Trolox (6-hydroxy-2,5,7,8-tetramethychroman-2-carboxylic acid) or by antioxidants present in studied oils. The detection limit of the method is determined to be 0.5 mg/L of Trolox equivalent, being a slightly lower than the corresponding UV-VIS spectrophotometric method. Applying the proposed voltammetric method the total antioxidant capacity of three types of commercially available cold-pressed edible oils are determined, and the results are found to be in a very good agreement with those obtained by UV-VIS spectrophotometry. The reported voltammetric method is cheap, rapid and simple, and it can be used as a sustainable alternative to the UV-VIS methods for the determination of total antioxidant capacitance of oils and other liquid lipophilic nutrients. Potent antioxidant capacity of studied oils was also confirmed by electron paramagnetic resonance spectroscopy of superoxide anion produced by macrophages.

  3. Discrimination of Rice with Different Pretreatment Methods by Using a Voltammetric Electronic Tongue

    PubMed Central

    Wang, Li; Niu, Qunfeng; Hui, Yanbo; Jin, Huali

    2015-01-01

    In this study, an application of a voltammetric electronic tongue for discrimination and prediction of different varieties of rice was investigated. Different pretreatment methods were selected, which were subsequently used for the discrimination of different varieties of rice and prediction of unknown rice samples. To this aim, a voltammetric array of sensors based on metallic electrodes was used as the sensing part. The different samples were analyzed by cyclic voltammetry with two sample-pretreatment methods. Discriminant Factorial Analysis was used to visualize the different categories of rice samples; however, radial basis function (RBF) artificial neural network with leave-one-out cross-validation method was employed for prediction modeling. The collected signal data were first compressed employing fast Fourier transform (FFT) and then significant features were extracted from the voltammetric signals. The experimental results indicated that the sample solutions obtained by the non-crushed pretreatment method could efficiently meet the effect of discrimination and recognition. The satisfactory prediction results of voltammetric electronic tongue based on RBF artificial neural network were obtained with less than five-fold dilution of the sample solution. The main objective of this study was to develop primary research on the application of an electronic tongue system for the discrimination and prediction of solid foods and provide an objective assessment tool for the food industry. PMID:26205274

  4. An Acetone Microsensor with a Ring Oscillator Circuit Fabricated Using the Commercial 0.18 μm CMOS Process

    PubMed Central

    Yang, Ming-Zhi; Dai, Ching-Liang; Shih, Po-Jen

    2014-01-01

    This study investigates the fabrication and characterization of an acetone microsensor with a ring oscillator circuit using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The acetone microsensor contains a sensitive material, interdigitated electrodes and a polysilicon heater. The sensitive material is α-Fe2O3 synthesized by the hydrothermal method. The sensor requires a post-process to remove the sacrificial oxide layer between the interdigitated electrodes and to coat the α-Fe2O3 on the electrodes. When the sensitive material adsorbs acetone vapor, the sensor produces a change in capacitance. The ring oscillator circuit converts the capacitance of the sensor into the oscillation frequency output. The experimental results show that the output frequency of the acetone sensor changes from 128 to 100 MHz as the acetone concentration increases 1 to 70 ppm. PMID:25036331

  5. Correlation of Chemisorption and Electronic Effects for Metal Oxide Interfaces: Transducing Principles for Temperature Programmed Gas Microsensors (Final Report)

    SciTech Connect

    S. Semancik; R. E. Cavicchi; D. L. DeVoe; T. J. McAvoy |

    2001-12-21

    This Final Report describes efforts and results for a 3-year DoE/OST-EMSP project centered at NIST. The multidisciplinary project investigated scientific and technical concepts critical for developing tunable, MEMS-based, gas and vapor microsensors that could be applied for monitoring the types of multiple analytes (and differing backgrounds) encountered at DoE waste sites. Micromachined ''microhotplate'' arrays were used as platforms for fabricating conductometric sensor prototypes, and as microscale research tools. Efficient microarray techniques were developed for locally depositing and then performance evaluating thin oxide films, in order to correlate gas sensing characteristics with properties including composition, microstructure, thickness and surface modification. This approach produced temperature-dependent databases on the sensitivities of sensing materials to varied analytes (in air) which enable application-specific tuning of microsensor arrays. Mechanistic studies on adsorb ate transient phenomena were conducted to better understand the ways in which rapid temperature programming schedules can be used to produce unique response signatures and increase information density in microsensor signals. Chemometric and neural network analyses were also employed in our studies for recognition and quantification of target analytes.

  6. Microsensors based on a whispering gallery mode in AlGaN microdisks undercut by hydrogen-environment thermal etching.

    PubMed

    Kouno, Tetsuya; Sakai, Masaru; Takeshima, Hoshi; Suzuki, Sho; Kikuchi, Akihiko; Kishino, Katsumi; Hara, Kazuhiko

    2017-04-20

    AlGaN microdisks were fabricated via a top-down process using electron-beam lithography, inductively coupled plasma reactive-ion etching, and hydrogen-environment thermal etching from commercial epitaxial wafers with a 100-300 nm thick AlGaN layer grown on a c-plane GaN layer by metal-organic chemical vapor deposition. The hydrogen-environment thermal etching performed well in undercutting the AlGaN microdisks owing to the selective etching for the GaN layer. The AlGaN microdisks acted as the whispering gallery mode (WGM) optical microresonators, exhibiting sharp resonant peaks in room temperature photoluminescence spectra. The evanescent component of the whispering gallery mode (WGM) is influenced by the ambient condition of the microdisk, resulting in the shift of the resonant peaks. The phenomenon is considered to be used for microsensors. Using the WGM in the AlGaN microdisks, we demonstrated microsensors and a microsensor system, which can potentially be used to evaluate biological and chemical actions in a microscale area in real time.

  7. Voltammetric detection of As(III) with Porphyridium cruentum based modified carbon paste electrode biosensor.

    PubMed

    Zaib, M; Saeed, A; Hussain, I; Athar, M M; Iqbal, M

    2014-12-15

    A novel biosensor based on carbon paste electrode modified with Porphyridium cruentum biomass was developed for the determination of As(III) in contaminated water. As(III) was first biosorbed-accumulated on the electrode surface at open circuit potential and then stripped off by applying anodic scan range of -0.8 to +0.8 V using differential pulse anodic stripping voltammetric technique. The best result was obtained at pH 6.0 with 0.1M HNO3 solution as stripping medium, allowing biosorption-accumulation time of 8 min using 5% P. cruentum biomass in graphite-mineral oil paste. Linear range for As(III) detection with the modified electrode-biosensor was observed between 2.5 and 20 µg L(-1). The FTIR spectrum of P. cruentum biomass confirmed the presence of active functional groups that participate in the binding of As(III). Scanning Electron Microscopy (SEM) indulged the surface morphology of modified electrode-biosensor before and after As(III) adsorption. Similarly, Atomic Force Microscopy (AFM) showed that the average roughness of the modified electrode decreased indicating the successful incorporation of P. cruentum biomass. Efficiency of the biosensor in the presence of different interfering metal (Na(+), K(+), Ca(2+), and Mg(2+)) ions were also evaluated. The application of P. cruentum modified biosensor was successfully used for the detection of As(III) in the binary metal (Fe(3+), Mn(2+), Cd(2+), Cu(2+), Ni(2+), Hg(2+), and Pb(2+)) contaminated system. The accuracy of application of biosorption based biosensor for the detection of As(III) is as low as 2.5 µg L(-1).

  8. Structural and electrochemical properties of lutetium bis-octachloro-phthalocyaninate nanostructured films. Application as voltammetric sensors.

    PubMed

    Alessio, P; Apetrei, C; Rubira, R J G; Constantino, C J L; Medina-Plazal, C; De Saja, J A; Rodríguez-Méndez, M L

    2014-09-01

    Thin films of the bis[2,3,9,10,16,17,23,24-octachlorophthalocyaninate] lutetium(III) complex (LuPc2Cl32) have been prepared by the Langmuir-Blodgett and the Langmuir-Schaefer (LS) techniques. The influence of the chlorine substituents in the structure of the films and in their spectroscopic, electrochemical and sensing properties has been evaluated. The π-A isotherms exhibit a monolayer stability greater than the observed in the unsubstituted analogue (LuPc2), being easily transferred to solid substrates, also in contrast to LuPc2. The LB and LS films present a linear growth forming stratified layers, monitored by UV-VIS absorption spectroscopy. The latter also revealed the presence of LuPc2Cl32 in the form of monomers and aggregates in both films. The FTIR data showed that the LuPc2Cl32 molecules present a non-preferential arrangement in both films. Monolayers of LB and LS were deposited onto 6 nm Ag island films to record surface-enhanced resonance Raman scattering (SERRS), leading to enhancement factors close to 2 x 10(3). Finally, LB and LS films deposited onto ITO glass have been successfully used as voltammetric sensors for the detection of catechol. The improved electroactivity of the LB and LS films has been confirmed by the reduction of the overpotential of the oxidation of catechol. The enhancement of the electrocatalytic effect observed in LB and LS films is the result of the nanostructured arrangement of the surface which increases the number of active sites. The sensors show a limit of detection in the range of 10(-5) mol/L.

  9. Potential application of microsensor technology in radioactive waste management with emphasis on headspace gas detection.

    SciTech Connect

    Davis, Chad Edward; Thomas, Michael Loren; Wright, Jerome L.; Pohl, Phillip Isabio; Hughes, Robert Clark; Wang, Yifeng; McGrath, Lucas K.; Ho, Clifford Kuofei; Gao, Huizhen

    2004-09-01

    Waste characterization is probably the most costly part of radioactive waste management. An important part of this characterization is the measurements of headspace gas in waste containers in order to demonstrate the compliance with Resource Conservation and Recovery Act (RCRA) or transportation requirements. The traditional chemical analysis methods, which include all steps of gas sampling, sample shipment and laboratory analysis, are expensive and time-consuming as well as increasing worker's exposure to hazardous environments. Therefore, an alternative technique that can provide quick, in-situ, and real-time detections of headspace gas compositions is highly desirable. This report summarizes the results obtained from a Laboratory Directed Research & Development (LDRD) project entitled 'Potential Application of Microsensor Technology in Radioactive Waste Management with Emphasis on Headspace Gas Detection'. The objective of this project is to bridge the technical gap between the current status of microsensor development and the intended applications of these sensors in nuclear waste management. The major results are summarized below: {sm_bullet} A literature review was conducted on the regulatory requirements for headspace gas sampling/analysis in waste characterization and monitoring. The most relevant gaseous species and the related physiochemical environments were identified. It was found that preconcentrators might be needed in order for chemiresistor sensors to meet desired detection {sm_bullet} A long-term stability test was conducted for a polymer-based chemresistor sensor array. Significant drifts were observed over the time duration of one month. Such drifts should be taken into account for long-term in-situ monitoring. {sm_bullet} Several techniques were explored to improve the performance of sensor polymers. It has been demonstrated that freeze deposition of black carbon (CB)-polymer composite can effectively eliminate the so-called 'coffee ring

  10. Polymer Electrolyte-Based Ambient Temperature Oxygen Microsensors for Environmental Monitoring

    NASA Technical Reports Server (NTRS)

    Hunter, Gary W.; Xu, Jennifer C.; Liu, Chung-Chiun

    2011-01-01

    An ambient temperature oxygen microsensor, based on a Nafion polymer electrolyte, has been developed and was microfabricated using thin-film technologies. A challenge in the operation of Nafion-based sensor systems is that the conductivity of Nafion film depends on the humidity in the film. Nafion film loses conductivity when the moisture content in the film is too low, which can affect sensor operation. The advancement here is the identification of a method to retain the operation of the Nafion films in lower humidity environments. Certain salts can hold water molecules in the Nafion film structure at room temperature. By mixing salts with the Nafion solution, water molecules can be homogeneously distributed in the Nafion film increasing the film s hydration to prevent Nafion film from being dried out in low-humidity environment. The presence of organics provides extra sites in the Nafion film to promote proton (H+) mobility and thus improving Nafion film conductivity and sensor performance. The fabrication of ambient temperature oxygen microsensors includes depositing basic electrodes using noble metals, and metal oxides layer on one of the electrode as a reference electrode. The use of noble metals for electrodes is due to their strong catalytic properties for oxygen reduction. A conducting polymer Nafion, doped with water-retaining components and extra sites facilitating proton movement, was used as the electrolyte material, making the design adequate for low humidity environment applications. The Nafion solution was coated on the electrodes and air-dried. The sensor operates at room temperature in potentiometric mode, which measures voltage differences between working and reference electrodes in different gases. Repeat able responses to 21-percent oxygen in nitrogen were achieved using nitrogen as a baseline gas. Detection of oxygen from 7 to 21 percent has also been demonstrated. The room-temperature oxygen micro sensor developed has extremely low power

  11. Metrological characteristics of the flat voltammetric electrode in time domain with a reversible electrochemical reaction running on the surface

    NASA Astrophysics Data System (ADS)

    Suchocki, Krzysztof

    2016-11-01

    The study deals with metrological characteristics of the flat voltammetric electrode used for determination of ions concentration by the DC voltammetric method, where a reversible reaction of electrochemical oxidation/reduction takes place on the surface. The analysis shows that such voltammetric electrode acts as a transducer of the first order, where the input signal is a concentration of marked ions in tested solution and the output signal is the current associated with a reversible reaction of oxidation / reduction. Metrological characteristics of such electrode in the time domain are determined by its sensitivity and time constant. The values of these parameters are defined by measurements of characteristics of the voltammetric electrode, polarization voltage and marked ions. To determine the effect of a particular volume of each of these parameters several numerical simulations are presented.

  12. Surface Crystallographic Dependence of Voltammetric Oxidation of Polyhydric Alcohols and Related Systems at Monocrystalline Gold-Acidic Aqueous Interfaces

    DTIC Science & Technology

    1992-02-01

    reverse if necessary and identify by block number) FIELD GROUP SUB-GROUP voltammetric oxidation, ethylene glycol, glycerol, meso- I I " ’ erythritol , d...by block rlumber)ne voltammetric o’zation in aqzueOus 0.Mb HClO 4 of four polyhydric alcohols, ethylene lycol, glycerol, meso- erythritol , and d...alcohols, ethylene glycol, glycerol, meso- erythritol , and d-mannitol, on seven oriented gold surfaces, Au(lll), (100), (110), (221), (533), (311), and (210

  13. Design and implementation of a wireless passive microsensor for methanol detection

    NASA Astrophysics Data System (ADS)

    Sanz, Diego; Rosas, Walter; Unigarro, Edgar; Vargas, Watson; Segura-Quijano, Fredy

    2013-03-01

    Methanol is a public health concern due to its toxicity, characterized by metabolic acidosis and blindness, among others. The third world population affected by the exposure to this compound is increasing, mainly due to the consumption of illicit distilled or adulterated alcoholic beverages. Although methanol is naturally present in some alcoholic drinks, the maximum allowed concentration cannot exceed 10 g of methanol per liter of anhydrous alcohol (0.4% (v/v) at 40% of ethanol) according to the general EU limit. A wireless passive microsensor was designed to detect small amounts of methanol at 40% of alcoholic dissolutions. The sensor consists of a planar inductor in series with an interdigital capacitor that changes its capacitance with the solution's dielectric constant. An antenna is used to readout the real part of the impedance to obtain the resonant frequencies for different amounts of methanol in the solution. The aim of this work was to develop a low cost wireless sensor with the capability to detect concentrations of at least 0.4% (v/v) of methanol in a 40% of alcoholic solution. The results obtained show variations of 403 kHz in the resonant frequency for changes of 0.2% (v/v) on the concentration of methanol in a 40% alcoholic ethanol-based solution. This project was possible thanks to the collaboration of the Department of Electrical and Electronics Engineering and the Department of Chemical Engineering of Universidad de los Andes.

  14. Portable Electronic Tongue Based on Microsensors for the Analysis of Cava Wines

    PubMed Central

    Giménez-Gómez, Pablo; Escudé-Pujol, Roger; Capdevila, Fina; Puig-Pujol, Anna; Jiménez-Jorquera, Cecilia; Gutiérrez-Capitán, Manuel

    2016-01-01

    Cava is a quality sparkling wine produced in Spain. As a product with a designation of origin, Cava wine has to meet certain quality requirements throughout its production process; therefore, the analysis of several parameters is of great interest. In this work, a portable electronic tongue for the analysis of Cava wine is described. The system is comprised of compact and low-power-consumption electronic equipment and an array of microsensors formed by six ion-selective field effect transistors sensitive to pH, Na+, K+, Ca2+, Cl−, and CO32−, one conductivity sensor, one redox potential sensor, and two amperometric gold microelectrodes. This system, combined with chemometric tools, has been applied to the analysis of 78 Cava wine samples. Results demonstrate that the electronic tongue is able to classify the samples according to the aging time, with a percentage of correct prediction between 80% and 96%, by using linear discriminant analysis, as well as to quantify the total acidity, pH, volumetric alcoholic degree, potassium, conductivity, glycerol, and methanol parameters, with mean relative errors between 2.3% and 6.0%, by using partial least squares regressions. PMID:27801796

  15. Microfluidic channel-based wireless charging and communication platform for microsensors with miniaturized onboard antenna

    NASA Astrophysics Data System (ADS)

    Duan, G.; Zhao, X.; Seren, H. R.; Chen, C.; Li, A.; Zhang, X.

    2016-12-01

    A double layer spiral antenna with side length of 380 μm was fabricated by a multi-step electroplating process, and integrated with a commercialized passive RFID chip to realize the RF power harvesting and communication functions of a microsensor. To power up and communicate with the microchips, a single layer spiral reader antenna was fabricated on top of a glass substrate with side length of 1 mm. The microchips and the reader antenna were both optimized at the frequency of 915 MHz. Due to the small size of the reader antenna, the strength of the magnetic field decreased dramatically along the axial direction of the reader antenna, which limited the working distance to within 1 mm. To enclose the microchips within the reading range, a three-layer microfluidic channel was designed and fabricated. The channel and cover layers were fabricated by laser cutting of acrylic sheets, and bonded with the glass substrate to form the channel. To operate multiple microchips simultaneously, separation and focusing function units were also designed. Low loss pump oil was used to transport the microchips flowing inside the channel. Within the reading area, the microchips were powered up, and their ID information was retrieved and displayed on the computer interface successfully.

  16. Sensitive thermal microsensor with pn junction for heat measurement of a single cell

    NASA Astrophysics Data System (ADS)

    Yamada, Taito; Inomata, Naoki; Ono, Takahito

    2016-02-01

    A sensitive thermal microsensor based on a pn junction diode for heat measurements of biological single cells is developed and evaluated. Using a fabricated device, we demonstrated the heat measurement of a single brown fat cell. The principle of the sensor relies on the temperature dependence of the pn junction diode resistance. This method has a capability of the highly thermal sensitivity by downsizing and the advantage of a simple experimental setup using electrical circuits without any special equipment. To achieve highly sensitive heat measurement of single cells, downsizing of the sensor is necessary to reduce the heat capacity of the sensor itself. The sensor with the pn junction diode can be downsized by microfabrication. A bridge beam structure with the pn junction diode as a thermal sensor is placed in vacuum using a microfludic chip to decrease the heat loss to the surroundings. A temperature coefficient of resistance of 1.4%/K was achieved. The temperature and thermal resolutions of the fabricated device are 1.1 mK and 73.6 nW, respectively. The heat measurements of norepinephrine stimulated and nonstimulated single brown fat cells were demonstrated, and different behaviors in heat generation were observed.

  17. Development of Wireless Subsurface Microsensors for Health Monitoring of Thermal Protection Systems

    NASA Technical Reports Server (NTRS)

    Pallix, Joan; Milos, Frank; Arnold, James O. (Technical Monitor)

    2000-01-01

    Low cost access to space is a primary goal for both NASA and the U.S. aerospace industry. Integrated subsystem health diagnostics is an area where major improvements have been identified for potential implementation into the design of new reusable launch vehicles (RLVS) in order to reduce life cycle costs, increase safety margins and improve mission reliability. A number of efforts are underway to use existing and emerging technologies to establish new methods for vehicle health monitoring on operational vehicles as well as X-vehicles. This paper summarizes a joint effort between several NASA centers and industry partners to develop rapid wireless diagnostic tools for failure management and long-term TPS performance monitoring of thermal protection systems (TPS) on future RLVS. An embedded wireless microsensor suite is being designed to allow rapid subsurface TPS health monitoring and damage assessment. This sensor suite will consist of both passive overlimit sensors and sensors for continuous parameter monitoring in flight. The on-board diagnostic system can be used to radio in maintenance requirements before landing and the data could also be used to assist in design validation for X-vehicles. For a 3rd generation vehicle, wireless diagnostics should be at a stage of technical development that will allow use for intelligent feedback systems for guidance and navigation control applications and can also serve as feedback for TPS that can intelligently adapt to its environment.

  18. Fiber optic microsensor hydrogen leak detection system on Delta IV launch vehicle

    NASA Astrophysics Data System (ADS)

    Kazemi, Alex A.; Goepp, John W.; Larson, David B.; Wuestling, Mark E.

    2008-04-01

    This paper describes the successful development and test of a multipoint fiber optic hydrogen microsensors system during the static firing of an Evolved Expandable Launch Vehicle (EELV)/Delta's common booster core (CBC) rocket engine at NASA's Stennis Space Center. The hydrogen sensitive chemistry is fully reversible and has demonstrated a response to hydrogen gas in the range of 0% to 10% with a resolution of 0.1% and a response time of <=5 seconds measured at a gas flow rate of 1 cc/min. The system consisted of a reversible chemical interaction causing a change in reflective of a thin film of coated Palladium. The sensor using a passive element consisting of chemically reactive microcoatings deposited on the surface of a glass microlens, which is then bonded to an optical fiber. The system uses a multiplexing technique with a fiber optic driver-receiver consisting of a modulated LED source that is launched into the sensor, and photodiode detector that synchronously measures the reflected signal. The system incorporates a microprocessor to perform the data analysis and storage, as well as trending and set alarm function. The paper illustrates the sensor design and performance data under field deployment conditions.

  19. Development and characterization of an NMR microsensor for nanoliter sample volumes

    NASA Astrophysics Data System (ADS)

    Dechow, Joern; Forchel, Alfred W. B.; Lanz, Titus; Haase, Axel

    1999-11-01

    The fabrication and performance of a micro-sensor for NMR- spectroscopy of nanoliter-sample volumes is presented. On both glass and GaAs-substrate. Planar coils with inner diameter from 50 micrometers to 400 micrometers including a coplanar wave-guide leading to the bonding pads were fabricated. A chamber for the liquid samples of 200 - 500 micrometers diameter was etched isotropically on the backside of the substrate, located under the coil. In initial experiments, the spectrum of a 20 - 50 nl-volumes of pure silicon-oil is analyzed in a 1H-NMR experiment in a 11T spectrometer (500 MHz). The microcoil serves as a receiver, while the RF-power was transmitted by a macroscopic coil perpendicular to the receiver coil. We observe characteristic lines from the silicon-oil spectrum which clearly indicates the high sensitivity of the microcoil. Additional signal from different materials in the experiment are suppressed by gradient fields and an adequate design of the sensor.

  20. Gold nanospikes based microsensor as a highly accurate mercury emission monitoring system

    PubMed Central

    Sabri, Ylias M.; Ippolito, Samuel J.; Tardio, James; Bansal, Vipul; O'Mullane, Anthony P.; Bhargava, Suresh K.

    2014-01-01

    Anthropogenic elemental mercury (Hg0) emission is a serious worldwide environmental problem due to the extreme toxicity of the heavy metal to humans, plants and wildlife. Development of an accurate and cheap microsensor based online monitoring system which can be integrated as part of Hg0 removal and control processes in industry is still a major challenge. Here, we demonstrate that forming Au nanospike structures directly onto the electrodes of a quartz crystal microbalance (QCM) using a novel electrochemical route results in a self-regenerating, highly robust, stable, sensitive and selective Hg0 vapor sensor. The data from a 127 day continuous test performed in the presence of volatile organic compounds and high humidity levels, showed that the sensor with an electrodeposted sensitive layer had 260% higher response magnitude, 3.4 times lower detection limit (~22 μg/m3 or ~2.46 ppbv) and higher accuracy (98% Vs 35%) over a Au control based QCM (unmodified) when exposed to a Hg0 vapor concentration of 10.55 mg/m3 at 101°C. Statistical analysis of the long term data showed that the nano-engineered Hg0 sorption sites on the developed Au nanospikes sensitive layer play a critical role in the enhanced sensitivity and selectivity of the developed sensor towards Hg0 vapor. PMID:25338965

  1. Denitrification and photosynthesis in stream sediment studied with microsensor and whole-core techniques

    SciTech Connect

    Nielsen, L.P.; Christensen, P.B.; Revsbech, N.P.; Soerensen, J. )

    1990-07-01

    The effect of light on benthic photosynthesis, denitrification, and assimilation of NH{sub 4}{sup +} and NO{sub 3}{sup {minus}} in stream sediments was studied with whole-core techniques and with O{sub 2} and N{sub 2}O microsensors. Photosynthetic oxygen production increased the thickness of the aerobic surface layer from 1.5 mm in the dark to {approximately} 3.5 mm at a light intensity saturating photosynthesis. The O{sub 2} flux change concurrently from net uptake to net release and the overall rate of denitrification was reduced by 70%. Denitrification was always restricted to a narrow zone immediately below the aerobic-anaerobic interface. Calculated NO{sub 3}{sup {minus}} microprofiles showed that overall denitrification was primarily dependent on the thickness of the aerobic layer which acted as a barrier for diffusion of NO{sub 3}{sup {minus}} from the overlying water. In the light, algal NO{sub 3}{sup {minus}} assimilation could exceed NO{sub 3}{sup {minus}} consumption by denitrification when availability of NH{sub 4}{sup +} was low. Assimilation of NO{sub 3}{sup {minus}}, however, had no influence on the flux of NO{sub 3}{sup {minus}} to the denitrification zone, since assimilation occurred relatively close to the sediment surface.

  2. A flexible polymer tube lab-chip integrated with microsensors for smart microcatheter.

    PubMed

    Li, Chunyan; Wu, Pei-Ming; Han, Jungyoup; Ahn, Chong H

    2008-10-01

    A flexible polymer tube lab-chip integrated with physical and biochemical sensor modules mounted on a flexible spiral structure for measuring physiological (temperature/flow rate) and metabolic data (glucose concentration) in a catheter application was designed, fabricated and characterized in this work. This new approach not only provides a unique way to assemble multiple sensors on both the inside and outside the flexible polymer tube using standard microfabrication methods while avoiding wiring and assembling problems associated with previous methods, but also maintains catheter inherent lumen potency for in situ drug delivery or insertion of medical tools. Three well-known sensors: temperature sensor (RTD), flow rate sensor (hot film anemometry) and glucose biosensor (amperometric sensor) have been successfully fabricated and fully integrated outside the spirally rolled polymer tube (ID = 500 microm, OD = 650 microm) of this demonstration device. The fabricated sensors showed good performances not only in a planar configuration but also in a spirally rolled configuration. This flexible micro tube lab-chip system provides a generic platform for developing patient-specific "smart" microcatheters that incorporate microsensors, microactuators, microfluidic devices and wireless signal communication modules that are tailored for the patients' unique condition.

  3. Torsional bridge setup for the characterization of integrated circuits and microsensors under mechanical shear stress.

    PubMed

    Herrmann, M; Gieschke, P; Ruther, P; Paul, O

    2011-12-01

    We present a torsional bridge setup for the electro-mechanical characterization of devices integrated in the surface of silicon beams under mechanical in-plane shear stress. It is based on the application of a torsional moment to the longitudinal axis of the silicon beams, which results in a homogeneous in-plane shear stress in the beam surface. The safely applicable shear stresses span the range of ±50 MPa. Thanks to a specially designed clamping mechanism, the unintended normal stress typically stays below 2.5% of the applied shear stress. An analytical model is presented to compute the induced shear stress. Numerical computations verify the analytical results and show that the homogeneity of the shear stress is very high on the beam surface in the region of interest. Measurements with piezoresistive microsensors fabricated using a complementary metal-oxide-semiconductor process show an excellent agreement with both the computational results and comparative measurements performed on a four-point bending bridge. The electrical connection to the silicon beam is performed with standard bond wires. This ensures that minimal forces are applied to the beam by the electrical interconnection to the external instrumentation and that devices with arbitrary bond pad layout can be inserted into the setup.

  4. High temperature gradient micro-sensor for wall shear stress and flow direction measurements

    NASA Astrophysics Data System (ADS)

    Ghouila-Houri, C.; Claudel, J.; Gerbedoen, J.-C.; Gallas, Q.; Garnier, E.; Merlen, A.; Viard, R.; Talbi, A.; Pernod, P.

    2016-12-01

    We present an efficient and high-sensitive thermal micro-sensor for near wall flow parameters measurements. By combining substrate-free wire structure and mechanical support using silicon oxide micro-bridges, the sensor achieves a high temperature gradient, with wires reaching 1 mm long for only 3 μm wide over a 20 μm deep cavity. Elaborated to reach a compromise solution between conventional hot-films and hot-wire sensors, the sensor presents a high sensitivity to the wall shear stress and to the flow direction. The sensor can be mounted flush to the wall for research studies such as turbulence and near wall shear flow analysis, and for technical applications, such as flow control and separation detection. The fabrication process is CMOS-compatible and allows on-chip integration. The present letter describes the sensor elaboration, design, and micro-fabrication, then the electrical and thermal characterizations, and finally the calibration experiments in a turbulent boundary layer wind tunnel.

  5. Microsensor Measurements of Sulfate Reduction and Sulfide Oxidation in Compact Microbial Communities of Aerobic Biofilms

    PubMed Central

    Kühl, Michael; Jørgensen, Bo Barker

    1992-01-01

    The microzonation of O2 respiration, H2S oxidation, and SO42- reduction in aerobic trickling-filter biofilms was studied by measuring concentration profiles at high spatial resolution (25 to 100 μm) with microsensors for O2, S2-, and pH. Specific reaction rates were calculated from measured concentration profiles by using a simple one-dimensional diffusion reaction model. The importance of electron acceptor and electron donor availability for the microzonation of respiratory processes and their reaction rates was investigated. Oxygen respiration was found in the upper 0.2 to 0.4 mm of the biofilm, whereas sulfate reduction occurred in deeper, anoxic parts of the biofilm. Sulfate reduction accounted for up to 50% of the total mineralization of organic carbon in the biofilms. All H2S produced from sulfate reduction was reoxidized by O2 in a narrow reaction zone, and no H2S escaped to the overlying water. Turnover times of H2S and O2 in the reaction zone were only a few seconds owing to rapid bacterial H2S oxidation. Anaerobic H2S oxidation with NO3- could be induced by addition of nitrate to the medium. Total sulfate reduction rates increased when the availability of SO42- or organic substrate increased as a result of deepening of the sulfate reduction zone or an increase in the sulfate reduction intensity, respectively. PMID:16348687

  6. Tackle and impact detection in elite Australian football using wearable microsensor technology.

    PubMed

    Gastin, Paul B; McLean, Owen C; Breed, Ray V P; Spittle, Michael

    2014-01-01

    The effectiveness of a wearable microsensor device (MinimaxX(TM) S4, Catapult Innovations, Melbourne, VIC, Australia) to automatically detect tackles and impact events in elite Australian football (AF) was assessed during four matches. Video observation was used as the criterion measure. A total of 352 tackles were observed, with 78% correctly detected as tackles by the manufacturer's software. Tackles against (i.e. tackled by an opponent) were more accurately detected than tackles made (90% v 66%). Of the 77 tackles that were not detected at all, the majority (74%) were categorised as low-intensity. In contrast, a total of 1510 "tackle" events were detected, with only 18% of these verified as tackles. A further 57% were from contested ball situations involving player contact. The remaining 25% were in general play where no contact was evident; these were significantly lower in peak Player Load™ than those involving player contact (P < 0.01). The tackle detection algorithm, developed primarily for rugby, was not suitable for tackle detection in AF. The underlying sensor data may have the potential to detect a range of events within contact sports such as AF, yet to do so is a complex task and requires sophisticated sport and event-specific algorithms.

  7. Novel magnetic and chemical microsensors for in-situ, real-time, and unattended use

    NASA Astrophysics Data System (ADS)

    Datskou, Irene; Rajic, Slobodan; Datskos, Panos G.

    1999-07-01

    There exists a need to develop novel, advanced, unattended magnetic and chemical micro-sensor systems for successful detection, localization, classification and tracking of ground time critical targets of interest. Consistent with the underlying long-term objectives of the development of unattended ground sensors program we have investigated the use of a new planted ground sensor platform based on Micro- Electro-Mechanical Systems that can offer magnetic, chemical and possibly acoustic detection. The envisioned micro-system will be low-power and low-cost and will be built around a single type of microstructure element integration a monolithic optical system and electronics package. This micro sensor can also incorporate burst telemetry to transmit the information, a renewable power source and will be capable of operating under field conditions, with sufficient sensitivity to permit high detection rates, and with sufficient chemical selectivity to prevent high false alarm rates. Preliminary studies, initial designs, and key predicted performance parameters will be presented. Possible applications of such as system include sensitive perimeter monitoring such as minefields and military/nuclear bases, vehicle detection, and aircraft navigation systems, and drug enforcement operations. The results of the present work demonstrate that the microcalorimetric spectroscopy technique can be applied to detect and identify chemicals in the ppm level and the studied microcantilever-based magnetometer can provide sensitivities in the order of 1(mu) T.

  8. Torsional bridge setup for the characterization of integrated circuits and microsensors under mechanical shear stress

    NASA Astrophysics Data System (ADS)

    Herrmann, M.; Gieschke, P.; Ruther, P.; Paul, O.

    2011-12-01

    We present a torsional bridge setup for the electro-mechanical characterization of devices integrated in the surface of silicon beams under mechanical in-plane shear stress. It is based on the application of a torsional moment to the longitudinal axis of the silicon beams, which results in a homogeneous in-plane shear stress in the beam surface. The safely applicable shear stresses span the range of ±50 MPa. Thanks to a specially designed clamping mechanism, the unintended normal stress typically stays below 2.5% of the applied shear stress. An analytical model is presented to compute the induced shear stress. Numerical computations verify the analytical results and show that the homogeneity of the shear stress is very high on the beam surface in the region of interest. Measurements with piezoresistive microsensors fabricated using a complementary metal-oxide-semiconductor process show an excellent agreement with both the computational results and comparative measurements performed on a four-point bending bridge. The electrical connection to the silicon beam is performed with standard bond wires. This ensures that minimal forces are applied to the beam by the electrical interconnection to the external instrumentation and that devices with arbitrary bond pad layout can be inserted into the setup.

  9. Pattern recognition of estradiol, testosterone and dihydrotestosterone in children's saliva samples using stochastic microsensors

    NASA Astrophysics Data System (ADS)

    Staden, Raluca-Ioana Stefan-Van; Gugoaşă, Livia Alexandra; Calenic, Bogdan; Legler, Juliette

    2014-07-01

    Stochastic microsensors based on diamond paste and three types of electroactive materials (maltodextrin (MD), α-cyclodextrin (α-CD) and 5,10,15,20-tetraphenyl-21H,23H porphyrin (P)) were developed for the assay of estradiol (E2), testosterone (T2) and dihydrotestosterone (DHT) in children's saliva. The main advantage of utilization of such tools is the possibility to identify and quantify all three hormones within minutes in small volumes of childen's saliva. The limits of quantification obtained for DHT, T2, and E2 (1 fmol/L for DHT, 1 pmol/L for T2, and 66 fmol/L for E2) determined using the proposed tools allows the utilization of these new methods with high reliability for the screening of saliva samples from children. This new method proposed for the assay of the three hormones overcomes the limitations (regarding limits of determination) of ELISA method which is the standard method used in clinical laboratories for the assay of DHT, T2, and E2 in saliva samples. The main feature of its utilization for children's saliva is to identify earlier problems related to early puberty and obesity.

  10. Adsorptive cathodic stripping voltammetric determination of cefoperazone in bulk powder, pharmaceutical dosage forms, and human urine.

    PubMed

    Hoang, Vu Dang; Huyen, Dao Thi; Phuc, Phan Hong

    2013-01-01

    The electroreduction behaviour and determination of cefoperazone using a hanging mercury drop electrode were investigated. Cyclic voltammograms of cefoperazone recorded in universal Britton-Robinson buffers pH 3-6 exhibited a single irreversible cathodic peak. The process was adsorption-controlled. Britton-Robinson buffer 0.04 M pH 4.0 was selected as a supporting electrolyte for quantitative purposes by differential pulse and square wave adsorptive cathodic stripping voltammetry. The experimental voltammetric conditions were optimized using Central Composite Face design. A reduction wave was seen in the range from -0.7 to -0.8 V. These voltammetric techniques were successfully validated as per ICH guidelines and applied for the determination of cefoperazone in its single and sulbactam containing powders for injection and statistically comparable to USP-HPLC. They were further extended to determine cefoperazone in spiked human urine with no matrix effect.

  11. Voltammetric Electronic Tongue for Different Varieties of Rice Classification Based on Square Wave Voltammetry

    NASA Astrophysics Data System (ADS)

    Hu, Hongsheng; Niu, Qunfeng; Pan, Yinqing; Wang, Li

    A classification method of discriminate rice from different varieties with voltammetric electronic tongue based on square wave voltammetry is investigated. The rice samples are crushed and mixed with distilled water to get the rice solution, and the solution should be stirred and filtered before the experiment. In order to obtain the electrochemical response signals of the rice samples and extract the characteristic value of the singles, the electronic tongue which works respectively with titanium (Ti) electrode and tungsten electrode (W) to test the sample solution under square wave voltammetry. The Principal Component Analysis (PCA) and Clustering Analysis (CA) are adopted to classify and recognize the rice samples. Experimental results show that good classification and recognition results are got in this paper when using Principal Component Analysis and Cluster Analysis to analyze the response signals which are obtained by voltammetric electronic tongue worked with Ti electrode and W electrode under square wave potential.

  12. A zeolite modified carbon paste electrode as useful sensor for voltammetric determination of acetaminophen.

    PubMed

    Ahmadpour-Mobarakeh, Leila; Nezamzadeh-Ejhieh, Alireza

    2015-04-01

    The voltammetric behavior of a carbon paste electrode modified with Co(II)-exchanged zeolite A (Co(II)-A/ZMCPE) for determination of acetaminophen was studied. The proposed electrode showed a diffusion controlled reaction with the electron transfer rate constant (Ks) of 0.44s(-1) and charge transfer coefficient of 0.73 in the absence of acetaminophen. A linear voltammetric response was obtained in the range of 0.1 to 190μmolL(-1) of acetaminophen [r(2)=0.9979, r=0.9989 (n=10)] with a detection limit of 0.04μmolL(-1). The method was successfully applied to the analysis of acetaminophen in some drugs.

  13. Voltammetric determination of salicylic acid in pharmaceuticals formulations of acetylsalicylic acid.

    PubMed

    Torriero, Angel A J; Luco, Juan M; Sereno, Leonides; Raba, Julio

    2004-02-06

    The electrochemical oxidation of salicylic acid (SA) has been studied on a glassy carbon electrode using cyclic voltammetry and differential pulse voltammetric (DPV) method. SA gives a single irreversible oxidation wave over the wide pH range studied. The irreversibility of the electrode process was verified by different criteria. The mechanism of oxidation is discussed. Using differential pulse voltammetry, SA yielded a well-defined voltammetric response in Britton-Robinson buffer solution, pH 2.37 at 1.088V (versus Ag/AgCl). The method was linear over the SA concentration range: 1-60mugml(-1). The method was successfully applied for the analysis of SA as a hydrolysis product, in solid pharmaceutical formulations containing acetylsalicylic acid (ASA).

  14. Adsorptive Cathodic Stripping Voltammetric Determination of Cefoperazone in Bulk Powder, Pharmaceutical Dosage Forms, and Human Urine

    PubMed Central

    Hoang, Vu Dang; Huyen, Dao Thi; Phuc, Phan Hong

    2013-01-01

    The electroreduction behaviour and determination of cefoperazone using a hanging mercury drop electrode were investigated. Cyclic voltammograms of cefoperazone recorded in universal Britton-Robinson buffers pH 3–6 exhibited a single irreversible cathodic peak. The process was adsorption-controlled. Britton-Robinson buffer 0.04 M pH 4.0 was selected as a supporting electrolyte for quantitative purposes by differential pulse and square wave adsorptive cathodic stripping voltammetry. The experimental voltammetric conditions were optimized using Central Composite Face design. A reduction wave was seen in the range from −0.7 to −0.8 V. These voltammetric techniques were successfully validated as per ICH guidelines and applied for the determination of cefoperazone in its single and sulbactam containing powders for injection and statistically comparable to USP-HPLC. They were further extended to determine cefoperazone in spiked human urine with no matrix effect. PMID:24109542

  15. Novel electrochemical sensor based on N-doped carbon nanotubes and Fe3O4 nanoparticles: simultaneous voltammetric determination of ascorbic acid, dopamine and uric acid.

    PubMed

    Fernandes, Diana M; Costa, Marta; Pereira, Clara; Bachiller-Baeza, Belén; Rodríguez-Ramos, Inmaculada; Guerrero-Ruiz, Antonio; Freire, Cristina

    2014-10-15

    A new modified electrode based on N-doped carbon nanotubes functionalized with Fe3O4 nanoparticles (Fe3O4@CNT-N) has been prepared and applied on the simultaneous electrochemical determination of small biomolecules such as dopamine (DA), uric acid (UA) and ascorbic acid (AA) using voltammetric methods. The unique properties of CNT-N and Fe3O4 nanoparticles individually and the synergetic effect between them led to an improved electrocatalytic activity toward the oxidation of AA, DA and UA. The overlapping anodic peaks of these three biomolecules could be resolved from each other due to their lower oxidation potentials and enhanced oxidation currents when using the Fe3O4@CNT-N modified electrode. The linear response ranges for the square wave voltammetric determination of AA, DA and UA were 5-235, 2.5-65 and 2.5-85μmoldm(-3) with detection limit (S/N=3) of 0.24, 0.050 and 0.047μmoldm(-3), respectively. These results show that Fe3O4@CNT-N nanocomposite is a promising candidate of cutting-edge electrode materials for electrocatalytic applications.

  16. Ion-transfer voltammetric determination of folic acid at meso-liquid-liquid interface arrays.

    PubMed

    Jiang, Xuheng; Gao, Kui; Hu, Daopan; Wang, Huanhuan; Bian, Shujuan; Chen, Yong

    2015-04-21

    Voltammetric studies on the simple ion transfer (IT) behaviors of an important water-soluble B-vitamin, folic acid (FA), at the liquid-liquid (L-L) interface were firstly performed and then applied as a novel detection method for FA under physiological conditions. Meso-water-1,6-dichlorohexane (W-DCH) and meso-water-organogel interface arrays were built by using a hybrid mesoporous silica membrane (HMSM) with a unique structure of pores-in-pores and employed as the new platforms for the IT voltammetric study. In view of the unique structure of the HMSM, the impact of the ionic surfactant cetyltrimethylammonium bromide (CTAB), self-assembled within the silica nanochannels of the HMSM, was investigated. In particular, its effect on the IT voltammetric behavior and detection of FA at meso-L-L interface arrays was systematically examined by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and differential pulse stripping voltammetry (DPSV). It was found that all the voltammetric responses of CV, DPV, and DPSV and the corresponding detection limit of FA at such meso-L-L interface arrays are closely related to the CTAB in the HMSM. Significantly, the calculated detection limit of FA could be improved to 80 nM after the combination of the DPSV technique with the additional preconcentration of FA in the silica-CTAB nanochannels, achieved through an anion-exchange process between FA(-) and the bromide of CTAB in HMSM. This provides a new and attractive strategy for the detection of those biological anions.

  17. Voltammetric Studies of Zomepirac Sodium and Its Determination in Tablets by Differential-Pulse Polarography.

    DTIC Science & Technology

    1984-01-06

    min in order to promote disintegration of the tablets . The remaining larger lumps of tablet mass were crushed with a glass rod and the mixture stirred...D-A136 982 VOLTAMMETRIC STUDIES OF ZOMEPIRAC SODIUM AND ITS i/i DETERMINATION IN TABLETS .. U) UTAH UNIV SALT LAKE CITY DEPT OF CHEMISTRY L G CHATTEN...TYPE OF REPORT &PEMOCVE Voltaninetric Studies of Zomepirac Sodium and its Dete~rmrination in Tablets by Differential-Pulse ,Technical Reportf 24 Pol

  18. Emerging trends in biosensing using stripping voltammetric detection of metal-containing nanolabels - A review.

    PubMed

    Kokkinos, Christos; Economou, Anastasios

    2017-04-08

    Over the last years, nanomaterials have found many applications in the development of electrochemical biosensors. Among other functions, metal nanoparticles (NPs) and quantum dots (QDs) (semiconducting nanocrystals composed of metal salts) are increasingly being used as voltammetric labels in affinity biosensing. Labeling is based on the attachment of the label(s) on the target biomolecules or on a biorecognition reporting probe. After an appropriate specific affinity interaction between the target and the reporting probe, the metallic nanolabels are converted to the respective cations which are quantified by a voltammetric technique. The very use of metal-containing nanoprobes as labels provides a first amplification step since each nanoprobe can release a very significant number of detectable cations. When anodic stripping voltammetry (ASV) (in which a preconcentration step precedes the actual voltammetric scan) is further employed as the detection format, ultra-sensitive bioassays can be developed. The present paper reviews the emerging trends in affinity biosensing using ASV detection of metal-containing nanolabels. It provides a critical discussion of recent developments in ASV transduction and electrodes, novel strategies for signal enhancement, approaches for multiplexed detection as well as fluidics, paper-based and lab-on-a-chip devices.

  19. An Integrated Surface Acoustic Wave-Based Chemical Microsensor Array for Gas-Phase Chemical Analysis Microsystems

    SciTech Connect

    Casalnuovo, stephen A.; Frye-Mason, Gregory C.; Heller, Edwin J.; Hietala, Vincent M.; Kottenstette, Richard J.; Lewis, Patrick R.; Manginell, Ronald P.; Matzke, Carolyn M.

    1999-07-20

    This paper describes preliminary results in the development of an acoustic wave (SAW) microsensor array. The array is based on a novel configuration that allows for three sensors and a phase reference. Two configurations of the integrated array are discussed: a hybrid multichip-module based on a quartz SAW sensor with GaAs microelectronics and a fully monolithic GaAs-based SAW. Preliminary data are also presented for the use of the integrated SAW array in a gas-phase chemical micro system that incorporates microfabricated sample collectors and concentrators along with gas chromatography (GC) columns.

  20. Non-invasive quantification of endogenous root auxin transport using an integrated flux microsensor technique.

    PubMed

    McLamore, Eric S; Diggs, Alfred; Calvo Marzal, Percy; Shi, Jin; Blakeslee, Joshua J; Peer, Wendy A; Murphy, Angus S; Porterfield, D Marshall

    2010-09-01

    Indole-3-acetic acid (IAA) is a primary phytohormone that regulates multiple aspects of plant development. Because polar transport of IAA is an essential determinant of organogenesis and dynamic tropic growth, methods to monitor IAA movement in vivo are in demand. A self-referencing electrochemical microsensor was optimized to non-invasively measure endogenous IAA flux near the surface of Zea mays roots without the addition of exogenous IAA. Enhanced sensor surface modification, decoupling of acquired signals, and integrated flux analyses were combined to provide direct, real time quantification of endogenous IAA movement in B73 maize inbred and brachytic2 (br2) auxin transport mutant roots. BR2 is localized in epidermal and hypodermal tissues at the root apex. br2 roots exhibit reduced shootward IAA transport at the root apex in radiotracer experiments and reduced gravitropic growth. IAA flux data indicates that maximal transport occurs in the distal elongation zone of maize roots, and net transport in/out of br2 roots was decreased compared to B73. Integration of short term real time flux data in this zone revealed oscillatory patterns, with B73 exhibiting shorter oscillatory periods and greater amplitude than br2. IAA efflux and influx were inhibited using 1-N-naphthylphthalamic acid (NPA), and 2-naphthoxyacetic acid (NOA), respectively. A simple harmonic oscillation model of these data produced a correlation between modeled and measured values of 0.70 for B73 and 0.69 for br2. These results indicate that this technique is useful for real-time IAA transport monitoring in surface tissues and that this approach can be performed simultaneously with current live imaging techniques.

  1. O2, pH, and Redox Potential Microprofiles around Potamogeton malaianus Measured Using Microsensors

    PubMed Central

    Dong, Bin; Han, Ruiming; Wang, Guoxiang; Cao, Xun

    2014-01-01

    This study aimed to elucidate the effects of periphyton on the microprofiles of oxygen (O2), pH, and oxidation-reduction potential around the stems and leaves of a submerged macrophyte Potamogeton malaianus and on the plant growth in the eutrophic shallow Taihu Lake, China. The microprofiles were measured using a motorized microprofiling system equipped with microsensors. The leaf age of the macrophyte and periphyton exerted significant effects on the microprofiles of O2, pH, and oxidation-reduction potential. O2 concentration and pH increased whereas the oxidation-reduction potential decreased with decreasing distance to the stem/leaf surface. The fluctuation amplitudes of O2, pH, and oxidation-reduction potential were the largest in the microprofiles of mature leaves and the lowest in senescent leaves. The periphyton increased the thickness of the broad diffusive boundary layer and fluctuation amplitudes of O2, pH, and oxidation-reduction potential. When the periphyton was removed, the thickness of the broad diffusive boundary layer in the microprofiles of stems, senescent leaves, and mature leaves reduced by 29.0%, 49.72%, and 70.34%, and the O2, pH, and oxidation-reduction potential fluctuation amplitudes also declined accordingly. Our results suggest that a thick periphyton exerted negative effects on the growth of macrophytes by providing extensive shading and creating a barrier that hindered the transport of dissolved substances such as O2, and led to premature decline in macrophytes in the eutrophic Taihu Lake. The consequent implications can help to elucidate the control mechanism of the broad diffusive boundary layer around macrophytes on nutrient cycling in eutrophic waters and to better understand the role of this layer in the Taihu Lake and other similar eutrophic waters. PMID:25004129

  2. A Multiscale Approach to the Smart Deployment of Micro-Sensors over Lightweight Structures

    PubMed Central

    Capellari, Giovanni

    2017-01-01

    A topology optimization approach has been recently proposed to maximize the sensitivity to damage of measurements, collected through a network of sensors to be deployed over thin plates for structural health monitoring purposes. Within such a frame, damage is meant as a change in the structural health characterized by a reduction of relevant stiffness and load-carrying properties. The sensitivity to a damage of unknown amplitude and location is computed by comparing the response to the external actions of the healthy structure and of a set of auxiliary damaged structures, each one featuring reduced mechanical properties in a small region only. The topology optimization scheme has been devised to properly account for the information coming from all of the sensors to be placed on the structure and for damage depending on its location. In this work, we extend the approach within a multiscale frame to account for three different length scales: a macroscopic one, linked to the dimensions of the whole structure to be monitored; a mesoscopic one, linked to the characteristic size of the damaged region; a microscopic one, linked to the size of inertial microelectromechanical systems (MEMS) to be used within a marginally-invasive health monitoring system. Results are provided for a square plate and for a section of fuselage with stiffeners, to show how the micro-sensors have to be deployed to maximize the capability to detect a damage, to assess the sensitivity of the results to the measurement noise and to also discuss the speedup in designing the network topology against a standard single-scale approach. PMID:28714888

  3. Determination of microcystins in river waters using microsensor arrays on disk.

    PubMed

    Morais, Sergi; Tamarit-López, Jesús; Puchades, Rosa; Maquieira, Angel

    2010-12-01

    The development of simple, accurate, and rapid multisample analytical methodologies to find out critical targets in waters is highly demanded. Optical microsensor arrays to determine microcystins in river waters are developed on the polycarbonate side of compact discs. The working principle of the sensors relied on an indirect competitive microimmunoassay, where free microcystin LR (MC-LR) competes with immobilized conjugate for specific monoclonal antibody. The results of the immunoreaction are detected with a DVD drive, showing the readouts in minutes. The method reached a sensitivity (IC(50)) for MC-LR of 1.04 μg/L and a linear response in the range 0.12-2.00 μg/L, allowing its determination below the upper limit proposed by the World Health Organization in drinking water. The developed analytical approach shows simplicity, good sensitivity, high throughput capability, and rapidity (37 min) in field use. The optimized assay showed also high congener reactivity to MC-LY (144%), MC-LA (125%), MC-LF (119%), MC-LW (102%), MC-YR (83%), and nodularin (94%). Furthermore, the suitability of the disk biosensor to quantify MC-LR was successfully evaluated analyzing river water samples, obtaining excellent recoveries (78-113%). Precoated discs are stable for at least seven weeks without loosing their analytical performances. Also, the portability of the analytical system permits on-site analysis and quantification, saving time and other resources. To our knowledge, this is the only work where a portable, easy-to-use, array based system has been developed for on-site microcystin quantification and applied to simultaneously analyze 42 samples plus the calibration curve, reaching microgram per liter sensitivity.

  4. Laboratory and field evaluation of a SAW microsensor array for measuring perchloroethylene in breath.

    PubMed

    Groves, William A; Achutan, Chandran

    2004-12-01

    This article describes the laboratory and field performance evaluation of a small prototype instrument employing an array of six polymer-coated surface acoustic wave (SAW) sensors and a thermal desorption preconcentration unit for rapid analysis of perchloroethylene in breath. Laboratory calibrations were performed using breath samples spiked with perchloroethylene to prepare calibration standards spanning a concentration range of 0.1-10 ppm. A sample volume of 250 mL was preconcentrated on 40 mg of Tenax GR at a flow rate of 100 mL/min, followed by a dry air purge and thermal desorption at a temperature of 200 degrees C. The resulting pulse of vapor was passed over the sensor array at a flow rate of 20 mL/min and sensor responses were recorded and displayed using a laptop computer. The total time per analysis was 4.5 min. SAW sensor responses were linear, and the instrument's limit of detection was estimated to be 50 ppb based on the criterion that four of the six sensors show a detectable response. Field performance was evaluated at a commercial dry-cleaning operation by comparing prototype instrument results for breath samples with those of a portable gas chromatograph (NIOSH 3704). Four breath samples were collected from a single subject over the course of the workday and analyzed using the portable gas chromatograph (GC) and SAW instruments. An additional seven spiked breath samples were prepared and analyzed so that a broader range of perchloroethylene concentrations could be examined. Linear regression analysis showed excellent agreement between prototype instrument and portable GC breath sample results with a correlation coefficient of 0.99 and a slope of 1.04. The average error for the prototype instrument over a perchloroethylene breath concentration range of 0.9-7.2 ppm was 2.6% relative to the portable GC. These results demonstrate the field capabilities of SAW microsensor arrays for rapid analysis of organic vapors in breath.

  5. O2, pH, and redox potential microprofiles around Potamogeton malaianus measured using microsensors.

    PubMed

    Dong, Bin; Han, Ruiming; Wang, Guoxiang; Cao, Xun

    2014-01-01

    This study aimed to elucidate the effects of periphyton on the microprofiles of oxygen (O2), pH, and oxidation-reduction potential around the stems and leaves of a submerged macrophyte Potamogeton malaianus and on the plant growth in the eutrophic shallow Taihu Lake, China. The microprofiles were measured using a motorized microprofiling system equipped with microsensors. The leaf age of the macrophyte and periphyton exerted significant effects on the microprofiles of O2, pH, and oxidation-reduction potential. O2 concentration and pH increased whereas the oxidation-reduction potential decreased with decreasing distance to the stem/leaf surface. The fluctuation amplitudes of O2, pH, and oxidation-reduction potential were the largest in the microprofiles of mature leaves and the lowest in senescent leaves. The periphyton increased the thickness of the broad diffusive boundary layer and fluctuation amplitudes of O2, pH, and oxidation-reduction potential. When the periphyton was removed, the thickness of the broad diffusive boundary layer in the microprofiles of stems, senescent leaves, and mature leaves reduced by 29.0%, 49.72%, and 70.34%, and the O2, pH, and oxidation-reduction potential fluctuation amplitudes also declined accordingly. Our results suggest that a thick periphyton exerted negative effects on the growth of macrophytes by providing extensive shading and creating a barrier that hindered the transport of dissolved substances such as O2, and led to premature decline in macrophytes in the eutrophic Taihu Lake. The consequent implications can help to elucidate the control mechanism of the broad diffusive boundary layer around macrophytes on nutrient cycling in eutrophic waters and to better understand the role of this layer in the Taihu Lake and other similar eutrophic waters.

  6. Surface acoustic wave (SAW) microsensor array for measuring VOCs in drinking water.

    PubMed

    Groves, W A; Grey, A B; O'Shaughnessy, P T

    2006-09-01

    Exposure to volatile organic chemicals (VOCs) in drinking water has been linked to a number of adverse health effects including cancer, liver, and kidney damage. However, the large number of potential contaminants and the cost and complexity of existing analytical methods limits the extent to which water quality is routinely characterized. This project focused on the laboratory development and evaluation of an instrument for field analysis of VOCs in drinking water. The instrument is based on an array of six polymer-coated surface-acoustic-wave microsensors. A test-set consisting of dichloromethane, chloroform, 1,1,1-trichloroethane, perchloroethylene, and m-xylene was used in a series of experiments designed to optimize the purge-trap preconcentration system, calibrate the instrument over the concentration range of 0.2-2 times the USEPA maximum contaminant levels (MCLs), and compare results to those of a reference laboratory. The primary goal was to develop a cost-effective alternative for on-site evaluation of VOCs in water. Calibration and evaluation test results for spiked water samples demonstrate adequate sensitivity for 19 of the 21 regulated VOCs considered using a ten minute sampling and analysis cycle. Monte Carlo simulations characterized the performance of trained artificial neural networks (ANNs) which had correct classification rates of 99%, 90%, and 80% for the five individual test-set vapors and their binary and ternary mixtures, respectively. These results demonstrate the excellent potential of this technology for addressing the need for improved VOC field-screening methods for water supplies.

  7. Microsensor measurements of sulfate reduction and sulfide oxidation in compact microbial communities of aerobic biofilms

    SciTech Connect

    Kuehl, M.; Joergensen, B.B. )

    1992-04-01

    The microzonation of O{sub 2} respiration, H{sub 2}S oxidation, and SO{sub 4}{sup 2{minus}} reduction in aerobic trickling-filter biofilms was studied by measuring concentration profiles at high spatial resolution (25 to 100 {mu}m) with microsensors for O{sub 2}, S{sup 2{minus}}, and pH. Specific reaction rates were calculated from measured concentration profiles by using a simple one-dimensional diffusion reaction model. The importance of electron acceptor and electron donor availability for the microzonation of respiratory processes and their reaction rates was investigated. Oxygen respiration was found in the upper 0.2 to 0.4 mm of the biofilm, whereas sulfate reduction occurred in deeper, anoxic parts of the biofilm. Sulfate reduction accounted for up to 50% of the total mineralization of organic carbon in the biofilms. All H{sub 2}S produced from sulfate reduction was reoxidized by O{sub 2} in a narrow reaction zone, and no H{sub 2}S escaped to the overlying water. Turnover times of H{sub 2}S and O{sub 2} in the reaction zone were only a few seconds owing to rapid bacterial H{sub 2}S oxidation. Anaerobic H{sub 2}S oxidation with NO{sub 3}{sup {minus}} could be induced by addition of nitrate to the medium. Total sulfate reduction rates increased when the availability of SO{sub 4}{sup 2{minus}} or organic substrate increased as a result of deepening of the sulfate reduction zone or an increase in the sulfate reduction intensity, respectively.

  8. Microsensors to the Model Forecasts: Multiscale Embedded Networked Sensing of Nutrients in the Watershed

    NASA Astrophysics Data System (ADS)

    Harmon, T. C.

    2005-12-01

    Hydrologic and water quality observatories are being planned with a vision of enhancing our ability to better understand, forecast and adaptively manage both water quantity and quality. To adequately cover these spatially and temporally variable systems, distributed, embedded sensor networks must be designed with the proper mix (multimodality) of sensors to quantify key system properties, including temperature and chemical distributions, as well as mass and energy fluxes, and to do so across multiple scales. Given resource limitations, process models need to be coupled to the sensor network to interpolate between sensor data. This work focuses on the spatially distributed flux of nutrients, specifically nitrate, in surface-subsurface environments. It begins at the sensor level, describing the development and testing of nitrate microsensors that are scaleable to large, dense sensor networks required to cover heterogeneous watersheds, including associated soil and sediment systems. First and second generation miniature and inexpensive nitrate sensors (ion selective electrodes) fabricated by depositing conducting polymers on carbon substrates are presented in the context of laboratory and field tests. While these sensors are limited to relatively short deployments (4-8 weeks), there are potential strategies for overcoming this problem. Scale-up to one- and three-dimensional soil/sediment sensor arrays is discussed in the context of two deployments: (1) a groundwater quality protection network, where recycled wastewater that is potentially high in nitrate is being used for agricultural irrigation, and (2) nonpoint source nitrate pollution in rivers and groundwater in agricultural watersheds. Recent hardware (wireless transceivers) and software advancements (e.g., network topology design and debugging, energy management) intended for networks spanning 100s of m in space are outlined in these examples. The discussion extends to sensor form factor, in situ calibration

  9. Dynamic characterization of external and internal mass transport in heterotrophic biofilms from microsensors measurements.

    PubMed

    Guimerà, Xavier; Dorado, Antonio David; Bonsfills, Anna; Gabriel, Gemma; Gabriel, David; Gamisans, Xavier

    2016-10-01

    Knowledge of mass transport mechanisms in biofilm-based technologies such as biofilters is essential to improve bioreactors performance by preventing mass transport limitation. External and internal mass transport in biofilms was characterized in heterotrophic biofilms grown on a flat plate bioreactor. Mass transport resistance through the liquid-biofilm interphase and diffusion within biofilms were quantified by in situ measurements using microsensors with a high spatial resolution (<50 μm). Experimental conditions were selected using a mathematical procedure based on the Fisher Information Matrix to increase the reliability of experimental data and minimize confidence intervals of estimated mass transport coefficients. The sensitivity of external and internal mass transport resistances to flow conditions within the range of typical fluid velocities over biofilms (Reynolds numbers between 0.5 and 7) was assessed. Estimated external mass transfer coefficients at different liquid phase flow velocities showed discrepancies with studies considering laminar conditions in the diffusive boundary layer near the liquid-biofilm interphase. The correlation of effective diffusivity with flow velocities showed that the heterogeneous structure of biofilms defines the transport mechanisms inside biofilms. Internal mass transport was driven by diffusion through cell clusters and aggregates at Re below 2.8. Conversely, mass transport was driven by advection within pores, voids and water channels at Re above 5.6. Between both flow velocities, mass transport occurred by a combination of advection and diffusion. Effective diffusivities estimated at different biofilm densities showed a linear increase of mass transport resistance due to a porosity decrease up to biofilm densities of 50 g VSS·L(-1). Mass transport was strongly limited at higher biofilm densities. Internal mass transport results were used to propose an empirical correlation to assess the effective diffusivity

  10. Sensitive determination of capsaicin in pepper samples using a voltammetric platform based on carbon nanotubes and ruthenium nanoparticles.

    PubMed

    Baytak, Aysegul Kutluay; Aslanoglu, Mehmet

    2017-08-01

    A voltammetric platform based on modifying glassy carbon electrodes (GCEs) with ruthenium nanoparticles decorated carbon nanotubes (CNTs) was applied for the determination of capsaicin in pepper samples. The nanoparticles of ruthenium (RuNPs) were obtained at carbon nanotubes modified GCE by cyclic voltammetry. The composite of RuNPs-CNTs was characterized by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX). The proposed voltammetric platform, RuNPs/CNTs/GCE, highly improved the voltammetric process of capsaicin in comparison to the CNTs/GCE and bare GCE. A linear concentration range was obtained from 1.0×10(-8) to 4.1×10(-7)M (R(2)=0.9987) with a detection limit of 2.5×10(-9)M. The voltammetric platform has successfully been applied for quantifying capsaicin in various pepper samples including Isot. The proposed voltammetric platform offers advantages such as high sensitivity, selectivity and precision. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Stripping voltammetric analysis of organophosphate pesticides using Ni/Al layered double hydroxides as solid-phase extraction.

    PubMed

    Gong, Jingming; Wang, Lianyi; Song, Dandan; Zhu, Xiaolei; Zhang, Lizhi

    2009-10-15

    A sensitive electrochemical stripping voltammetric biosensor is designed for organophosphate pesticides (OPs) based on solid-phase extraction (SPE) using Ni/Al layered double hydroxides (LDHs) modified glassy carbon electrode (labeled as Ni/Al-LDHs/GCE). The Ni/Al-LDHs as the host are highly efficient to capture OPs, which dramatically facilitates the enrichment of nitroaromatic OPs onto their surface and realizes the stripping voltammetric detection of OPs. The stripping voltammetric performances of methyl parathion (MP) intercalated into LDHs were evaluated by cyclic voltammetric and square-wave voltammetric (SWV) analysis. The combination of the host-guest supramolecular structure, SPE, and stripping voltammetry provides a fast, simple, and sensitive electrochemical method for detecting nitroaromatic OPs by using MP as a model. The stripping analysis is linear over the MP concentration ranges of 0.001-0.1 and 0.2-1.0 microg mL(-1) with a detection limit of 0.6 ng mL(-1) (S/N=3). The developed biosensor exhibits good reproducibility and acceptable stability. This study offers a new promising protocol for OPs analysis.

  12. A sensitive bisphenol A voltammetric sensor relying on AuPd nanoparticles/graphene composites modified glassy carbon electrode.

    PubMed

    Su, Bingyuan; Shao, Huilin; Li, Na; Chen, Xiaomei; Cai, Zhixiong; Chen, Xi

    2017-05-01

    In this work, a sensitive bisphenol A (BPA) electrochemical sensor was assembled using a surfactant-free AuPd nanoparticles-loaded graphene nanosheets (AuPdNPs/GNs) modified electrode. The AuPdNPs monodispersed on GNs were successfully prepared by the spontaneous redox reaction between bimetallic precursors and GNs. Because no surfactant or halide ions were involved in the proposed synthesis, the prepared composite was enabled to directly modify a glassy carbon electrode without any pre-treatments. Moreover, due to the synergetic effect of Au and Pd, AuPdNPs/GNs displayed high electrochemical activity with well-defined voltammetric peaks of BPA oxidation and lower overpotential compared with monometallic PdNPs and AuNPs supported GNs. According to the results of differential pulse voltammetry (DPV), under optimized conditions, a good linear response was observed for the concentration of BPA in the range of 0.05-10μM with a detection limit of 8nM. The developed electrochemical sensor was successfully applied to determine BPA in food package. This study indicated that AuPdNPs/GNs based electrochemical sensor can be a promising and reliable tool for rapid analysis of emergency pollution affairs of BPA.

  13. Surface crystallographic dependence of voltammetric oxidation of polyhydric alcohols and related systems at monocrystalline gold-acidic aqueous interfaces

    NASA Astrophysics Data System (ADS)

    Hamelin, Antoinette; Ho, Yeunghaw; Chang, Si-Chung; Gao, Xiaoping; Weaver, Michael J.

    1992-02-01

    The voltammetric oxidation in aqueous 0.1 Molar perchloric acid of four polyhydric alcohols, ethylene glycol, glycerol, meso-erythritol, and d-mannitol, on seven oriented gold surfaces is reported with the objective of assessing the role of surface crystallographic orientation on the catalytic electrooxidation of such poly-functional reactants. The automatically well-ordered nature of these gold surfaces has been scrutinized by in-situ scanning tunneling microscopy. In particular, the Au(221) and (533) faces were selected since they provide stepped surfaces, 4(111)-(111) and 4(111)-(100), respectively. The results are compared with corresponding data for simple unifunctional reactants, specifically for formic acid oxidation and with results reported previously for carbon monoxide oxidation. In contrast to the last reaction, the electrooxidation rates for both the polyhydric alcoholic and formic acid are greatest on Au(111), with Au(110) displaying unusually low activity. While formic acid electrooxidation is insensitive to the presence of monoatomic surface steps, the polyhydric alcohols (especially mannitol) are substantially less reactive on AU(221) and (533) relative to Au(111).

  14. Voltammetric determination of glutathione in haemolysed erythrocyte and tablet samples using modified-multiwall carbon nanotubes paste electrode.

    PubMed

    Ensafi, Ali A; Dadkhah-Tehrani, Samira; Karimi-Maleh, Hassan

    2012-12-01

    A chemically modified electrode was prepared by incorporating p-aminophenol into multiwall carbon nanotubes paste matrix. Cyclic voltammetry, square wave voltammetry, double potential step chronoamperometry, and electrochemical impedance spectroscopy were used to investigate the electrochemical behaviour of glutathione at the chemically modified electrode prepared. According to the results, p-aminophenol multiwall carbon nanotubes paste electrode (p-APMWCNTPE) showed high electrocatalytic activity for glutathione oxidation, producing a sharp oxidation peak current at about +0.285 vs Ag/AgCl reference electrode at pH 5.0. Chronoamperometry was also used to determine glutathione's catalytic rate constant and diffusion coefficient at p-APMWCNTPE. The square wave voltammetric peak current of glutathione increased linearly with glutathione concentration in the range of 2.0 × 10(-7) - 1.0 × 10(-4) mol L(-1) with a detection limit of 9.0 × 10(-8) mol L(-1). The method was also successfully employed as a selective, simple, and precise method for the determination of glutathione in haemolysed erythrocyte, tablet, and urine samples.

  15. Voltammetric determination of antibacterial drug gemifloxacin in solubilized systems at multi-walled carbon nanotubes modified glassy carbon electrode.

    PubMed

    Jain, Rajeev; Rather, Jahangir Ahmad

    2011-04-01

    A sensitive electroanalytical method for determination of gemifloxacin in pharmaceutical formulation has been investigated on the basis of the enhanced electrochemical response at multi-walled carbon nanotubes modified glassy carbon electrode in the presence of CTAB. Solubilized system of different surfactants including SDS, Tween-20 and CTAB were taken for the study of electrochemical behaviour of gemifloxacin at modified electrode. The reduction peak current increases in the presence of CTAB while other surfactants show opposite effect. The modified electrode exhibits catalytic activity, high sensitivity, stability and is applicable over wide range of concentration for the determination of gemifloxacin. The mechanism of electrochemical reduction of gemifloxacin has been proposed on the basis of CV, SWV, DPV and coulometeric techniques. The proposed squarewave voltammetric method shows linearity over the concentration range 2.47-15.5 μg/mL. The achieved limits of detection (LOD) and quantification (LOQ) are 0.90 ng/mL and 3.0 ng/mL respectively. Crown Copyright © 2010. Published by Elsevier B.V. All rights reserved.

  16. A novel poly(cyanocobalamin) modified glassy carbon electrode as electrochemical sensor for voltammetric determination of peroxynitrite.

    PubMed

    Wang, Yan; Chen, Zhen-zhen

    2010-07-15

    This report described the direct voltammetric detection of peroxynitrite (ONOO(-)) at a novel cyanocobalamin modified glassy carbon electrode prepared by electropolymeriation method. The electrochemical behaviors of peroxynitrite at the modified electrode were studied by cyclic voltammetry. The results showed that this new electrochemical sensor exhibited an excellent electrocatalytic activity to oxidation of peroxynitrite. The mechanism of catalysis was discussed. Based on electrocatalytic oxidation of peroxynitrite at the poly(cyanocobalamin) modified electrode, peroxynitrite was sensitively detected by differential pulse voltammetry. Under optimum conditions, the anodic peak current was linear to concentration of peroxynitrite in the range of 2.0x10(-6) to 3.0x10(-4) mol L(-1) with a detection limit of 1.0x10(-7) mol L(-1) (S/N of 3). The proposed method has been applied to determination of peroxynitrite in human serum with satisfactory results. This poly(cyanocobalamin) modified electrode showed high selectivity and sensitivity to peroxynitrite determination, which could be used in quantitative detection of peroxynitrite in vivo and in vitro. Copyright 2010 Elsevier B.V. All rights reserved.

  17. A graphene-based label-free voltammetric immunosensor for sensitive detection of the egg allergen ovalbumin.

    PubMed

    Eissa, Shimaa; L'Hocine, Lamia; Siaj, Mohamed; Zourob, Mohammed

    2013-08-07

    A graphene-based label-free voltammetric immunosensor for the sensitive detection of the egg white allergen ovalbumin has been developed. Graphene-modified screen printed carbon electrodes have been covalently functionalized using electrochemical reduction of in situ generated aryl diazonium salt forming a carboxyphenyl film on the graphene surface. The blocking property of the carboxyphenyl film grafted on to the graphene electrodes using different cyclic voltammetry cycles has been characterized using differential pulse voltammetry in [Fe(CN)6](3-/4-) solution. Then, the terminal carboxylic groups on the graphene surface were activated using EDC/NHS and used to immobilize the ovalbumin antibody and construct the immunosensor. The fabrication steps of the immunosensor have also been characterized using differential pulse voltammetry. The decrease in the [Fe(CN)6](3-/4-) reduction peak current after the immunochemical reaction with ovalbumin has been used for the ovalbumin detection. The developed immunosensor has been used for ovalbumin detection in the concentration range of 1 pg mL(-1) to 0.5 μg mL(-1) with a detection limit of 0.83 pg mL(-1) in PBS buffer. The food matrix effect studied with ovalbumin spiked cake extract showed a good percentage of recovery, indicating the possible applicability of the developed immunosensor in real food samples.

  18. Determination of fenitrothion in water using a voltammetric sensor based on a polymer-modified glassy carbon electrode.

    PubMed

    Amare, Meareg; Abicho, Samuel; Admassie, Shimelis

    2014-01-01

    A glassy carbon electrode (GCE) modified with poly(4-amino-3-hydroxynaphthalene sulfonic acid) (poly-AHNSA) was used for the selective and sensitive determination of fenitrothion (FT) organophosphorus pesticide in water. The electrochemical behavior of FT at the bare GCE and the poly-AHNSA/GCE were compared using cyclic voltammetry. Enhanced peak current response and shift to a lower potential at the polymer-modified electrode indicated the electrocatalytic activity of the polymer film towards FT. Under optimized solution and method parameters, the adsorptive stripping square wave voltammetric reductive peak current of FT was linear to FT concentration in the range of 0.001 to 6.6 x 10(-6) M, and the LOD obtained (3delta/m) was 7.95 x 10(-10) M. Recoveries in the range 96-98% of spiked FT in tap water and reproducible results with RSD of 2.6% (n = 5) were obtained, indicating the potential applicability of the method for the determination of trace levels of FT in environmental samples.

  19. Sensitive voltammetric detection of DNA damage at carbon electrodes using DNA repair enzymes and an electroactive osmium marker.

    PubMed

    Havran, Ludek; Vacek, Jan; Cahová, Katerina; Fojta, Miroslav

    2008-07-01

    This paper presents a new approach to electrochemical sensing of DNA damage, using osmium DNA markers and voltammetric detection at the pyrolytic graphite electrode. The technique is based on enzymatic digestion of DNA with a DNA repair enzyme exonuclease III (exoIII), followed by single-strand (ss) selective DNA modification by a complex of osmium tetroxide with 2,2'-bipyridine. In double-stranded DNA possessing free 3'-ends, the exoIII creates ss regions that can accommodate the electroactive osmium marker. Intensity of the marker signal measured at the pyrolytic graphite electrode responded well to the extent of DNA damage. The technique was successfully applied for the detection of (1) single-strand breaks (ssb) introduced in plasmid DNA by deoxyribonuclease I, and (2) apurinic sites generated in chromosomal calf thymus DNA upon treatment with the alkylating agent dimethyl sulfate. The apurinic sites were converted into the ssb by DNA repair endonuclease activity of the exoIII enzyme. We show that the presented technique is capable of detection of one lesion per approximately 10(5) nucleotides in supercoiled plasmid DNA.

  20. Application of renewable silver amalgam annular band electrode to voltammetric determination of vitamins C, B1 and B2.

    PubMed

    Baś, Bogusław; Jakubowska, Małgorzata; Górski, Łukasz

    2011-05-30

    In this work, the design and results of applying silver liquid amalgam film-modified silver solid amalgam annular band electrode (AgLAF-AgSAE), refreshed before each measurement, to voltammetric determination of vitamins C (VC), B(1) (VB1) and B(2) (VB2) are presented. The method is based on adsorptive accumulation of analytes at the AgLAF-AgSAE in a phosphate buffer (VB1), phosphate buffer with Triton X-100 (VB2) and an alkaline borate buffer with Triton X-100 (VC). The analytical parameters and procedure of electrode activation were optimized. The calibration graphs obtained for vitamins C, B(1) and B(2) are linear, respectively, for concentration range 0.05-12, 0.01-0.1 and 0.05-3 mg L(-1). The detection limits were calculated and equaled 0.02, 0.003 and 0.009 mg L(-1), while repeatability of the peak current was 2%, 1% and 3%, respectively. These results are comparable with results obtained for polarographic determination of the same vitamins using mercury electrodes. Finally, the AgLAF-AgSAE was applied to the determination of vitamins in pharmaceutical samples and fruit juices with satisfactory results.

  1. Voltammetric Determination of Homocysteine Using Multiwall Carbon Nanotube Paste Electrode in the Presence of Chlorpromazine as a Mediator

    PubMed Central

    Gholami-Orimi, Fathali; Taleshi, Farshad; Biparva, Pourya; Karimi-Maleh, Hassan; Beitollahi, Hadi; Ebrahimi, Hamid R.; Shamshiri, Mohamad; Bagheri, Hasan; Fouladgar, Masoud; Taherkhani, Ali

    2012-01-01

    We propose chlorpromazine (CHP) as a new mediator for the rapid, sensitive, and highly selective voltammetric determination of homocysteine (Hcy) using multiwall carbon nanotube paste electrode (MWCNTPE). The experimental results showed that the carbon nanotube paste electrode has a highly electrocatalytic activity for the oxidation of Hcy in the presence of CHP as a mediator. Cyclic voltammetry, double potential step chronoamperometry, and square wave voltammetry (SWV) are used to investigate the suitability of CHP at the surface of MWCNTPE as a mediator for the electrocatalytic oxidation of Hcy in aqueous solutions. The kinetic parameters of the system, including electron transfer coefficient, and catalytic rate constant were also determined using the electrochemical approaches. In addition, SWV was used for quantitative analysis. SWV showed wide linear dynamic range (0.1–210.0 μM Hcy) with a detection limit of 0.08 μM Hcy. Finally, this method was also examined as a selective, simple, and precise electrochemical sensor for the determination of Hcy in real samples. PMID:22675657

  2. Voltammetric determination of homocysteine using multiwall carbon nanotube paste electrode in the presence of chlorpromazine as a mediator.

    PubMed

    Gholami-Orimi, Fathali; Taleshi, Farshad; Biparva, Pourya; Karimi-Maleh, Hassan; Beitollahi, Hadi; Ebrahimi, Hamid R; Shamshiri, Mohamad; Bagheri, Hasan; Fouladgar, Masoud; Taherkhani, Ali

    2012-01-01

    We propose chlorpromazine (CHP) as a new mediator for the rapid, sensitive, and highly selective voltammetric determination of homocysteine (Hcy) using multiwall carbon nanotube paste electrode (MWCNTPE). The experimental results showed that the carbon nanotube paste electrode has a highly electrocatalytic activity for the oxidation of Hcy in the presence of CHP as a mediator. Cyclic voltammetry, double potential step chronoamperometry, and square wave voltammetry (SWV) are used to investigate the suitability of CHP at the surface of MWCNTPE as a mediator for the electrocatalytic oxidation of Hcy in aqueous solutions. The kinetic parameters of the system, including electron transfer coefficient, and catalytic rate constant were also determined using the electrochemical approaches. In addition, SWV was used for quantitative analysis. SWV showed wide linear dynamic range (0.1-210.0 μM Hcy) with a detection limit of 0.08 μM Hcy. Finally, this method was also examined as a selective, simple, and precise electrochemical sensor for the determination of Hcy in real samples.

  3. Cost-effective and highly sensitive cholesterol microsensors with fast response based on the enzyme-induced conductivity change of polyaniline

    NASA Astrophysics Data System (ADS)

    Fang, Kuan-Chung; Chu, Chia-Ho; Hsu, Chen-Pin; Kang, Yen-Wen; Fang, Jung-Ying; Hsu, Chia-Hsien; Huang, Yu-Fen; Chen, Chih-Chen; Li, Sheng-Shian; Andrew Yeh, J.; Yao, Da-Jeng; Wang, Yu-Lin

    2014-09-01

    In this study, a cost-effective and highly sensitive cholesterol microsensor, which is consisted of cholesterol oxidase (ChOx), horseradish peroxidase (HRP), and polyaniline (PANI), was developed based on the enzyme-induced conductivity change of PANI with fast response. Hydrogen peroxide is produced via the reaction between cholesterol and ChOx, which was immobilized in a dialysis membrane. The produced hydrogen peroxide can oxidize HRP, which can be reduced by oxidizing PANI, thus resulting in decreased conductivity of the polyaniline thin film. The reduced HRP can be oxidized again by hydrogen peroxide and the cycle of the oxidation/reduction continues until all hydrogen peroxide are reacted, leading to the high sensitivity of the sensor due to the signal contributed from all hydrogen peroxide molecules. Cholesterol was detected near the physiological concentrations ranging from 100 mg/dl to 400 mg/dl with the cholesterol microsensors. The results show linear relation between cholesterol concentration and the conductivity change of the PANI. The microsensor showed no response to cholesterol when the PANI was standalone without cholesterol oxidase immobilized, indicating that the enzymatic reaction is required for cholesterol detection. The simple process of the sensor fabrication allows the sensor to be cost-effective and disposable usage. This electronic cholesterol microsensor is promising for point-of-care health monitoring in cholesterol level with low cost and fast response.

  4. Cost-effective and highly sensitive cholesterol microsensors with fast response based on the enzyme-induced conductivity change of polyaniline

    SciTech Connect

    Fang, Kuan-Chung; Chu, Chia-Ho; Hsu, Chen-Pin; Kang, Yen-Wen; Fang, Jung-Ying; Chen, Chih-Chen; Li, Sheng-Shian; Andrew Yeh, J.; Yao, Da-Jeng; Wang, Yu-Lin; Hsu, Chia-Hsien; Huang, Yu-Fen

    2014-09-15

    In this study, a cost-effective and highly sensitive cholesterol microsensor, which is consisted of cholesterol oxidase (ChOx), horseradish peroxidase (HRP), and polyaniline (PANI), was developed based on the enzyme-induced conductivity change of PANI with fast response. Hydrogen peroxide is produced via the reaction between cholesterol and ChOx, which was immobilized in a dialysis membrane. The produced hydrogen peroxide can oxidize HRP, which can be reduced by oxidizing PANI, thus resulting in decreased conductivity of the polyaniline thin film. The reduced HRP can be oxidized again by hydrogen peroxide and the cycle of the oxidation/reduction continues until all hydrogen peroxide are reacted, leading to the high sensitivity of the sensor due to the signal contributed from all hydrogen peroxide molecules. Cholesterol was detected near the physiological concentrations ranging from 100 mg/dl to 400 mg/dl with the cholesterol microsensors. The results show linear relation between cholesterol concentration and the conductivity change of the PANI. The microsensor showed no response to cholesterol when the PANI was standalone without cholesterol oxidase immobilized, indicating that the enzymatic reaction is required for cholesterol detection. The simple process of the sensor fabrication allows the sensor to be cost-effective and disposable usage. This electronic cholesterol microsensor is promising for point-of-care health monitoring in cholesterol level with low cost and fast response.

  5. A direct in situ fingerprinting method for acid rock drainage using voltammetric techniques with a single renewable gold microelectrode.

    PubMed

    Nuzzio, Donald B; Zettler, Erik R; Aguilera, Angeles; Amaral-Zettler, Linda A

    2011-04-15

    Electrochemistry allows for rapid identification of multiple metals and other chemical complexes common in acid rock drainage (ARD) systems. Voltammetric scans using a single gold microelectrode of water samples from geochemically distinct areas of the Río Tinto (RT) in southwestern Spain were clearly recognizable in the field and in samples stored at room temperature for over 6 months. Major voltammetric peaks of iron(III) and copper(II) were identified on a single constantly renewable gold microelectrode. Confirmation of these peaks was performed by spiking with standard metal solutions in the laboratory. This voltammetric technique is a rapid, direct and inexpensive in situ method for identification of water sources and their chemical characteristics, as well as an economical way to monitor environmental changes and remediation efforts.

  6. Fusion of Potentiometric & Voltammetric Electronic Tongue for Classification of Black Tea Taste based on Theaflavins (TF) Content

    NASA Astrophysics Data System (ADS)

    Bhattacharyya, Nabarun; Legin, Andrey; Papieva, Irina; Sarkar, Subrata; Kirsanov, Dmitry; Kartsova, Anna; Ghosh, Arunangshu; Bandyopadhyay, Rajib

    2011-09-01

    Black tea is an extensively consumed beverage worldwide with an expanding market. The final quality of black tea depends upon number of chemical compounds present in the tea. Out of these compounds, theaflavins (TF), which is responsible for astringency in black tea, plays an important role in determining the final taste of the finished black tea. The present paper reports our effort to correlate the theaflavins contents with the voltammetric and potentiometric electronic tongue (e-tongue) data. Noble metal-based electrode array has been used for collecting data though voltammetric electronic tongue where as liquid filled membrane based electrodes have been used for potentiometric electronic tongue. Black tea samples with tea taster score and biochemical results have been collected from Tea Research Association, Tocklai, India for the analysis purpose. In this paper, voltammetric and potentiometric e-tongue responses are combined to demonstrate improvement of cluster formation among tea samples with different ranges of TF values.

  7. Voltammetric and spectrophotometric techniques for the determination of the antihypertensive drug Prazosin in urine and formulations.

    PubMed

    Arranz, A; de Betoño, S F; Echevarria, C; Moreda, J M; Cid, A; Valentín, J F

    1999-12-01

    A sensitive method was developed to determine Prazosin using a nafion modified carbon paste electrode (NMCPE). Prazosin was accumulated at a potential of 750 mV in Britton-Robinson buffer (pH 6.0) and then a negative sweep was made obtaining a cathodic peak close to 0 V. Cyclic voltammetric studies indicated that the process was quasi-reversible, and fundamentally controlled by adsorption. To obtain a good sensitivity, the instrumental and accumulation variables were studied using differential pulse voltammetry (DPV). Adsorptive voltammetric peak currents showed a linear response for Prazosin concentrations in the range between 4.0 x 10(-11) and 4.0 x 10(-8) M with two different slopes, and a detection limit (LOD) of 3.1 x 10(-11)M was obtained. The variation coefficient (CV) for a 8.0 x 10(-10) M solution (n = 10) was 4.08%. A spectrophotometric study of Prazosin was also carried out and two absorption bands were obtained at 246 and 329 nm (pH 1.8). The band at 329 nm was pH-dependent and its height and position changed with the pH values, so this allowed the pK'a determination (7.14 +/- 0.20) using different methods. The detection limit reached by means of UV-spectrophotometry was 0.9 x 10(-7) M, and the variation coefficient for 1.5 x 10(-5) M Prazosin solutions was 1.14% (n = 10). Although the sensitivity of the UV-spectrophotometric method was lower than that obtained using adsorptive stripping-differential pulse voltammetry (AdS-DPV), it could be applied to the determination of Prazosin in Minipres tablets. The voltammetric method was used for the determination of the drug in human urine samples at trace levels with good recoveries.

  8. Electrochemical Behavior and Voltammetric Determination of a Manganese(II) Complex at a Carbon Paste Electrode

    PubMed Central

    Karastogianni, Sophia; Girousi, Stella

    2016-01-01

    Investigation of the electrochemical behavior using cyclic voltammetry and detection of [Mn2+(thiophenyl-2-carboxylic acid)2 (triethanolamine)] with adsorptive stripping differential pulse voltammetry. The electrochemical behavior of a manganese(II) complex [Mn2+(thiophenyl-2-carboxylic acid)2(triethanolamine)] (A) was investigated using cyclic and differential pulse voltammetry in an acetate buffer of pH 4.6 at a carbon paste electrode. Further, an oxidation–reduction mechanism was proposed. Meanwhile, an adsorptive stripping differential pulse voltammetric method was developed for the determination of manganese(II) complex. PMID:26819548

  9. Spectroscopic and voltammetric characteristics of α-Zn2SiO4:V luminophor

    NASA Astrophysics Data System (ADS)

    Krasnenko, T. I.; Yanchenko, M. Yu.; Zaitseva, N. A.; Zabolotskaya, E. V.; Baklanova, I. V.; Buldakova, L. Yu.; Onufrieva, T. A.; Samigullina, R. F.

    2017-09-01

    Single-phase luminophor Zn2SiO4:V with willemite structure is prepared by hydrothermal method. It is found that the Zn: Si: V ratio between cations is 2: 0.9: 0.1. It is shown that the inclusion of vanadium in the willemite structure reduces the width of the bandgap by Δ E g ≈ 2 eV. Using a combination of spectroscopic and voltammetric techniques, it is found the zinc silicate matrix contains vanadium ions with charge states V5+, V4+, and V3+. In addition, magnetic ions form clusters.

  10. Voltammetric and RP-LC assay for determination of benidipine HCl.

    PubMed

    Karadas, Nurgul; Sanli, Senem; Gumustas, Mehmet; Ozkan, Sibel A

    2012-07-01

    The detailed electrooxidative behavior of benidipine (BEN) has been studied by using glassy carbon (GC) and boron-doped diamond (BDD) electrodes. Using cyclic voltammetry, depending on the pH values and the working electrodes, BEN showed one or two sharp and irreversible oxidation responses. The voltammetric experiments on some model compounds allowed elucidation of the oxidation mechanism of BEN. Highly sensitive, selective, rapid, and fully validated voltammetric methods for the determination of BEN in tablet dosage form were also presented. Under optimized conditions, the peak current showed a linear dependence with concentration in the range between 3.25 μg mL(-1) and 54.20 μg mL(-1) for GC and 1.08 μg mL(-1) and 54.20 μg mL(-1) for BDD electrodes by using differential pulse (DPV) and square wave (SWV) voltammetric techniques. In this study, acid dissociation constant (pK(a)) value of BEN was determined by using the dependence of the retention factor on the pH of the mobile phase using reverse phase-liquid chromatographic (RP-LC) method. The effect of the composition of the mobile phase on the ionization constant was studied by measuring the pK(a) at different acetonitrile-water mixtures, ranging between 50 and 65% (v/v). Also simple, accurate, precise and fully validated RP-LC method for the assay of BEN in dosage form has been developed. XTerra RP-18 column at 25 °C with the mobile phase of acetonitrile:water 55:45 (v/v) adjusted to pH 3.0 with 15 mM o-phosphoric acid was used. Isocratic elution was performed in less than 5.0 min with a flow rate of 1.0 mL min(-1). The RP-LC method allowed quantitation over the 0.25-15.00 μg mL(-1) range for BEN. The proposed voltammetric and RP-LC methods allow a number of cost and time saving benefits. BEN was also exposed to thermal, photolytic, oxidative stress, acid-base catalyzed hydrolyses, and the stressed samples were detected by the proposed RP-LC method. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Stripping voltammetric determination of mercury(II) at antimony-coated carbon paste electrode.

    PubMed

    Ashrafi, Amir M; Vytřas, Karel

    2011-10-15

    A new procedure was elaborated to determine mercury(II) using an anodic stripping square-wave voltammetry at the antimony film carbon paste electrode (SbF-CPE). In highly acidic medium of 1M hydrochloric acid, voltammetric measurements can be realized in a wide potential window. Presence of cadmium(II) allows to separate peaks of Hg(II) and Sb(III) and apparently catalyses reoxidation of electrolytically accumulated mercury, thus allowing its determination at ppb levels. Calibration dependence was linear up to 100 ppb Hg with a detection limit of 1.3 ppb. Applicability of the method was tested on the real river water sample.

  12. Electrochemical Behavior and Voltammetric Determination of a Manganese(II) Complex at a Carbon Paste Electrode.

    PubMed

    Karastogianni, Sophia; Girousi, Stella

    2016-01-01

    Investigation of the electrochemical behavior using cyclic voltammetry and detection of [Mn(2+)(thiophenyl-2-carboxylic acid)2 (triethanolamine)] with adsorptive stripping differential pulse voltammetry. The electrochemical behavior of a manganese(II) complex [Mn(2+)(thiophenyl-2-carboxylic acid)2(triethanolamine)] (A) was investigated using cyclic and differential pulse voltammetry in an acetate buffer of pH 4.6 at a carbon paste electrode. Further, an oxidation-reduction mechanism was proposed. Meanwhile, an adsorptive stripping differential pulse voltammetric method was developed for the determination of manganese(II) complex.

  13. Detection of trace cobalt ions in in vivo plant cells using a voltammetric interlocking system.

    PubMed

    Ly, Suw Young; Shin, Myoung Ho; Lee, Chang Hyun; Lee, Jin Hui; Kim, Mi Sook; Ji, Sang Woo; Park, Dong Won

    2013-01-01

    This experiment was conducted to establish a system for detecting trace cobalt ions in water and plant tissues using a voltammetric in vivo sensor. Cyclic and stripping voltammetry was devised from hand-made, macro-type implantable three-electrode systems. The results reached micro and nano working ranges at 100 sec accumulation time. The statistical detection limit (S/N) was attained at 6.0 ng L(-1). For the in vivo application, direct assay of cobalt ions was carried out in Eichhornia crassipes (EC) deep tissue in real time with a preconcentration time of 100 s. Interfaced techniques can be interlocked with other control systems.

  14. A miniature electronic nose system based on an MWNT-polymer microsensor array and a low-power signal-processing chip.

    PubMed

    Chiu, Shih-Wen; Wu, Hsiang-Chiu; Chou, Ting-I; Chen, Hsin; Tang, Kea-Tiong

    2014-06-01

    This article introduces a power-efficient, miniature electronic nose (e-nose) system. The e-nose system primarily comprises two self-developed chips, a multiple-walled carbon nanotube (MWNT)-polymer based microsensor array, and a low-power signal-processing chip. The microsensor array was fabricated on a silicon wafer by using standard photolithography technology. The microsensor array comprised eight interdigitated electrodes surrounded by SU-8 "walls," which restrained the material-solvent liquid in a defined area of 650 × 760 μm(2). To achieve a reliable sensor-manufacturing process, we used a two-layer deposition method, coating the MWNTs and polymer film as the first and second layers, respectively. The low-power signal-processing chip included array data acquisition circuits and a signal-processing core. The MWNT-polymer microsensor array can directly connect with array data acquisition circuits, which comprise sensor interface circuitry and an analog-to-digital converter; the signal-processing core consists of memory and a microprocessor. The core executes the program, classifying the odor data received from the array data acquisition circuits. The low-power signal-processing chip was designed and fabricated using the Taiwan Semiconductor Manufacturing Company 0.18-μm 1P6M standard complementary metal oxide semiconductor process. The chip consumes only 1.05 mW of power at supply voltages of 1 and 1.8 V for the array data acquisition circuits and the signal-processing core, respectively. The miniature e-nose system, which used a microsensor array, a low-power signal-processing chip, and an embedded k-nearest-neighbor-based pattern recognition algorithm, was developed as a prototype that successfully recognized the complex odors of tincture, sorghum wine, sake, whisky, and vodka.

  15. Differential pulse voltammetric determination of acyclovir in pharmaceutical preparations using a pencil graphite electrode.

    PubMed

    Dilgin, Didem Giray; Karakaya, Serkan

    2016-06-01

    In this study, a new selective and sensitive voltammetric procedure for determination of acyclovir (ACV) was proposed using a disposable electrode, pencil graphite electrode (PGE). Cyclic and differential pulse voltammograms of ACV were recorded in Britton-Robinson buffer solution containing 0.10 M KCl with pH of 4.0 at PGE. The PGE displayed a very good electrochemical behavior with significant enhancement of the peak current compared to a glassy carbon electrode (GCE). Under experimental conditions, the PGE had a linear response range from 1.0 μM to 100.0 μM ACV with a detection limit of 0.3 μM (based on 3 Sb). Relative standard deviations of 4.8 and 3.6% were obtained for five successive determinations of 10.0 and 50.0 μM ACV, respectively, which indicate acceptable repeatability. This voltammetric method was successfully applied to the direct determination of ACV in real pharmaceutical samples. The effect of various interfering compounds on the ACV peak current was studied. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Development of Conductive Boron-Doped Diamond Electrode: A microscopic, Spectroscopic, and Voltammetric Study

    PubMed Central

    Bennet, Kevin E.; Lee, Kendall H.; Kruchowski, James N.; Chang, Su-Youne; Marsh, Michael P.; Orsow, Alexander A. Van; Paez, Aurelio; Manciu, Felicia S.

    2013-01-01

    Building on diamond characteristics such as hardness, chemical inertness and low electron emission threshold voltage, the current microscopic, spectroscopic and voltammetric investigations are directed towards improving the properties of electrode coating materials for their future use in clinical studies of deep brain stimulation via fast-scan cyclic voltammetry (FSCV). In this study we combine the capabilities of confocal Raman mapping in providing detailed and accurate analysis of local distributions of material constituents in a series of boron-doped polycrystalline diamond films grown by chemical vapor deposition, with information from the more conventional techniques of scanning electron microscopy (SEM) and infrared absorption spectroscopy. Although SEM images show a uniform distribution of film crystallites, they have the limitation of being unable to differentiate the distribution of boron in the diamond. Values of 1018–1021 atoms/cm3 of boron content have been estimated from the absorption coefficient of the 1290 cm−1 infrared absorption band and from the 500 cm−1 Raman vibration. The observed accumulation of boron atoms and carbon sp2 impurities at the grain boundaries suggests that very high doping levels do not necessarily contribute to improvement of the material’s conductivity, corroborating with voltammetric data. FSCV results also indicate an enhanced stability of analyte detection. PMID:28788420

  17. Evaluation of antimony microparticles supported on biochar for application in the voltammetric determination of paraquat.

    PubMed

    Gevaerd, Ava; de Oliveira, Paulo R; Mangrich, Antonio S; Bergamini, Márcio F; Marcolino-Junior, Luiz H

    2016-05-01

    This work describes the construction and application of carbon paste electrodes modified with biochar and antimony microparticles (SbBCPE) for voltammetric determination of paraquat using a simple and sensitive procedure based on voltammetric stripping analysis. Some parameters such as amount of biochar and antimony used in the composition of the carbon paste and instrumental parameters were examined in detail. Under optimized conditions, an analytical curve was obtained for paraquat determination employing SbBCPE, which showed a linear response ranging from 0.2 to 2.9 μmol L(-1), with limit of detection and quantification of 34 nmol L(-1) and 113 nmol L(-1), respectively, after paraquat pre-concentration of 120 s. The repeatability study presented a RSD=2.0% for 10 consecutive measurements using the same electrode surface and the reproducibility study showed a RSD=2.7% for measurements with 10 different electrode surfaces. The proposed sensor was successfully applied for paraquat determination in tap water and citric fruit juice spiked samples and good recoveries were obtained without any sample pre-treatment, showing its promising analytical performance.

  18. Voltammetric behaviour of drotaverine hydrochloride in surfactant media and its enhancement determination in Tween-20.

    PubMed

    Jain, Rajeev; Vikas; Rather, Jahangir Ahmad

    2011-02-01

    Simple, sensitive and rapid adsorptive voltammetric behaviour of drotaverine hydrochloride onto the HMDE has been explored and validated in surfactant media by using cyclic, differential pulse and square-wave voltammetry. Addition of Tween-20 to the drotaverine hydrochloride containing electrolyte enhances the reduction current signal. The voltammograms of the drug with Tween-20 in phosphate buffers of pH 2.5-11.0 exhibit a single well defined reduction peak which may be due to the reduction of -CC- group. The cyclic voltammetric studies indicated the reduction of drotaverine hydrochloride at the electrode surface through two electron irreversible step and diffusion-controlled. The peak current showed a linear dependence with the drug concentration over the range 0.8-7.2μgmL(-1). The calculated LOD and LOQ are 1.8 and 6.0ngmL(-1) by SWCAdSV and 8.1 and 27.2ngmL(-1) by DPCAdSV, respectively. The procedure was applied to the assay of the drug in tablet form with mean percentage recoveries of 100.2% with SWCAdSV and 99.7% with DPCAdSV. The validity of the proposed methods was further assessed by applying a standard addition technique.

  19. Development of Conductive Boron-Doped Diamond Electrode: A microscopic, Spectroscopic, and Voltammetric Study.

    PubMed

    Bennet, Kevin E; Lee, Kendall H; Kruchowski, James N; Chang, Su-Youne; Marsh, Michael P; Van Orsow, Alexander A; Paez, Aurelio; Manciu, Felicia S

    2013-12-06

    Building on diamond characteristics such as hardness, chemical inertness and low electron emission threshold voltage, the current microscopic, spectroscopic and voltammetric investigations are directed towards improving the properties of electrode coating materials for their future use in clinical studies of deep brain stimulation via fast-scan cyclic voltammetry (FSCV). In this study we combine the capabilities of confocal Raman mapping in providing detailed and accurate analysis of local distributions of material constituents in a series of boron-doped polycrystalline diamond films grown by chemical vapor deposition, with information from the more conventional techniques of scanning electron microscopy (SEM) and infrared absorption spectroscopy. Although SEM images show a uniform distribution of film crystallites, they have the limitation of being unable to differentiate the distribution of boron in the diamond. Values of 10(18)-10(21) atoms/cm³ of boron content have been estimated from the absorption coefficient of the 1290 cm(-1) infrared absorption band and from the 500 cm(-1) Raman vibration. The observed accumulation of boron atoms and carbon sp² impurities at the grain boundaries suggests that very high doping levels do not necessarily contribute to improvement of the material's conductivity, corroborating with voltammetric data. FSCV results also indicate an enhanced stability of analyte detection.

  20. Spectroscopic and voltammetric studies of pefloxacin bound to calf thymus double-stranded DNA.

    PubMed

    Radi, A; El Ries, M A; Kandil, S

    2005-01-01

    Spectral and electrochemical studies have been carried out on the interaction of pefloxacin with calf thymus double-stranded dsDNA. The voltammetric behavior of pefloxacin was investigated at glassy carbon, carbon paste and dsDNA-modified carbon paste electrodes using cyclic voltammetry. Pefloxacin was oxidized, yielding one irreversible oxidation peak. The modification of the carbon paste surface with dsDNA allowed an accumulation process to take place for pefloxacin such that higher sensitivity was achieved compared with the bare surface. The response was characterized with respect to ionic strength, accumulation time, pefloxacin concentration, and other variables. The stripping differential pulse voltammetric response showed a linear calibration curve in the range 1.0 x 10(-7)-1.0 x 10(-5) mol l(-1) with a detection limit of 5.0 x 10(-8) mol l(-1) at the dsDNA modified electrode. The method was applied to the direct determination of pefloxacin in diluted urine samples.

  1. Vapor permeation-stepwise injection simultaneous determination of methanol and ethanol in biodiesel with voltammetric detection.

    PubMed

    Shishov, Andrey; Penkova, Anastasia; Zabrodin, Andrey; Nikolaev, Konstantin; Dmitrenko, Maria; Ermakov, Sergey; Bulatov, Andrey

    2016-02-01

    A novel vapor permeation-stepwise injection (VP-SWI) method for the determination of methanol and ethanol in biodiesel samples is discussed. In the current study, stepwise injection analysis was successfully combined with voltammetric detection and vapor permeation. This method is based on the separation of methanol and ethanol from a sample using a vapor permeation module (VPM) with a selective polymer membrane based on poly(phenylene isophtalamide) (PA) containing high amounts of a residual solvent. After the evaporation into the headspace of the VPM, methanol and ethanol were transported, by gas bubbling, through a PA membrane to a mixing chamber equipped with a voltammetric detector. Ethanol was selectively detected at +0.19 V, and both compounds were detected at +1.20 V. Current subtractions (using a correction factor) were used for the selective determination of methanol. A linear range between 0.05 and 0.5% (m/m) was established for each analyte. The limits of detection were estimated at 0.02% (m/m) for ethanol and methanol. The sample throughput was 5 samples h(-1). The method was successfully applied to the analysis of biodiesel samples.

  2. Trace level voltammetric determination of heavy metals and total mercury in tea matrices (Camellia sinensis).

    PubMed

    Melucci, Dora; Locatelli, Marcello; Locatelli, Clinio

    2013-12-01

    An analytical procedure regarding the voltammetric determination of mercury(II), copper(II), lead(II), cadmium(II) and zinc(II) by square wave anodic stripping voltammetry (SWASV) in matrices involved in food chain is proposed. In particular, tea leaves were analyzed as real samples. The digestion of each matrix was carried out using a concentrated HCl-HNO3-H2SO4 acidic attack mixture; 0.01 mol L(-1) EDTA-Na2+ 0.15 mol L(-1) NaCl + 0.5 mol L(-1) HCl was employed as the supporting electrolyte. The voltammetric measurements were carried out using a conventional three electrode cell, employing, as working electrodes, a gold electrode (GE) and a stationary hanging mercury drop electrode (HMDE). The analytical procedure has been verified on the standard reference materials Spinach Leaves NIST-SRM 1570a, Tomato Leaves NIST-SRM 1573a and Apple Leaves NIST-SRM 1515. For all the elements, the precision as repeatability, expressed as relative standard deviation (sr) was of the order of 3-5%, while the trueness, expressed as relative error (e) was of the order of 3-7%. Once set up on the standard reference materials, the analytical procedure was applied to commercial tea leaves samples. A critical comparison with spectroscopic measurements is also discussed.

  3. TRACE LEVEL VOLTAMMETRIC DETERMINATION OF HEAVY METALS AND TOTAL MERCURY IN TEA MATRICES (Camellia sinensis).

    PubMed

    Melucci, Dora; Locatelli, Marcello; Locatelli, Clinio

    2013-10-24

    An analytical procedure regarding the voltammetric determination of mercury(II), copper(II), lead(II), cadmium(II) and zinc(II) by square wave anodic stripping voltammetry (SWASV) in matrices involved in food chain is proposed. In particular, tea leaves were analysed as real samples. The digestion of each matrix was carried out using a concentrated HCl-HNO3-H2SO4 acidic attack mixture; 0.01 mol L(-1) EDTA-Na2 + 0.15 mol L(-1) NaCl + 0.5 mol L(-1) HCl was employed as the supporting electrolyte. The voltammetric measurements were carried out using a conventional three electrode cell, employing, as working electrodes, a gold electrode (GE) and a stationary hanging mercury drop electrode (HMDE). The analytical procedure has been verified on the standard reference materials Spinach Leaves NIST-SRM 1570a, Tomato Leaves NIST-SRM 1573a and Apple Leaves NIST-SRM 1515. For all the elements, the precision as repeatability, expressed as relative standard deviation (sr) was of the order of 3-5 %, while the trueness, expressed as relative error (e) was of the order of 3-7 %. Once set up on the standard reference materials, the analytical procedure was applied to commercial tea leaves samples. A critical comparison with spectroscopic measurements is also discussed.

  4. Voltammetric Determination of the Herbicide Linuron Using a Tricresyl Phosphate-Based Carbon Paste Electrode

    PubMed Central

    Đorđević, Jelena; Papp, Zsigmond; Guzsvány, Valéria; Švancara, Ivan; Trtić-Petrović, Tatjana; Purenović, Milovan; Vytřas, Karel

    2012-01-01

    This paper summarises the results of voltammetric studies on the herbicide 3-(3,4-dichlorophenyl)-1-methoxy-1-methylurea (Linuron), using a carbon paste electrode containing tricresyl phosphate (TCP-CPE) as liquid binder. The principal experimental conditions, such as the pH effect, investigated in Britton-Robinson buffer solutions (pH 2.0–7.0), the peak characteristics for the analyte of interest, or instrumental parameters for the differential pulse voltammetric mode were optimized for the method. As found out, the best electroanalytical performance of the TCP-CPE was achieved at pH 2.0, whereby the oxidation peak of Linuron appeared at ca. +1.3 V vs. SCE. The analytical procedure developed offers good linearity in the concentration range of 1.25–44.20 μg mL−1 (1.77 × 10−4–5.05 × 10−6 mol L−1), showing—for the first time—the applicability of the TCP-CPE for anodic oxidations in direct voltammetry (without accumulation). The method was then verified by determining Linuron in a spiked river water sample and a commercial formulation and the results obtained agreed well with those obtained by the reference HPLC/UV determination. PMID:22368461

  5. Voltammetric studies on the electrochemical determination of methylmercury in chloride medium at carbon microelectrodes.

    PubMed

    Ribeiro, F; Neto, M M M; Rocha, M M; Fonseca, I T E

    2006-10-10

    Electroanalytical techniques have been used to determine methylmercury at low levels in environmental matrices. The electrochemical behaviour of methylmercury at carbon microelectrodes in a hydrochloric acid medium using cyclic, square wave and fast-scan linear-sweep voltammetric techniques has been investigated. The analytical utility of the methylmercury reoxidation peak has been explored, but the recorded peak currents were found to be poorly reproducible. This is ascribed to two factors: the adsorption of insoluble chloromercury compounds on the electrode surface, which appears to be an important contribution to hinder the voltammetric signal of methylmercury; and the competition between the reoxidation of the methylmercury radical and its dimerization reaction, which limits the reproducibility of the methylmercury peak. These problems were successfully overcome by adopting the appropriate experimental conditions. Fast-scan rates were employed and an efficient electrochemical regeneration procedure of the electrode surface was achieved, under potentiostatic conditions in a mercury-free solution containing potassium thiocyanate--a strong complexing agent. The influence of chloride ion concentration was analysed. Interference by metals, such as lead and cadmium, was considered. Calibration plots were obtained in the micromolar and submicromolar concentration ranges, allowing the electrochemical determination of methylmercury in trace amounts. An estuarine water sample was analysed using the new method with a glassy carbon microelectrode.

  6. Voltammetric determination of dopamine at a zirconium phosphated silica gel modified carbon paste electrode.

    PubMed

    Shams, Esmaeil; Babaei, Ali; Taheri, Ali Reza; Kooshki, Mojtaba

    2009-06-01

    Zirconium phosphated amorphous silica gel (devoted briefly as Si-ZrPH) modified carbon paste electrode (CPE) was used for detection of dopamine (DA) in the presence of ascorbic acid (AA) and uric acid (UA). Cyclic voltammetry demonstrated improved reversibility of the DA on the modified electrode. Cyclic voltammetry of Fe(CN)(6)(3-/4-) as a negatively charged probe revealed that the surface of the Si-ZrPH modified CPE surface had a high density of negative charge. As a result, the modified carbon paste electrode could inhibit the voltammetric response of AA and UA while the redox reaction of dopamine was promoted. Based on this, a selective method has been developed to detect DA in the presence of 2500 and 1000 time higher concentration of AA and UA, respectively. The effect of various experimental parameters on the voltammetric response of dopamine was investigated. Under the chosen conditions, the differential pulse voltammetry peak current was found to be linear with DA concentration in the ranges of 0.04 to 50 microM and 50 to 400 microM. The detection limit of the proposed method in the presence of 100 microM of AA and 40 microM of UA was found to be 0.02 microM for DA determination. Satisfying results are achieved when detecting the DA in injection and human serum samples.

  7. Voltammetric determination of copper in selected pharmaceutical preparations--validation of the method.

    PubMed

    Lutka, Anna; Maruszewska, Małgorzata

    2011-01-01

    It were established and validated the conditions of voltammetric determination of copper in pharmaceutical preparations. The three selected preparations: Zincuprim (A), Wapń, cynk, miedź z wit. C (B), Vigor complete (V) contained different salts and different quantity of copper (II) and increasing number of accompanied ingredients. For the purpose to transfer copper into solution, the samples of powdered tablets of the first and second preparation were undergone extraction and of the third the mineralization procedures. The concentration of copper in solution was determined by differential pulse voltammetry (DP) using comparison with standard technique. In the validation process, the selectivity, accuracy, precision and linearity of DP determination of copper in three preparations were estimated. Copper was determined within the concentration range of 1-9 ppm (1-9 microg/mL): the mean recoveries approached 102% (A), 100% (B), 102% (V); the relative standard deviations of determinations (RSD) were 0.79-1.59% (A), 0.62-0.85% (B) and 1.68-2.28% (V), respectively. The mean recoveries and the RSDs of determination satisfied the requirements for the analyte concentration at the level 1-10 ppm. The statistical verification confirmed that the tested voltammetric method is suitable for determination of copper in pharmaceutical preparation.

  8. Copper(II) complexes of prion protein PEG11-tetraoctarepeat fragment: spectroscopic and voltammetric studies.

    PubMed

    Bonomo, Raffaele P; Di Natale, Giuseppe; Rizzarelli, Enrico; Tabbì, Giovanni; Vagliasindi, Laura I

    2009-04-14

    Spectroscopic (UV-Vis and EPR) and voltammetric studies have been carried out on the copper(II) complexes with the Ac-PEG11-(PHGGGWGQ)4-NH2 (L) polypeptide. In the ratios Cu : L 3 : 1 and 4 : 1, the two [Cu3(L)H(-6)] and [Cu4(L)H(-8)] complex species have been characterized at neutral pH values. All the copper atoms occupy similar coordination sites formed by imidazole, peptidic nitrogen atoms and carbonyl oxygen atoms in a square base pyramidal geometry. Voltammetric measurements on these systems point out the cooperativity in the electron transfer processes among the copper(II) sites during their reduction. NO interaction with these polynuclear copper species is characterized by the reduction of the copper sites through the formation of two different intermediate complex species. When an excess of the Ac-PEG11-(PHGGGWGQ)4-NH2 ligand is considered, frozen solution EPR parameters and UV-Vis spectroscopic data identify the [Cu(N(im))4]2+ chromophore, which does not interact with NO.

  9. Electrochemical investigation of the voltammetric determination of hydrochlorothiazide using a nickel hydroxide modified nickel electrode.

    PubMed

    Machini, Wesley B S; David-Parra, Diego N; Teixeira, Marcos F S

    2015-12-01

    The preparation and electrochemical characterization of a nickel hydroxide modified nickel electrode as well as its behavior as electrocatalyst toward the oxidation of hydrochlorothiazide (HCTZ) were investigated. The electrochemical behavior of the modified electrode and the electrooxidation of HCTZ were explored using cyclic voltammetry. The voltammetric response of the modified electrode in the detection of HCTZ is based on the electrochemical oxidation of the Ni(II)/Ni(III) and a chemical redox process. The analytical parameters for the electrooxidation of HCTZ by the nickel hydroxide modified nickel electrode were obtained in NaOH solution, in which the linear voltammetric response was in the concentration range from 1.39×10(-5) to 1.67×10(-4)mol L(-1) with a limit of detection of 7.92×10(-6)mol L(-1) and a sensitivity of 0.138 μA Lmmol(-1). Tafel analysis was used to elucidate the kinetics and mechanism of HCTZ oxidation by the modified electrode.

  10. Electrooxidation of New Synthetic Cannabinoids: Voltammetric Determination of Drugs in Seized Street Samples and Artificial Saliva.

    PubMed

    Dronova, Marina; Smolianitski, Evgeny; Lev, Ovadia

    2016-04-19

    The electrochemical sensing of new psychoactive substances, synthetic cannabinoids (SCs), commonly marketed under the trade name "Spice" is explored for the first time. The electrooxidative transformations of 11 new indole and indazole SCs which are currently the predominant illicit smoking mixtures on the drug market is performed using cyclic and differential pulse voltammetry with various commercially available electrodes (Pt, GC, Bdd). It is found that SCs exhibit voltammetric responses that can be used for their detection in smoking mixtures and artificial saliva with limits of detection in the nanomolar range. The indole-based SCs exhibited an anodic peak at ∼1.5 V (vs Ag/Ag(+)) and ∼1.2 V (vs Ag/AgCl) in acetonitrile and artificial saliva, respectively, and the indazoles exhibited corresponding peaks at ∼1.7 V and ∼1.5 V. The voltammetric procedure was evaluated by prescreening of SCs in 12 confiscated street samples that were also independently analyzed by GC-MS and LC-MS techniques. A good agreement between the three analytical protocols was found. Voltammetry provides a tool for the prescreening of synthetic cannabinoid derivatives in seized materials and biological samples.

  11. Cathodic stripping voltammetric determination of doxazosin in urine and pharmaceutical tablets using carbon paste electrodes.

    PubMed

    Arranz, A; Fernández de Betoño, S; Moreda, J M; Cid, A; Arranz, J F

    1997-08-01

    Several voltammetric techniques were used to explore the reductive behaviour of the antihypertensive agent doxazosin on a bare carbon paste (CPE) and a Tenax-modified carbon paste electrode (TMCPE). The results indicate that the process is irreversible and fundamentally controlled by adsorption, which allows doxazosin to be accumulated at the electrode surface. The cathodic adsorptive stripping (AdS) response was evaluated with respect to pH, accumulation variables and instrumental parameters, using differential-pulse (DPV) and square-wave voltammetry (SWV) as redissolution techniques. In both cases, a voltammetric peak close to 0 V in Britton-Robinson buffer (pH 6.6) was obtained after a preconcentration step at 0.55 V for 3 min (2000 rpm) and a subsequent cathodic scan. When the TMCPE was used, the limits of detection were 4.35 x 10(-11) and 5.18 x 10(-11) M for AdS-DPV and AdS-SWV, respectively. The deposition time (3 min) was improved relative to that obtained by means of CPE (6 min). Under the optimum operational conditions, the doxazosin reduction peak showed a linear response in the range from 6 x 10(-11) to 1 x 10(-9) M by using AdS-DPV, with an RSD of 3.39% for 3 x 10(-8) M doxazosin solution (n = 10). A method was developed for the determination of doxazosin in human urine and formulations.

  12. Computational approach to the rational design of molecularly imprinted polymers for voltammetric sensing of homovanillic acid.

    PubMed

    Diñeiro, Yolanda; Menéndez, M Isabel; Blanco-López, M Carmen; Lobo-Castañón, M Jesús; Miranda-Ordieres, Arturo J; Tuñón-Blanco, Paulino

    2005-10-15

    A methodology based on density functional theory calculations for the design of molecularly imprinted polymers (MIPs) is described. The method allows the rational choice of the most suitable monomer and polymerization solvent among a set of chemicals traditionally used in MIP formulations for the molecular imprinting of a given template. It is based on the comparison of the stabilization energies of the prepolymerization adducts between the template and different functional monomers. The effect of the polymerization solvent is included using the polarizable continuum model. A voltammetric sensor for homovanillic acid was constructed using different MIPs as recognition element, confirming that the solvent (toluene) and functional monomer (methacrylic acid) selected according to the theoretical predictions lead to the most efficient molecular recognition sensing phase. With the voltammetric sensor prepared using the MIP designed according to the theoretical predictions, a linear response for concentrations of homovanillic acid between 5 x 10(-8) and 1 x 10(-5) M can be obtained. The limit of detection is 7 x 10(-9) M. The selectivity obtained for homovanillic acid over other structurally related compounds buttresses the validity of this strategy of design.

  13. Technological Barriers in the Use of Electrochemical Microsensors and Microbiosensors for in vivo Analysis of Neurological Relevant Substances

    PubMed Central

    Bucur, Bogdan

    2012-01-01

    In this paper is presented an overview of the technological barriers faced by the in vivo brain analysis with microelectrodes. Numerous microsensors and enzymatic microbiosensors have been developed for the real time monitoring of neurotransmitters, neuromodulators, drugs and diverse other biological relevant substances. A clear understanding of the working principle, advantages and limitations is essential for the acquisition of valid data in neurological investigations. Some of the aspects presented here refer to: microelectrode insertion and positioning related to possibilities to minimize tissue damage, spatial and temporal resolution of the measurements, actual controversies in data interpretation and sensor calibration, simultaneous detection of multiple analytes, interferences and state of the art in the development of wireless devices. PMID:23449399

  14. Technological Barriers in the Use of Electrochemical Microsensors and Microbiosensors for in vivo Analysis of Neurological Relevant Substances.

    PubMed

    Bucur, Bogdan

    2012-09-01

    In this paper is presented an overview of the technological barriers faced by the in vivo brain analysis with microelectrodes. Numerous microsensors and enzymatic microbiosensors have been developed for the real time monitoring of neurotransmitters, neuromodulators, drugs and diverse other biological relevant substances. A clear understanding of the working principle, advantages and limitations is essential for the acquisition of valid data in neurological investigations. Some of the aspects presented here refer to: microelectrode insertion and positioning related to possibilities to minimize tissue damage, spatial and temporal resolution of the measurements, actual controversies in data interpretation and sensor calibration, simultaneous detection of multiple analytes, interferences and state of the art in the development of wireless devices.

  15. Mapping urban air quality in real-time: Applications of crowdsourced microsensor data

    NASA Astrophysics Data System (ADS)

    Schneider, Philipp; Castell, Nuria; Vogt, Matthias; Lahoz, William; Bartonova, Alena

    2017-04-01

    crowdsourced network of low-cost microsensors in conjunction with model information is able to provide realistic high-resolution maps of urban air quality. Comparisons with observations made at air quality monitoring stations equipped with reference instruments show that the resulting maps are able to replicate the average true NO2 measurements with a root mean squared error of 14.3 μg/m3 and an R2 value of 0.89. In addition, we show that the resulting maps are able to replicate the typical bi-modal diurnal cycle related to traffic emissions. Detailed urban air quality maps such as those derived from data fusion techniques can then further be used for providing personalized information about air quality to the citizens. We present examples of how this kind of real-time data allows end users to find the currently least polluted route through a city or to track their individual personal exposure to air pollutants while moving through the urban environment.

  16. Cathodic Voltammetric Behavior of Pillar[5]quinone in Nonaqueous Media. Symmetry Effects on the Electron Uptake Sequence.

    PubMed

    Cheng, Beijun; Kaifer, Angel E

    2015-08-12

    The cathodic voltammetric behavior of pillar[5]quinone was investigated in dichloromethane solution. Our data show that the symmetry of the macrocycle has a pronounced effect on the electron uptake sequence. The uptake of the first five electrons follows a 2-1-2 pattern, and only a total of eight electrons could be injected into the macrocycle under our experimental conditions.

  17. Anodic voltammetric behavior and determination of rosiglitazone in pharmaceutical dosage forms and biological fluids on solid electrode.

    PubMed

    Dogan-Topal, Burcu; Tuncel, Secil; Ozkan, Sibel A

    2010-09-01

    The anodic voltammetric behavior and electroanalytical determination of rosiglitazone was studied using cyclic, linear sweep, differential pulse and square wave voltammetric techniques on glassy carbon electrode. The oxidation of rosiglitazone was irreversible and exhibited diffusion controlled process depending on pH. Different parameters were tested to optimize the conditions for the determination of the oxidation mechanism of rosiglitazone. The dependence of current intensities and potentials on pH, concentration, scan rate, nature of the buffer was also investigated. According to the linear relationship between the peak current and the concentration, differential pulse and square wave voltammetric methods for rosiglitazone assay in pharmaceutical dosage forms and biological fluids were developed. A linear response was obtained within the range of 1x10-6M - 6x10-5M in 0.1 M H2SO4 and acetate buffer at pH 5.70 for both voltammetric methods in human serum samples. The practical analytical value of the method is demonstrated by quantitative determination of rosiglitazon in pharmaceutical formulation and human serum, without the need for separation or complex sample preparation, since there was no interference from the excipients and endogenous substances. The methods were fully validated and successfully applied to the high throughput determination of the drug in tablets and human serum with good recoveries.

  18. A VOLTAMMETRIC FLAVIN MICROELECTRODE FOR USE IN BIOFILMS

    PubMed Central

    Nguyen, Hung Duc; Renslow, Ryan; Babauta, Jerome; Ahmed, Bulbul; Beyenal, Haluk

    2011-01-01

    Biofilms used in bioelectrochemical systems are expected to transfer electrons using electron transfer mediators. One mediator type, flavins, which includes flavin mononucleotide, riboflavin, and flavin adenine dinucleotide, has been found to be endogenously produced by Shewanella oneidensis MR-1. However, the presence and concentration of flavins inside a S. oneidensis MR-1 biofilm have never been reported. The goal of this study was to develop a flavin microelectrode capable of measuring flavins inside a living biofilm and apply it to a biofilm which produces flavins. Because flavins are electrochemically active molecules, the flavin microelectrode was based on detection via square-wave voltammetry. The microelectrode consisted of a carbon working electrode with a 10–30 μm tip diameter, a built-in platinum counter electrode, and a Ag/AgCl reference electrode, all enclosed in a glass outer case. The microelectrode was calibrated between 0.1 μM and 10 μM flavins and showed a linear correlation between flavin concentration and peak currents located at −424 mVAg/AgCl on a square-wave voltammogram. We also developed a model to explain the electrochemical mechanism of flavin detection, and to determine the effective surface area of the microelectrode, the standard reduction potential, and the transfer coefficient. We found that the effective surface area of the microelectrode was close to 100 times the projected surface area. The model predicted a standard reduction potential for RF/RFH2 of −419 mVAg/AgCl at 20 °C and a transfer coefficient of 0.45. Lastly, we measured flavin concentration inside a S. oneidensis MR-1 biofilm grown on a glass surface using oxygen as the electron acceptor. The flavin concentration reached 0.7 μM, increasing near the bottom of the biofilm, where no oxygen was present. This shows the possibility that flavins are produced in the anaerobic zone to act as intermediate electron acceptors in the deeper parts of the biofilm, where

  19. Development of boron-doped diamond thin-films as voltammetric and amperometric detectors

    NASA Astrophysics Data System (ADS)

    Xu, Jishou

    2000-10-01

    The utilization of boron-doped diamond thin-films for applications in electroanalysis was investigated. Voltammetric analysis in static solution, and amperometric detection coupled with flow injection analysis and HPLC were performed. The results were compared to those for glassy carbon. The electroactivity, the merit of detection figures, the adsorption of polar organic molecules, and the resistance to fouling were studied. Surface characterization was performed to elucidate the surface property-electroacticvity relationship. The results showed that diamond thin-films, compared with glassy carbon, had comparable electroactivity to simple electron transfer processes (e.g., Ru(NH3)6+2/+3, Fe(CN)6 -3/-4, IrCl6-2/-3, azide, chlorpromazine), but had lower electroactivity for the electron transfer processes involving surface-confined intermediate (e.g., hydrogen evolution, oxygen evolution, 4-methyl catechol, hydrazine). The diamond thin-films had a wide working potential up to 4.0 V in aqueous media. They also had small double layer capacitance, voltammetric background current, and amperometric residual current. These properties had leaded to higher signal-to-background ratios and signal-to-noise ratios. The diamond thin-films had lower limits of detection in voltammetric measurements of several analytes, and had lower limits of detection in amperometric measurements of all compounds studied. The diamond thin-films had negligible adsorption of polar organic molecules (e.g., anthraquinone 2,6-disulfonate, chlorpromazine), compared to glassy carbon. This is due to the fact that the diamond surfaces are primarily composed of sp3 carbon and hydrogen terminated. This leaded to less decay of the electroactivity by storage and operation, and higher resistance to fouling. The surface property-electroactivity relationship depends on the specific mechanism for electron transfer. The extent of non-diamond impurities (e.g., oxygen evolution), diamond crystalline size, surface

  20. Carbon Paste Electrode Modified With Cuo–Nanoparticles as a Probe for Square Wave Voltammetric Determination of Atrazine

    PubMed Central

    Rahbar, Nadereh; Parham, Hooshang

    2013-01-01

    Background Atrazine (ATZ) is a widely used herbicide in most countries because of its low cost and good selectivity. The concentration of ATZ that the EPA considers safe to consume in drinking water is 3 ppb. Therefore, recently, there have been concerns about its determination in trace levels. This compound is not electro-active, so in this research indirect electrochemical method for its detection in low levels was proposed. Objectives The main aim of this study is the indirect determination of ATZ in water samples by voltammetry using nano-particle modified electrode. Materials and Methods A nano-CuO modified carbon paste electrode (NMCPE) is constructed and its application for indirect square wave voltammetric (SWV) detection of ATZ is reported. The sensing performance mechanism of the nano-CuO modified carbon paste electrode toward atrazine is due to complexation of the analyte with Cu (II) ion. The peak current for copper (II) reduction decreases with increase in the ATZ concentration and is monitored for its determination. Instrumental and chemical parameters influencing the detection of ATZ were optimized. Results The results revealed that decrease in peak current was proportional to ATZ concentration over the range of 5-75 ng/mL. The limit of detection (LOD) and limit of quantification (LOQ) were 2 ng/mL and 5.6 ng/mL (n = 20), respectively. The relative standard deviation (n = 10) for the determination of 10 and 50 ng/mL of ATZ solution was estimated as 4.9% and 4.2 %, respectively. Conclusions This easily fabricated electrode together with the fast and sensitive SW voltammetry was successfully applied for the determination of concentration of ATZ at trace levels, in different water samples. PMID:24624200

  1. A Flexible Three-in-One Microsensor for Real-Time Monitoring of Internal Temperature, Voltage and Current of Lithium Batteries

    PubMed Central

    Lee, Chi-Yuan; Peng, Huan-Chih; Lee, Shuo-Jen; Hung, I-Ming; Hsieh, Chien-Te; Chiou, Chuan-Sheng; Chang, Yu-Ming; Huang, Yen-Pu

    2015-01-01

    Lithium batteries are widely used in notebook computers, mobile phones, 3C electronic products, and electric vehicles. However, under a high charge/discharge rate, the internal temperature of lithium battery may rise sharply, thus causing safety problems. On the other hand, when the lithium battery is overcharged, the voltage and current may be affected, resulting in battery instability. This study applies the micro-electro-mechanical systems (MEMS) technology on a flexible substrate, and develops a flexible three-in-one microsensor that can withstand the internal harsh environment of a lithium battery and instantly measure the internal temperature, voltage and current of the battery. Then, the internal information can be fed back to the outside in advance for the purpose of safety management without damaging the lithium battery structure. The proposed flexible three-in-one microsensor should prove helpful for the improvement of lithium battery design or material development in the future. PMID:25996509

  2. A Flexible Three-in-One Microsensor for Real-Time Monitoring of Internal Temperature, Voltage and Current of Lithium Batteries.

    PubMed

    Lee, Chi-Yuan; Peng, Huan-Chih; Lee, Shuo-Jen; Hung, I-Ming; Hsieh, Chien-Te; Chiou, Chuan-Sheng; Chang, Yu-Ming; Huang, Yen-Pu

    2015-05-19

    Lithium batteries are widely used in notebook computers, mobile phones, 3C electronic products, and electric vehicles. However, under a high charge/discharge rate, the internal temperature of lithium battery may rise sharply, thus causing safety problems. On the other hand, when the lithium battery is overcharged, the voltage and current may be affected, resulting in battery instability. This study applies the micro-electro-mechanical systems (MEMS) technology on a flexible substrate, and develops a flexible three-in-one microsensor that can withstand the internal harsh environment of a lithium battery and instantly measure the internal temperature, voltage and current of the battery. Then, the internal information can be fed back to the outside in advance for the purpose of safety management without damaging the lithium battery structure. The proposed flexible three-in-one microsensor should prove helpful for the improvement of lithium battery design or material development in the future.

  3. Indirect voltammetric detection of fluoride ions in toothpaste on a comb-shaped interdigitated microelectrode array.

    PubMed

    Cernanská, Monika; Tomcík, Peter; Jánosíková, Zuzana; Rievaj, Miroslav; Bustin, Dusan

    2011-02-15

    A novel technique based on dynamic electrochemistry for the detection of fluoride ions was developed. It is based on its strong complexation with ferric ion. Formed fluoroferric complex is cathodically inactive at the potential of the reduction of free ferric aquo ion. The voltammetric and amperometric response of platinum comb-shaped interdigitated microelectrode array is decreased after fluoride addition. This decrease serves for the quantification of fluoride ions added to the solution. The detection limit of 4.5×10(-5) mol dm(-3) was achieved when one of the segments of interdigitated microelectrode array (IDA) was used as an indicating electrode. The detection limit is about one order of magnitude lower than in the case of conventional platinum macroelectrode. In comparison with ISE electrodes this method is faster and also avoiding large error resulting from the antilogarithmization of ISE Nerstian response. The method was applied to the analysis of toothpaste.

  4. Modified Carbon Nanotube Paste Electrode for Voltammetric Determination of Carbidopa, Folic Acid, and Tryptophan

    PubMed Central

    Esfandiari Baghbamidi, Sakineh; Beitollahi, Hadi; Karimi-Maleh, Hassan; Soltani-Nejad, Somayeh; Soltani-Nejad, Vahhab; Roodsaz, Sara

    2012-01-01

    A simple and convenient method is described for voltammetric determination of carbidopa (CD), based on its electrochemical oxidation at a modified multiwall carbon nanotube paste electrode. Under optimized conditions, the proposed method exhibited acceptable analytical performances in terms of linearity (over the concentration range from 0.1 to 700.0 μM), detection limit (65.0 nM), and reproducibility (RSD = 2.5%) for a solution containing CD. Also, square wave voltammetry (SWV) was used for simultaneous determination of CD, folic acid (FA), and tryptophan (TRP) at the modified electrode. To further validate its possible application, the method was used for the quantification of CD, FA, and TRP in urine samples. PMID:22666634

  5. Synthesis and application of a molecularly imprinted polymer for the voltammetric determination of famciclovir.

    PubMed

    El Gohary, Nesrine Abdelrehim; Madbouly, Adel; El Nashar, Rasha Mohamed; Mizaikoff, Boris

    2015-03-15

    A molecularly imprinted polymer (MIP) was synthesized and applied as additive within a carbon paste electrode for the cyclic voltammetric determination of famciclovir (FCV). Complementary computational studies were performed to study the intermolecular interactions in the pre-polymerization mixture. Derived from the computational studies, four MIP ratios were synthesized and their performance was evaluated using equilibrium rebinding assays. The MIP with the highest binding capacity was selected. A linear response was obtained in the range of 2.5×10(-6)-1.0×10(-3)M with a limit of detection at 7.5×10(-7)M. Finally, the developed MIP-voltammetry system was successfully applied for the determination of FCV in pure solutions and pharmaceutical preparations.

  6. Detection of the peanut allergen Ara h 6 in foodstuffs using a voltammetric biosensing approach.

    PubMed

    Alves, Rita C; Pimentel, Filipa B; Nouws, Henri P A; Correr, Wagner; González-García, María Begoña; Oliveira, M Beatriz P P; Delerue-Matos, Cristina

    2015-09-01

    A voltammetric biosensor for Ara h 6 (a peanut allergen) detection in food samples was developed. Gold nanoparticle-modified screen-printed carbon electrodes were used to develop a sandwich-type immunoassay using two-monoclonal antibodies. The antibody-antigen interaction was detected through the electrochemical detection of enzymatically deposited silver. The immunosensor presented a linear range between 1 and 100 ng/ml, as well as high precision (inter-day RSD ≤9.8%) and accuracy (recoveries ≥96.7%). The detection and quantification limits were 0.27 and 0.88 ng/ml, respectively. It was possible to detect small levels of Ara h 6 in complex food matrices.

  7. Development of a voltammetric electronic tongue for discrimination of edible oils.

    PubMed

    Oliveri, Paolo; Baldo, M Antonietta; Daniele, Salvatore; Forina, Michele

    2009-10-01

    In this paper, we propose a novel strategy to perform cyclic voltammetric measurements with a platinum microelectrode directly in edible oil samples. The microelectrode was employed as an electronic tongue that, along with the application of chemometrics to the current-potential responses, proved useful for discriminating oils on the basis of their quality and geographical origin. The method proposed here is based on the use of suitable room temperature ionic liquids, added to oils as supporting electrolytes to provide conductivity to the low-polarity samples. The entire voltammograms, recorded directly on the oil/RTIL mixtures, were processed via principal component analysis and a classification technique (K nearest neighbors), to extract information on samples characteristics. Data processing showed that oils having different nature (i.e. maize and olive) or geographical origin (i.e. olive oils coming from different regions) can be distinguished.

  8. Unsupervised pattern recognition methods in ciders profiling based on GCE voltammetric signals.

    PubMed

    Jakubowska, Małgorzata; Sordoń, Wanda; Ciepiela, Filip

    2016-07-15

    This work presents a complete methodology of distinguishing between different brands of cider and ageing degrees, based on voltammetric signals, utilizing dedicated data preprocessing procedures and unsupervised multivariate analysis. It was demonstrated that voltammograms recorded on glassy carbon electrode in Britton-Robinson buffer at pH 2 are reproducible for each brand. By application of clustering algorithms and principal component analysis visible homogenous clusters were obtained. Advanced signal processing strategy which included automatic baseline correction, interval scaling and continuous wavelet transform with dedicated mother wavelet, was a key step in the correct recognition of the objects. The results show that voltammetry combined with optimized univariate and multivariate data processing is a sufficient tool to distinguish between ciders from various brands and to evaluate their freshness.

  9. Anodic adsorptive stripping voltammetric determination of the anesthetic drug: methohexital sodium.

    PubMed

    Farghaly, O A; El-Wadood, H M; Ghandour, M A

    1999-11-01

    Methohexital (MS) determination is based on the formation of insoluble mercury salt on a hanging mercury drop electrode after preaccumulation by adsorption. This property was exploited in developing a highly sensitive stripping voltammetric procedure for the determination of the drug. The anodic current of adsorbed compound is measured by linear sweep anodic stripping voltammetry (LSASV), preceded by a period of preconcentration. The effect of various parameters such as supporting electrolyte composition, pH, initial potential, scan rate, accumulation time and ionic strength are discussed to characterize the interfacial and redox behavior. The detection limit was found to be 2x10(-7) M (56.8 ppb) with 180-s accumulation time. The interference of some amino acids, ascorbic acid and some metal ions was investigated. The application of this method was tested in the determination of methohexital in spiked urine samples. The precision of the method is satisfactory with a relative standard deviation of 2.5%.

  10. Cathodic adsorptive stripping voltammetric determination of uranium with potassium hydrogen phthalate.

    PubMed

    Farghaly, O A; Ghandour, M A

    1999-06-01

    The adsorption properties of dioxouranium (II)-Phathalate complexes onto hanging mercury drop electrode are exploited in developing a highly sensitive and selective stripping voltammetric procedure for the determination of uranium (VI). The reduction current of adsorbed complex ions of U(VI) was measured by both linear sweep (LSCSV) and differential pulse cathodic stripping voltammetry (DPCSV), preceded by a period of preconcentration onto the electrode surface. As low as 2x10(-9) mol dm(-3) (0.5 mug/l) and 2x10(-8) mol dm(-3) (4.8 mug/l) with accumulation time 240 and 120 s using DPCSV and LSCSV, respectively, have been determined successfully. The relative standard deviation of 2.2% at the 5 ppm level was obtained. The interferences of some metal ions and anions were studied. The application of this method was tested in the determination of uranium in superphosphate fertilizer.

  11. Sensitive Voltammetric Determination of Natural Flavonoid Quercetin on a Disposable Graphite Lead

    PubMed Central

    Vu, Dai Long; Žabčíková, Simona; Ertek, Bensu; Dilgin, Yusuf

    2015-01-01

    Summary In this paper, a pencil graphite electrode was pretreated using chronoamperometry technique in phosphate buffer solution (pH=7.0) for sensitive determination of quercetin. Oxidation of quercetin was investigated using pretreated pencil graphite electrode and anodic stripping differential pulse voltammetry. Under optimal conditions, the anodic current of quercetin exhibited linear response to its concentration in the range from 0.001 to 1.5 µmol/L with the limit of detection of 0.3·10–3 µmol/L. The proposed method was successfully applied for the determination of quercetin in cranberry and blackcurrant juices with recovery rate from 93.2 to 94.7%. Solid-phase extraction was found to be necessary prior to voltammetric determination of quercetin in fruit juice samples using pretreated pencil graphite electrode. PMID:27904372

  12. A self-polishing platinum ring voltammetric sensor and its application to complex media.

    PubMed

    Cavanillas, Santiago; Winquist, Fredrik; Eriksson, Mats

    2015-02-15

    A self-polishing voltammetric sensor was recently developed and has been applied to samples of urea, milk and sewage water. The polishing device continuously grinds a platinum ring electrode, offering a reproducible and clean electrode surface. Principal component analysis (PCA) and partial least squares (PLS) techniques were applied to interpret the data and to build prediction models. In an evaluation of samples with different urea concentrations, the grinding step allows for repeatable measurements, similar to those after electrochemical cleaning. Furthermore, for the determination of sewage water concentrations in drinking water and for the evaluation of different fat contents in milk samples, the polishing eliminates sensor drift produced by electrode fouling. The results show that the application of a self-polishing unit offers a promising tool for electrochemical studies of difficult analytes and complex media. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Anodic stripping tin titration: a method for the voltammetric determination of platinum at trace levels.

    PubMed

    Giussani, Barbara; Roncoroni, Simone; Nemenyi, Anna; Dal Santo, Vladimiro; Monticelli, Damiano; Recchia, Sandro

    2014-07-01

    We propose here a novel voltammetric method for the determination of platinum at trace levels. The method is based on the interference that platinum generates on the anodic stripping signal of tin acidic solutions: in appropriate conditions platinum uses the intermediate formation of tin(II) ions, taking place during the tin cathodic reduction, to reduce itself and to form mixed Pt(II)-Sn(II) chloro-complexes. From the analysis of the anodic stripping plots obtained after subsequent additions of tin in a Pt-containing solution, it is possible to quantify accurately and precisely the Pt concentration from 3 ppb to more than 10 ppm. This novel method is validated for the analysis of Pt in heterogeneous catalysts, but in principle could be extended to other matrixes.

  14. Voltammetric Behaviour of Sulfamethoxazole on Electropolymerized-Molecularly Imprinted Overoxidized Polypyrrole.

    PubMed

    Ozkorucuklu, Sabriye Perçin; Sahin, Yücel; Alsancak, Güleren

    2008-12-18

    In this work, preparation of a molecularly imprinted polymer (MIP) film and its recognition properties for sulfamethoxazolewere investigated. The overoxidized polypyrrole (OPPy) film was prepared by the cyclic voltammetric deposition of pyrrole (Py) in the presence of supporting electrolyte (tetrabutylammonium perchlorate-TBAP) with and without a template molecule (sulfamethoxazole) on a pencil graphite electrode (PGE). The voltammetric behaviour of sulfamethoxazole on imprinted and non-imprinted (NIP) films was investigated by differential pulse voltammetry (DPV) in Britton-Robinson (BR) buffer solutions prepared in different ratio of acetonitrile-water binary mixture, between the pH 1.5 and 7.0. The effect of the acetonitrile-water ratio and pH, monomer and template concentrations, electropolymerization cycles on the performance of the MIP electrode was investigated and optimized. The MIP electrode exhibited the best reproducibility and highest sensitivity. The results showed that changing acetonitrile-water ratio and pH of BR buffer solution changes the oxidation peak current values. The highest anodic signal of sulfamethoxazole was obtained in BR buffer solution prepared in 50% (v/v) acetonitrile-water at pH 2.5. The calibration curve for sulfamethoxazole at MIP electrode has linear region for a concentration range of 25.10(-3) to 0.75 mM (R²=0.9993). The detection limit of sulfamethoxazole was found as 3.59.10(-4) mM (S/N=3). The same method was also applied to determination of sulfamethoxazole in commercial pharmaceutical samples. Method precision (RSD87%) were satisfactory. The proposed method is simple and quick. The polypyrrole (PPy) electrodes have low response time, good mechanical stability and are disposable simple to construct.

  15. Discrimination of Apple Liqueurs (Nalewka) Using a Voltammetric Electronic Tongue, UV-Vis and Raman Spectroscopy

    PubMed Central

    Śliwińska, Magdalena; Garcia-Hernandez, Celia; Kościński, Mikołaj; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek; Śliwińska-Bartkowiak, Małgorzata; Jurga, Stefan; Garcia-Cabezon, Cristina; Rodriguez-Mendez, Maria Luz

    2016-01-01

    The capability of a phthalocyanine-based voltammetric electronic tongue to analyze strong alcoholic beverages has been evaluated and compared with the performance of spectroscopic techniques coupled to chemometrics. Nalewka Polish liqueurs prepared from five apple varieties have been used as a model of strong liqueurs. Principal Component Analysis has demonstrated that the best discrimination between liqueurs prepared from different apple varieties is achieved using the e-tongue and UV-Vis spectroscopy. Raman spectra coupled to chemometrics have not been efficient in discriminating liqueurs. The calculated Euclidean distances and the k-Nearest Neighbors algorithm (kNN) confirmed these results. The main advantage of the e-tongue is that, using PLS-1, good correlations have been found simultaneously with the phenolic content measured by the Folin–Ciocalteu method (R2 of 0.97 in calibration and R2 of 0.93 in validation) and also with the density, a marker of the alcoholic content method (R2 of 0.93 in calibration and R2 of 0.88 in validation). UV-Vis coupled with chemometrics has shown good correlations only with the phenolic content (R2 of 0.99 in calibration and R2 of 0.99 in validation) but correlations with the alcoholic content were low. Raman coupled with chemometrics has shown good correlations only with density (R2 of 0.96 in calibration and R2 of 0.85 in validation). In summary, from the three holistic methods evaluated to analyze strong alcoholic liqueurs, the voltammetric electronic tongue using phthalocyanines as sensing elements is superior to Raman or UV-Vis techniques because it shows an excellent discrimination capability and remarkable correlations with both antioxidant capacity and alcoholic content—the most important parameters to be measured in this type of liqueurs.  PMID:27735832

  16. Discrimination of Apple Liqueurs (Nalewka) Using a Voltammetric Electronic Tongue, UV-Vis and Raman Spectroscopy.

    PubMed

    Śliwińska, Magdalena; Garcia-Hernandez, Celia; Kościński, Mikołaj; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek; Śliwińska-Bartkowiak, Małgorzata; Jurga, Stefan; Garcia-Cabezon, Cristina; Rodriguez-Mendez, Maria Luz

    2016-10-09

    The capability of a phthalocyanine-based voltammetric electronic tongue to analyze strong alcoholic beverages has been evaluated and compared with the performance of spectroscopic techniques coupled to chemometrics. Nalewka Polish liqueurs prepared from five apple varieties have been used as a model of strong liqueurs. Principal Component Analysis has demonstrated that the best discrimination between liqueurs prepared from different apple varieties is achieved using the e-tongue and UV-Vis spectroscopy. Raman spectra coupled to chemometrics have not been efficient in discriminating liqueurs. The calculated Euclidean distances and the k-Nearest Neighbors algorithm (kNN) confirmed these results. The main advantage of the e-tongue is that, using PLS-1, good correlations have been found simultaneously with the phenolic content measured by the Folin-Ciocalteu method (R² of 0.97 in calibration and R² of 0.93 in validation) and also with the density, a marker of the alcoholic content method (R² of 0.93 in calibration and R² of 0.88 in validation). UV-Vis coupled with chemometrics has shown good correlations only with the phenolic content (R² of 0.99 in calibration and R² of 0.99 in validation) but correlations with the alcoholic content were low. Raman coupled with chemometrics has shown good correlations only with density (R² of 0.96 in calibration and R² of 0.85 in validation). In summary, from the three holistic methods evaluated to analyze strong alcoholic liqueurs, the voltammetric electronic tongue using phthalocyanines as sensing elements is superior to Raman or UV-Vis techniques because it shows an excellent discrimination capability and remarkable correlations with both antioxidant capacity and alcoholic content-the most important parameters to be measured in this type of liqueurs.

  17. Voltammetric Behaviour of Sulfamethoxazole on Electropolymerized-Molecularly Imprinted Overoxidized Polypyrrole

    PubMed Central

    Özkorucuklu, Sabriye Perçin; Şahin, Yücel; Alsancak, Güleren

    2008-01-01

    In this work, preparation of a molecularly imprinted polymer (MIP) film and its recognition properties for sulfamethoxazole were investigated. The overoxidized polypyrrole (OPPy) film was prepared by the cyclic voltammetric deposition of pyrrole (Py) in the presence of supporting electrolyte (tetrabutylammonium perchlorate-TBAP) with and without a template molecule (sulfamethoxazole) on a pencil graphite electrode (PGE). The voltammetric behaviour of sulfamethoxazole on imprinted and non-imprinted (NIP) films was investigated by differential pulse voltammetry (DPV) in Britton-Robinson (BR) buffer solutions prepared in different ratio of acetonitrile-water binary mixture, between the pH 1.5 and 7.0. The effect of the acetonitrile-water ratio and pH, monomer and template concentrations, electropolymerization cycles on the performance of the MIP electrode was investigated and optimized. The MIP electrode exhibited the best reproducibility and highest sensitivity. The results showed that changing acetonitrile-water ratio and pH of BR buffer solution changes the oxidation peak current values. The highest anodic signal of sulfamethoxazole was obtained in BR buffer solution prepared in 50% (v/v) acetonitrile-water at pH 2.5. The calibration curve for sulfamethoxazole at MIP electrode has linear region for a concentration range of 25.10-3 to 0.75 mM (R2=0.9993). The detection limit of sulfamethoxazole was found as 3.59.10-4 mM (S/N=3). The same method was also applied to determination of sulfamethoxazole in commercial pharmaceutical samples. Method precision (RSD<1%) and recoveries (>87%) were satisfactory. The proposed method is simple and quick. The polypyrrole (PPy) electrodes have low response time, good mechanical stability and are disposable simple to construct. PMID:27873996

  18. A disposable voltammetric cell for determining the titratable acidity in vinegar.

    PubMed

    Kotani, Akira; Miyaguchi, Yuji; Harada, Dai; Kusu, Fumiyo

    2003-11-01

    A disposable voltammetric cell using three pencil leads as working, reference, and counter electrodes was developed for determining the titratable acidity, i.e. the acid content in vinegar. The materials of the pencil leads were graphite-reinforcement carbons (GRCs). A voltammetric determination of acid was made by measuring the reduction prepeak current of 3,5-di-t-butyl-1,2-benzoquinone (DBBQ) due to the presence of acids in unbuffered solution. The potential stability of the pseudo-reference electrode of GRC was examined. The prepeak current was found to be proportional to the acetic acid concentration from 0.05 to 2.7 mM with a correlation coefficient of 0.999. The cell-to-cell reproducibility for 1 mM acetic acid was evaluated with ten individual disposable cells. The RSD of the prepeak current and the SD of the prepeak potential were 2.56% and 0.008, respectively. The titratable acidity in five vinegar samples was determined by voltammetry using disposable cells and compared with that of the titratable acidity determined by the conventional potentiometric titration method. We then observed the results by both methods, and found a correlation coefficient of 0.972. As such, the voltammetry using disposable-cell required only one thousandth the volume of a vinegar sample for the titration method. The disposable cell was superior to the conventional electrochemical cell, in terms of facility, environment-friendly, and economy, and thus a sensor using the present cell would be useful for routine work in the quality control of vinegar.

  19. In-Situ Measurement of High-Temperature Proton Exchange Membrane Fuel Cell Stack Using Flexible Five-in-One Micro-Sensor.

    PubMed

    Lee, Chi-Yuan; Weng, Fang-Bor; Kuo, Yzu-Wei; Tsai, Chao-Hsuan; Cheng, Yen-Ting; Cheng, Chih-Kai; Lin, Jyun-Ting

    2016-10-18

    In the chemical reaction that proceeds in a high-temperature proton exchange membrane fuel cell stack (HT-PEMFC stack), the internal local temperature, voltage, pressure, flow and current nonuniformity may cause poor membrane material durability and nonuniform fuel distribution, thus influencing the performance and lifetime of the fuel cell stack. In this paper micro-electro-mechanical systems (MEMS) are utilized to develop a high-temperature electrochemical environment-resistant five-in-one micro-sensor embedded in the cathode channel plate of an HT-PEMFC stack, and materials and process parameters are appropriately selected to protect the micro-sensor against failure or destruction during long-term operation. In-situ measurement of the local temperature, voltage, pressure, flow and current distributions in the HT-PEMFC stack is carried out. This integrated micro-sensor has five functions, and is favorably characterized by small size, good acid resistance and temperature resistance, quick response, real-time measurement, and the goal is being able to be put in any place for measurement without affecting the performance of the battery.

  20. In-Situ Measurement of High-Temperature Proton Exchange Membrane Fuel Cell Stack Using Flexible Five-in-One Micro-Sensor

    PubMed Central

    Lee, Chi-Yuan; Weng, Fang-Bor; Kuo, Yzu-Wei; Tsai, Chao-Hsuan; Cheng, Yen-Ting; Cheng, Chih-Kai; Lin, Jyun-Ting

    2016-01-01

    In the chemical reaction that proceeds in a high-temperature proton exchange membrane fuel cell stack (HT-PEMFC stack), the internal local temperature, voltage, pressure, flow and current nonuniformity may cause poor membrane material durability and nonuniform fuel distribution, thus influencing the performance and lifetime of the fuel cell stack. In this paper micro-electro-mechanical systems (MEMS) are utilized to develop a high-temperature electrochemical environment-resistant five-in-one micro-sensor embedded in the cathode channel plate of an HT-PEMFC stack, and materials and process parameters are appropriately selected to protect the micro-sensor against failure or destruction during long-term operation. In-situ measurement of the local temperature, voltage, pressure, flow and current distributions in the HT-PEMFC stack is carried out. This integrated micro-sensor has five functions, and is favorably characterized by small size, good acid resistance and temperature resistance, quick response, real-time measurement, and the goal is being able to be put in any place for measurement without affecting the performance of the battery. PMID:27763559

  1. OPTIMIZATION OF VOLTAMMETRIC METHODS FOR AN IN SITU DETERMINATION OF TOTAL SULFIDE IN ANOXIC POREWATER USING A MERCURY PLATED GOLD ELECTRODE

    EPA Science Inventory

    Voltammetric methods for determination of total sulfide concentrations in anoxic sediments utilizing a previously described [1] gold-based mercury amalgam microelectrode were optimized. Systematic studies in NaCl (supporting electrolyte) and porewater indicate variations in ionic...

  2. OPTIMIZATION OF VOLTAMMETRIC METHODS FOR AN IN SITU DETERMINATION OF TOTAL SULFIDE IN ANOXIC POREWATER USING A MERCURY PLATED GOLD ELECTRODE

    EPA Science Inventory

    Voltammetric methods for determination of total sulfide concentrations in anoxic sediments utilizing a previously described [1] gold-based mercury amalgam microelectrode were optimized. Systematic studies in NaCl (supporting electrolyte) and porewater indicate variations in ionic...

  3. Voltammetric investigation of oxidation of zuclopenthixol and application to its determination in dosage forms and in drug dissolution studies.

    PubMed

    Sentürk, Z; Ozkan, S A; Ozkan, Y; Aboul-Enein, H Y

    2000-03-01

    The oxidative voltammetric behaviour of zuclopenthixol (ZPT) at a glassy carbon has been studied using cyclic, linear sweep and differential pulse voltammetry. Oxidation of the drug produced three pH dependent anodic steps (representing an irreversible oxidation). Using differential pulse voltammetry, the drug yielded a well-defined voltammetric response in phosphate buffer, pH 5.2 at + 0.82 V (vs. Ag/AgCl). This process could be used to determine ZPT concentrations in the range 8 x 10(-7)-2 x 10(-4) M. The method was applied, without any interferences from the excipients, to the determination of the drug in tablets and oral drops, and in drug dissolution studies.

  4. The effect of an electrical double layer on the voltammetric performance of nanoscale interdigitated electrodes: a simulation study.

    PubMed

    Yang, Xiaoling; Zhang, Guigen

    2008-11-19

    Finite-element based computational simulation is performed to investigate the effect of an electrical double layer (EDL) on the electrochemical processes of nanometer-scale interdigitated electrodes (nano-IDEs). Results show that the EDL structure will alter the voltammetric current response of nano-IDEs due to the expansion of the diffuse layer into the diffusion layer at the electrode surfaces and the overlap of the electrical fields of the neighboring electrodes. The EDL induced change in the voltammetric current response is more severe for nano-IDEs with a smaller electrode size and gap spacing, and the EDL effect is influenced by the compact layer thickness, the charge valence of the redox species, the electron transfer rate, and the absence of the supporting electrolyte.

  5. Selenocystine modified screen-printed electrode as an alternative sensor for the voltammetric determination of metal ions.

    PubMed

    Puy-Llovera, Jaume; Pérez-Ràfols, Clara; Serrano, Núria; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

    2017-12-01

    A novel selenium based screen-printed electrode was developed based on the immobilization of selenocystine on aryl diazonium salt monolayers anchored to a carbon-nanofiber screen-printed electrode support (SeCyst-SPCNFE). SeCyst-SPCNFE was analytically compared to a screen-printed carbon nanofiber electrode modified with L-Cystine (Cyst-SPCNFE) for the determination of Pb(II) and Cd(II) by stripping voltammetric techniques. Their analytical performance suggests that SeCyst-SPCNFE could be a much better alternative for metal ion determination at trace levels than Cyst-SPCNFE. The proposed electrode was successfully applied for the simultaneous voltammetric determination of trace Pb(II) and Cd(II) in a wastewater reference material with a very high reproducibility (3.2%) and good trueness (2.6%). Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Simultaneous voltammetric determination of nitrate and nitrite ions using a copper electrode pretreated by dissolution/redeposition.

    PubMed

    Shariar, Shovon Mohammad; Hinoue, Teruo

    2010-01-01

    Nitrate and nitrite ions were found to be successfully electroreduced at an in situ electrochemically pretreated copper electrode in acidic media, and their reduction peaks of a cyclic voltammogram were found at two distinct electrode potentials. Cyclic voltammetric experiments revealed a highly sensitive behavior of the pretreated copper electrode upon the electroreduction of nitrate and nitrite ions, and showed that a simultaneous voltammetric determination of the ions was achievable. Differential pulse voltammetry (DPV) was applied to the simultaneous determination. As a result, the detection limits were 0.26 and 0.17 µmol dm(-3) for nitrate and nitrite ions, respectively. Simultaneous determinations for real samples (river water) were carried out by DPV at the pretreated copper electrode and spectrophotometry (the Griess method). The determination values obtained by both methods were in a good agreement with each other.

  7. Denitrification, Dissimilatory Reduction of Nitrate to Ammonium, and Nitrification in a Bioturbated Estuarine Sediment as Measured with 15N and Microsensor Techniques

    PubMed Central

    Binnerup, Svend Jørgen; Jensen, Kim; Revsbech, Niels Peter; Jensen, Mikael Hjorth; Sørensen, Jan

    1992-01-01

    Nitrogen and oxygen transformations were studied in a bioturbated (reworked by animals) estuarine sediment (Norsminde Fjord, Denmark) by using a combination of 15N isotope (NO3-), specific inhibitor (C2H2), and microsensor (N2O and O2) techniques in a continuous-flow core system. The estuarine water was NO3- rich (125 to 600 μM), and NO3- was consistently taken up by the sediment on the four occasions studied. Total NO3- uptake (3.6 to 34.0 mmol of N m-2 day-1) corresponded closely to N2 production (denitrification) during the experimental steady state, which indicated that dissimilatory, as well as assimilatory, NO3- reduction to NH4+ was insignificant. When C2H2 was applied in the flow system, denitrification measured as N2O production was often less (58 to 100%) than the NO3- uptake because of incomplete inhibition of N2O reduction. The NO3- formed by nitrification and not immediately denitrified but released to the overlying water, uncoupled nitrification, was calculated both from 15NO3- dilution and from changes in NO3- uptake before and after C2H2 addition. These two approaches gave similar results, with rates ranging between 0 and 8.1 mmol of N m-2 day-1 on the four occasions. Attempts to measure total nitrification activity by the difference between NH4+ fluxes before and after C2H2 addition failed because of non-steady-state NH4+ fluxes. The vertical distribution of denitrification and oxygen consumption was studied by use of N2O and O2 microelectrodes. The N2O profiles measured during the experimental steady state were often irregularly shaped, and the buildup of N2O after C2H2 was added was much too fast to be described by a simple diffusion model. Only bioturbation by a dense population of infauna could explain these observations. This was corroborated by the relationship between diffusive and total fluxes, which showed that only 19 to 36 and 29 to 62% of the total O2 uptake and denitrification, respectively, were due to diffusion-reaction processes at

  8. Development of Voltammetric Double-Polymer-Modified Electrodes for Nanomolar Ion Detection for Environmental and Biological Applications

    NASA Astrophysics Data System (ADS)

    Kim, Yushin

    Qualitative and quantitative electrochemical methods for trace ion analysis of organic and inorganic species with environmental and biological attention have been developed and reported during past decades. The development of fast and accurate electrochemical methods is critical for field applications with various blocking contaminants. Voltammetric method is attractive not only to analyze selective ion species due to its characteristic based on ion lipophilicity, but also to lower the limit of detection by combining with stripping analysis. In my PhD work, I have developed and studied a highly selective and sensitive electrochemical method that can be used to characterize fundamental transport dynamics and to develop electrochemical sensors at liquid/liquid interfaces based on electrochemically-controlled ion transfer and recognition. The understanding of the kinetic and thermodynamic properties of the voltammetric ion transfer through polymer-modified ion-selective electrodes leads to realize the highly selective and sensitive analytical method. The ultrathin polymer membrane is used to maximize a current response by complete exhaustion of preconcentrated ions. Therefore, nanomolar detection is achieved and confirmed by a thermodynamic mechanism that controls the detection limit. It was also demonstrated experimentally and theoretically that more lipophilic ionic species gives a significantly lower detection limit. The voltammetric method was expanded into inexpensive and disposable applications based on pencil lead modified with the thin polymer membrane. In the other hand, micropipet/nanopipet voltammetry as an artificial cell membrane was used to study the interface between two immiscible solutions for environmental and biomedical applications. It is very useful to get quantitative kinetic and thermodynamic information by studying numerical simulations of ion transfer and diffusion. Molecular recognition and transport of heparin and low

  9. Voltammetric method for determining the trace moisture content of organic solvents based on hydrogen-bonding interactions with quinones.

    PubMed

    Hui, Yanlan; Chng, Elaine Lay Khim; Chua, Louisa Pei-Lyn; Liu, Wan Zhen; Webster, Richard D

    2010-03-01

    Voltammetry experiments were performed on the natural quinone, vitamin K(1) (VK(1)), in a range of organic solvents of varying dielectric constant that are commonly used for electrochemical measurements [dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), acetonitrile (MeCN), propionitrile (EtCN), butyronitrile (PrCN), 1,2-dichloroethane (DCE), dichloromethane (DCM), and 1,1,2,2-tetrachloroethane (TCE)]. The water content of the solvents was accurately measured using Karl Fischer (KF) coulometric titrations, and the voltammetric data were used to estimate the degree of hydrogen-bonding interactions between the reduced forms of VK(1) and variable levels of water, thereby allowing a ranking of water-substrate interactions in the different solvents. The voltammetric data were analyzed based on interactions that occur between reduced forms of VK(1) and the water, the solvent, and the supporting electrolyte. Calibration data were obtained that are independent of the nature of the reference electrode and allow the water content of the solvents to be calculated by performing a single voltammetric scan in the presence of VK(1) and 0.2 M supporting electrolyte (Bu(4)NPF(6)).

  10. A new method based on the Butler-Volmer formalism to evaluate voltammetric cation and anion sensors.

    PubMed

    Cano, Manuel; Rodríguez-Amaro, Rafael; Fernández Romero, Antonio J

    2008-12-11

    A new method based on the Butler-Volmer formalism is applied to assess the capability of two voltammetric ion sensors based on polypyrrole films: PPy/DBS and PPy/ClO4 modified electrodes were studied as voltammetric cation and anion sensors, respectively. The reversible potential versus electrolyte concentrations semilogarithm plots provided positive calibration slopes for PPy/DBS and negative ones for PPy/ClO4, as was expected from the proposed method and that based on the Nernst equation. The slope expressions deduced from Butler-Volmer include the electron-transfer coefficient, which allows slope values different from the ideal Nernstian value to be explained. Both polymeric films exhibited a degree of ion-selectivity when they were immersed in mixed-analyte solutions. Selectivity coefficients for the two proposed voltammetric cation and anion sensors were obtained by several experimental methods, including the separated solution method (SSM) and matched potential method (MPM). The K values acquired by the different methods were very close for both polymeric sensors.

  11. Thermoelectric infrared microsensors based on a periodically suspended thermopile integrating nanostructured Ge/SiGe quantum dots superlattice

    SciTech Connect

    Ziouche, K. E-mail: Zahia.bougrioua@iemn.univ-lille1.fr; Bougrioua, Z. E-mail: Zahia.bougrioua@iemn.univ-lille1.fr; Lejeune, P.; Lasri, T.; Leclercq, D.; Savelli, G.; Hauser, D.; Michon, P.-M.

    2014-07-28

    This paper presents an original integration of polycrystalline SiGe-based quantum dots superlattices (QDSL) into Thermoelectric (TE) planar infrared microsensors (μSIR) fabricated using a CMOS technology. The nanostructuration in QDSL results into a considerably reduced thermal conductivity by a factor up to 10 compared to the one of standard polysilicon layers that are usually used for IR sensor applications. A presentation of several TE layers, QDSL and polysilicon, is given before to describe the fabrication of the thermopile-based sensors. The theoretical values of the sensitivity to irradiance of μSIR can be predicted thanks to an analytical model. These findings are used to interpret the experimental measurements versus the nature of the TE layer exploited in the devices. The use of nanostructured QDSL as the main material in μSIR thermopile has brought a sensitivity improvement of about 28% consistent with theoretical predictions. The impact of QDSL low thermal conductivity is damped by the contribution of the thermal conductivity of all the other sub-layers that build up the device.

  12. A highly sensitive Pb(Zr,Ti)O3 thin film ultrasonic micro-sensor with a grooved diaphragm.

    PubMed

    Matsushima, Tomoaki; Xiong, Sibei; Kawada, Hiroshi; Yamanaka, Hiroshi; Muralt, Paul

    2007-12-01

    A highly sensitive piezoelectric ultrasonic micro-sensor with a grooved multilayer membrane was developed by a Si-based MEMS technique. The groove was located at one-quarter of the distance away from the edge of the membrane and opened into piezoelectric layer. The piezoelectric layer Pb(Zr,Ti)O(3) (PZT) was 2.2 microm thick and was prepared by a sol-gel method. The prepared PZT film was pure perovskite and showed a highly (100) textured structure. The sensitivity of the fabricated piezoelectric ultrasonic sensor without the groove structure was 100 microV/Pa. In comparison, the sensitivity of the ultrasonic sensor with the groove structure was about 500 microV/Pa, which is 5 times that without the groove structure. The diaphragm having grooves showed a corrugate-like structure that was formed by residual stress. The high sensitivity of the membrane with the grooved diaphragm is considered to relate to the corrugate-like structure.

  13. Electrochemical properties of silver-copper alloy microelectrodes for use in voltammetric field apparatus.

    PubMed

    Skogvold, Silje M; Mikkelsen, Oyvind; Billon, Gabriel; Garnier, Cedric; Lesven, Ludovic; Barthe, Jean-Francois

    2006-04-01

    Microelectrodes of silver-copper alloys have been evaluated for use in voltammetric analyses. Increased overpotential towards the hydrogen overvoltage reaction (HER) was found as a function of increased copper content in the silver. A study of oxidizing products by cyclic voltammetry (CV) in NaOH solution showed ten anodic and eight cathodic peaks which are described in the present paper. The behaviour of these alloy electrodes is somewhere between pure silver and pure copper electrodes. Differential pulse anodic stripping voltammetry (DPASV) was used to measure zinc, cadmium and lead in ultrapure water only (18 MOmegacm), and good linearity was found for all metals (r (2)=0.998) in the range of 0.5 to 5 ppb with a 600- to 1,200-s plating time. It was additionally found that cadmium and lead were better separated on the alloy electrodes compared to pure silver electrodes. Measurements of nickel were carried out on alloy electrodes by use of adsorptive differential pulse cathodic stripping voltammetry (Ad-DPCSV), and good linearity (r (2)=1.000) was found in the range from 0.5 to 5 ppb with an adsorption time of 120 s. The alloy electrodes were also found to be sensitive to nitrate, and good linearity (r (2)=0.997) was found in the range from 1 mg L(-1) to 100 mg L(-1) using differential pulse voltammetry (DPV) scanning from -450 mV to -1,500 mV. Addition of nitrate in ultrapure water afforded two different peaks related to the successive reductions of nitrate and nitrite. In ammonium buffer solution (pH 8.6) only one peak resulting from reduction of nitrate was observed. Furthermore, the use of alloy electrodes containing 17% Cu was tested in real samples, by installing it in a voltammetric system for monitoring of zinc and lead in a polluted river, the river Deûle, near the town of Douai in northern France. Results were found to be in agreement with parallel measurements carried out by ICP-MS.

  14. Stripping voltammetric determination of palladium, platinum and rhodium in freshwater and sediment samples from South African water resources.

    PubMed

    van der Horst, C; Silwana, B; Iwuoha, E; Somerset, V

    2012-01-01

    Stripping voltammetry as technique has proved to be very useful in the analysis of heavy and other metal ions due to its excellent detection limits and its sensitivity in the presence of different metal species or interfering ions. Recent assessments of aquatic samples have shown increased levels of platinum group metals (PGMs) in aquatic ecosystems, caused by automobile exhaust emissions and mining activities. The development of an analytical sensor for the detection and characterisation of PGMs were investigated, since there is an ongoing need to find new sensing materials with suitable recognition elements that can respond selectively and reversibly to specific metal ions in environmental samples. The work reported shows the successful application of another mercury-free sensor electrode for the determination of platinum group metals in environmental samples. The work reported in this study entails the use of a glassy carbon electrode modified with a bismuth film for the determination of platinum (Pt(2+)), palladium (Pd(2+)) or rhodium (Rh(2+)) by means of adsorptive cathodic stripping voltammetry. Optimised experimental conditions included composition of the supporting electrolyte, complexing agent concentration, deposition potential, deposition time and instrumental voltammetry parameters for Pt(2+), Pd(2+) and Rh(2+) determination. Adsorptive differential pulse stripping voltammetric measurements for PGMs were performed in the presence of dimethylglyoxime (DMG) as complexing agent. The glassy carbon bismuth film electrode (GC/BiFE) employed in this study exhibit good and reproducible sensor characteristics. Application of GC/BiFE sensor exhibited well-defined peaks and highly linear behaviour for the stripping analysis of the PGMs in the concentration range between 0 and 3.5 μg/L. The detection limit of Pd, Pt and Rh was found to be 0.12 μg/L, 0.04 μg/L and 0.23 μg/L, respectively for the deposition times of 90 s (Pd) and 150 s (for both Pt and Rh). Good

  15. Redox speciation and biogeochemical gradients: Assessing spatial niches and monitoring dynamics in natural systems with voltammetric microelectrodes

    NASA Astrophysics Data System (ADS)

    Druschel, G. K.; Lorenson, G. W.; Eastmann, D. A.; Macalady, J. L.

    2005-12-01

    Biogeochemical gradients may be described by the spatial distribution of redox species distributed in water, where overlap of electron donors and acceptors out of equilibrium defines available sources of potential energy and essentially determines possible microbial metabolisms. Observed changes in redox speciation along a gradient associated with microbial biofilms may additionally provide some environmental basis for assessing physiology of sampled microorganisms. Voltammetric microelectrodes have been used in a variety of environments to describe the links between ecology and geochemistry (Luther et al., 2001). Recent work in Yellowstone National Park hydrothermal waters, the Frassassi caves in central Italy (a sulfidic cave system), and Green Lake in New York (a meromictic lake) have expanded our abilities to use microelectrodes for assessing As(III) concentrations and uncovering more details of sulfur speciation in a wide range of natural waters. We are using these data to design redox-specific culture media, make inferences about microbial physiology, constrain biogeochemical gradients over very fine scales, and observe dynamics in biogeochemical systems. Describing microbial communities and the geochemical environments that surround them at appropriate scales is of importance to begin assessing the links between microbial activity and geochemical cycling. Diversity in an environment may be better assessed if we first know how many different geochemical environments there are in that environment and if the microbial ecology in those environments is essentially independent from environments neighboring it. Because microelectrodes measure multiple redox species simultaneously and do so in matter of seconds, they are also useful in monitoring the dynamics of a biogeochemical system, which will be of use in studying the response of communities to perturbation. We will present results showing the characterization of lateral and vertical gradients over different

  16. Relative reactivity of dihydropyridine derivatives to electrogenerated superoxide ion in DMSO solutions: a voltammetric approach.

    PubMed

    Oriz, María Eugenia; Núñez-Vergara, Luis Joaquin; Squella, Juan Arturo

    2003-02-01

    To evaluate the reaction of a large series of pharmacologically significant 1,4-dihydropyridine (1,4-DHP) compounds with superoxide (O2.-) in dimethylsulfoxide using differential pulse voltammetry and controlled potential electrolysis. Differential pulse voltammetry was used to track the consumption of O2.-, and controlled potential electrolysis was used to electrogenerate O2.-. With the addition of 1,4-DHP, the oxidation peak current of O2.- decreased concentration dependently, suggesting that 1,4-DHP reacts with O2.-, that is, 1,4-DHP scavenges O2.- in dimethylsulfoxide. very easy and direct voltammetric procedure to study the relative reactivity of different 1,4-DHP with O2.- is proposed. Using the proposed method we have found that all commercial 1,4-DHP reacts with O2.-. The following order of rates was obtained: felodipine > or = vitamin E > isradipine > nimodipine > furnidipine > nitrendipine > nisoldipine > nifedipine. Furthermore, it was demonstrated that the hydrogen at the N-position of 1,4-DHP compounds could be released as a proton in the presence of O2.-, thus the electrogenerated O2.- worked as a proton acceptor to 1,4-DHP.

  17. Stripping voltammetric determination of indapamide in serum at castor oil-based carbon paste electrodes.

    PubMed

    Radi, A

    2001-01-01

    The diuretic drug indapamide has been characterized voltammetrically at carbon paste electrodes by means of cyclic and differential pulse voltammetry. An adsorptive stripping method at carbon paste electrode modified with castor oil for trace determination of indapamide was described. A study of the variation of the peak current with solution variables such as pH, ionic strength, concentration of indapamide, possible interference, and instrumental variables such as scan rate, pulse amplitude, preconcentration time, accumulation potential, paste composition has resulted in the optimization of the oxidation signal for analytical purposes. By anodic stripping differential pulse voltammetry, the calibration plot was linear in the range 5 x 10(-8) x 10(-7) M with a detection limit of 5 x 10(-9) M at carbon paste electrode modified with castor oil in pH 4.0. The preconcentration medium-exchange approach was utilized for selective determination of indapamide in spiked serum. A detection limit of 15 ng ml(-1) was obtained for dilute serum sample after 3 min accumulation and medium-exchange procedure.

  18. Adsorptive cathodic stripping voltammetric determination of dexamethasone in formulations and biological fluids.

    PubMed

    Ghoneim, Enass M; El-Attar, Mona A; Ghoneim, Mohamed M

    2009-01-01

    The electrochemical behavior of dexamethasone at a hanging mercury drop electrode (HMDE) in a universal buffer series of pH 2-10 was studied using cyclic voltammetry. Based on the interfacial adsorptive character of dexamethasone onto the HMDE (electrode surface coverage = 1.4 x 10(-10) mol/cm2), a fully validated simple square-wave adsorptive cathodic stripping voltammetric method is described for its determination in bulk form with a limit of detection (LOD) of 3.1 x 10(-9) M. The described method was successfully applied to analysis of dexamethasone in its pharmaceutical formulations (deltasone tablets and fortecortin ampule) and in spiked samples of human urine, bovine urine, and protein-free bovine milk. The achieved LODs of dexamethasone in human urine, bovine urine, and protein-free bovine milk were 1.5 x 10(-8), 2 x 10(-8), and 9 x 10(-9) M, respectively. The mean percentage recoveries of 4 x 10(-7) M dexamethasone in bulk form, spiked human urine, bovine urine, and bovine milk, based on the average of 3 replicate measurements, were 99.8 +/- 0.25, 100.4 +/- 0.96, 99.6 +/- 0.79, and 100.1 +/- 0.26, respectively.

  19. Monitoring dissolved orthophosphate in a struvite precipitation reactor with a voltammetric electronic tongue.

    PubMed

    Aguado, Daniel; Barat, Ramón; Soto, Juan; Martínez-Mañez, Ramón

    2016-10-01

    This study demonstrates the feasibility of using a voltammetric electronic tongue to monitor effluent dissolved orthophosphate concentration in a struvite precipitation reactor. The electrochemical response of the electronic tongue to the presence of orthophosphate in samples collected from the effluent of the precipitation reactor is used to predict orthophosphate concentration via a statistical model based on Partial Least Squares (PLS) Regression. PLS predictions were suitable for this monitoring application in which precipitation efficiencies higher than 80% (i.e., effluent dissolved orthophosphate concentrations lower than 40mg P-PO4(3-) L(-1)) could be considered as indicator of good process performance. The electronic tongue consisted of a set of metallic (noble and non-noble) electrodes housed inside a stainless steel cylinder which was used as the body of the electronic tongue system. Fouling problems were prevented via a simple mechanical polishing of the electrodes. The measurement of each sample with the electronic tongue was done in less than 3s. Conductivity of the samples only affected the electronic tongue marginally, being the main electrochemical response due to the orthophosphate concentration in the samples. Copper, silver, iridium and rhodium were the electrodes that exhibited noticeable response correlated with the dissolved orthophosphate concentration variations, while gold, platinum and especially cobalt and nickel were the less useful electrodes for this application.

  20. Voltammetric determination of zinc in compound pharmaceutical preparations--validation of method.

    PubMed

    Lutka, Anna; Bukowska, Honorata

    2009-01-01

    The conditions of voltammetric determination of zinc in compound pharmaceutical preparations were established and validated. The three investigated preparations (Organic zinc (A), Calcium, zinc, copper with vitamin C (B), Vigor complete (V) contained different salts of zinc (II) and increasing number of other components. The samples of powdered tablets of each preparation were undergone mineralization or extraction procedures for the purpose to transfer the zinc ions into solution. The concentration of zinc in solution was determined by differential pulse voltammetry (DP). The selectivity, accuracy, precision and linearity of DP determination of zinc in three preparations were estimated in validation process. Zinc was determined within the concentration range of 1-12 ppm (1-12 microg/mL): the mean recoveries approached 96-99% (A), 96-102% (B), 106% (V); the relative standard deviations of determinations (RSD) were 2,97-2,98% (A), 2,83-3,84% (B) and 2,65% (V). The mean recoveries and the errors of determination satisfied the requirements for the analyte concentration at the level 1-20 ppm (12).

  1. Voltammetric detection of cadmium ions at glutathione-modified gold electrodes.

    PubMed

    Chow, Edith; Hibbert, D Brynn; Gooding, J Justin

    2005-06-01

    An electrochemical sensor for the detection of cadmium ions is described using immobilized glutathione as a selective ligand. First, a self-assembled monolayer of 3-mercaptopropionic acid (MPA) was formed on a gold electrode. The carboxyl terminus then allowed attachment of glutathione (GSH)via carbodiimide coupling to give the MPA-GSH modified electrode. A cadmium ion forms a complex with glutathione via the free sulfhydryl group and also to the carboxyl groups. The complexed ion is reduced by linear and Osteryoung square wave voltammetry with a detection limit of 5 nM. The effect of the kinetics of accumulation of cadmium on the measured current was investigated and modeled. Increasing the temperature of accumulation and electrochemical analysis caused an increase in the voltammetric peak of approximately 4% per degrees C around room temperature. The modified electrode could be regenerated, being stable for more than 16 repeated uses and more than two weeks if used once a day. Some interference from Pb(2+) and Cu(2+) was observed but the effects of Zn(2+), Ni(2+), Cr(3+) and Ba(2+) were insignificant.

  2. Electrodeposited apatite coating for solid-phase microextraction and sensitive indirect voltammetric determination of fluoride ions.

    PubMed

    Mao, Yuehong; Chen, Yufei; Chu, Lin; Zhang, Xiaoli

    2013-10-15

    Electrodeposition was used to prepare a new solid phase microextraction (SPME) coatings. Two apatite SPME coatings, dicalcium phosphate dihydrate (DCPD or brushite) and hydroxyapatite (HAP) were validly and homogeneously one-step electrodeposited on glassy carbon electrode (GCE) under different conditions. The coatings were characterized by XRD, FTIR, SEM, CV and EIS. The apatite SPME coatings showed excellent and selective adsorbability to fluoride ions. A novel indirect voltammetric strategy for sensitive detection of fluoride was proposed using K3Fe(CN)6 as indicating probe. The detection principle of fluoride ions was based on the increment of steric hindrance after fluoride adsorption, which resulting in the decrease of the amperometric signal to Fe(CN)6(3-). The liner ranges were 0.5-20.0 μmol/L for n-DCPD/GCE with the limit of detection of 0.14 μmol/L and 0.1-50.0 μmol/L for n-HAP/GCE with the limit of detection of 0.069 μmol/L, respectively. The developed method was applied to the analysis of water samples (lake, spring and tap water) and the recovery values were found to be in the range of 90-106%. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Ion-transfer voltammetric behavior of propranolol at nanoscale liquid-liquid interface arrays.

    PubMed

    Liu, Yang; Strutwolf, Jörg; Arrigan, Damien W M

    2015-04-21

    In this work, the ion-transfer voltammetric detection of the protonated β-blocker propranolol was explored at arrays of nanoscale interfaces between two immiscible electrolyte solutions (ITIES). Silicon nitride nanoporous membranes with 400 pores in a hexagonal arrangement, with either 50 or 17 nm radius pores, were used to form regular arrays of nanoITIES. It was found that the aqueous-to-organic ion-transfer current continuously increased steadily rather than reaching a limiting current plateau after the ion-transfer wave; the slope of this limiting current region was concentration dependent and associated with the high ion flux at the nanointerfaces. Electrochemical data were examined in terms of an independent nanointerface approach and an equivalent microdisc approach, supported by finite element simulation. In comparison to the larger interface configuration (50 nm radius), the array of 17 nm radius nanoITIES exhibited a 6.5-times higher current density for propranolol detection due to the enhanced ion flux arising from the convergent diffusion to smaller electrochemical interfaces. Both nanoITIES arrays achieved the equivalent limits of detection, 0.8 μM, using cyclic voltammetry. Additionally, the effect of scan rate on the charging and faradaic currents at these nanoITIES arrays, as well as their stability over time, was investigated. The results demonstrate that arrays of nanoscale liquid-liquid interfaces can be applied to study electrochemical drug transfer, and provide the basis for the development of miniaturized and integrated detection platforms for drug analysis.

  4. Determination of detergents in washing machine wastewater with a voltammetric electronic tongue.

    PubMed

    Olsson, J; Ivarsson, P; Winquist, F

    2008-06-30

    A voltammetric electronic tongue (ET) and a conductivity meter were used to predict amounts of detergents in process water from washing machines. The amount of detergent in over sixty samples was also determined by a HPLC reference method. Prediction was more accurate for the electronic tongue, but both techniques could be used. The composition of the detergent, e.g. supporting electrolyte, is an important factor for the ability to predict the detergent quantity by conductivity. Also two different surfactants, alkyl benzyl sulfonate (ABS) and etoxylated fatty alcohol (EOA), were fingerprinted by the HPLC. Their behaviour during the wash cycle differs from each other, ABS rinses away in the same proportions as the supporting electrolyte, but EOA appears to stay within the machine and laundry. Prediction models for ABS are accurate both with ET and conductivity meter, mostly due to the correlation with supporting electrolyte. The behaviour of EOA, with almost no correlation to the supporting electrolyte makes it difficult to predict using conductivity but ET prediction models give promising indications of its capabilities.

  5. Synthesis, spectroscopic and voltammetric studies of a novel Schiff-base of cysteine and saccharin

    NASA Astrophysics Data System (ADS)

    Çakır, Semiha; Odabaşoğlu, Mustafa; Biçer, Ender; Yazar, Zehra

    2009-01-01

    In this study, a novel Schiff-base of cysteine and saccharin [( 2R)-2-(1, 1-dioxo-1, 2-dihydro-1λ6-benzo[ d]isothiazol-3-ylideneamino)-3-mercapto-propionic acid] was synthesized and characterized by UV-Vis, FT-IR, 1H NMR and elemental analysis. The voltammetric behaviour of Schiff-base was investigated on the static mercury drop electrode (SMDE) by using Square-Wave voltammetry (SWV) and Cyclic voltammetry (CV). The voltammograms of the Schiff-base gave three reduction waves in Britton-Robinson buffer (pH 5.0-9.0) for the potential range from 0.0 to -1.4 V. The first reversible cathodic peak is due to reduction of the mercury thiolate, produced by the thiol group of Schiff-base which adsorbs at Hg electrode surface, to metallic mercury and free thiol. The second reduction peak may be assigned to the reduction of azomethine center (>C dbnd N sbnd ) in the Schiff-base and the last peak may be related to the catalytic hydrogen reduction.

  6. Improvement of the ultra-trace voltammetric determination of Rh in environmental samples using signal transformation.

    PubMed

    Almécija, C; Cobelo-García, A; Santos-Echeandía, J

    2016-01-01

    Rhodium (Rh) is present at the Earth's surface at ultra-trace concentrations (0.06 ng g(-1)); however, its use in catalytic converters has increased its deposition nearby traffic pressure and therefore the interest in analytical techniques for Rh determination has raised in the recent years. In this study we propose an improvement of Rh measurement by adsorptive voltammetry applying second-derivative signal transformation. The optimization of experimental parameters affecting the voltammetric analysis were carried out using sediment samples; these include the amount of sample digest used, the hydrochloric acid and formaldehyde concentrations, deposition potential and equilibration time. The use of the second derivative transformation provided well-defined peaks due to the minimization of background interferences, leading to a significant decrease in the detection limits. Accordingly, a detection limit of 200 fM Rh in the cell was obtained, which corresponds to 14 pg g(-1) of Rh for 200mg of sediments. The optimized methodology was applied to the analysis of Rh in a sediment core collected close to a motorway bridge from Tagus Estuary (Lisbon, Portugal). Here, Rh concentrations ranged from 0.06 to 0.47 ng g(-1), showing a surface Rh-enrichment linked to traffic, which was consistent with a Pt superficial peak. Reference materials were also analyzed, including road dust (BCR-723) and river sediment (JSD-2), and values obtained were in agreement with certified concentrations and previously values reported in the literature. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Differential pulse voltammetric determination of eugenol at a pencil graphite electrode.

    PubMed

    Sağlam, Özlem; Dilgin, Didem Giray; Ertek, Bensu; Dilgin, Yusuf

    2016-03-01

    In this study, the electrochemical behavior of eugenol, a widely used herbal drug, was investigated at a pencil graphite electrode (PGE). A low-cost, disposable, sensitive and selective electrochemical sensor is proposed for the determination of eugenol by recording its differential pulse voltammograms in Britton-Robinson buffer solution containing 0.1 M KCl with pH of 2.0 at the PGE. The PGE displayed a very good electrochemical behavior with significant enhancement of the peak current compared to a glassy carbon electrode. Under experimental conditions, the PGE had a linear response range from 0.3 μM to 50.0 μM eugenol with a detection limit of 0.085 μM (based on 3S(b)). Relative standard deviations of 2.4 and 4.8% were obtained for five successive determinations of 30.0 and 5.0 μM eugenol, respectively, which indicate acceptable repeatability. This voltammetric method was successfully applied for the direct determination of eugenol in real samples. The effect of various interfering compounds on the eugenol peak current was also studied. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Voltammetric electronic tongue and support vector machines for identification of selected features in Mexican coffee.

    PubMed

    Domínguez, Rocio Berenice; Moreno-Barón, Laura; Muñoz, Roberto; Gutiérrez, Juan Manuel

    2014-09-24

    This paper describes a new method based on a voltammetric electronic tongue (ET) for the recognition of distinctive features in coffee samples. An ET was directly applied to different samples from the main Mexican coffee regions without any pretreatment before the analysis. The resulting electrochemical information was modeled with two different mathematical tools, namely Linear Discriminant Analysis (LDA) and Support Vector Machines (SVM). Growing conditions (i.e., organic or non-organic practices and altitude of crops) were considered for a first classification. LDA results showed an average discrimination rate of 88% ± 6.53% while SVM successfully accomplished an overall accuracy of 96.4% ± 3.50% for the same task. A second classification based on geographical origin of samples was carried out. Results showed an overall accuracy of 87.5% ± 7.79% for LDA and a superior performance of 97.5% ± 3.22% for SVM. Given the complexity of coffee samples, the high accuracy percentages achieved by ET coupled with SVM in both classification problems suggested a potential applicability of ET in the assessment of selected coffee features with a simpler and faster methodology along with a null sample pretreatment. In addition, the proposed method can be applied to authentication assessment while improving cost, time and accuracy of the general procedure.

  9. Voltammetric Electronic Tongue and Support Vector Machines for Identification of Selected Features in Mexican Coffee

    PubMed Central

    Domínguez, Rocio Berenice; Moreno-Barón, Laura; Muñoz, Roberto; Gutiérrez, Juan Manuel

    2014-01-01

    This paper describes a new method based on a voltammetric electronic tongue (ET) for the recognition of distinctive features in coffee samples. An ET was directly applied to different samples from the main Mexican coffee regions without any pretreatment before the analysis. The resulting electrochemical information was modeled with two different mathematical tools, namely Linear Discriminant Analysis (LDA) and Support Vector Machines (SVM). Growing conditions (i.e., organic or non-organic practices and altitude of crops) were considered for a first classification. LDA results showed an average discrimination rate of 88% ± 6.53% while SVM successfully accomplished an overall accuracy of 96.4% ± 3.50% for the same task. A second classification based on geographical origin of samples was carried out. Results showed an overall accuracy of 87.5% ± 7.79% for LDA and a superior performance of 97.5% ± 3.22% for SVM. Given the complexity of coffee samples, the high accuracy percentages achieved by ET coupled with SVM in both classification problems suggested a potential applicability of ET in the assessment of selected coffee features with a simpler and faster methodology along with a null sample pretreatment. In addition, the proposed method can be applied to authentication assessment while improving cost, time and accuracy of the general procedure. PMID:25254303

  10. On the Nature of Voltammetric Signals Originating from Hydrogen Electrosorption into Palladium-Noble Metal Alloys

    PubMed Central

    Łukaszewski, Mariusz; Hubkowska, Katarzyna; Koss, Urszula; Czerwiński, Andrzej

    2013-01-01

    Hydrogen sorption/desorption signals observed on cyclic voltammograms in experiments on hydrogen electrosorption into Pd-noble metal alloys (Pd-Au, Pd-Pt, Pd-Rh, Pd-Ru, Pd-Pt-Rh, Pd-Pt-Au) were characterized. The influence of electrosorption potential, scan rate and alloy bulk composition on the features of the hydrogen peaks was investigated. The experimental results were compared with those obtained on the basis of a model taken from the literature. It was confirmed that the rate of the α-β phase transition controls the overall rate of the process of hydrogen absorption/desorption into/from thin Pd-based electrodes. It was demonstrated that from the analysis of the changes of the hydrogen oxidation peak potential with the hydrogen electrosorption potential in cyclic voltammetric experiments it is possible to determine the limiting Pd bulk content, below which the β-phase in the alloy-hydrogen system is not formed. PMID:28788362

  11. New insights into the chemistry of Coenzyme Q-0: A voltammetric and spectroscopic study.

    PubMed

    Gulaboski, Rubin; Bogeski, Ivan; Kokoskarova, Pavlinka; Haeri, Haleh H; Mitrev, Sasa; Stefova, Marina; Stanoeva, Jasmina Petreska; Markovski, Velo; Mirčeski, Valentin; Hoth, Markus; Kappl, Reinhard

    2016-10-01

    Coenzyme Q-0 (CoQ-0) is the only Coenzyme Q lacking an isoprenoid group on the quinoid ring, a feature important for its physico-chemical properties. Here, the redox behavior of CoQ-0 in buffered and non-buffered aqueous media was examined. In buffered aqueous media CoQ-0 redox chemistry can be described by a 2-electron-2-proton redox scheme, characteristic for all benzoquinones. In non-buffered media the number of electrons involved in the electrode reaction of CoQ-0 is still 2; however, the number of protons involved varies between 0 and 2. This results in two additional voltammetric signals, attributed to 2-electrons-1H(+) and 2-electrons-0H(+) redox processes, in which mono- and di-anionic compounds of CoQ-0 are formed. In addition, CoQ-0 exhibits a complex chemistry in strong alkaline environment. The reaction of CoQ-0 and OH(-) anions generates several hydroxyl derivatives as products. Their structures were identified with HPLC/MS. The prevailing radical reaction mechanism was analyzed by electron paramagnetic resonance spectroscopy. The hydroxyl derivatives of CoQ-0 have a strong antioxidative potential and form stable complexes with Ca(2+) ions. In summary, our results allow mechanistic insights into the redox properties of CoQ-0 and its hydroxylated derivatives and provide hints on possible applications. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. A voltammetric electronic tongue as tool for water quality monitoring in wastewater treatment plants.

    PubMed

    Campos, Inmaculada; Alcañiz, Miguel; Aguado, Daniel; Barat, Ramón; Ferrer, José; Gil, Luis; Marrakchi, Mouna; Martínez-Mañez, Ramón; Soto, Juan; Vivancos, José-Luis

    2012-05-15

    The use of a voltammetric electronic tongue as tool for the prediction of concentration levels of certain water quality parameters from influent and effluent wastewater from a Submerged Anaerobic Membrane Bioreactor pilot plant applied to domestic wastewater treatment is proposed here. The electronic tongue consists of a set of noble (Au, Pt, Rh, Ir, and Ag) and non-noble (Ni, Co and Cu) electrodes that were housed inside a stainless steel cylinder which was used as the body of the electronic tongue system. As a previous step an electrochemical study of the response of the ions sulphate, orthophosphate, acetate, bicarbonate and ammonium was carried out in water using the electrodes contained in the electronic tongue. The second part of the work was devoted to the application of the electronic tongue to the characterization of the influent and effluent waters from the wastewater treatment plant. Partial Least Squares analysis was used to obtain a correlation between the data from the tongue and the pollution parameters measured in the laboratory such as soluble chemical oxygen demand (CODs), soluble biological oxygen demand (BODs), ammonia (NH(4)-N), orthophosphate (PO(4)-P), Sulphate (SO(4)-S), acetic acid (HAC) and alkalinity (Alk). A total of 28 and 11 samples were used in the training and the validation steps, respectively, for both influent and effluent water samples. The electronic tongue showed relatively good predictive power for the determination of BOD, COD, NH(4)-N, PO(4)-P, SO(4)-S, and Alk.

  13. Square Wave Voltammetric Determination of Diclofenac in Pharmaceutical Preparations and Human Serum.

    PubMed

    Ciltas, Ulvihan; Yilmaz, Bilal; Kaban, Selcuk; Akcay, Bilge Kaan; Nazik, Gulsah

    2015-01-01

    In this study, a simple and reliable square wave voltammetric (SWV) method was developed and validated for determination of diclofenac in pharmaceutical preparations and human serum. The proposed method was based on electrooxidation of diclofenac at platinum electrode in 0.1 M TBAClO4/acetonitrile solution. The well-defined two oxidation peaks were observed at 0.87 and 1.27 V, respectively. Calibration curves that were obtained by using current values measured for second peak were linear over the concentration range of 1.5-17.5 μg mL(-1) and 2-20 μg mL(-1) in supporting electrolyte and serum, respectively. Precision and accuracy were also checked in all media. Intra- and inter-day precision values for diclofenac were less than 3.64, and accuracy (relative error) was better than 2.49%. Developed method in this study is accurate, precise and can be easily applied to Diclomec, Dicloflam and Voltaren tablets as pharmaceutical preparation. Also, the proposed technique was successfully applied to spiked human serum samples. No electroactive interferences from the endogenous substances were found in human serum.

  14. Square Wave Voltammetric Determination of Diclofenac in Pharmaceutical Preparations and Human Serum

    PubMed Central

    Ciltas, Ulvihan; Yilmaz, Bilal; Kaban, Selcuk; Akcay, Bilge Kaan; Nazik, Gulsah

    2015-01-01

    In this study, a simple and reliable square wave voltammetric (SWV) method was developed and validated for determination of diclofenac in pharmaceutical preparations and human serum. The proposed method was based on electrooxidation of diclofenac at platinum electrode in 0.1 M TBAClO4/acetonitrile solution. The well-defined two oxidation peaks were observed at 0.87 and 1.27 V, respectively. Calibration curves that were obtained by using current values measured for second peak were linear over the concentration range of 1.5-17.5 μg mL-1 and 2-20 μg mL-1 in supporting electrolyte and serum, respectively. Precision and accuracy were also checked in all media. Intra- and inter-day precision values for diclofenac were less than 3.64, and accuracy (relative error) was better than 2.49%. Developed method in this study is accurate, precise and can be easily applied to Diclomec, Dicloflam and Voltaren tablets as pharmaceutical preparation. Also, the proposed technique was successfully applied to spiked human serum samples. No electroactive interferences from the endogenous substances were found in human serum. PMID:26330859

  15. Convolution-deconvolution cyclic voltammetric equilibria study on cadmium(II)-L-histidinate in aqueous solutions.

    PubMed

    Abdel-Hamid, R; Rabia, M K; El-Nady, A B

    1994-09-01

    POLAG computer programme was employed for processing convoluted-deconvoluted cyclic voltammetric data to study cadmium(II)-L-histidinate system. This was performed in 0.1 mol/dm(3) NAClO(4) aqueous solution at different pH's at 298K. The results show that the reduction of cadmium(II) and its complexes proceeds via a reversible and diffusion-controlled wave of two electrons at the entire range of pH. The system was studied at two ranges of pH (6.73-7.44 and 8.53-8.92). It was evident that the system at the first range of pH is well described by the presence of a mixture of binary complexes, [Cd(HisO.H)], [Cd(HisO.H(2))(2)] and a ternary one [Cd(HisO.H)(HisO.H(2))]. For the second pH range, it was revealed that the most likely model corresponds to the presence of a mixture of [Cd(HisO)(2)] and [Cd(OH)] species. The overall stability constants were computed. The structure of the detected complexes was discussed on the basis of ligating sites of histidine.

  16. Voltammetric determination of 4-nitrophenol at a sodium montmorillonite-anthraquinone chemically modified glassy carbon electrode.

    PubMed

    Hu, S; Xu, C; Wang, G; Cui, D

    2001-03-30

    A new method for the determination of 4-nitrophenol(4-NP) by differential pulse voltammetry (DPV) based on adsorptive stripping technique was described. Cyclic voltammetry (CV) and linear scan voltammetry (LSV) were used in a comparative investigation into the electrochemical reduction of 4-NP at a Na-montmorillonite(SWy-2) and anthraquione (AQ) modified glassy carbon electrode. With this chemically modified electrode, 4-NP was first irreversibly reduced from phiNO(2) to phiNHOH at -0.78 V. A couple of well-defined redox peaks at +0.22 V (vs. SCE) were responsible for a two-electron redox peak between phiNHOH and phiNO. Studies on the effect of pH on the peak height and peak potential were carried out over the pH range 2.0-9.0 with the phosphate buffer solution. A pH of 3.4 was chosen as the optimum pH. The other experimental parameters, such as film thickness, accumulation time and potential etc. were optimized. Anodic peak currents were found to be linearly related to concentration of 4-NP over the range 0.3-45 mg l(-1), with a detection limit of 0.02 mg l(-1). The interference of organic and inorganic species on the voltammetric response have been studied. This modified electrode can be used to the determination of 4-NP in water samples.

  17. Voltammetric determination of polyphenolic content as rosmarinic acid equivalent in tea samples using pencil graphite electrodes.

    PubMed

    David, Iulia Gabriela; Buleandră, Mihaela; Popa, Dana Elena; Bîzgan, Ana-Maria Cristina; Moldovan, Zenovia; Badea, Irinel-Adriana; Iorgulescu, Emilia Elena; Tekiner, Tuğçe Ayça; Basaga, Huveyda

    2016-06-01

    The quasi-reversible, diffusion controlled behavior of rosmarinic acid (RA) on a disposable pencil graphite electrode (PGE) was established by cyclic voltammetry. Using the anodic oxidation peak presented by RA on the PGE a differential pulse voltammetric (DPV) method was developed for the quantitative determination of RA. The linear range was 10(-8) - 10(-5) M RA and the detection and quantification limits were 7.93 × 10(-9) M and 2.64 × 10(-8) M RA, respectively. The applicability of the developed method was tested by recovery studies and by the assessment of the total polyphenolic contents (TPCDPV) of green, white and black Turkish teas, which were found to be 40.74, 30.04 and 23.97 mg rosmarinic acid equivalent/g dry tea, respectively. These results were in good agreement with those obtained by the Folin-Ciocalteu method. The developed method is a sensitive and cheap tool for the rapid and precise evaluation of TPCDPV of tea samples.

  18. Gold nanoparticles modified carbon paste electrode for differential pulse voltammetric determination of eugenol.

    PubMed

    Afzali, Daryoush; Zarei, Somaye; Fathirad, Fariba; Mostafavi, Ali

    2014-10-01

    In the present study, a carbon paste electrode chemically modified with gold nanoparticles was used as a sensitive electrochemical sensor for determination of eugenol. The differential pulse voltammetric method was employed to study the behavior of eugenol on this modified electrode. The effect of variables such as percent of gold nanoparticles, pH of solution, accumulation potential and time on voltammogram peak current were optimized. The proposed electrode showed good oxidation response for eugenol in 0.1 mol L(-1) phosphate buffer solution (pH8) and the peak potential was about +285 mV (vs. Ag/AgCl). The peak current increased linearly with the eugenol concentration in the range of 5-250 μmol L(-1). The detection limit was found to be 2.0 μmol L(-1) and the relative standard deviation was 1.2% (n=7). The effect of interferences on the eugenol peak current was studied. The method has been applied to the determination of eugenol in different real samples, spiked recoveries were in the range of 96%-99%. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Voltammetric and mathematical evidence for dual transport mediation of serotonin clearance in vivo.

    PubMed

    Wood, Kevin M; Zeqja, Anisa; Nijhout, H Frederik; Reed, Michael C; Best, Janet; Hashemi, Parastoo

    2014-08-01

    The neurotransmitter serotonin underlies many of the brain's functions. Understanding serotonin neurochemistry is important for improving treatments for neuropsychiatric disorders such as depression. Antidepressants commonly target serotonin clearance via serotonin transporters and have variable clinical effects. Adjunctive therapies, targeting other systems including serotonin autoreceptors, also vary clinically and carry adverse consequences. Fast scan cyclic voltammetry is particularly well suited for studying antidepressant effects on serotonin clearance and autoreceptors by providing real-time chemical information on serotonin kinetics in vivo. However, the complex nature of in vivo serotonin responses makes it difficult to interpret experimental data with established kinetic models. Here, we electrically stimulated the mouse medial forebrain bundle to provoke and detect terminal serotonin in the substantia nigra reticulata. In response to medial forebrain bundle stimulation we found three dynamically distinct serotonin signals. To interpret these signals we developed a computational model that supports two independent serotonin reuptake mechanisms (high affinity, low efficiency reuptake mechanism, and low affinity, high efficiency reuptake system) and bolsters an important inhibitory role for the serotonin autoreceptors. Our data and analysis, afforded by the powerful combination of voltammetric and theoretical methods, gives new understanding of the chemical heterogeneity of serotonin dynamics in the brain. This diverse serotonergic matrix likely contributes to clinical variability of antidepressants. © 2014 International Society for Neurochemistry.

  20. Ensembles-of Gold Nanowires for the Anodic Stripping Voltammetric Determination of Inorganic Arsenic.

    PubMed

    Mardegan, Andrea; Scopece, Paolo; Ugo, Paolo; Moretto, Ligia Maria

    2015-05-01

    3D-ensembles of gold nanowires electrodes (3D-NEEs) are produced by electroless gold deposition in track-etched polycarbonate (PC) membranes, followed by partial etching (plama or chemical) of the polymeric membrane. These electrodes are applied to the anodic stripping voltammetric determination of inorganic As. The controlled etching of the PC template increased the gold surface area, widening the linear range of the analytical response with respect to ensembles of gold nanodisk electrodes (2D-NEEs). 3D-NEEs prepared using a chemical etching time of 10 s allows the anodic stripping determination of As(III) with a detection limit of 0.08 μg/L and a linear range extended up to 20 μg/L. The speciation of inorganic As (As(III) and (As(V)) in river water is possible by difference between As(III) and total inorganic As, determined after reduction of As(V) with cysteine. The proposed method is successfully validated by comparison with lCP-MS determination.

  1. Electrochemical behaviour and voltammetric sensitivity at arrays of nanoscale interfaces between immiscible liquids.

    PubMed

    Rimboud, Mickaël; Hart, Robert D; Becker, Thomas; Arrigan, Damien W M

    2011-11-21

    Arrays of nanoscale interfaces between immiscible electrolyte solutions were formed using silicon nitride nanopore array membranes. Nanopores in the range from 75 nm radius down to 17 nm radius were used to form the nano-interfaces. It was found that the liquid organic phase electrolyte solution filled the pores so that inlaid nano-interfaces were formed with the aqueous phase. Cyclic voltammetry at these nano-interface arrays demonstrated steady-state behaviour at the larger interfaces but the voltammetric wave-shape became progressively worse as the interface size decreased. It was found that the ion transfer currents were ca. 50% of those expected based on theoretical calculations, which is attributed to overlap of diffusion zones at adjacent nano-interfaces. Here, the separation between adjacent nano-interfaces was 20-times the interface radius. The analytical sensitivity for ion transfer from the aqueous to the 1,6-dichlorohexane organic phase was estimated from calibration plots of current density versus concentration of aqueous tetraethylammonium cation. The sensitivity was in the range of 65 μA cm(-2) μM(-1) (at 75 nm radius interfaces) to 265 μA cm(-2) μM(-1) (at 17 nm radius interfaces). The sensitivity depended directly on the inverse of the nano-interface radius, implying that smaller interfaces will provide better sensitivity, due to the enhanced flux of analyte arising from convergent diffusion to smaller electrochemical interfaces.

  2. Simultaneous Voltammetric/Amperometric Determination of Sulfide and Nitrite in Water at BDD Electrode.

    PubMed

    Baciu, Anamaria; Ardelean, Magdalena; Pop, Aniela; Pode, Rodica; Manea, Florica

    2015-06-19

    This work reported new voltammetric/amperometric-based protocols using a commercial boron-doped diamond (BDD) electrode for simple and fast simultaneous detection of sulfide and nitrite from water. Square-wave voltammetry operated under the optimized working conditions of 0.01 V step potential, 0.5 V modulation amplitude and 10 Hz frequency allowed achieving the best electroanalytical parameters for the simultaneous detection of nitrite and sulfide. For practical in-field detection applications, the multiple-pulsed amperometry technique was operated under optimized conditions, i.e., -0.5 V/SCE for a duration of 0.3 s as conditioning step, +0.85 V/SCE for a duration of 3 s that assure the sulfide oxidation and +1.25 V/SCE for a duration of 0.3 s, where the nitrite oxidation occurred, which allowed the simultaneously detection of sulfide and nitrite without interference between them. Good accuracy was found for this protocol in comparison with standardized methods for each anion. Also, no interference effect was found for the cation and anion species, which are common in the water matrix.

  3. Simultaneous Voltammetric/Amperometric Determination of Sulfide and Nitrite in Water at BDD Electrode

    PubMed Central

    Baciu, Anamaria; Ardelean, Magdalena; Pop, Aniela; Pode, Rodica; Manea, Florica

    2015-01-01

    This work reported new voltammetric/amperometric-based protocols using a commercial boron-doped diamond (BDD) electrode for simple and fast simultaneous detection of sulfide and nitrite from water. Square-wave voltammetry operated under the optimized working conditions of 0.01 V step potential, 0.5 V modulation amplitude and 10 Hz frequency allowed achieving the best electroanalytical parameters for the simultaneous detection of nitrite and sulfide. For practical in-field detection applications, the multiple-pulsed amperometry technique was operated under optimized conditions, i.e., −0.5 V/SCE for a duration of 0.3 s as conditioning step, +0.85 V/SCE for a duration of 3 s that assure the sulfide oxidation and +1.25 V/SCE for a duration of 0.3 s, where the nitrite oxidation occurred, which allowed the simultaneously detection of sulfide and nitrite without interference between them. Good accuracy was found for this protocol in comparison with standardized methods for each anion. Also, no interference effect was found for the cation and anion species, which are common in the water matrix. PMID:26102487

  4. Fourier transform analysis of chronoamperometric currents obtained during staircase voltammetric experiments.

    PubMed

    Chang, Byoung-Yong; Park, Su-Moon

    2007-07-01

    We report a novel comprehensive Fourier transform electrochemical impedance spectroscopic (FTEIS) analysis method of a series of chronoamperometric currents obtained during staircase cyclic voltammetric (SCV) experiments. In our method, FTEIS analysis of a set of chronoamperometric currents recorded upon applying a series of small potential steps during an SCV experiment provides a complete description of an electron-transfer reaction at the electrode/electrolyte interface in forms of equivalent circuit elements. Conversion of the circuit elements thus obtained from the analysis allows electrode kinetic parameters including the electron-transfer rate constant, transfer coefficient, diffusion coefficient, and double layer capacitance as well as thermodynamic parameters such as the half-wave potential and the apparent number of electrons transferred to be determined. Theories for obtaining an ac admittance voltammogram, as well as both the thermodynamic and mass-transfer kinetic parameters thereof, from the SCV data have been developed and verified. A decided advantage of the method is that it provides completely self-contained information regarding an electron-transfer reaction from a single pass of the SCV experiment.

  5. Application of XRF, XRD, thermal analysis, and voltammetric techniques to the study of ancient ceramics.

    PubMed

    Sánchez Ramos, S; Bosch Reig, F; Gimeno Adelantado, J V; Yusá Marco, D J; Doménech Carbó, A

    2002-04-01

    An in-depth chemical-analytical study has been performed on biscuit and mortar from 17th-18th century tiles from a mediaeval hermitage in the province of Valencia (Spain). Representative samples were chosen from the tile fragments available, using appearance, essentially color and consistency, as the criterion. The chemical composition was analyzed by X-ray fluorescence of the samples in the form of glass disks after a previous qualitative study to choose the standard materials for calibration and the experimental conditions used in the analysis. X-ray diffraction of the samples provided information about the mineralogical composition which was consistent with the firing of the original materials; it also gave information about the range of temperatures used in the firing. From thermal gravimetric analysis of the limestone, and from historical considerations, it was possible to deduce the raw materials used and their approximate composition in the tiles. In the same way it was possible to determine the nature of the mortars used to fix the tiles. Cyclic voltammetric study of the iron(II) and iron(III) system in the biscuit showed the simultaneous presence of both oxidation states, corroborating the results.

  6. Nanostructured electrochemical sensors based on functionalized nanoporous silica for voltammetric analysis of lead, mercury, and copper.

    PubMed

    Yantasee, Wassana; Fryxell, Glen E; Conner, Marianne M; Lin, Yuehe

    2005-09-01

    We have successfully developed electrochemical sensors based on functionalized nanostructured materials for voltammetric analysis of toxic metal ions. Glycinylurea self-assembled monolayers on mesoporous silica (Gly-UR SAMMS) were incorporated in carbon paste electrodes for the detection of toxic metal ions such as lead, copper, and mercury based on adsorptive stripping voltammetry (AdSV). The electrochemical sensor yields a linear response at a low ppb level of Pb2+ (i.e., 2.5-50 ppb) after a 2-min preconcentration period, with reproducible measurements (%RSD = 3.5, N = 6) and an excellent detection limit (1 ppb). By exploiting the interfacial functionality of Gly-UR SAMMS, the sensor is selective for the target species, does not require the use of a mercury film, and can be easily regenerated in dilute acid solution. The rigid, open, parallel pore structure, combined with suitable interfacial chemistry of SAMMS, also results in fast analysis times (2-3 min). The nanostructured SAMMS materials enable the development of miniature sensing devices that are compact and low cost, have low energy consumption, and are easily integrated into field-deployable units.

  7. Synthesis, characterization and cyclic voltammetric study of copper(II) and nickel(II) polymer chelates.

    PubMed

    Azmeera, Venkanna; Rastogi, Pankaj Kumar; Adhikary, Pubali; Ganesan, Vellaichamy; Krishnamoorthi, S

    2014-09-22

    Graft copolymers based on dextran (Dx) and 2-acrylamido-2-methyl-1-propane sulphonic acid (AMPS) were synthesized by free radical initiated solution polymerization technique using ceric ammonium nitrate as initiator. These graft copolymers were used to prepare Cu(II) and Ni(II) chelates by reactions with Cu(II) and Ni(II) metal ions respectively. Graft copolymer and metal chelates were characterized by elemental analysis, intrinsic viscosity, FT-IR, scanning electron microscopy (SEM), atomic force microscopy (AFM), thermogravimetric analysis (TGA) and powder X-ray diffraction (XRD). Elemental analysis, intrinsic viscosity and FT-IR studies revealed the incorporation of metal ions to form metal chelates. SEM studies showed the change in morphology due to metal incorporation. From AFM studies it was observed that there was increase in Root mean square (RMS) roughness values in case of metal complexes. Metal chelates were observed to be thermally more stable than graft copolymer from TGA. UV-vis spectroscopy study revealed increase in absorbance values and cyclic voltammetric (CV) studies showed more than tenfold increase in redox current due to formation of Cu(II) and Ni(II) metal chelates. The binding constants of each complex determined by using UV-visible spectroscopy revealed that Cu(II) has more binding ability than Ni(II).

  8. Voltammetric Thin-Layer Ionophore-Based Films: Part 1. Experimental Evidence and Numerical Simulations.

    PubMed

    Yuan, Dajing; Cuartero, Maria; Crespo, Gaston A; Bakker, Eric

    2017-01-03

    Voltammetric thin layer (∼200 nm) ionophore-based polymeric films of defined ion-exchange capacity have recently emerged as a promising approach to acquire multi-ion information about the sample, in analogy to performing multiple potentiometric measurements with individual membranes. They behave under two different regimes that are dependent on the ion concentration. A thin layer control (no mass transport limitation of the polymer film or solution) is identified for ion concentrations of >10 μM, in which case the peak potential serves as the readout signal, in analogy to a potentiometric sensor. On the other hand, ion transfer at lower concentrations is chiefly controlled by diffusional mass transport from the solution to the sensing film, resulting in an increase of peak current with ion concentration. This concentration range is suitable for electrochemical ion transfer stripping analysis. Here, the transition between the two mentioned scenarios is explored experimentally, using a highly silver-selective membrane as a proof-of-concept under different conditions (variation of ion concentration in the sample from 0.1 μM to 1 mM, scan rate from 25 mV s(-1) to 200 mV s(-1), and angular frequency from 100 rpm to 6400 rpm). Apart from experimental evidence, a numerical simulation is developed that considers an idealized conducting polymer behavior and permits one to predict experimental behavior under diffusion or thin-layer control.

  9. Voltammetric methods for determination and speciation of inorganic arsenic in the environment--a review.

    PubMed

    Mays, Douglas E; Hussam, Abul

    2009-07-30

    The measurement of inorganic arsenic in the environment has received considerable attention over the past 40+ years due to its toxicity and prevalence in drinking water. This paper provides an overview of voltammetric techniques used since 2001. More than fifty papers from refereed analytical chemistry journals on the speciation and measurement of inorganic arsenic (As(III) and As(V)) in practical and environmental samples are included. The present review shows that stripping voltammetry is a sensitive and inexpensive technique. The new approaches include development of novel measurement protocols through media variation, development and use of new boron doped diamond electrodes modified with metals, nano Au-modified electrodes on carbon or carbon nano-tubes, novel rotating disc and vibrating electrodes to enhance mass transfer, and modified Hg(l) and thin film Bi on carbon for cathodic stripping voltammetry are discussed. Although, majority of the papers were of exploratory in nature, the trend towards developing a commercial standalone instrument for field use is still in progress.

  10. Fabrication of a novel microsensor consisting of electrodeposited ZnO nanorod-coated crossed Cu micropillars and the effects of nanorod coating morphology on the gas sensing.

    PubMed

    Tseng, Yao-Tien; Lin, Jing-Chie; Ciou, Yong-Jie; Hwang, Yean-Ren

    2014-07-23

    A novel microsensor, consisting of crossed Cu micropillars coated with ZnO nanorods, was fabricated by electrochemical methods for detecting gas in a small space. The Cu micropillars (80 μm diameter, 10 mm long) were prepared by microanode-guided electroplating (MAGE) on the periphery of a square copper pad (dimensions 5.0 mm × 5.0 mm × 1.0 mm). The micropillars were electrochemically coated with a 500 nm thick layer of ZnO nanorods deposited from a bath containing 2.0 mM zinc chloride and H2O2 varying in 5, 10, 15, and 20 mM. Two ZnO-coated pillars were crossed to form a microsensor by approaching the Cu pads below, which was adhered to an alumina substrate with silver paste and connected to conducting wires for measurement. The morphology of the coating of ZnO nanorods, which was found to be determined by the concentration of H2O2 in the bath, influenced the gas sensing. The morphology of the coating was characterized by scanning electron microscopy; the structural analysis was carried out by X-ray diffraction and high-resolution transmission electron microscopy (HRTEM); the surface analysis was carried out by X-ray photoelectron spectroscopy; and the defects were determined with photoluminescence (PL) spectra. We thus investigated the effect of the morphology of the coating on the sensing properties by introducing a stream of gases varying in CO/air ratios to understand the sensing mechanism of the microsensor.

  11. Experimental and theoretical study of possible correlation between the electrochemistry of canthin-6-one and the anti-proliferative activity against human cancer stem cells

    NASA Astrophysics Data System (ADS)

    Cebrián-Torrejón, G.; Doménech-Carbó, A.; Scotti, M. T.; Fournet, A.; Figadère, B.; Poupon, E.

    2015-12-01

    This work presents an approach to study the performance of novel targets able to overcome cancer stem cell chemoresistance, based on the voltammetric data for microparticulate films of natural or synthetic alkaloids from the canthin-6-one series. A comparison of this voltammetric technique with conventional solution phase electrochemistry suggests the differences in the anti-proliferative activity of canthin-6-ones could be tentatively correlated to their different capacity to generate semiquinone radical anions. These data also match theoretical calculations.

  12. Characterization of MgFe2O4 nanoparticles as a novel electrochemical sensor: application for the voltammetric determination of ciprofloxacin.

    PubMed

    Ensafi, Ali A; Allafchian, Ali R; Mohammadzadeh, R

    2012-01-01

    A new sensor containing MgFe2O4 nanoparticles in modified multiwall carbon nanotubes (MgFe2O4-MWCNTs) was prepared, and its electrochemical behavior was investigated. MgFe2O4-MWCNTs were used as a voltammetric sensor for the electrocatalytic determination of ciprofloxacin. The synthesized materials were characterized by different methods such as transmission electron microscopy (TEM), X-ray diffraction (XRD), cyclic voltammetry, and electrochemical impedance spectroscopy. The MgFe2O4-MWCNTs electrode showed an oxidation peak potential at around 250 mV. The immobilized composite films facilitate interfacial electron transfer and electrocatalytic activity on the oxidation of ciprofloxacin. The oxidation peak current was dependent on the ciprofloxacin concentration, which was linear over the range of 0.10 - 1000 µmol L(-1) with a detection limit and quantification limit of 0.01 and 0.08 µmol L(-1), respectively. The relative standard deviation for the determination of 1.0 µmol L(-1) ciprofloxacin was 1.1%. The repeatability of the sensor was investigated by preparing nine similar electrodes. The proposed sensor is a selective and fast tool for the determination of ciprofloxacin in tablet, plasma, and urine samples.

  13. Acetylene black paste electrode modified with graphene as the voltammetric sensor for selective determination of tryptophan in the presence of high concentrations of tyrosine.

    PubMed

    Deng, Peihong; Xu, Zhifeng; Feng, Yonglan

    2014-02-01

    A reliable sensor was fabricated by modifying an acetylene black paste electrode with graphene (denoted as GR/ABPE) for sensitive and selective determination of tryptophan (Trp). Due to the high sorption ability, large surface area and numerous active sites, the GR/ABPE showed a strong enhancement effect on the oxidation of Trp, and greatly increased the peak current. The parameters affecting the Trp determination were investigated. In 1.0 M H2SO4 the voltammetric responses of Trp and tyrosine (Tyr) were well separated into two distinct peaks with peak potential difference (ΔE(pa)) of 115 mV. Under the optimized conditions, in the presence of 0.1 mM Tyr, the oxidation peak current of Trp was proportional to its concentration in the range between 0.1 μM and 0.1 mM, with the limit of detection of 60 nM (S/N=3). The GR/ABPE was applied to the direct detection of Trp in pharmaceutical and biological samples with satisfactory results. This work provides a simple and easy approach to selective detection of Trp in the presence of Tyr.

  14. Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films.

    PubMed

    Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

    2014-12-01

    Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1-65 μM with a low detection limit of 0.01 μM (S/N=3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets.

  15. In Vivo Voltammetric Monitoring of Norepinephrine Release in the Rat Ventral Bed Nucleus of the Stria Terminalis and Anteroventral Thalamic Nucleus

    PubMed Central

    Park, Jinwoo; Kile, Brian M.; Wightman, R. Mark

    2010-01-01

    The role and contribution of the dense noradrenergic innervation in the ventral bed nucleus of the stria terminalis (vBNST) and anteroventral thalamic nucleus (AV) to biological function and animal behaviors is poorly understood due to the small size of these nuclei. The aim of this study was to compare norepinephrine release and uptake in the vBNST with that in the AV of anesthetized rats. Measurements were made in vivo with fast-scan cyclic voltammetry following electrical stimulation of noradrenergic projection pathways, either the dorsal noradrenergic bundle (DNB) or the ventral noradrenergic bundle (VNB). The substance detected was identified as norepinephrine based upon voltammetric, anatomical, neurochemical, and pharmacological evidence. Fast-scan cyclic voltammetry enables the selective monitoring of local norepinephrine overflow in the vBNST evoked by the stimulation of either the DNB or VNB while norepinephrine in the AV was only evoked by DNB stimulation. The α2-adrenoceptor antagonist, yohimbine, and the norepinephrine uptake inhibitor, desipramine, increased norepinephrine overflow and slowed its disappearance in both regions. However, control of extracellular norepinephrine by both autoreceptors and uptake was greater in the AV. The greater control exerted by autoreceptors and uptake in the AV resulted in reduced extracellular concentration compared to the vBNST when large numbers of stimulation pulses were employed. The differences in noradrenergic transmission observed in the terminal fields of the vBNST and the AV may differentially regulate activity in these two regions that both contain high densities of norepinephrine terminals. PMID:20128849

  16. Langmuir-Blodgett and Langmuir-Schaefer films of homoleptic and heteroleptic phthalocyanine complexes as voltammetric sensors:. Applications to the study of antioxidants

    NASA Astrophysics Data System (ADS)

    Casilli, Serena; De Luca, Mariangela; Apetrei, Constantin; Parra, Vicente; Arrieta, Álvaro A.; Valli, Ludovico; Jiang, Jianzhuang; Rodríguez-Méndez, María L.; De Saja, José A.

    2005-06-01

    Double- and triple-decker phthalocyanine derivatives have been successfully used as the sensitive materials for liquid electrochemical sensors. The materials include homoleptic and heteroleptic phthalocyanine complexes formed by phthalocyanine, porphyrin and naphthalocyanine rings. A high degree of cross-selectiviy towards antioxidant compounds (including vannilic acid, pyrogallol, ascorbic acid and catechin) has been attained by using different phthalocyanine complexes. The features observed in the cyclic voltammograms reflect the rich electrochemistry of either the phthalocyanine molecules or the studied solutions. In consequence, each sensor shows a selective response to the antioxidant analysed. The obtained voltammograms from by using highly ordered electrodes prepared using the Langmuir-Blodgett (LB) or the Langmuir-Schaefer (LS) techniques show better resolution and stability than those of disordered electrodes prepared by casting. For this reason, ordered films have been chosen to construct an array of liquid sensors. The principal component analysis (PCA) of the obtained signals has allowed that a clear discrimination of the antioxidant solutions be achieved. The rich and varied responses produced by antioxidant molecules evidences that voltammetric electrodes based on phthalocyanines, are especially suitable for the analysis of compounds with electrochemical activity.

  17. Glassy carbon electrode modified with horse radish peroxidase/organic nucleophilic-functionalized carbon nanotube composite for enhanced electrocatalytic oxidation and efficient voltammetric sensing of levodopa.

    PubMed

    Shoja, Yalda; Rafati, Amir Abbas; Ghodsi, Javad

    2016-01-01

    A novel and selective enzymatic biosensor was designed and constructed for voltammetric determination of levodopa (L-Dopa) in aqueous media (phosphate buffer solution, pH=7). Biosensor development was on the basis of to physically immobilizing of horse radish peroxidase (HRP) as electrochemical catalyst by sol-gel on glassy carbon electrode modified with organic nucleophilic carbon nanotube composite which in this composite p-phenylenediamine (pPDA) as organic nucleophile chemically bonded with functionalized MWCNT (MWCNT-COOH). The results of this study suggest that prepared bioorganic nucleophilic carbon nanotube composite (HRP/MWCNT-pPDA) shows fast electron transfer rate for electro oxidation of L-Dopa because of its high electrochemical catalytic activity toward the oxidation of L-Dopa, more--NH2 reactive sites and large effective surface area. Also in this work we measured L-Dopa in the presence of folic acid and uric acid as interferences. The proposed biosensor was characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), FT-IR spectroscopy and cyclic voltammetry (CV). The differential pulse voltammetry (DPV) was used for determination of L-Dopa from 0.1 μM to 1.9 μM with a low detection limit of 40 nM (for S/N=3) and sensitivity was about 35.5 μA/μM. Also this biosensor has several advantages such as rapid response, high stability and reproducibility.

  18. Electro-Oxidation Mechanism and Direct Square-Wave Voltammetric Determination of Lidocaine With a Carbon-Paste Electrode

    PubMed Central

    Rahbar, Nadereh; Ramezani, Zahra; Babapour, Ahmad

    2015-01-01

    Background Lidocaine hydrochloride (LH) is one of the most extensively used local anesthetics and peripheral analgesics. Availability of a simple and sensitive assay method for this analyte in pharmaceutical preparations as well as development of new voltammetric detectors that can be applied in chromatographic systems for determination of this analyte in biological samples are of great importance. Objectives In this study, a square-wave voltammetric (SWV) determination of LH at a bare carbon-paste electrode (CPE) was reported. Moreover, the oxidation mechanism for LH molecule at this electrode was investigated. Materials and Methods The SW voltammogram of LH solution at CPE showed a well-defined peak between +0.80 and +0.88 V depending on a scan rate in potassium nitrate (KNO3) solution. Different chemical and instrumental parameters influencing the voltammetric response, such as the pH level and scan rate were optimized for LH determination. Results A linear range of 8.0 - 1000.0 μmol L-1 (r2 = 0.999) was obtained. The limit of detection (LOD) was 0.29 μmol L-1. The relative standard deviations of 2.1% obtained for 0.8 800 μmol L-1 solution of LH indicated a reasonable reproducibility of the method. Conclusions The results of this study show that LH in different pharmaceutical preparations could be determined with good reliability. In addition, the results reveal that the equal numbers of electrons and protons are involved in the oxidation of LH and the irreversible oxidation of an analyte was performed via amine groups of LH molecule. PMID:25866720

  19. Controlled functionalisation of single-walled carbon nanotube network electrodes for the enhanced voltammetric detection of dopamine.

    PubMed

    E, Sharel P; Miller, Thomas S; Macpherson, Julie V; Unwin, Patrick R

    2015-10-21

    Voltammetric studies of dopamine (DA) oxidation on pristine and acid-treated single-walled carbon nanotube (SWNT) network electrodes were undertaken in order to investigate both the effect of network density and acid treatment times on the voltammetric characteristics for DA oxidation and the susceptibility of the electrodes to fouling. Through careful control of catalysed chemical vapour deposition growth parameters, multiply interconnected and randomly oriented SWNT networks of two significantly different densities were grown (high density, HD, coverage ≫10 μm length of SWNT per μm(-2) and low density, LD, coverage = 5 (±1) μmSWNTμm(-2)). Acid treatment was performed to provide materials with different electrochemical properties and SWNT coverage, as determined by field emission-scanning electron microscopy, atomic force microscopy and micro-Raman spectroscopy. A high concentration of DA (100 μM) was deliberately employed to accelerate the fouling phenomenon associated with DA oxidation in order to evaluate the lifetime of the electrodes. HD pristine SWNT networks were found to promote more facile electron transfer (ET) and were less susceptible to blocking, compared to LD pristine SWNT networks. Acid treatment resulted in both a further enhancement of the ET rate and a reduction in susceptibility towards electrode fouling. However, lengthy acid treatment detrimentally affected ET, due to a decrease in network density and significant damage to the SWNT network structure. These studies highlight the subtle interplay between SWNT coverage and degree of acid functionalisation when seeking to achieve the optimal SWNT electrode for the voltammetric detection of DA.

  20. Voltammetric determination of cysteine using carbon paste electrode modified with Co(II)-Y zeolite.

    PubMed

    Nezamzadeh-Ejhieh, Alireza; Hashemi, Habibeh-Sadat

    2012-01-15

    A novel zeolite modified electrode for use in voltammetric determination of l-cysteine (CySH) was described. The electrode comprises a Co(II)-exchanged zeolite Y as modifier in carbon paste matrix. First, the electrochemical behavior of Co(II) in modified carbon paste electrode was studied. The results demonstrated that diffusion can control the redox process of cobalt cations at the surface of the modified electrode. Then, the behavior of the electrode in the presence of CySH was studied by using cyclic voltammetry and a novel behavior was observed. In high concentration of CySH (above 10 mmol L(-1)), one pair of semi-reversible electrochemical extra peak was observed which was assigned to the processes of oxidation-reduction of CySH at the unmodified and modified electrode. Acidic conditions with respect to the neutral one cause an increase in the electrode response. The modified electrode showed a suitable linear calibration graph in the concentration range of 1.0×10(-9)-1.0×10(-3)mol L(-1) cysteine with a detection limit of 2.37×10(-10)mol L(-1). The influence of potential interfering substances on the peak current was studied and the results showed that the method was highly selective for determination of CySH. Thus, the proposed electrode was used for the determination of CySH in real samples including human blood serum, urine, N-acetylcysteine tablet and powdered poultry feed and the satisfactory results were obtained. Typical features of the sensor can be summarized as: low cost, simple preparation, fast response, good stability and selectivity, wide linear range, low detection limit and high reproducibility.

  1. Voltammetric determination of nitrite in meat products using polyvinylimidazole modified carbon paste electrode.

    PubMed

    Yildiz, Gulcemal; Oztekin, Nevin; Orbay, Ayca; Senkal, Filiz

    2014-01-01

    A simple and sensitive voltammetric method was developed to determine the amount of nitrite by using Carbon Paste Electrode (CPE) which is modified with polyvinylimidazole (PVI). A buffer solution of phosphate with a pH 4 value was used in the experiments. The amount of the nitrite-ion was determined by cyclic voltammetry (CV). The electro-chemical behaviour of nitrite-ion was investigated by using CV on the PVI modified CPE. A well-defined oxidation peak was obtained at 0.83 V against a reference Ag/AgCl electrode. Differential pulse voltammetry (DPV) was applied for the calibration plot and for the detection limit. The optimisation procedure was done in two steps: using a two-level factorial design for preliminary evaluation of the contributing factors, and the Box-Behnken Design (BBD) to assess the optimal experimental conditions. These are done with the analysis of 3 different factors in 15 runs of DPV. The optimum conditions are obtained within a linear response range of 5×10(-7)-1×10(-4) mol L(-1). Regression analysis is performed within this range showed the linear equation of y=0.028x+3.93×10(-7) with r(2)=0.9982, and for n=7. Limit of Detection (LOD) was 9×10(-8) mol L(-1) with S/N=3, and Limit of Quantification (LOQ) was 3×10(-7) mol L(-1) with S/N=10. The procedure was used successfully to detect the amount of nitrite in meat products.

  2. Glyphosate Detection by Means of a Voltammetric Electronic Tongue and Discrimination of Potential Interferents

    PubMed Central

    Bataller, Román; Campos, Inmaculada; Laguarda-Miro, Nicolas; Alcañiz, Miguel; Soto, Juan; Martínez-Máñez, Ramón; Gil, Luís; García-Breijo, Eduardo; Ibáñez-Civera, Javier

    2012-01-01

    A new electronic tongue to monitor the presence of glyphosate (a non-selective systemic herbicide) has been developed. It is based on pulse voltammetry and consists in an array of three working electrodes (Pt, Co and Cu) encapsulated on a methacrylate cylinder. The electrochemical response of the sensing array was characteristic of the presence of glyphosate in buffered water (phosphate buffer 0.1 mol·dm−3, pH 6.7). Rotating disc electrode (RDE) studies were carried out with Pt, Co and Cu electrodes in water at room temperature and at pH 6.7 using 0.1 mol·dm−3 of phosphate as a buffer. In the presence of glyphosate, the corrosion current of the Cu and Co electrodes increased significantly, probably due to the formation of Cu2+ or Co2+ complexes. The pulse array waveform for the voltammetric tongue was designed by taking into account some of the redox processes observed in the electrochemical studies. The PCA statistical analysis required four dimensions to explain 95% of variance. Moreover, a two-dimensional representation of the two principal components differentiated the water mixtures containing glyphosate. Furthermore, the PLS statistical analyses allowed the creation of a model to correlate the electrochemical response of the electrodes with glyphosate concentrations, even in the presence of potential interferents such as humic acids and Ca2+. The system offers a PLS prediction model for glyphosate detection with values of 098, −2.3 × 10−5 and 0.94 for the slope, the intercept and the regression coefficient, respectively, which is in agreement with the good fit between the predicted and measured concentrations. The results suggest the feasibility of this system to help develop electronic tongues for glyphosate detection. PMID:23250277

  3. Indirect differential pulse voltammetric determination of aluminum by a pyrocatechol violet-modified electrode

    SciTech Connect

    Chen, G.; Bi, S.; Dai, L.; Cao, M.; Chen, Y. Wang, X.

    1999-03-01

    Aluminum is one of the abundant elements in the earth`s crust. It has been considered to be a causative agent for various neurological disorders such as Alzheimer Senile, presenile dementia and amyotrophic lateral sclerosis. It is also very harmful to plants and aquatic organisms. Therefore, the determination of Al is very important. A Pyrocatechol Violet (PCV) modified electrode for the voltammetric determination of aluminum is reported. The modified electrode is simply prepared by dip-coating a pyrolytic graphite electrode in a NaAc-HAc buffer solution of PCV. Optimum experimental conditions for aluminum determination include a 0.2 mol/L NaAc-HAc buffer solution of pH 4.8, a PCV concentration of 0.02 mol/L used to modify the electrode and the use of differential-pulse mode for measurement. The peak currents of differential pulse voltammograms (DPV) decrease with the addition of Al into the buffer solution while the peak potentials remain the same. The decreasing value of peak current {Delta}i{sub p} is linear with Al concentration in the range of 1{times}10{sup {minus}8} to 1{times}10{sup {minus}7} mol/L and 1{times}10{sup {minus}7} to 1{times}10{sup {minus}6} mol/L. The detection limit is 5{times}10{sup {minus}9} mol/L and the relative standard deviation for 4{times}10{sup {minus}8} mol/L Al is 2.9% (n=8). The stability of this electrode is satisfactory. No serious interference is found. This method has been applied to determine Al in drinking water samples.

  4. Study of the voltammetric behaviour of metam and its application to an amperometric flow system.

    PubMed

    Barroso, M Fátima; Paíga, Paula; Vaz, M Carmo V F; Delerue-Matos, Cristina

    2005-11-01

    The electrochemical behaviour of the pesticide metam (MT) at a glassy carbon working electrode (GCE) and at a hanging mercury drop electrode (HMDE) was investigated. Different voltammetric techniques, including cyclic voltammetry (CV) and square wave voltammetry (SWV), were used. An anodic peak (independent of pH) at +1.46 V vs AgCl/Ag was observed in MT aqueous solution using the GCE. SWV calibration curves were plotted under optimized conditions (pH 2.5 and frequency 50 Hz), which showed a linear response for 17-29 mg L(-1). Electrochemical reduction was also explored, using the HMDE. A well defined cathodic peak was recorded at -0.72 V vs AgCl/Ag, dependent on pH. After optimizing the operating conditions (pH 10.1, frequency 150 Hz, potential deposition -0.20 V for 10 s), calibration curves was measured in the concentration range 2.5 x 10(-1) to 1.0 mg L(-1) using SWV. The electrochemical behaviour of this compound facilitated the development of a flow injection analysis (FIA) system with amperometric detection for the quantification of MT in commercial formulations and spiked water samples. An assessment of the optimal FIA conditions indicated that the best analytical results were obtained at a potential of +1.30 V, an injection volume of 207 muL and an overall flow rate of 2.4 ml min(-1). Real samples were analysed via calibration curves over the concentration range 1.3 x 10(-2) to 1.3 mg L(-1). Recoveries from the real samples (spiked waters and commercial formulations) were between 97.4 and 105.5%. The precision of the proposed method was evaluated by assessing the relative standard deviation (RSD %) of ten consecutive determinations of one sample (1.0 mg L(-1)), and the value obtained was 1.5%.

  5. Voltammetric study of the control of striatal dopamine release by glutamate.

    PubMed

    Borland, Laura M; Michael, Adrian C

    2004-10-01

    The central dopamine systems are involved in several aspects of normal brain function and are implicated in a number of human disorders. Hence, it is important to understand the mechanisms that control dopamine release in the brain. The striatum of the rat receives both dopaminergic and glutamatergic projections that synaptically target striatal neurons but not each other. Nevertheless, these afferents do form frequent appositional contacts, which has engendered interest in the question of whether they communicate with each other despite the absence of a direct synaptic connection. In this study, we used voltammetry in conjunction with carbon fiber microelectrodes in anesthetized rats to further examine the effect of the ionotropic glutamate antagonist, kynurenate, on extracellular dopamine levels in the striatum. Intrastriatal infusions of kynurenate decreased extracellular dopamine levels, suggesting that glutamate acts locally within the striatum via ionotropic receptors to regulate the basal extracellular dopamine concentration. Infusion of tetrodotoxin into the medial forebrain bundle or the striatum did not alter the voltammetric response to the intrastriatal kynurenate infusions, suggesting that glutamate receptors control a non-vesicular release process that contributes to the basal extracellular dopamine level. However, systemic administration of the dopamine uptake inhibitor, nomifensine (20 mg/kg i.p.), markedly decreased the amplitude of the response to kynurenate infusions, suggesting that the dopamine transporter mediates non-vesicular dopamine release. Collectively, these findings are consistent with the idea that endogenous glutamate acts locally within the striatum via ionotropic receptors to control a tonic, impulse-independent, transporter-mediated mode of dopamine release. Although numerous prior in vitro studies had suggested that such a process might exist, it has not previously been clearly demonstrated in an in vivo experiment.

  6. Penicillamine-modified sensor for the voltammetric determination of Cd(II) and Pb(II) ions in natural samples.

    PubMed

    Pérez-Ràfols, Clara; Serrano, Núria; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

    2015-11-01

    A new penicillamine-GCE was developed based on the immobilization of d-penicillamine on aryl diazonium salt monolayers anchored to the glassy carbon electrode (GCE) surface and it was applied for the first time to the simultaneous determination of Cd(II) and Pb(II) ions by stripping voltammetric techniques. The detection and quantification limits at levels of µg L(-1) suggest that the penicillamine-GCE could be fully suitable for the determination of the considered ions in natural samples.

  7. Potential shift correction in multivariate curve resolution of voltammetric data. General formulation and application to some experimental systems.

    PubMed

    Alberich, Arístides; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

    2008-01-01

    A new mathematical algorithm is proposed to correct the progressive potential shift of some voltammetric signals that decrease the linearity of the data. The corrected data matrix can be further analysed by Multivariate Curve Resolution by Alternating Least Squares (MCR-ALS) and the vector including the potential shift corrections can be fitted to specific equations such as that by DeFord-Hume. A detailed discussion is given on the different cases of potential shift correction, and, in some of them, mathematical simulation is made or experimental systems [Cd(ii)-glutathione and Zn(ii)-glycine] are analysed.

  8. The study and application of four kinds of organic ion-selective microsensors

    NASA Astrophysics Data System (ADS)

    Yu, Bi; Zheng, Xiao; Feng, Chu; Hong, Wen-Bing; Liu, Jun-Tao; Wang, Ru-Jiang

    1991-09-01

    Four kinds of organic ion-selective microelectrodes (two barrels, tip diameter 0.1-0.5 micron) have been developed for the measurement of acetylcholine, histamine, serotonin, and bile acid. Physiological and pathological models on the cellular or sub-cellular level have been established for the purpose of basic and clinical pharmacological research, treatment or diagnosis of certain diseases. The acetylcholine sensitive microelectrode has been applied to the study of acetylcholine activity in single erythrocytes of normal human subjects and patients suffering from manic depressive disorders. The bile acid selective microelectrode has been used for the direct measurement of intracellular bile acid activities both in colorectal cancer and colorectal mucosa in living condition.

  9. Review on Hydrogel-based pH Sensors and Microsensors

    PubMed Central

    Richter, Andreas; Paschew, Georgi; Klatt, Stephan; Lienig, Jens; Arndt, Karl-Friedrich; Adler, Hans-Jürgen P.

    2008-01-01

    Stimuli-responsive hydrogels are materials with great potential for development of active functionalities in fluidics and micro-fluidics. Based on the current state of research on pH sensors, hydrogel sensors are described qualitatively and quantitatively for the first time. The review introduces the physical background of the special properties of stimuli-responsive hydrogels. Following, transducers are described which are able to convert the non-electrical changes of the physical properties of stimuli-responsive hydrogels into an electrical signal. Finally, the specific sensor properties, design rules and general conditions for sensor applications are discussed. PMID:27879722

  10. Anodic-stripping voltammetric immunoassay for ultrasensitive detection of low-abundance proteins using quantum dot aggregated hollow microspheres.

    PubMed

    Zhang, Bing; Tang, Dianping; Goryacheva, Irina Yu; Niessner, Reinhard; Knopp, Dietmar

    2013-02-11

    A new anodic-stripping voltammetric immunoassay protocol for detection of IgG1, as a model protein, was designed by using CdS quantum dot (QD) layer-by-layer assembled hollow microspheres (QDHMS) as molecular tags. Initially, monoclonal anti-human IgG1 specific antibodies were anchored on amorphous magnetic beads preferably selective to capture F(ab) of IgG1 analyte from the sample. For detection, monoclonal anti-human IgG1 (F(c)-specific) antibodies were covalently coupled to the synthesized QDHMS. In a sandwich-type immunoassay format, subsequent anodic-stripping voltammetric detection of cadmium released under acidic conditions from the coupled QDs was conducted at an in situ prepared mercury film electrode. The immunoassay combines highly efficient magnetic separation with signal amplification by the multilayered QD labels. The dynamic concentration range spanned from 1.0 fg mL(-1) to 1.0 μg mL(-1) of IgG1 with a detection limit of 0.1 fg mL(-1). The electrochemical immunoassay showed good reproducibility, selectivity, and stability. The analysis of clinical serum specimens revealed good accordance with the results obtained by an enzyme-linked immunosorbent assay method. The new immunoassay is promising for enzyme-free, and cost-effective analysis of low-abundance biomarkers. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Square wave voltammetric determination of methyl parathion using ZrO2-nanoparticles modified carbon paste electrode.

    PubMed

    Parham, H; Rahbar, N

    2010-05-15

    A carbon paste electrode is modified with ZrO(2)-nanoparticles and its application for square wave voltammetric (SWV) detection of methyl parathion, MP (organophosphate pesticide) is reported. The nano-ZrO(2) shows a strong affinity toward the phosphate group on methyl parathion molecules, which provides sensitivity and selectivity of the modified carbon paste electrode. Instrumental and chemical parameters influencing the voltammetric response are optimized for MP determination. Under optimum experimental conditions the peak current is linear to MP concentration over the range of 5.0-3000.0 ng mL(-1) with a correlation coefficient of 0.9992. The limit of detection (LOD) and limit of quantification (LOQ) for MP based on three and ten times the standard deviation of the blank (3S(b), 10S(b)) were 2.0 and 5.7 ng mL(-1) (n=20) for MP, respectively. The recovery values from quality control (QC) samples of water solutions containing low, middle and high concentrations of MP (50, 100 and 800 ng mL(-1)) were 98.0+/-2.3%, 92.5+/-4.9% and 97.6+/-2.8%, respectively. The electrode is successfully applied for the determination of MP in different water samples.

  12. Sensitive voltammetric determination of lead released from ceramic dishes by using of bismuth nanostructures anchored on biochar.

    PubMed

    Agustini, Deonir; Mangrich, Antonio Salvio; Bergamini, Márcio F; Marcolino-Junior, Luiz Humberto

    2015-09-01

    A simple and sensitive electroanalytical method was developed for determination of nanomolar levels of Pb(II) based on the voltammetric stripping response at a carbon paste electrode modified with biochar (a special charcoal) and bismuth nanostructures (nBi-BchCPE). The proposed methodology was based on spontaneous interactions between the highly functionalized biochar surface and Pb(II) ions followed by reduction of these ions into bismuth nanodots which promote an improvement on the stripping anodic current. The experimental procedure could be summarized in three steps: including an open circuit pre-concentration, reduction of accumulated lead ions at the electrode surface and stripping step under differential pulse voltammetric conditions (DPAdSV). SEM images revealed dimensions of bismuth nanodots ranging from 20 nm to 70 nm. The effects of main parameters related to biochar, bismuth and operational parameters were examined in detail. Under the optimal conditions, the proposed sensor has exhibited linear range from 5.0 to 1000 nmol L(-1) and detection limit of 1.41 nmol L(-1) for Pb(II). The optimized method was successfully applied for determination of Pb(II) released from overglaze-decorated ceramic dishes. Results obtained were compared with those given by inductively coupled plasma optical emission spectroscopy (ICP-OES) and they are in agreement at 99% of confidence level.

  13. A new voltammetric strategy for sensitive and selective determination of gallium using cupferron as a complexing agent.

    PubMed

    Grabarczyk, Malgorzata; Wardak, Cecylia

    2014-01-01

    This article describes a differential pulse adsorptive stripping voltammetric method for the trace determination of gallium in environmental water samples. It is based on the adsorptive deposition of the complex Ga(III)-cupferron at the hanging mercury drop electrode (HMDE) at -0.4 V (versus Ag/AgCl) and its cathodic stripping during the potential scan. The method was optimized as concerns the main electrochemical parameters that affect the voltammetric determination (supporting electrolyte, pH, cupferron concentration, deposition potential and time). The calibration graph is linear from 5 × 10(-10) to 5 × 10(-7) mol L(-1) with a detection limit calculated as 1.3 × 10(-10) mol L(-1) for deposition time of 30 s. The influence of interfering substances such as surfactants and humic substances present in the matrices of natural water samples on the Ga(III) signal was examined and a satisfying minimization of these interferences was proposed. The procedure was applied to direct determination of gallium in environmental water samples.

  14. Indirect voltammetric determination of caffeine content in coffee using 1,4-benzoquinone modified carbon paste electrode.

    PubMed

    Aklilu, Muluken; Tessema, Merid; Redi-Abshiro, Mesfin

    2008-08-15

    In this paper a simple and highly sensitive electroanalytical method for the determination of caffeine content using 1,4-benzoquinone modified carbon paste electrode is presented. The method is based on suppression of 1,4-benzoquinone peak current on addition of caffeine. Square-wave and cyclic voltammetric techniques were utilised for the investigation. The 1,4-benzoquinone modified electrode exhibited a well-defined peak with reproducible peak current values for repetitive measurements; and showed a decrease in peak current value with an increase in caffeine content. The result revealed two linear range regions between 0 mmol L(-1) and 0.5 mmol L(-1) and 0.5 mmol L(-1) and 8.0 mmol L(-1), with detection limits of 0.3 micromol L(-1) and 5.1 micromol L(-1), respectively. The method was then successfully applied to the determination of caffeine content in coffee samples. The effects of pH, electrode composition, step potential, pulse amplitude and square-wave frequency on the voltammetric responses were also investigated.

  15. Second-order advantage maintenance with voltammetric data modeling for quantitation of ethiofencarb in the presence of interferences.

    PubMed

    Diez, Nielene Mora; Cabanillas, Agustina Guiberteau; Silva Rodríguez, Antonio; Goicoechea, Héctor C

    2015-01-01

    This work presents the development of a method based on a voltammetric determination coupled to second-order data modeling with multivariate curve resolution-alternating least-square (MCR-ALS) and unfolded partial least squares regression followed by residual bilinearization (U-PLS/RBL) for the quantitation of the pesticide ethiofencarb in the presence of interferences in tap water. The determination of ethiofencarb by voltammetry is possible on the basis that this pesticide is hydrolysed in alkaline media giving rise to a compound which shows an oxidation peak at Ep=0.80 V. But some other pesticides belonging to the same family can be considered as interferences due to the high overlapping in their signals. The two such interferences are fenobucarb and bendiocarb, which have not been included in the calibration step. The possibility of second-order multivariate calibration was studied by using the hydrolysis time as the third variable, and MCR-ALS and U-PLS/RBL. Good results were obtained in this determination in spite of the high overlapping in voltammetric signals.

  16. Computational design and synthesis of a high selective molecularly imprinted polymer for voltammetric sensing of propazine in food samples.

    PubMed

    Gholivand, Mohammad Bagher; Karimian, Nashmil; Malekzadeh, Ghodratollah

    2012-01-30

    Using a molecularly imprinted polymer (MIP) as a recognition element, the design and construction of a high selective voltammetric sensor for propazine were introduced. A computational approach was developed to study the intermolecular interactions in the pre-polymerization mixture and to find a suitable functional monomer in MIP preparation. Having confirmed the results of computational method, three MIPs were synthesized with functional monomers methacrylic acid (MAA), acrylamide (AAM) and 4-vinylpyridine (4-VP). The results indicated that to prepare MIPs, acrylamide (AAM) is the best candidate. A propazine selective MIP and a nonimprinted polymer (NIP) were synthesized and then incorporated in the carbon paste electrodes (CPEs). The sensor was applied for propazine determination through the cathodic stripping voltammetric method. Two dynamic linear ranges of 0.01-1.0 μmol L(-1) and 1.0-55.0 μmol L(-1) were obtained. The detection limit of the sensor was calculated as 0.001 μmol L(-1). This sensor was used successfully for propazine determination in food samples.

  17. Field Programmable Gate Array (FPGA) Respiratory Monitoring System Using a Flow Microsensor and an Accelerometer

    NASA Astrophysics Data System (ADS)

    Mellal, Idir; Laghrouche, Mourad; Bui, Hung Tien

    2017-04-01

    This paper describes a non-invasive system for respiratory monitoring using a Micro Electro Mechanical Systems (MEMS) flow sensor and an IMU (Inertial Measurement Unit) accelerometer. The designed system is intended to be wearable and used in a hospital or at home to assist people with respiratory disorders. To ensure the accuracy of our system, we proposed a calibration method based on ANN (Artificial Neural Network) to compensate the temperature drift of the silicon flow sensor. The sigmoid activation functions used in the ANN model were computed with the CORDIC (COordinate Rotation DIgital Computer) algorithm. This algorithm was also used to estimate the tilt angle in body position. The design was implemented on reconfigurable platform FPGA.

  18. Compact autonomous voltammetric sensor for sulfide monitoring in deep sea vent habitats

    NASA Astrophysics Data System (ADS)

    Contreira-Pereira, Leonardo; Yücel, Mustafa; Omanovic, Dario; Brulport, Jean-Pierre; Le Bris, Nadine

    2013-10-01

    In situ chemical monitoring at deep-sea hydrothermal vents remains a challenge. Particularly, tools are still scarce for assessing the ranges and temporal variability of sulfide in these harsh environmental conditions. There is a particular need for compact and relatively simple devices to enlarge the capacity of in situ measurements of this major energy source in chemosynthetic ecosystems. With this objective, a voltammetric sensor based on a bare-silver working electrode was developed and tested in real conditions. In the laboratory, the sensor presented a linear response from 10 to 1000 μM sulfide, together with a low pH sensitivity and moderate temperature dependence. The device was operated at 850 and 2500 m depth during 3 cruises over two different vent fields. The autonomous potentiostat (290 mm length, ∅ 35 mm) equipped with laboratory-made electrodes was mounted on a wand, for manipulation from a submersible, or on a holder for unattended deployments. The system was applied in mussel, tubeworm and annelid worm habitats, characterized by different ranges of sulfide concentration, pH and temperature. Calibrations performed before and after each deployment confirmed the stability of the sensor response over a few hours to 11 days, with a maximum drift of 11.4% during this period. Short-term measurements in the vicinity of Riftia pachyptila and Alvinella pompejana were consistent with previous results on these habitats, with concentrations ranging from 20 to 140 μM and 100 to 450 μM and sulfide versus temperature ratio of 14 μM °C-1 and 20 μM °C-1, respectively. A continuous 4-day record on a bed of Bathymodiolus Thermophilus mussels furthermore illustrated the capacity of the sensor to capture fluctuating sulfide concentration between 0 and 70 μM, in combination to temperature, and to investigate the changes in the sulfide versus temperature ratio over time. The method has a higher detection limit (<10 μM) than previous in situ sulfide measurement

  19. Observations on intrauterine oxygen tension measured by fibre-optic microsensors.

    PubMed

    Ottosen, Lars D M; Hindkaer, Johnny; Husth, Merete; Petersen, Dorrit Elschner; Kirk, John; Ingerslev, Hans Jakob

    2006-09-01

    Understanding the biology of reproductive organs is essential for the development of assisted reproductive techniques. There is at present no direct evidence for either the concentration and dynamics of intrauterine oxygen tension at the endometrial surface, nor its importance for the receptiveness of the endometrium. In this study a new method measured mid-cycle (ranging from day 12-18) endometrial surface oxygen tension in 21 patients referred to intrauterine insemination (IUI). Time series was measured online for a period of 5-10 min. The (mean) individual oxygen tension among patients varied from 4 to 27% air saturation. Overall mean oxygen tension among all patients was 11.8% air saturation. Within the same patient, considerable time-related variations were observed. Some patients exhibited rhythmic oscillations with a frequency in the order of 1 min, whereas others did not show any regular patterns. A good description of endometrial surface oxygen concentration and dynamics was thus obtained, but given the relatively small number of participants, an association with pregnancy following insemination could not be established. Further studies using this new method could elucidate the association between individual intrauterine activity, embryo implantation and endometrial surface oxygen tension.

  20. A zirconium dioxide ammonia microsensor integrated with a readout circuit manufactured using the 0.18 μm CMOS process.

    PubMed

    Lin, Guan-Ming; Dai, Ching-Liang; Yang, Ming-Zhi

    2013-03-15

    The study presents an ammonia microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The integrated sensor chip consists of a heater, an ammonia sensor and a readout circuit. The ammonia sensor is constructed by a sensitive film and the interdigitated electrodes. The sensitive film is zirconium dioxide that is coated on the interdigitated electrodes. The heater is used to provide a working temperature to the sensitive film. A post-process is employed to remove the sacrificial layer and to coat zirconium dioxide on the sensor. When the sensitive film adsorbs or desorbs ammonia gas, the sensor produces a change in resistance. The readout circuit converts the resistance variation of the sensor into the output voltage. The experiments show that the integrated ammonia sensor has a sensitivity of 4.1 mV/ppm.

  1. 5A Zirconium Dioxide Ammonia Microsensor Integrated with a Readout Circuit Manufactured Using the 0.18 μm CMOS Process

    PubMed Central

    Lin, Guan-Ming; Dai, Ching-Liang; Yang, Ming-Zhi

    2013-01-01

    The study presents an ammonia microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The integrated sensor chip consists of a heater, an ammonia sensor and a readout circuit. The ammonia sensor is constructed by a sensitive film and the interdigitated electrodes. The sensitive film is zirconium dioxide that is coated on the interdigitated electrodes. The heater is used to provide a working temperature to the sensitive film. A post-process is employed to remove the sacrificial layer and to coat zirconium dioxide on the sensor. When the sensitive film adsorbs or desorbs ammonia gas, the sensor produces a change in resistance. The readout circuit converts the resistance variation of the sensor into the output voltage. The experiments show that the integrated ammonia sensor has a sensitivity of 4.1 mV/ppm. PMID:23503294

  2. A high-Q resonant pressure microsensor with through-glass electrical interconnections based on wafer-level MEMS vacuum packaging.

    PubMed

    Luo, Zhenyu; Chen, Deyong; Wang, Junbo; Li, Yinan; Chen, Jian

    2014-12-16

    This paper presents a high-Q resonant pressure microsensor with through-glass electrical interconnections based on wafer-level MEMS vacuum packaging. An approach to maintaining high-vacuum conditions by integrating the MEMS fabrication process with getter material preparation is presented in this paper. In this device, the pressure under measurement causes a deflection of a pressure-sensitive silicon square diaphragm, which is further translated to stress build up in "H" type doubly-clamped micro resonant beams, leading to a resonance frequency shift. The device geometries were optimized using FEM simulation and a 4-inch SOI wafer was used for device fabrication, which required only three photolithographic steps. In the device fabrication, a non-evaporable metal thin film as the getter material was sputtered on a Pyrex 7740 glass wafer, which was then anodically bonded to the patterned SOI wafer for vacuum packaging. Through-glass via holes predefined in the glass wafer functioned as the electrical interconnections between the patterned SOI wafer and the surrounding electrical components. Experimental results recorded that the Q-factor of the resonant beam was beyond 22,000, with a differential sensitivity of 89.86 Hz/kPa, a device resolution of 10 Pa and a nonlinearity of 0.02% F.S with the pressure varying from 50 kPa to 100 kPa. In addition, the temperature drift coefficient was less than -0.01% F.S/°C in the range of -40 °C to 70 °C, the long-term stability error was quantified as 0.01% F.S over a 5-month period and the accuracy of the microsensor was better than 0.01% F.S.

  3. Development and application of a self-referencing glucose microsensor for the measurement of glucose consumption by pancreatic beta-cells.

    PubMed

    Jung, S K; Trimarchi, J R; Sanger, R H; Smith, P J

    2001-08-01

    Glucose gradients generated by an artificial source and beta-cells were measured using an enzyme-based glucose microsensor, 8-microm tip diameter, as a self-referencing electrode. The technique is based on a difference measurement between two locations in a gradient and thus allows us to obtain real-time flux values with minimal impact of sensor drift or noise. Flux values were derived by incorporation of the measured differential current into Fick's first equation. In an artificial glucose gradient, a flux detection limit of 8.2 +/- 0.4 pmol.cm(-2).s(-1) (mean +/- SEM, n = 7) with a sensor sensitivity of 7.0 +/- 0.4 pA/ mM (mean +/- SEM, n = 16) was demonstrated. Under biological conditions, the glucose sensor showed no oxygen dependence with 5 mM glucose in the bulk medium. The addition of catalase to the bulk medium was shown to ameliorate surface-dependent flux distortion close to specimens, suggesting an underlying local accumulation of hydrogen peroxide. Glucose flux from beta-cell clusters, measured in the presence of 5 mM glucose, was 61.7 +/- 9.5 fmol.nL(-1).s(-1) (mean +/- SEM, n = 9) and could be pharmacologically modulated. Glucose consumption in response to FCCP (1 microM) transiently increased, subsequently decreasing to below basal by 93 +/- 16 and 56 +/- 6%, respectively (mean +/- SEM, n = 5). Consumption was decreased after the application of 10 microM rotenone by 74 +/- 5% (mean +/- SEM, n = 4). These results demonstrate that an enzyme-based amperometric microsensor can be applied in the self-referencing mode. Further, in obtaining glucose flux measurements from small clusters of cells, these are the first recordings of the real-time dynamic of glucose movements in a biological microenvironment.

  4. Simultaneous, real-time measurement of nitric oxide and oxygen dynamics during cardiac ischemia-reperfusion of the rat utilizing sol-gel-derived electrochemical microsensors.

    PubMed

    Kang, Sung Wook; Kim, Ok Kyun; Seo, Bochan; Lee, Sung Ho; Quan, Fu Shi; Shin, Jae Ho; Lee, Gi-Ja; Park, Hun-Kuk

    2013-11-13

    In this study, we simultaneously measured nitric oxide (NO) and oxygen (O2) dynamics in the myocardium during myocardial ischemia-reperfusion (IR) utilizing sol-gel modified electrochemical NO and O2 microsensors. In addition, we attempted to clarify the correlation between NO release in the ischemic period and O2 restoration in the myocardium after reperfusion, comparing a control heart with a remote ischemic preconditioning (RIPC)-treated heart as an attractive strategy for myocardial protection. Rat hearts were randomly divided into two groups: a control group (n=5) and an RIPC group (n=5, with RIPC treatment). Myocardia that underwent RIPC treatment (182±70 nM, p<0.05) released more NO during the ischemic period than those of the control group (63±41 nM). The restoration value of oxygen tension (pO2) in the RIPC group significantly increased and was restored to pre-ischemic levels (92.6±36.8%); however, the pO2 of the control group did not increase throughout the reperfusion period (5.7±7.5%, p=0.001). Myocardial infarct size measurements revealed a significant decrease in cell death in the myocardium region of the RIPC group (41.44±6.42%, p=0.001) compared with the control group (60.05±10.91%). As a result, we showed that the cardioprotective effect of RIPC could be attributed to endogenous NO production during the ischemic period, which subsequently promoted reoxygenation in post-ischemic myocardia during early reperfusion. Our results suggest that the promotion of endogenous formation during an ischemic episode might be helpful as a therapeutic strategy for protecting the myocardium from IR injury. Additionally, our NO and O2 perm-selective microsensors could be utilized to evaluate the effect of drug or treatment.

  5. A High-Q Resonant Pressure Microsensor with Through-Glass Electrical Interconnections Based on Wafer-Level MEMS Vacuum Packaging

    PubMed Central

    Luo, Zhenyu; Chen, Deyong; Wang, Junbo; Li, Yinan; Chen, Jian

    2014-01-01

    This paper presents a high-Q resonant pressure microsensor with through-glass electrical interconnections based on wafer-level MEMS vacuum packaging. An approach to maintaining high-vacuum conditions by integrating the MEMS fabrication process with getter material preparation is presented in this paper. In this device, the pressure under measurement causes a deflection of a pressure-sensitive silicon square diaphragm, which is further translated to stress build up in “H” type doubly-clamped micro resonant beams, leading to a resonance frequency shift. The device geometries were optimized using FEM simulation and a 4-inch SOI wafer was used for device fabrication, which required only three photolithographic steps. In the device fabrication, a non-evaporable metal thin film as the getter material was sputtered on a Pyrex 7740 glass wafer, which was then anodically bonded to the patterned SOI wafer for vacuum packaging. Through-glass via holes predefined in the glass wafer functioned as the electrical interconnections between the patterned SOI wafer and the surrounding electrical components. Experimental results recorded that the Q-factor of the resonant beam was beyond 22,000, with a differential sensitivity of 89.86 Hz/kPa, a device resolution of 10 Pa and a nonlinearity of 0.02% F.S with the pressure varying from 50 kPa to 100 kPa. In addition, the temperature drift coefficient was less than −0.01% F.S/°C in the range of −40 °C to 70 °C, the long-term stability error was quantified as 0.01% F.S over a 5-month period and the accuracy of the microsensor was better than 0.01% F.S. PMID:25521385

  6. Application of Global Positioning System and Microsensor Technology in Competitive Rugby League Match-Play: A Systematic Review and Meta-analysis.

    PubMed

    Hausler, Joanne; Halaki, Mark; Orr, Rhonda

    2016-04-01

    The use of global positioning system (GPS) devices with the inclusion of microsenor technology in rugby league enables measurement of player activity profiles to understand the demands of match-play and optimise on-field performance. The aim of this review was to systematically review the use of GPS and microsensor technology to quantify player activity profiles in match-play, and conduct a meta-analysis of relevant movement variables in order to present the contemporary and emerging themes within rugby league. A systematic search of electronic databases (MEDLINE, SPORTDiscus, CINAHL, Web of Science, Scopus, ScienceDirect, EMBASE, and Google Scholar) from the earliest record to February 2015 was conducted. Permutations of key words included GPS, microtechnology, activity profiles, match demands (movement or physical demands), and rugby league. A meta-analysis was conducted to provide a pooled mean and confidence intervals on comparable data from at least three studies. Twenty-seven studies met the eligibility criteria and included 1270 male participants. The studies reported on GPS use in elite competition (n = 16) with limited representation of other competition standards: sub-elite (n = 6), amateur (n = 1) and junior (n = 3). All studies reported on movement variables (distance, relative distance, speed and accelerations), with studies analysing movement at high speed (n = 18, 66.7%), evaluating collision or impact variables (n = 15, 55.6%) and determining the metabolic energy (n = 2, 7.4%) associated with rugby league match-play. Activity profiles of varying positions, positional groups and levels of rugby league competition were described. Meta-analysis indicated that the total distance covered by backs and adjustables were both greater than forward positions, but adjustables covered greater relative distance than forwards and backs. Speed zones were typically categorised into six speed zones ranging from 0 to 36 km·h(-1), or into low- and high

  7. Voltammetric Detection of Urea on an Ag-Modified Zeolite-Expanded Graphite-Epoxy Composite Electrode

    PubMed Central

    Manea, Florica; Pop, Aniela; Radovan, Ciprian; Malchev, Plamen; Bebeselea, Adriana; Burtica, Georgeta; Picken, Stephen; Schoonman, Joop

    2008-01-01

    In this paper, a modified expanded graphite composite electrode based on natural zeolitic volcanic tuff modified with silver (EG-Ag-Z-Epoxy) was developed. Cyclic voltammetry measurements revealed a reasonably fast electron transfer and a good stability of the electrode in 0.1 M NaOH supporting electrolyte. This modified electrode exhibited moderate electrocatalytic effect towards urea oxidation, allowing its determination in aqueous solution. The linear dependence of the current versus urea concentration was reached using square-wave voltammetry in the concentrations range of urea between 0.2 to 1.4 mM, with a relatively low limit of detection of 0.05 mM. A moderate enhancement of electroanalytical sensitivity for the determination of urea at EG-Ag-Z-Epoxy electrode was reached by applying a chemical preconcentration step prior to voltammetric/amperometric quantification. PMID:27873841

  8. Voltammetric analysis of Cu (II), Cd (II) and Zn (II) complexes and their cyclic voltammetry with several cephalosporin antibiotics.

    PubMed

    Abo El-Maali, N; Osman, A H; Aly, A A M; Al-Hazmi, G A A

    2005-02-01

    Both osteryoung square wave voltammetry and cyclic voltammetry have been utilized to elucidate and confirm the possible complexation reaction that occur between the various cephalosporin antibiotics and either the toxic, non-essential metal ion, viz. Cd (II), or the essential but toxic (when their concentration exceeds certain level in serum) metal ions, viz. Cu (II) and Zn (II). Voltammetric measurements indicated the existence of 1:1 metal-to-ligand ratio (as in cephalexin and cephapirin complexes), 1:2 ratio (such as in cefamandole, cefuroxime and cefotaxime complexes) and 2:1 ratio in case of ceftazidime complexes. Adsorption behavior was evidenced for Cu (II)-cefuroxime or ceftazidime complexes as well as for those for Zn (II)-cephalexin or cephapirin. This phenomenon could be used for the determination of either the antibiotic or the metal ion using adsorptive stripping voltammetry. Detection limits down to 7x10(-10) M have been easily achieved.

  9. The Application of Nafion Metal Catalyst Free Carbon Nanotube Modified Gold Electrode: Voltammetric Zinc Detection in Serum

    PubMed Central

    Yue, Wei; Bange, Adam; Riehl, Bill L.; Johnson, Jay M.; Papautsky, Ian; Heineman, William R.

    2013-01-01

    Metal catalyst free carbon nanotube (MCFCNT) whiskers were first used as an electrode modification material on a gold electrode surface for zinc voltammetric measurements. A composite film of Nafion and MCFCNT whiskers was applied to a gold electrode surface to form a mechanically stable sensor. The sensor was then used for zinc detection in both acetate buffer solution and extracted bovine serum solution. A limit of detection of 53 nM was achieved for a 120 s deposition time. The zinc in bovine serum was extracted via a double extraction procedure using dithizone in chloroform as a zinc chelating ligand. The modified electrode was found to be both reliable and sensitive for zinc measurements in both matrices. PMID:24436574

  10. Differential pulse voltammetric determination of nanomolar concentrations of antiviral drug acyclovir at polymer film modified glassy carbon electrode.

    PubMed

    Dorraji, Parisa S; Jalali, Fahimeh

    2016-04-01

    An electrochemical sensor for the sensitive detection of acyclovir was developed by the electropolymerization of Eriochrome black T at a pretreated glassy carbon electrode. The surface morphology of the modified electrode was characterized by field emission scanning electron microscopy. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of acyclovir on the modified electrode surface relative to the unmodified electrode. The detection limit of 12 nM and two linear calibration ranges of 0.03-0.3 μM and 0.3-1.5 μM were obtained for acyclovir determination using a differential pulse voltammetric method in acetate buffer (0.1 M, pH 4.0). Real sample studies were carried out in human blood serum and pharmaceutical formulations, which offered good recovery (98-102%). The electrode showed excellent reproducibility, selectivity and antifouling effects.

  11. Voltammetric Behavior and Determination of Trace Amounts of Omeprazole Using an Edge-plane Pyrolytic Graphite Electrode

    PubMed Central

    Shahrokhian, Saeed; Ghalkhani, Masoumeh; Bayat, Maryam; Ghorbani-Bidkorbeh, Fatemeh

    2015-01-01

    The voltammetric performance of edge-plane pyrolytic graphite (EPG) electrode via adsorptive stripping voltammetry was investigated for study of the electrochemical behavior of omeprazole (OMZ) in aqueous solution. The results revealed that the oxidation of OMZ is an irreversible pH-dependent process that proceeds with the transfer of one electron and one proton in an adsorption-controlled mechanism. The determination conditions, such as the pH values of the supporting electrolyte, accumulation time and scan rate were optimized. Simplicity, high reproducibility and low detection limit (3 nM) of the electrode response as well as wide linear range (0.01 to 4.0 µM) can be stated as significant features of this electrode. The EPG electrode was successfully applied for the determination of OMZ in pharmaceutical formulations and satisfactory results were obtained. PMID:25901153

  12. Voltammetric iodometric titration of ascorbic acid with dead-stop end-point detection in fresh vegetables and fruit samples.

    PubMed

    Verdini, R A; Lagier, C M

    2000-07-01

    The present work describes a method for determining ascorbic acid, which combines iodometry with a voltammetric technique to detect the end point of the titration. In addition, the validity of the method applied to natural vegetable or fruit samples was assessed. The results were compared with those obtained by an accurate method such as HPLC using UV detection. Similar values of ascorbic acid for different natural samples were obtained by means of this approach (p > 0.05). The limit of quantification was 0.1 mg. This technique presents the advantage of other electroanalytical methods such as avoiding filtration or ultracentrifugation steps, with the additional benefit of using the platinum electrodes, which are routinely used in the laboratory. These facts allow a rapid and efficient quantification of ascorbic acid with very low cost of reagents and equipment.

  13. Data Fusion from Voltammetric and Potentiometric Sensors to Build a Hybrid Electronic Tongue Applied in Classification of Beers

    NASA Astrophysics Data System (ADS)

    Haddi, Zouhair; Amari, Aziz; Bouchikhi, Benachir; Gutiérrez, Juan Manuel; Cetó, Xavier; Mimendia, Aitor; del Valle, Manel

    2011-09-01

    A hybrid electronic tongue based on data fusion of two different sensor families was built and used to recognize three types of beer. The employed sensor array was formed by three modified graphite-epoxy voltammetric sensors plus six potentiometric sensors with cross-sensitivity. The sensors array coupled with feature extraction and pattern recognition methods, namely Principal Component Analysis (PCA) and Discriminant Factor Analysis (DFA), were trained to classify the data clusters related to different beer types. PCA was used to visualize the different categories of taste profiles and DFA with leave-one-out cross validation approach permitted the qualitative classification. According to the DFA model, 96% of beer samples were correctly classified. The aim of this work is to prove performance of hybrid electronic tongue systems by exploiting the new approach of data fusion of different sensor families, in comparison of electronic tongue with only one sensor type.

  14. Remaining useful life measurements of diesel engine oils, automotive engine oils, hydraulic fluids, and greases using cyclic voltammetric methods

    SciTech Connect

    Kauffman, R.E.

    1995-03-01

    This paper presents the results of research designed to develop a remaining useful life evaluation rig (RULER) from cyclic voltammetric methods for diesel engine oils, automotive engine oils, hydraulic fluids, and greases. The RULER requires less than one millimeter of sample, less than one minute to perform, and very little technical expertise. Samples of laboratory-stressed and authentic-used oils, fluids, and greases were used in the development of the RULER. The results of this research demonstrate that remaining useful life measurements made by the RULER can be used by oil analysis programs to quantify antioxidant levels of incoming and stored supplies, to predict and extend oil change intervals for normally operating equipment, and to detect abnormally operating equipment prior to malfunction. 13 refs., 8 figs.

  15. Voltammetric Detection of Oxalic Acid by Using Glassy Carbon Electrodes with Covalently Attached Nitrogen-containing Functional Groups.

    PubMed

    Matsuura, Hiroaki; Akabe, Syuhei; Kitamura, Tsubasa; Takahashi, Takuto; Uchiyama, Shunichi

    2015-01-01

    We report on a novel voltammetric detection of oxalic acid by using glassy carbon electrodes with covalently attached nitrogen-containing functional groups prepared by stepwise electrolysis. A glassy carbon electrode electrooxidized in an ammonium carbamate solution was electroreduced at -1.0 V (vs. Ag/AgCl) in 1.0 M sulfuric acid for a long time. We found that the electrocatalytic oxidation wave of oxalic acid obtained by this modified glassy carbon electrode was moved to a more negative potential region than that obtained by a platinum electrode in an acidic medium. A good linearity for the peak current signals was observed in the concentration range from 0.1 to 50 mM.

  16. Dual-Frequency Alternating Current Designer Waveform for Reliable Voltammetric Determination of Electrode Kinetics Approaching the Reversible Limit.

    PubMed

    Li, Jiezhen; Bentley, Cameron L; Bond, Alan M; Zhang, Jie

    2016-02-16

    Alternating current (ac) voltammetry provides access to faster electrode kinetics than direct current (dc) methods. However, difficulties in ac and other methods arise when the heterogeneous electron-transfer rate constant (k(0)) approaches the reversible limit, because the voltammetric characteristics become insensitive to electrode kinetics. Thus, in this near-reversible regime, even small uncertainties associated with bulk concentration (C), diffusion coefficient (D), electrode area (A), and uncompensated resistance (Ru) can lead to significant systematic error in the determination of k(0). In this study, we have introduced a kinetically sensitive dual-frequency designer waveform into the Fourier-transformed large-amplitude alternating current (FTAC) voltammetric method that is made up of two sine waves having the same amplitude but with different frequencies (e.g., 37 and 615 Hz) superimposed onto a dc ramp to quantify the close-to-reversible Fc(0/+) process (Fc = ferrocene) in two nonhaloaluminate ionic liquids. The concept is that from a single experiment the lower-frequency data set, collected on a time scale where the target process is reversible, can be used as an internal reference to calibrate A, D, C, and Ru. These calibrated values are then used to calculate k(0) from analysis of the harmonics of the higher-frequency data set, where the target process is quasi-reversible. With this approach, k(0) values of 0.28 and 0.11 cm·s(-1) have been obtained at a 50 μm diameter platinum microdisk electrode for the close-to-diffusion-controlled Fc(0/+) process in two ionic liquids, 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide and 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, respectively.

  17. Voltammetric extraction of heparin and low-molecular-weight heparin across 1,2-dichloroethane/water interfaces.

    PubMed

    Jing, Ping; Kim, Yushin; Amemiya, Shigeru

    2009-12-01

    Heparin and low-molecular-weight heparin are voltammetrically extracted across 1,2-dichloroethane/water interfaces for the detection of these highly sulfated polysaccharides widely used as anticoagulants/antithrombotics in many medical procedures. A new heparin ionophore, 1-[4-(dioctadecylcarbamoyl)butyl]guanidinium, is the first to enable the voltammetric extraction of various polyanionic heparins with average molecular weights of up to approximately 20 kDa including those in commercial preparations (i.e., Arixtra (1.5 kDa), Lovenox (4.5 kDa), and unfractionated heparin (15 kDa), as well as chromatographically fractionated heparins (7, 9, 15, and 20 kDa)). Facilitated Arixtra extraction is fully and quantitatively characterized by micropipet voltammetry to propose that cooperative effects from strong heparin-binding capability and high lipophilicity of this ionophore are required for the formation of an electrically neutral and highly lipophilic complex of a heparin molecule with multiple ionophore molecules to be extracted into the nonpolar organic phase. At the same time, the participation of multiple ionophore molecules in interfacial complexation with a heparin molecule slows down its extraction across the interface. This kinetic limitation is enhanced by fast mass transfer at a micropipet-supported interface to compromise thermodynamically favorable selectivity for heparin and an important contaminant, oversulfated chondroitin sulfate, thereby requiring a macroscopic interface for sensing applications. Another highly lipophilic guanidinium ionophore, N,N-dioctadecylguanidinium, cannot completely extract even Arixtra, which indicates the importance of elaborate ionophore design for heparin extraction.

  18. The redox behaviour of diazepam (Valium®) using a disposable screen-printed sensor and its determination in drinks using a novel adsorptive stripping voltammetric assay.

    PubMed

    Honeychurch, Kevin C; Crew, Adrian; Northall, Hannah; Radbourne, Stuart; Davies, Owian; Newman, Sam; Hart, John P

    2013-11-15

    In this study we investigated the possibility of applying disposable electrochemical screen-printed carbon sensors for the rapid identification and quantitative determination of diazepam in beverages. This was achieved utilising a previously unreported oxidation peak. The origin of this peak was investigated further by cyclic voltammetry and gas chromatography/mass spectroscopy. At pH 6 the voltammetric behaviour of this oxidation process was found to involve adsorption of the drug allowing for the development of an adsorptive stripping voltammetric assay. Experimental conditions were then optimised for the determination of diazepam in a beverage sample using a medium exchange technique. It was shown that no elaborate extraction procedures were required as the calibration plots obtained in the absence and presence of the beverage were very similar. © 2013 Elsevier B.V. All rights reserved.

  19. Using of multi-walled carbon nanotubes electrode for adsorptive stripping voltammetric determination of ultratrace levels of RDX explosive in the environmental samples.

    PubMed

    Rezaei, Behzad; Damiri, Sajjad

    2010-11-15

    A study of the electrochemical behavior and determination of RDX, a high explosive, is described on a multi-walled carbon nanotubes (MWCNTs) modified glassy carbon electrode (GCE) using adsorptive stripping voltammetry and electrochemical impedance spectroscopy (EIS) techniques. The results indicated that MWCNTs electrode remarkably enhances the sensitivity of the voltammetric method and provides measurements of this explosive down to the sub-mg/l level in a wide pH range. The operational parameters were optimized and a sensitive, simple and time-saving cyclic voltammetric procedure was developed for the analysis of RDX in ground and tap water samples. Under optimized conditions, the reduction peak have two linear dynamic ranges of 0.6-20.0 and 8.0-200.0 mM with a detection limit of 25.0 nM and a precision of <4% (RSD for 8 analysis).

  20. Preparation, characterization and electrochemical application of Ag-ZnO nanoplates for voltammetric determination of glutathione and tryptophan using modified carbon paste electrode.

    PubMed

    Beitollahi, Hadi; Gholami, Abbas; Ganjali, Mohammad Reza

    2015-12-01

    Ag-ZnO nanoplates and 2-chlorobenzoyl ferrocene were synthesized and used to construct a modified carbon paste electrode. The electrooxidation of glutathione at the surface of the modified electrode was studied. Under the optimized conditions, the square wave voltammetric (SWV) peak current of glutathione increased linearly with glutathione concentrations in the range of 5.0 × 10(-8) to 2.0 × 10(-4)M with sensitivity of 0.659 μA μM(-1) and method detection limit of 20.0 nM was obtained for glutathione. The prepared modified electrode exhibits a very good resolution between the voltammetric peaks of glutathione and tryptophan which makes it suitable for the detection of glutathione in the presence of tryptophan in real samples.

  1. Microfabricated tin-film electrodes for protein and DNA sensing based on stripping voltammetric detection of Cd(II) released from quantum dots labels.

    PubMed

    Kokkinos, Christos; Economou, Anastasios; Petrou, Panagiota S; Kakabakos, Sotirios E

    2013-11-19

    A novel disposable microfabricated tin-film electrochemical sensor was developed for the detection of proteins and DNA. The sensor was fabricated on a silicon wafer through photolithography to define the sensor geometry followed by tin sputtering. A sandwich-type immunoassay with biotinylated reporter antibody was employed for the determination of prostate-specific antigen (PSA) in human serum samples. For the detection of C533G mutation of the RET gene, biotinylated oligonucleotide probes were used. The biotinylated biomolecular probes were labeled with streptavidin (STV)-conjugated CdSe/ZnS quantum dots (QDs); quantification of the analytes was performed through acidic dissolution of the QDs and stripping voltammetric detection of the Cd(II) released. The proposed QD-based electrochemical sensor overcomes the limitations of existing voltammetric sensors and provides a mercury-free sensing platform with scope for mass-production and further potential for application in clinical diagnostics.

  2. Highly selective and sensitive voltammetric sensor based on modified multiwall carbon nanotube paste electrode for simultaneous determination of ascorbic acid, acetaminophen and tryptophan.

    PubMed

    Keyvanfard, Mohsen; Shakeri, Razieh; Karimi-Maleh, Hassan; Alizad, Khadijeh

    2013-03-01

    A carbon-paste electrode modified with multiwall carbon nanotubes (MWCNTs) was used for the sensitive and selective voltammetric determination of ascorbic acid (AA) in the presence of 3,4-dihydroxycinnamic acid (3,4-DHCA) as mediator. The mediated oxidation of AA at the modified electrode was investigated by cyclic voltammetry (CV), chronoamperommetry and electrochemical impedance spectroscopy (EIS). Also, the values of catalytic rate constant (k), and diffusion coefficient (D) for AA were calculated. Using square wave voltammetry (SWV), a highly selective and simultaneous determination of AA, acetaminophen (AC) and tryptophan (Trp) has been explored at the modified electrode. The modified electrode displayed strong function for resolving the overlapping voltammetric responses of AA, AC and Trp into three well-defined voltammetric peaks. In the mixture containing AA, AC and Trp, the three compounds can well separate from each other with potential differences of 200, 330 and 530 mV between AA and AC, AC and Trp and AA and Trp, respectively, which was large enough to determine AA, AC and Trp individually and simultaneously.

  3. The renewable bismuth bulk annular band working electrode: fabrication and application in the adsorptive stripping voltammetric determination of nickel(II) and cobalt(II).

    PubMed

    Baś, Bogusław; Węgiel, Krystian; Jedlińska, Katarzyna

    2015-06-30

    The paper presents the first report on fabrication and application of a user friendly and mercury free electrochemical sensor, with the renewable bismuth bulk annular band working electrode (RBiABE), in stripping voltammetry (SV). The sensor body is partly filled with the internal electrolyte solution, in which the RBiABE is cleaned and activated before each measurement. Time of the RBiABE contact with the sample solution is precisely controlled. The usefulness of this sensor was tested by Ni(II) and Co(II) traces determination by means of differential pulse adsorptive stripping voltammetry (DP AdSV), after complexation with dimethylglyoxime (DMG) in ammonia buffer (pH 8.2). The experimental variables (composition of the supporting electrolyte, pre-concentration potential and time, potential of the RBiABE activation, and DP parameters), as well as possible interferences, were investigated. The linear calibration graphs for Ni(II) and Co(II), determined individually and together, in the range from 1×10(-8) to 70×10(-8)molL(-1) and from 1×10(-9) to 70×10(-9)molL(-1) respectively, were obtained. The calculated limit of detection (LOD), for 30s of the accumulation time, was 3×10(-9)molL(-1) for Ni(II) in case of a single element's analysis, whereas the LOD was 5×10(-9)molL(-1) for Ni(II) and 3×10(-10)molL(-1) for Co(II), when both metal ions were measured together. The repeatability of the Ni(II) and Co(II) adsorptive stripping voltammetric signals obtained at the RBiABE were equal to 5.4% and 2.5%, respectively (n=5). Finally, the proposed method was validated by determining Ni(II) and Co(II) in the certified reference waters (SPS-SW1 and SPS-SW2) with satisfactory results.

  4. Electrochemical studies of DNA interaction and antimicrobial activities of MnII, FeIII, CoII and NiII Schiff base tetraazamacrocyclic complexes

    NASA Astrophysics Data System (ADS)

    Kumar, Anuj; Vashistha, Vinod Kumar; Tevatia, Prashant; Singh, Randhir

    2017-04-01

    Tetraazamacrocyclic complexes of MnII, FeIII, CoII and NiII have been synthesized by template method. These tetraazamacrocycles have been analyzed with various techniques like molar conductance, IR, UV-vis, mass spectral and cyclic voltammetric studies. On the basis of all these studies, octahedral geometry has been assigned to these tetraazamacrocyclic complexes. The DNA binding properties of these macrocyclic complexes have been investigated by electronic absorption spectra, fluorescence spectra, cyclic voltammetric and differential pulse voltammetric studies. The cyclic voltammetric data showed that ipc and ipa were effectively decreased in the presence of calf thymus DNA, which is a strong evidence for the interaction of these macrocyclic complexes with the calf thymus DNA (ct-DNA). The heterogeneous electron transfer rate constant found in the order: KCoII > KNiII > KMnII which indicates that CoII macrocyclic complex has formed a strong intercalated intermediate. The Stern-Volmer quenching constant (KSV) and voltammetric binding constant were found in the order KSV(CoII) > KSV(NiII) > KSV(MnII) and K+(CoII) > K+(NiII) > K+(MnII) which shows that CoII macrocyclic complex exhibits the high interaction affinity towards ct-DNA by the intercalation binding. Biological studies of the macrocyclic complexes compared with the standard drug like Gentamycin, have shown antibacterial activities against E. coli, P. aeruginosa, B. cereus, S. aureus and antifungal activity against C. albicans.

  5. Electrochemical behavior and voltammetric determination of norfloxacin at glassy carbon electrode modified with multi walled carbon nanotubes/Nafion.

    PubMed

    Huang, Ke-Jing; Liu, Xue; Xie, Wan-Zhen; Yuan, Hong-Xia

    2008-07-15

    A simple and rapid electrochemical method is developed for the determination of trace-level norfloxacin, based on the excellent properties of multi-walled carbon nanotubes (MWCNTs). The MWCNTs/Nafion film-coated glassy carbon electrode (GCE) is constructed and the electrochemical behavior of norfloxacin at the electrode is investigated in detail. The results indicate that MWCNTs modified glassy carbon electrode exhibited efficiently electrocatalytic oxidation for norfloxacin (NFX) with relatively high sensitivity, stability and life time. Under conditions of cyclic voltammetry, the current for oxidation of selected analyte is enhanced significantly in comparison to the bare GCE. The electrocatalytic behavior is further exploited as a sensitive detection scheme for the analyte determinations by linear sweep voltammetry (LSV). Under optimized condition in voltammetric method the concentration calibration range and detection limit (S/N=3) are 0.1-100 micromol/L and 5 x 10(-8)mol/L for NFX. The proposed method was successfully applied to NFX determination in tablets. The analytical performance of this sensor has been evaluated for detection of the analyte in urine as a real sample.

  6. Rapid determination of total polyphenolic content in tea samples based on caffeic acid voltammetric behaviour on a disposable graphite electrode.

    PubMed

    David, Iulia Gabriela; Bizgan, Ana-Maria Cristina; Popa, Dana Elena; Buleandra, Mihaela; Moldovan, Zenovia; Badea, Irinel Adriana; Tekiner, Tuğçe Ayça; Basaga, Huveyda; Ciucu, Anton A

    2015-04-15

    The present paper describes the voltammetric behaviour and the quantitative determination of caffeic acid (CA) on a disposable pencil graphite electrode (PGE). The anodic peak current of CA recorded by differential pulse voltammetry (DPV) varies linearly with CA concentration in the range 1×10(-7)-3×10(-3) M. The detection and quantification limits were 8.83×10(-8) M and 2.94×10(-7) M caffeic acid, respectively. The mean recoveries of CA from Turkish green, white and black teas were 98.30%, 99.57% and 91.46%. For these three tea types the corresponding total polyphenolic contents (TPCs) evaluated by DPV on PGE were 35.81, 34.59 and 31.21 mg caffeic acid equivalent/g tea, respectively. These TPC values were in good accordance with those obtained by the Folin-Ciocalteu method. The developed DPV on PGE method constitutes a simple and inexpensive tool for the rapid assessment of TPC of tea samples.

  7. Sensitive voltammetric determination of tryptophan using an acetylene black paste electrode modified with a Schiff's base derivative of chitosan.

    PubMed

    Deng, Peihong; Fei, Junjie; Feng, Yonglan

    2011-12-21

    Chitosan was modified by salicylaldehyde via Schiff's base reaction and the resulting product was modified on the surface of an acetylene black paste electrode (ABPE) by the drop-coating method. In 0.5 mol L(-1) acetate buffer (pH 4.2), a substantial increase in the anodic stripping peak current of tryptophan (Trp) (compared to conventional bare carbon paste electrode (CPE) and bare ABPE) is observed at the Schiff's base chitosan-modified electrode. The parameters influencing voltammetric determination of Trp have been optimized. Under the selected conditions, the linearity between the anodic peak currents and concentrations of Trp demonstrated a wide range of 6.0 × 10(-8) mol L(-1) to 2.0 × 10(-6) mol L(-1), 2.0 × 10(-6) mol L(-1) to 4.0 × 10(-5) mol L(-1) and 4.0 × 10(-5) mol L(-1) to 1.0 × 10(-4) mol L(-1), a low detection limit of 2.0 × 10(-9) mol L(-1) was obtained after a 60 s accumulation. In addition, the developed electrochemical sensor has been successfully applied for the determination of Trp in pharmaceutical and biological samples with satisfactory assay results.

  8. Voltammetric heparin-selective electrode based on thin liquid membrane with conducting polymer-modified solid support.

    PubMed

    Guo, Jidong; Amemiya, Shigeru

    2006-10-01

    A novel, solid-supported voltammetric ion-selective electrode to detect anticoagulant/antithrombotic heparin at polarizable poly(vinyl chloride) (PVC) membrane/water interfaces was developed. An approximately 3-4.5-microm-thick PVC membrane plasticized with 2-nitrophenyl octyl ether was supported on a gold electrode modified with a poly(3-octylthiophene) (POT) film as an ion-to-electron transducer. Charge transport through the PVC-covered POT film is electrochemically reversible, as demonstrated by cyclic voltammetry with nonpolarizable membrane/water interfaces. In addition to the fast charge transport, adequate redox capacity of the POT film and a small ohmic potential drop in the thin PVC membrane enable ion transfer voltammetry at polarizable macroscopic membrane/water interfaces in a standard three-electrode cell. Reversible ClO4- transfer at the interfaces coupled with oxidation of a neutral POT film was examined by cyclic voltammetry to determine the distribution of the applied potential to the two polarizable interfaces by convolution technique. Interfacial adsorption and desorption of heparin facilitated by octadecyltrimethylammonium were studied also by cyclic voltammetry and convolution technique to demonstrate that the processes are electrochemically irreversible. Stripping voltammetry based on the interfacial processes gives a low detection limit of 0.005 unit/mL heparin in a saline solution, which is slightly lower than the detection limit of most sensitive heparin sensors reported so far (0.01 unit/mL).

  9. Separation and determination of the macrolide antibiotics (erythromycin, spiramycin and oleandomycin) by capillary electrophoresis coupled with fast reductive voltammetric detection.

    PubMed

    Zhou, J; Chen, Y; Cassidy, R

    2000-04-01

    Separation and determination of erythromycin, spiramycin and oleandomycin by capillary zone electrophoresis coupled with fast reductive voltammetric detection using an Hg-film electrode was investigated in a simple aqueous phosphate buffer system. The influence of pH, concentration of phosphate, applied voltage, capillary length and dimension on the separation was examined and optimized. The entire separation of erythromycin, spiramycin, and oleandomycin was achieved in a 0.2 mol/L phosphate buffer system without organic modifiers. The electrochemical detection parameters, such as electrode material, applied waveform, scan rate, preconcentration potentials and preconcentration times, were investigated and discussed. This approach provides high separation efficiency and high sensitivity for all compounds, with detection limits (3 x peak-to-peak baseline noise) of 7.5 x 10(-8) mol/L for spiramycin, and 3 x 10(-7) mol/ L for erythromycin and oleandomycin. The calibration plot of peak areas for each separated peak vs. concentration of analyte was found to be linear over three orders of magnitude.

  10. Catalytic-adsorptive stripping voltammetric determination of ultra-trace iridium(III). Application to fresh- and sea-water.

    PubMed

    Locatelli, Clinio

    2011-07-15

    An extremely sensitive stripping voltammetric procedure for ultra-trace determination of iridium(III) is reported. The method is based on the interfacial accumulation of the iridium(III)-CTAB complex onto the glassy carbon electrode, followed by the catalytic reduction of the adsorbed complex in the presence of bromate. 0.3 mol L(-1) acetate buffer pH 4.7+6.9×10(-2) mol L(-1) NaBrO(3)+2.7×10(-5)mol L(-1) cetyltrimethylammonium bromide (CTAB)+0.2 mol L(-1) KCl was employed as the supporting electrolyte. The analytical procedure was verified by the analysis of the standard reference materials: Sea Water BCR-CRM 403 and Fresh Water NIST-SRM 1643d. The accuracy, expressed as relative error e%, was satisfactory, being lower than 6%, while precision as repeatability, expressed as relative standard deviation s(r)%, was generally lower than 5%. The limit of detection was of the order of 2-3 ng L(-1). Once set up on the standard reference materials, the analytical procedure was transferred and applied to superficial water sampled in proximity to superhighway and in the Po river mouth area. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Voltammetric and spectroscopic studies on binding of antitumor Morin, Morin-Cu complex and Morin-β-cyclodextrin with DNA

    NASA Astrophysics Data System (ADS)

    Temerk, Y. M.; Ibrahim, M. S.; Kotb, M.

    2009-01-01

    A systematic comparative study of the binding of antitumor Morin and its complexes with DNA has been investigated in the Britton-Robison (BR) buffer solutions using voltammetric and spectroscopic methods. The results show that Morin molecule, acting as an intercalator, is inserted into the cavity of the β-cyclodextrin (β-CD) as well as into the base stacking domain of the DNA double helix. The interaction of Morin-Cu complex or the inclusion complex of Morin-β-CD with ds-DNA causes hypochromism in the absorption spectra, along with pronounced changes in the electrochemical behavior of the Morin complexes. An isobestic point and a new spectrum band appeared indicating the formation of the new system of Morin-Cu-DNA at λm = 391 nm and Morin-β-CD-DNA at λm = 375 nm. The intercalation of Morin-Cu and Morin-β-CD complexes with DNA produces an electrochemically inactive supramolecular complex. The binding constants were calculated from the increase of the solubility, the strong hypochromism, and the decrease in peak current of Morin and its complexes upon the addition of the host molecules. Calculation of the thermodynamic parameters of the interaction of the inclusion complex of Morin-β-CD with DNA, including Gibbs free energy change, Helmholz free energy and entropy change shows that the complexation is a spontaneous process of association.

  12. Design and Optimization of a New Voltammetric Method for Determination of Isoniazid by Using PEDOT Modified Gold Electrode in Pharmaceuticls.

    PubMed

    Demirkaya-Miloglu, Fatma; Oznuluer, Tuba; Ozdurak, Buket; Miloglu, Elmas

    2016-01-01

    Isoniazid (INH) was studied with regard to its electrochemical treatment on a strongly alkaline solution of a poly (3,4-ethylenedioxythiophene)-modified gold electrode, using both cyclic voltammetric and controlled potential techniques. Electrocatalytic performance measurements of this composite electrode toward oxidation of INH exhibited an increase of 4-folds in oxidation peak densities compared to the bare gold electrode. Central composite design method was used to obtain optimum experimental conditions, and used critical parameters (pH (A), scan rate (mV/s, B) and temperature (C, C) to assess the effects on amperometric response. Optimum experimental conditions were achieved by using a pH of 9.2 with a scan rate of 260 mV/s and a temperature of 30 C. Under these circumstances, a good linear relationship was observed between peak current densities and INH concentration in the range of 0.05-2 μM, with correlation coefficient of 0.9998. Furthermore, the method was very sensitive (limit of quantitation, 0.0043 μM), accurate (relative error, -5.65 to 4.03) and precise (relative standard deviation %, ≤ 7.97). The method was also applied to determine INH in pharmaceutical formulations, and statistically compared the results with the official method using the two one-sided equivalence test; the results were in good agreement with those obtained by the official and reported methods.

  13. Sensitive voltammetric determination of thymol in essential oil of Carum copticum seeds using boron-doped diamond electrode.

    PubMed

    Stanković, Dalibor M

    2015-10-01

    Essential oil of Carum copticum seeds, obtained from a local shop, was extracted and content of thymol was analyzed using square-wave voltammetry at boron-doped diamond electrode. The effect of various parameters, such as pH of supporting electrolyte and square-wave voltammetric parameters (modulation amplitude and frequency), was examined. In Britton-Robinson buffer solution (pH 4), thymol provided a single and oval-shaped irreversible oxidation peak at +1.13 V versus silver/silver chloride potassium electrode (3M). Under optimal experimental conditions, a plot of peak height against concentration of thymol was found to be linear over the range of 4 to 100μM consisting of two linear ranges: from 4 to 20μM (R(2)=0.9964) and from 20 to 100μM (R(2)=0.9993). The effect of potential interferences such as p-cymene and γ-terpinene (major components in essential oil of C. copticum seeds) was evaluated. Thus, the proposed method displays a sufficient selectivity toward thymol with a detection limit of 3.9μM, and it was successfully applied for the determination of thymol in essential oil of C. copticum seeds. The Prussian blue method was used for validation of the proposed electroanalytical method.

  14. Sensitive and Rapid Voltammetric Determination of Phenothiazine and Azaphenothiazine Derivatives in Pharmaceuticals Using a Boron-doped Diamond Electrode.

    PubMed

    Mielech-Łukasiewicz, Katarzyna; Staśkowska, Elżbieta

    2015-01-01

    Novel, sensitive and rapid electrochemical methods for the determination of phenothiazine and azaphenothiazine derivatives were developed. A boron-doped diamond (BDD) electrode was used for electrochemical oxidation of levomepromazine, promazine and prothipendyl. The electrooxidation of these substances demonstrated reversible peaks of oxidation at the potential range 0.55 - 0.75 V vs. SCE. Examining the influence of scan rate allowed is to demonstrate that the currents registered typical of the diffusion-controlled process. Determinations of the studied analytes were carried out by means of a square wave voltammetry (SWV) method and a differential pulse voltammetry (DPV) method. Linear ranges of determination with the use of the BDD electrode and the SWV method were obtained in the ranges: from 4 × 10(-7) to 1.38 × 10(-4) mol L(-1) for levomepromazine, from 4 × 10(-7) to 1.17 × 10(-5) mol L(-1) for promazine and from 4.95 × 10(-7) to 4.54 × 10(-5) mol L(-1) for prothipendyl. The influence of interferences on the voltammetric signal of the studied analytes was also checked. The proposed procedures were used for quantitative determination of the studied compounds in pharmaceutical preparations. The measurements showed high accuracy. The recovery values obtained ranged from 98.52 to 99.57%. The developed procedures were compared with pharmacopoeial reference methods.

  15. Design and Optimization of a New Voltammetric Method for Determination of Isoniazid by Using PEDOT Modified Gold Electrode in Pharmaceuticls

    PubMed Central

    Demirkaya-Miloglu, Fatma; Oznuluer, Tuba; Ozdurak, Buket; Miloglu, Elmas

    2016-01-01

    Isoniazid (INH) was studied with regard to its electrochemical treatment on a strongly alkaline solution of a poly (3,4-ethylenedioxythiophene)-modified gold electrode, using both cyclic voltammetric and controlled potential techniques. Electrocatalytic performance measurements of this composite electrode toward oxidation of INH exhibited an increase of 4-folds in oxidation peak densities compared to the bare gold electrode. Central composite design method was used to obtain optimum experimental conditions, and used critical parameters (pH (A), scan rate (mV/s, B) and temperature (C, C) to assess the effects on amperometric response. Optimum experimental conditions were achieved by using a pH of 9.2 with a scan rate of 260 mV/s and a temperature of 30 C. Under these circumstances, a good linear relationship was observed between peak current densities and INH concentration in the range of 0.05-2 μM, with correlation coefficient of 0.9998. Furthermore, the method was very sensitive (limit of quantitation, 0.0043 μM), accurate (relative error, -5.65 to 4.03) and precise (relative standard deviation %, ≤ 7.97). The method was also applied to determine INH in pharmaceutical formulations, and statistically compared the results with the official method using the two one-sided equivalence test; the results were in good agreement with those obtained by the official and reported methods. PMID:28228805

  16. Simultaneous square-wave voltammetric determination of aspartame and cyclamate using a boron-doped diamond electrode.

    PubMed

    Medeiros, Roberta Antigo; de Carvalho, Adriana Evaristo; Rocha-Filho, Romeu C; Fatibello-Filho, Orlando

    2008-07-30

    A simple and highly selective electrochemical method was developed for the simultaneous determination of aspartame and cyclamate in dietary products at a boron-doped diamond (BDD) electrode. In square-wave voltammetric (SWV) measurements, the BDD electrode was able to separate the oxidation peak potentials of aspartame and cyclamate present in binary mixtures by about 400 mV. The detection limit for aspartame in the presence of 3.0x10(-4) mol L(-1) cyclamate was 4.7x10(-7) mol L(-1), and the detection limit for cyclamate in the presence of 1.0x10(-4) mol L(-1) aspartame was 4.2x10(-6) mol L(-1). When simultaneously changing the concentration of both aspartame and cyclamate in a 0.5 mol L(-1) sulfuric acid solution, the corresponding detection limits were 3.5x10(-7) and 4.5x10(-6) mol L(-1), respectively. The relative standard deviation (R.S.D.) obtained was 1.3% for the 1.0x10(-4) mol L(-1) aspartame solution (n=5) and 1.1% for the 3.0x10(-3) mol L(-1) cyclamate solution. The proposed method was successfully applied in the determination of aspartame in several dietary products with results similar to those obtained using an HPLC method at 95% confidence level.

  17. Voltammetric studies of Azathioprine on the surface of graphite electrode modified with graphene nanosheets decorated with Ag nanoparticles.

    PubMed

    Asadian, Elham; Iraji Zad, Azam; Shahrokhian, Saeed

    2016-01-01

    By using graphene nanosheets decorated with Ag nanoparticles (AgNPs-G) as an effective approach for the surface modification of pyrolytic graphite electrode (PGE), a sensing platform was fabricated for the sensitive voltammetric determination of Azathioprine (Aza). The prepared AgNPs-G nanosheets were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), UV-vis and Raman spectroscopy techniques. The electrochemical behavior of Aza was investigated by means of cyclic voltammetry. Comparing to the bare PGE, a remarkable enhancement was observed in the response characteristics of Aza on the surface of the modified electrode (AgNPs-G/PGE) as well as a noticeable decrease in its reduction overpotential. These results can be attributed to the incredible enlargement in the microscopic surface area of the electrode due to the presence of graphene nanosheets together with strong adsorption of Aza on its surface. The effect of experimental parameters such as accumulation time, the amount of modifier suspension and pH of the supporting electrolyte were also optimized toward obtaining the maximum sensitivity. Under the optimum conditions, the calibration curve studies demonstrated that the peak current increased linearly with Aza concentrations in the range of 7 × 10(-7) to 1 × 10(-4)mol L(-1) with the detection limit of 68 nM. Further experiments revealed that the modified electrode can be successfully applied for the accurate determination of Aza in pharmaceutical preparations. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Simultaneous voltammetric determination of morphine and noscapine by adsorptive differential pulse stripping method and least-squares support vector machines.

    PubMed

    Niazi, Ali; Ghasemi, Jahanbakhsh; Zendehdel, Mojgan

    2007-11-30

    An adsorptive differential pulse stripping method for the simultaneous determination of morphine and noscapine is proposed. The procedure involves an adsorptive accumulation of morphine and noscapine on a hanging mercury drop electrode (HMDE), followed by oxidation of adsorbed morphine and noscapine by voltammetric scan using differential pulse modulation. The optimum experimental conditions are: pH 10.0, accumulation potential of -100 mV versus Ag/AgCl, accumulation time of 150 s, scan rate of 40 mV s(-1) and pulse height of 100 mV. Morphine and noscapine peak currents were observed in same potential region at about +0.25 V. The simultaneous determination of morphine and noscapine by using voltammetry is a difficult problem in analytical chemistry, due to voltammogram interferences. The resolution of mixture of morphine and noscapine by the application of least-squares support vector machines (LS-SVM) was performed. The linear dynamic ranges were 0.01-3.10 and 0.015-2.75 microg mL(-1) and detection limits were 3 and 7 ng mL(-1) for morphine and noscapine, respectively. The capability of the method for the analysis of real samples was evaluated by the determination of morphine and noscapine in addict's human plasma with satisfactory results.

  19. Voltammetric reduction and re-oxidation of solid coordination polymers of dihydroxybenzoquinone.

    PubMed

    Abrahams, Brendan F; Bond, Alan M; Le, Thanh Hai; McCormick, Laura J; Nafady, Ayman; Robson, Richard; Vo, Nguyen

    2012-12-04

    Crystalline (PMePh(3))(2)[Cd(2)(dhbq)(3)], (dhbq(2-) = deprotonated 2,5-dihydroxybenzoquinone, H(2)dhbq), attached to electrode surfaces, survives repeated cycles of reduction followed by re-oxidation when placed in contact with aqueous electrolyte media. The results afford encouragement that a range of coordination networks containing redox active connecting ligands and/or redox active metal centres may be reducible or oxidisable in the solid state.

  20. Development of square-wave adsorptive stripping voltammetric method for determination of acebutolol in pharmaceutical formulations and biological fluids

    PubMed Central

    2012-01-01

    A validated simple, rapid, sensitive and specific square-wave voltammetric technique is described for the determination of acebutolol (AC) following its accumulation onto a hanging mercury drop electrode in a Britton-Robinson universal buffer of pH 7.5. The optimal procedural conditions were: accumulation potential Eacc = - 0.8 V versus Ag/AgCl/KCl, accumulation duration tacc = 30 s, pulse-amplitude = 70 mV, scan rate = 100 mV/s, frequency = 30 Hz, surface area of the working electrode = 0.6 mm2 and the convection rate = 2000 rpm. Under these optimized conditions, the adsorptive stripping voltammetry (AdSV) peak current was proportional over the concentration range 5 × 10-7 - 6 × 10-6 M (r = 0.999). Recoveries for acebutolol from human plasma and urine were in the range 97-103% and 96-104% respectively. The method proved to be precise (intra-day precision expressed as %RSD in human plasma ranged from 2.9 - 3.2% and inter-day precision expressed as %RSD ranged from 3.4 - 3.8%) and accurate (intra-day accuracies expressed as % error in human urine ranged from -3.3 - 2.8% and inter-day accuracies ranged from -3.3 - 1.7%). The limit of quantitation (LOQ) and limit of detection (LOD) for acebutolol were 1.7 × 10-7 and 5 × 10-7 M, respectively. Possible interferences by substances usually present in the pharmaceutical formulations were investigated with a mean recovery of 101.6 ± 0.64%. Results of the developed square-wave adsorptive stripping voltammetry (SW-AdSV) method were comparable with those obtained by reference analytical method. PMID:22353684

  1. The decrease in hypothalamic dopamine secretion induced by suckling: comparison of voltammetric and radioisotopic methods of measurement. [Rats

    SciTech Connect

    Plotsky, P.M.; Neill, J.D.

    1982-03-01

    Previous in situ voltammetric microelectrode measurements of median eminence dopamine release during mammary nerve stimulation of anesthetized lactating rats revealed a transient (1-3 min) 70% decline of dopamine concentrations. This dopamine was believed to be destined for secretion into the hypophysial portal circulation, but direct experimental support for this supposition was lacking. Thus, in the present study, (3H)dopamine release into brief sequential samples of hypophysial portal blood was compared with dopamine release in the median eminence measured by voltammetry. Lactating female rats were urethane anesthetized, and the median eminence pituitary region was exposed. (3H)Tyrosine was injected into a jugular cannula (100 microCi) followed by continuous infusion (5 microCi/min). In a preliminary experiment, this regimen produced a steady state level of (3H)dopamine in the portal blood within 45 min. In subsequent experiments, portal blood was collected as sequential 3-min samples, and electrochemical sampling from a microelectrode placed in the median eminence occurred at 1-min intervals. Electrochemical current resulting from the oxidation of dopamine in the medial median eminence was unvarying throughout the 75-min experiment in control rats (n . 4) and during the 30-min control period preceding mammary nerve stimulation in the other group (n . 4). These results were paralled by (3H) dopamine levels in portal blood during the same periods of time. All animals showed simultaneous decreases in oxidation current and (3H)dopamine levels within 1-4 min after initiation of mammary nerve stimulation. These and earlier results demonstrate that mammary nerve stimulation (and by extension, suckling) induces a momentary, but profound, decrease in hypothalamic dopamine secretion which precedes or accompanies the rise in PRL secretion evoked by the same stimulus.

  2. A poly(3-acetylthiophene) modified glassy carbon electrode for selective voltammetric measurement of uric acid in urine sample.

    PubMed

    Aslanoglu, Mehmet; Kutluay, Aysegul; Abbasoglu, Sultan; Karabulut, Serpil

    2008-03-01

    A reliable and reproducible method for the determination of uric acid in urine samples has been developed. The method is based on the modification of a glassy carbon electrode by 3-acetylthiophene using cyclic voltammetry. The poly(3-acetylthiophene) modified glassy carbon electrode showed an excellent electrocatalytic effect towards the oxidation of uric acid in 0.1 m phosphate buffer solution (PBS) at pH 7.2. Compared with a bare glassy carbon electrode (GCE), an obvious shift of the oxidation peak potential in the cathodic direction and a marked enhancement of the anodic current response for uric acid were observed. The poly(3-acetylthiophene)/GCE was used for the determination of uric acid using square wave voltammetry. The peak current increased linearly with the concentration of uric acid in the range of 1.25 x 10(-5)-1.75 x 10(-4) M. The detection limit was 5.27 x 10(-7) M by square wave voltammetry. The poly(3-acetylthiophene)/GCE was also effective to determine uric acid and ascorbic acid in a mixture and resolved the overlapping anodic peaks of these two species into two well-defined voltammetric peaks in cyclic voltammetry at 0.030 V and 0.320 V (vs. Ag/AgCl) for ascorbic acid and uric acid, respectively. The modified electrode exhibited stable and sensitive current responses toward uric acid and ascorbic acid. The method has successfully been applied for determination of uric acid in urine samples.

  3. Label-free voltammetric aptasensor for the sensitive detection of microcystin-LR using graphene-modified electrodes.

    PubMed

    Eissa, Shimaa; Ng, Andy; Siaj, Mohamed; Zourob, Mohammed

    2014-08-05

    The development of successful biosensing platforms is highly dependent upon the biorecognition properties of the recognition receptor and the sensitivity of the transducer of the binding signal. The integration of the high affinity and specificity of DNA aptamers with the unique properties of the carbon nanomaterial graphene offers an excellent avenue for sensitive and selective biosensing architectures. In this work, a highly sensitive and selective aptasensor which utilizes an unlabeled DNA aptamer assembled on a graphene electrode for microcystin-LR detection was developed. A facile strategy was used for the aptasensor fabrication on the basis of the noncovalent assembly of DNA aptamer on graphene-modified screen printed carbon electrodes. Assembly of the DNA aptamer on the graphene-modified electrodes caused a marked drop in the square wave voltammetric reduction signal of the [Fe(CN)6](4-/3-) redox couple. The presence of microcystin-LR, on the other hand, caused a dose-responsive increase in peak current, allowing the quantification of microcystin-LR through the measurement of peak current change. Under optimal conditions, the detection limit of the developed aptasensor was 1.9 pM in buffer, a concentration much lower than those offered by previously reported biosensors for microcystin-LR. The developed aptasensor also exhibited excellent selectivity for microcystin-LR with no detectable cross-reactivity to okadaic acid, microcystin-LA, and microcystin-YR. Moreover, the proposed aptasensor has been applied for the analysis of spiked tap water and fish samples showing good recovery percentages. This novel, simple, high-performance, and low-cost detection platform would facilitate the routine monitoring of microcystin-LR in real samples.

  4. Mesoporous film of WO3-the "sunlight" assisted decomposition of surfactant in wastewater for voltammetric determination of Pb

    NASA Astrophysics Data System (ADS)

    Krasnodębska-Ostręga, Beata; Bielecka, Agnieszka; Biaduń, Ewa; Miecznikowski, Krzysztof

    2016-12-01

    In this paper we present the application of "sunlight" assisted digestion in the presence of WO3 to the decomposition of dissolved organic matter, using the anionic surfactant sodium dodecyl sulfate (SDS) and the nonionic surfactant (1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol (Triton™X-114) in natural water samples, prior to the determination of traces residues of lead by stripping voltammetry methods. The results of the study showed firstly that the preparation of reproducible WO3 layers characterized by high mechanical and chemical resistance was possible, and secondly that it was also possible to obtain a high efficiency of decomposition, equal in efficiency to that of the reference method, which was the hydrogen peroxide oxidation assisted by UV, with evaporation nearly to dryness. The developed procedure is suggested to be a no-reagents method for the decomposition of added SDS, leading to 100% recovery of added Pb (II). The anodic stripping voltammetric curves recorded in solution after 4 h irradiation with UV assisted by WO3 were repeatable and increased linearly with standard additions, but the data finally obtained were incorrect. The curves recorded in solution after "sunlight" assisted digestion in the presence of WO3 were repeatable, and increased linearly with an increasing of concentration of standard additions (100% recovery of Pb). In the case of a nonionic surfactant, the decomposition time is at least 6 h. The advantage of the proposed method is the fact that the digestion process does not need the addition of any chemicals for the complete decomposition of organic matter.

  5. A square-wave adsorptive stripping voltammetric method for the determination of Amaranth, a food additive dye.

    PubMed

    Alghamdi, Ahmad H

    2005-01-01

    Square-wave adsorptive stripping voltammetric (AdSV) determinations of trace concentrations of the azo coloring agent Amaranth are described. The analytical methodology used was based on the adsorptive preconcentration of the dye on the hanging mercury drop electrode, followed by initiation of a negative sweep. In a pH 10 carbonate supporting electrolyte, Amaranth gave a well-defined and sensitive AdSV peak at -518 mV. The electroanalytical determination of this azo dye was found to be optimal in carbonate buffer (pH 10) under the following experimental conditions: accumulation time, 120 s; accumulation potential, 0.0 V; scan rate, 600 mV/s; pulse amplitude, 90 mV; and frequency, 50 Hz. Under these optimized conditions the AdSV peak current was proportional over the concentration range 1 x 10(-8)-1.1 x 10(-7) mol/L (r = 0.999) with a detection limit of 1.7 x 10(-9) mol/L (1.03 ppb). This analytical approach possessed enhanced sensitivity, compared with conventional liquid chromatography or spectrophotometry and it was simple and fast. The precision of the method, expressed as the relative standard deviation, was 0.23%, whereas the accuracy, expressed as the mean recovery, was 104%. Possible interferences by several substances usually present as food additive azo dyes (E110, E102), gelatin, natural and artificial sweeteners, preservatives, and antioxidants were also investigated. The developed electroanalyticals method was applied to the determination of Amaranth in soft drink samples, and the results were compared with those obtained by a reference spectrophotometric method. Statistical analysis (paired t-test) of these data showed that the results of the 2 methods compared favorably.

  6. Sensitive voltammetric and amperometric responses of respiratory toxins at hemin-adsorbed carbon-felt.

    PubMed

    Hasebe, Yasushi; Wang, Yue

    2013-06-01

    A hemin [iron-Fe(III) protoporphyrin IX chloride] was adsorbed onto a carbon-felt (CF), which is a microelectrode ensemble of micro carbon fiber (ca. 7 microm diameter). The resulting hemin-adsorbed-CF (hemin-CF) showed a well-defined redox wave based on the hemin-Fe(III)/Fe(II) redox process with the formal potential of -0.225 V vs. Ag/AgCl in deoxygenated phosphate/citrate buffer solution (0.1 mol/L, pH 5.0). The apparent heterogenous electron transfer rate constant was estimated to be 8.6 sec(-1). In air-saturated electrolyte solution, the hemin-CF exhibited an excellent electrocatalytic activity for the reduction of dioxygen (O2). This activity was reversibly inhibited by respiratory toxins such as cyanide and azide, which bind sixth coordination position of iron active center of hemin. The electrocatalytic 02 reduction current at the hemin-CF was modulated by the toxins in a concentration-depending manner. Based on the relationship between the %inhibition and the toxin concentration, apparent inhibition constants of cyanide and azide were evaluated to be 4.52 and 1.98 micromol/L, respectively. When the hemin-CF was used as a working electrode unit of the CF-based electrochemical flow-through detector with air-saturated carrier, the injection of the azide induced peak-shape current responses, which allowed rapid and continuous flow-amperometric determination of azide with high sensitivity.

  7. Voltammetric studies on the potent carcinogen, 7,12-dimethylbenz[a]anthracene: Adsorptive stripping voltammetric determination in bulk aqueous forms and human urine samples and detection of DNA interaction on pencil graphite electrode.

    PubMed

    Yardim, Y; Keskin, E; Levent, A; Ozsöz, M; Sentürk, Z

    2010-01-15

    7,12-Dimethylbenz[a]anthracene (DMBA), is a widely studied polycyclic aromatic hydrocarbon that has long been recognized as a very potent carcinogen. Initially, the electrochemical oxidation of DMBA at the glassy carbon and pencil graphite electrodes in non-aqueous media (dimethylsulphoxide with lithium perchlorate) was studied by cyclic voltammetry. DMBA was irreversibly oxidized in two steps at high positive potentials, resulting in the ill-resolved formation of a couple with a reduction and re-oxidation wave at much lower potentials. Special attention was given to the use of adsorptive stripping voltammetry together with a medium exchange procedure on disposable pencil graphite electrode in aqueous solutions over the pH range of 3.0-9.0. The response was characterized with respect to pH of the supporting electrolyte, pre-concentration time and accumulation potential. Using square-wave stripping mode, the compound yielded a well-defined voltammetric response in acetate buffer, pH 4.8 at +1.15V (vs. Ag/AgCl) (a pre-concentration step being carried out at a fixed potential of +0.60V for 360s). The process could be used to determine DMBA concentrations in the range 2-10nM, with an extremely low detection limit of 0.194nM (49.7ngL(-1)). The applicability to assay of spiked human urine samples was also illustrated. Finally, the interaction of DMBA with fish sperm double-stranded DNA based on decreasing of the oxidation signal of adenine base was studied electrochemically by using differential pulse voltammetry with a pencil graphite electrode at the surface and also in solution. The favorable signal-to-noise characteristics of biosensor resulted in low detection limit (ca. 46nM) following a 300-s interaction. These results displayed that the electrochemical DNA-based biosensor could be used for the sensitive, rapid, simple and cost effective detection of DMBA-DNA interaction.

  8. Development of a selective and sensitive voltammetric sensor for propylparaben based on a nanosized molecularly imprinted polymer-carbon paste electrode.

    PubMed

    Gholivand, Mohammad Bagher; Shamsipur, Mojtaba; Dehdashtian, Sara; Rajabi, Hamid Reza

    2014-03-01

    The design and construction of a selective voltammetric sensor for propylparaben (PP) in cosmetics by using a molecularly imprinted polymer (MIP) as recognition element was introduced. The MIP was synthesized by using PP as template and methacrylic acid as functional monomer and then incorporated in the carbon paste electrode as PP sensor. The molecularly imprinted polymer-carbon paste electrode (MIP-CPE) showed very high recognition ability in comparison to non-imprinted polymer-carbon paste electrode (NIP-CPE). It was shown that electrode washing after PP extraction, led to enhanced selectivity, without noticeably decreasing the sensitivity. Some parameters affecting sensor response were optimized, and a calibration curve was then plotted using differential pulse voltammetric (DPV) technique. A dynamic linear range of 1 nM to 100 nM was obtained. The detection limit of the sensor was calculated to be equal to 0.32 nM. The imprinted electrode also displayed good selectivity for PP and selectivity coefficients were 2.29 and 1.66 for methylparaben (MP) and ethylparaben (EP) respectively. Structural analogs, such as phenol and p-hydroxybenzoic acid had almost no response. This sensor was used successfully for propylparaben determination in cosmetic sample.

  9. A novel and sensitive carbon paste electrode with clinoptilolite nano-particles containing hexadecyltrimethyl ammonium surfactant and dithizone for the voltammetric determination of Sn(II).

    PubMed

    Niknezhadi, Azin; Nezamzadeh-Ejhieh, Alireza

    2017-09-01

    Clinoptilolite nano-particles (CNP) were modified by hexadecyltrimethyl ammonium bromide surfactant (HDTMA) and dithizone (DZ). The modified zeolite was then used for the modification of carbon paste electrode (CPE). The resulted CNP-HDTMA-DZ-CPE was finally used for the voltammetric determination of Sn(II) in aqueous solution. The raw and modified CNP was characterized by SEM-EDX, BET, TG-DTG and FTIR techniques. The best voltammetric response was obtained in 0.1molL(-1) NaNO3+HCl at pH 2.2 as supporting electrolyte. The electrode showed a linear response in the concentration range of 1×10(-8) to 1×10(-2)molL(-1)Sn(II) with LOD about 9×10(-9)molL(-1)Sn(II). The electrode showed good selectivity and applicability for the determination of Sn(II) in real samples such as river water, an steel company wastewater, tomato paste and a canned tuna fish. Copyright © 2017 Elsevier Inc. All rights reserved.

  10. Differential pulse voltammetric determination of P(V) following adsorptive accumulation of alpha-[PMo(12)O(40)](3-) on a polypyrrole-modified glassy carbon electrode.

    PubMed

    Takamoto, Masayo; Himeno, Sadayuki

    2003-03-01

    On the basis of the formation and pre-concentration of an alpha-Keggin-type [PMo(12)O(40)](3-) complex, a novel voltammetric method was developed for the determination of trace levels of P(V). The alpha-[PMo(12)O(40)](3-) complex was formed by heating a 5x10(-4) M Mo(VI)-0.2 M HCl-40% (v/v) CH(3)CN system containing a trace amount of P(V) at 70 degrees C for 30 min. During the electrochemical polymerization of pyrrole in the alpha-[PMo(12)O(40)](3-) solution, the alpha-[PMo(12)O(40)](3-) complex was accumulated into the polypyrrole film on a glassy carbon electrode. The differential pulse voltammetric peak current due to the alpha-[PMo(12)O(40)](3-) complex incorporated in the polypyrrole film was linearly dependent on the P(V) concentration in the range of 5x10(-9)-5x10(-7) M; a detection limit of 2x10(-9) M was achieved.

  11. Electrochemical behavior and voltammetric determination of 2,4,6-triaminopyrimidine at glassy carbon electrode modified with multi-walled carbon nanotubes/nafion.

    PubMed

    Yang, Baocheng; Wang, Fei; Guo, Sujuan; Ye, Baoxian

    2010-01-01

    A multi-wall carbon nanotubes (MWCNTs) composite with Nafion was modified on a glass carbon electrode. The modified electrode was then used as a voltammetric sensor in detecting 2,4,6-triaminopyrimidine (TAP). The surface morphology of the Nafion/MWCNTs composite film was characterized by atomic force microscopy (AFM), and the electrochemical behavior of TAP at this sensor was investigated in detail. The results indicated that the Nafion/MWCNTs modified electrode exhibited efficient electrocatalytic oxidation for TAP with relatively high sensitivity, stability and lifetime. Under the optimized condition using linear sweep voltammetry (LSV), the Nafion/MWCNTs modified electrode exhibited a linear voltammetric response for TAP in the concentration range of 2.0 × 10(-7) to 3.6 × 10(-5) mol L(-1), with a detection limit of 5.0 × 10(-8) mol L(-1). The electrode was applied to detect TAP added to human blood serum, with an average recovery value of 101.3%.

  12. Langmuir-Blodgett film of p-tert-butylthiacalix[4]arene modified glassy carbon electrode as voltammetric sensor for the determination of Hg(II).

    PubMed

    Wang, Fei; Wei, Xiaohan; Wang, Chenbin; Zhang, Shusheng; Ye, Baoxian

    2010-01-15

    The pi-A isotherms and UV-vis spectra of the transferred films suggested that the monolayer of p-tert-butylthiacalix[4]arene can coordinate with Hg(2+) at the air-water surface. From these observations, a glassy carbon electrode coated with Langmuir-Blodgett film of p-tert-butylthiacalix[4] arene as a new voltammetric sensor is designed for the determination of trace amounts of Hg(2+). Compared with bare glassy carbon electrode and modified glassy carbon electrode using direct coating method, the Langmuir-Blodgett film-modified electrode can greatly improve the measuring sensitivity of Hg(2+). Under the selected conditions, the Langmuir-Blodgett film-modified electrode in 0.1molL(-1) H(2)SO(4)+0.01molL(-1) KCl solution shows a linear voltammetric response for Hg(2+) in the range of 5.0x10(-10) to 1.5x10(-7)molL(-1), with a detection limit of 2.0x10(-10)molL(-1). The proposed method was also applied to determine Hg(2+) in water samples (tap, lake and river water). In addition, the fabricated electrode exhibited a distinct advantage of simple preparation, non-toxicity, good reproducibility and good stability.

  13. Sensitive voltammetric determination of vanillin with an AuPd nanoparticles-graphene composite modified electrode.

    PubMed

    Shang, Lei; Zhao, Faqiong; Zeng, Baizhao

    2014-05-15

    In this work, graphene oxide was reduced to graphene with an endogenous reducing agent from dimethylformamide, and then AuPd alloy nanoparticles were electrodeposited on the graphene film. The obtained AuPd-graphene hybrid film was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction and voltammetry. The electrochemical behavior of vanillin was studied using the AuPd-graphene hybrid based electrode. It presented high electrocatalytic activity and vanillin could produce a sensitive oxidation peak at it. Under the optimal conditions, the peak current was linear to the concentration of vanillin in the ranges of 0.1-7 and 10-40 μM. The sensitivities were 1.60 and 0.170 mA mM(-1) cm(-2), respectively; the detection limit was 20 nM. The electrode was successfully applied to the detection of vanillin in vanilla bean, vanilla tea and biscuit samples.

  14. Voltammetric determination of melatonin using a graphene-based sensor in pharmaceutical products

    PubMed Central

    Apetrei, Irina Mirela; Apetrei, Constantin

    2016-01-01

    Melatonin can be sensitively detected in pharmaceuticals by cyclic voltammetry and fixed-potential amperometry using a graphene-based sensor. The sensor characterization of cyclic voltammetry constantly provides high values of electrode active area and heterogeneous rate constant. In optimal conditions, the sensor was applied for the determination of melatonin in different pharmaceutical samples. The sensitivity to melatonin was 0.0371 A M−1, and the limit of detection was 0.87×10−6 M. The data obtained by using the graphene-based sensor for the detection of melatonin in pharmaceutical products were in good agreement with the data provided by the producer. Since no interferences from the excipients were found, using a separation technique was not necessary. Additionally, the low price, ease of handling, small amount of sample, short time per analysis, and possibility of automation are the important advantages that recommend this methodology for quality control of pharmaceuticals. PMID:27194909

  15. Voltammetric Determination of Ferulic Acid Using Polypyrrole-Multiwalled Carbon Nanotubes Modified Electrode with Sample Application

    PubMed Central

    Abdel-Hamid, Refat; Newair, Emad F.

    2015-01-01

    A polypyrrole-multiwalled carbon nanotubes modified glassy carbon electrode-based sensor was devised for determination of ferulic acid (FA). The fabricated sensor was prepared electrochemically using cyclic voltammetry (CV) and characterized using CV and scanning electron microscope (SEM). The electrode shows an excellent electrochemical catalytic activity towards FA oxidation. Under optimal conditions, the anodic peak current correlates linearly to the FA concentration throughout the range of 3.32 × 10−6 to 2.59 × 10−5 M with a detection limit of 1.17 × 10−6 M (S/N = 3). The prepared sensor is highly selective towards ferulic acid without the interference of ascorbic acid. The sensor applicability was tested for total content determination of FA in a commercial popcorn sample and showed a robust functionality.

  16. Synthesis, characterization of amide substituted dexibuprofen derivatives and their spectral, voltammetric and docking investigations for DNA binding interactions.

    PubMed

    Arshad, Nasima; Zafran, Muhammad; Ashraf, Zaman; Perveen, Fouzia

    2017-04-01

    Three amide derivatives - methyl-2-[2-(4-isobutylphenyl)propanamido]propanoate (Dex-2), methyl 2-[2-(4-isobutylphenyl) propanamido]-3-phenylpropanoate (Dex-3) and methyl 2-[2-(4-isobutylphenyl)-propanamido]-4-methylpentanoate (Dex-4) of dexibuprofen (Dex-1) 2-(4-isobutylphenyl)propanoic acid were synthesized and conformed for structures by physical data and spectral analysis. Further, all the compounds were studied for their binding with ds.DNA through experimental (UV-visible/and fluorescence spectroscopy, cyclic voltammetry) and theoretical (molecular docking) techniques. Spectral and voltammetric responses as well as kinetic and thermodynamic data interpretations at stomach (4.7) and blood (7.4) pH and at human body temperature (37°C) indicated spontaneous interaction of all the compounds with DNA via intercalation and external bindings. The binding constants (Kb) and Gibbs free energy changes (-ΔG) were evaluated greater at pH7.4 attributing comparatively more significant binding of all the compounds with DNA at blood pH. Among all compounds, Dex-4 showed greater binding with DNA at both pH with greater Kb values i.e., {UV-visible: pH 4.7 (2.36×10(4)M(-1)); pH7.4 (2.42×10(4)M(-1)), fluorescence: pH4.7 (2.24×10(4)M(-1)); pH7.4 (2.56×10(4)M(-1)) and CV: pH4.7 (4.06×10(4)M(-1)); pH7.4 (4.89×10(4)M(-1))}. Binding site size (n) at both pH values was evaluated n≥1 for Dex-2 and Dex-4 which assured intercalation as a major mode of interaction between compounds and DNA. For Dex-1 and Dex-3 (n) was evaluated n≤1 at both pH values and the values n<1 indicated the possibility of binding via groove or electrostatic interactions. Electrochemical processes were found diffusion controlled and diffusion coefficients (Do) for all the compounds - DNA adducts were evaluated lesser than unbound compounds. Docking studies further supported DNA binding evidences obtained from spectral and electrochemical investigations. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Simultaneous multiplexed stripping voltammetric monitoring of marine toxins in seafood based on distinguishable metal nanocluster-labeled molecular tags.

    PubMed

    Zhang, Bing; Hou, Li; Tang, Dianping; Liu, Bingqian; Li, Jianrong; Chen, Guonan

    2012-09-12

    Marine toxins from microscopic algae can accumulate through the food chain and cause various neurological and gastrointestinal illnesses for human health. Herein, we designed a new ultrasensitive multiplexed immunoassay protocol for simultaneous electrochemical determination of brevetoxin B (BTX-2) and dinophysistoxin-1 (DTX-1) in seafood using distinguishable metal nanocluster-labeled molecular tags as traces on bifunctionalized magnetic capture probes. To construct such a bifunctionalized probe, monoclonal mouse anti-BTX-2 (mAb(1)) and anti-DTX-1 (mAb(2)) antibodies were co-immobilized on a magnetic bead (MB-mAb(1,2)). The distinguishable metal nanoclusters including cadmium nanoclusters (CdNC) and copper nanoclusters (CuNC) were synthesized using the artificial peptides with amino acid sequence CCCYYY, which were used as distinguishable signal tags for the label of the corresponding bovine serum albumin-BTX-2 and bovine serum albumin-DTX-1 conjugates. A competitive-type immunoassay format was adopted for the online simultaneous monitoring of BTX-2 and DTX-1 on a homemade flow-through magnetic detection cell. The assay was based on the stripping voltammetric behaviors of the labeled CdNC and CuNC at the various peak potentials in pH 2.5 HCl containing 0.01 M KCl using square wave anodic stripping voltammetry (SWASV). Under optimal conditions, the multiplexed immunoassays enabled simultaneous detection of BTX-2 and DTX-1 in a single run with wide working ranges of 0.005-5 ng mL(-1) for two marine toxins. The limit of detection (LOD) and limit of quantification (LOQ) were 1.8 and 6.0 pg mL(-1) for BTX-2, while those for DTX-1 were 2.2 and 7.3 pg mL(-1), respectively. No non-specific adsorption and electrochemical cross-talk between neighboring sites were observed during a series of procedures to detect target analytes. The covalent conjugation of biomolecules onto the nanoclusters and magnetic beads resulted in good repeatability and intermediate precision down to

  18. Voltammetric behavior of nitrazepam and its determination in serum using liquid chromatography with redox mode dual-electrode detection.

    PubMed

    Honeychurch, Kevin C; Smith, Gemma C; Hart, John P

    2006-01-15

    A method involving high-performance liquid chromatography with dual-electrode electrochemical detection in the redox mode (LC-DED) has been successfully developed for the determination of the benzodiazepine tranquilizer, nitrazepam, in serum. To elucidate the electrochemical mechanism occurring at a glassy carbon electrode, cyclic voltammetry was preformed with 1 mM solutions of nitrazepam at pH values between 2 and 12, using a potential range from -1.5 to +1.5 V. Two reduction peaks were observed over the whole pH range; the first, designated R1, was consistent with the 4e-, 4H+ reduction of the 7-nitro group to a hydroxylamine species; the second more negative peak, designated R2, was shown to be the result of a 2e-, 2H+ reduction of the 4-5 azomethine group. On the reverse anodic scan, an oxidation signal was observed, designated O1, which was considered to result from a 2e-, 2H+ oxidation of the hydroxylamine to a nitroso group. On the second forward scan, a new reduction peak, designated R3, was observed, which was considered to result from reduction of the nitroso species back to the hydroxylamine species. Studies were then undertaken to exploit the hydroxylamine/nitroso redox couple using LC-DED detection for the measurement of nitrazepam in serum. The optimal chromatographic conditions were found to comprise a mobile phase containing 60% methanol, 40% 50 mM pH 4.1 acetate buffer, in conjunction with a Hypersil C18 250 mm x 4.6 mm column. Hydrodynamic voltammetric studies were undertaken to optimize the operating potentials required for dual-electrode detection. It was found that an applied potential of -2.4 V was optimum for the "generator" cell and +0.5 V for the "detector" cell. The proposed method was evaluated by carrying out replicate nitrazepam determinations on spiked bovine and human serum samples. The former evaluation was preformed at a concentration of 11.2 microg mL(-1), and the latter at 1670 ng mL(-1). For bovine serum, the recovery of

  19. Theoretical voltammetric response of electrodes coated by solid polymer electrolyte membranes.

    PubMed

    Gómez-Marín, Ana M; Hernández-Ortíz, Juan P

    2014-09-24

    A model for the differential capacitance of metal electrodes coated by solid polymer electrolyte membranes, with acid/base groups attached to the membrane backbone, and in contact with an electrolyte solution is developed. With proper model parameters, the model is able to predict a limit response, given by Mott-Schottky or Gouy-Chapman-Stern theories depending on the dissociation degree and the density of ionizable acid/base groups. The model is also valid for other ionic membranes with proton donor/acceptor molecules as membrane counterions. Results are discussed in light of the electron transfer rate at membrane-coated electrodes for electrochemical reactions that strongly depend on the double layer structure. In this sense, the model provides a tool towards the understanding of the electro-catalytic activity on modified electrodes. It is shown that local maxima and minima in the differential capacitance as a function of the electrode potential may occur as consequence of the dissociation of acid/base molecular species, in absence of specific adsorption of immobile polymer anions on the electrode surface. Although the model extends the conceptual framework for the interpretation of cyclic voltammograms for these systems and the general theory about electrified interfaces, structural features of real systems are more complex and so, presented results only are qualitatively compared with experiments.

  20. Electrochemistry of metoclopramide at multi-walled carbon nanotube modified electrode and its voltammetric detection.

    PubMed

    Guo, Wei; Geng, Mingjiang; Zhou, Lingyun

    2012-01-01

    A simple, sensitive and inexpensive electrochemical method was developed for the determination of metoclopramide (MCP) with a multi-wall carbon nanotube (MWNT) modified glassy carbon electrode (GCE). MWNT was dispersed into polyacrylic acid (PAA); the aqueous suspension was then cast on GCE electrodes, forming MWNT-PAA films after evaporation of the solvent. The electrochemical behavior of MCP at the MWNT-modified electrode was investigated in detail. Compared with the bare GCE, the MWNT-modified electrode exhibits electrocatalytic activity to the oxidation of MCP because of the significant oxidation peak-current enhancement. Furthermore, various experimental parameters, such as the solution pH value, the amount of MWNT-PAA suspension and accumulation conditions were optimized for the determination of MCP. Based on the electrocatalytic effect of the MWNT-modified electrode, linear sweep voltammetry (LSV) was developed for the determination of MCP with the linear response in the range from 1.0 × 10(-7) to 1.0 × 10(-5) mol L(-1) and a detection limit of 5.0 × 10(-8) mol L(-1). The method has been successfully applied to the determination of MCP in commercial MCP tablets.

  1. A novel horseradish peroxidase biosensor towards the detection of dopamine: a voltammetric study.

    PubMed

    Raghu, P; Reddy, T Madhusudana; Gopal, P; Reddaiah, K; Sreedhar, N Y

    2014-04-10

    A polymerized film of glycine (Gly) was prepared on the surface of carbon paste electrode (CPE) through the cyclic voltammetry (CV) technique. A novel biosensor for the determination of dopamine (DA) has been constructed based on horseradish peroxidase (HRP) and multiwalled carbon nanotubes (MWCNTs) immobilizing on Poly (Gly)/CPE through silica sol-gel (SiSG) entrapment. CV measurements were employed in order to understand the feasibility of poly (Gly) as an electron carrier between the immobilized peroxidase and the surface of CPE. By using differential pulse voltammetry (DPV) the calibration curves of DA was obtained in the range of 15-865 μM. The limit of detection (LOD) and limit of quantification (LOQ) of DA was found to be 6×10⁻⁷ M and 2×10⁻⁶ M respectively. The apparent Michaelis-Menten constant (Km(app)) was found to be 0.5 mM and illustrated that the good biological activity of the fixed enzyme. Electrochemical impedance spectroscopy (EIS) results confirmed the rapid electron transfer and also the immobilization of enzyme on the electrode surface. The biosensor showed high sensitivity, selectivity and reproducibility. This method has been used to determine DA in the presence of various interferences and in clinical preparations.

  2. Sensitive voltammetric determination of rutin at an ionic liquid modified carbon paste electrode.

    PubMed

    Zhang, Ya; Zheng, Jianbin

    2008-10-19

    An ionic liquid modified carbon paste electrode (IL/CPE) had been fabricated by using hydrophilic ionic liquid 1-amyl-3-methylimidazolium bromide ([AMIM]Br) as a modifier. The IL/CPE was characterized by scanning electron microscope and voltammetry. Electrochemical behavior of rutin at the IL/CPE had been investigated in pH 3.29 Britton-Robinson (B-R) buffer solution by cyclic voltammetry (CV) and square wave voltammetry (SWV). The experimental results suggested that the modified electrode exhibited an electrocatalytic activity toward the redox of rutin. The electron transfer coefficient (alpha) and the standard rate constant (k(s)) of rutin at the modified electrode were calculated. Under the selected conditions, the reduction peak current was linearly dependent on the concentration of rutin in the range of 4.0x10(-8) to 1.0x10(-5)mol L(-1) (r=0.9998), with a detection limit of 1.0x10(-8)mol L(-1)(S/N=3). The relative standard deviation (R.S.D.) for six times successful determination of 8.0x10(-7)mol L(-1) rutin was 1.2%. The proposed method was applied to determine rutin in tablet and urine sample. In addition, the IL/CPE exhibited a distinct advantage of simple preparation, surface renewal, good reproducibility and good stability.

  3. Toluidine blue adsorbed on alcohol dehydrogenase modified glassy carbon electrode for voltammetric determination of ethanol.

    PubMed

    Periasamy, Arun Prakash; Umasankar, Yogeswaran; Chen, Shen-Ming

    2011-01-15

    A novel toluidine blue O (TBO) adsorbed alcohol dehydrogenase (ADH) biocomposite film have been prepared through simple adsorption technique with the help of electrostatic interaction between oppositely charged layers. Nafion (NF) coating was made on top of the biocomposite film modified glassy carbon electrode (GCE) to protect ADH from leaching. The fabricated ADH/TBO/NF biocomposite electrode remains highly stable in the pH range from 4 to 13. More facile electron transfer process occurs at ADH/TBO/NF biocomposite than at TBO/NF film, which is obvious from the six folds increase in k(s) value. Maximum surface coverage concentration (Γ) of TBO is noticed at ADH/TBO/NF film, which is 82% higher than at TBO/NF and 15% higher than at ADH/TBO film modified GCEs. Electrochemical impedance spectroscopy studies reveal that ADH has been well immobilized in the biocomposite film. Scanning electron microscopy studies confirm the discriminate surface morphology of various components present in the biocomposite film. Cyclic voltammetry studies validate that ADH/TBO/NF biocomposite film exhibits excellent electrocatalytic activity for ethanol oxidation at low over potential (I(pa)=-0.14 V). The same studies show biocomposite film possesses a good sensitivity of 7.91 μAM(-1)cm(-2) for ethanol determination. This above sensitivity value is 17.40% higher than the sensitivity obtained for TBO/NF film (6.74 μAM(-1)cm(-2)). Further, using differential pulse voltammetry, a sensitivity of 1.70 μAM(-1)cm(-2) has been achieved for ADH/TBO/NF biocomposite film. Copyright © 2010 Elsevier B.V. All rights reserved.

  4. Lens-free imaging-based low-cost microsensor for in-line wear debris detection in lube oils

    NASA Astrophysics Data System (ADS)

    Mabe, Jon; Zubia, Joseba; Gorritxategi, Eneko

    2017-02-01

    The current paper describes the application of lens-free imaging principles for the detection and classification of wear debris in lubricant oils. The potential benefits brought by the lens-free microscopy techniques in terms of resolution, deep of field and active areas have been tailored to develop a micro sensor for the in-line monitoring of wear debris in oils used in lubricated or hydraulic machines as gearboxes, actuators, engines, etc. The current work presents a laboratory test-bench used for evaluating the optical performance of the lens-free approach applied to the wear particle detection in oil samples. Additionally, the current prototype sensor is presented, which integrates a LED light source, CMOS imager, embedded CPU, the measurement cell and the appropriate optical components for setting up the lens-free system. The imaging performance is quantified using micro structured samples, as well as by imaging real used lubricant oils. Probing a large volume with a decent 2D spatial resolution, this lens-free micro sensor can provide a powerful tool at very low cost for inline wear debris monitoring.

  5. Electrochemical behavior and voltammetric determination of vanillin based on an acetylene black paste electrode modified with graphene-polyvinylpyrrolidone composite film.

    PubMed

    Deng, Peihong; Xu, Zhifeng; Zeng, Rongying; Ding, Chunxia

    2015-08-01

    The graphene-polyvinylpyrrolidone composite film modified acetylene black paste electrode (GR-PVP/ABPE) was fabricated and used to determine vanillin. In 0.1M H3PO4 solution, the oxidation peak current of vanillin increased significantly at GR-PVP/ABPE compared with bare ABPE, PVP/ABPE and GR/ABPE. The oxidation mechanism was discussed. The experimental conditions that exert influence on the voltammetric determination of vanillin, such as supporting electrolytes, pH values, accumulation potential and accumulation time, were optimized. Besides, the interference, repeatability, reproducibility and stability measurements were also evaluated. Under the optimal experimental conditions, the oxidation peak current was proportional to vanillin concentration in the range of 0.02-2.0 μM, 2.0-40 μM and 40-100 μM. The detection limit was 10nM. This sensor was used successfully for vanillin determination in various food samples.

  6. A Voltammetric Biosensor Based on Glassy Carbon Electrodes Modified with Single-Walled Carbon Nanotubes/Hemoglobin for Detection of Acrylamide in Water Extracts from Potato Crisps.

    PubMed

    Krajewska, Agnieszka; Radecki, Jerzy; Radecka, Hanna

    2008-09-23

    The presence of toxic acrylamide in a wide range of food products such as potato crisps, French fries or bread has been confirmed by Swedish scientists from Stockholm University. The neurotoxicity, possible carcinogenicity of this compound and its metabolites compels us to control them by quantitative and qualitative assays. Acrylamide forms adduct with hemoglobin (Hb) as a result of the reaction the -NH2 group of the Nterminal valine with acrylamide. In this work we present the use of glassy carbon electrodes coated with single-walled carbon nanotubes (SWCNTs) and Hb for voltammetric detection of acrylamide in water solutions. The electrodes presented a very low detection limit (1.0×10(-9) M). The validation made in the matrix obtained by water extraction of potato crisps showed that the electrodes presented are suitable for the direct determination of acrylamide in food samples.

  7. Post-column coulometric generation and cyclic voltammetric identification of the free radical of the antineoplastic agent etoposide (VP 16-213).

    PubMed

    Ploegmakers, H H; van Oort, W J

    1988-01-01

    It has been suggested that etoposide can be transformed 'in vivo' into a radical intermediate, which may be involved in the irreversible binding of etoposide to microsomal proteins and in DNA damage. To investigate some physico-chemical properties, the on-line coulometric production of this free radical and its subsequent cyclic voltammetric detection is described. For the synthesis, a coulometric ESA Coulochem 5100A module, equipped with an ESA 5010 analytical cell, has been used. For its detection the computerized cyclic voltammetric detection system after HPLC controlled by an Apple IIe computer, using home-made software and a home-made glassy-carbon wall-jet detector, has been used. Application of a ramdisk allows storage of 68 cyclic voltammograms. In a methanol-phosphate buffer (pH=8) (40:60 w/w) containing mobile phase, the forward scan of the on-line cyclic voltammogram of etoposide shows two oxidation steps, caused by a double one-electron transfer. Post-column electrolysis at +500 mV versus the H(+)/H2 reference electrode results into total disappearance of the first oxidation step, whereas a reduction wave arises. The limiting current of this wave, and the remaining second oxidation wave, are of equal heights, indicating one-electron processes. Under these conditions, the half-life time of the product, and consequently the free radical, is 100 s, determined by stopped-flow analysis. Decreasing the pH of the buffer in the mobile phase to pH 2.2 results in merging of the two oxidation steps to a single two-electron transfer, disabling radical formation. Under physiological conditions ('in vivo') the established half-life time of the radical enables participation of the intermediate in metabolic processes.

  8. Sensor Fusion of Position- and Micro-Sensors (MEMS) integrated in a Wireless Sensor Network for movement detection in landslide areas

    NASA Astrophysics Data System (ADS)

    Arnhardt, Christian; Fernández-Steeger, Tomas; Azzam, Rafig

    2010-05-01

    technologies were chosen. The MEMS-Sensors are acceleration-, tilt- and barometric pressure sensors. The positionsensors are draw wire and linear displacement transducers. In first laboratory tests the accuracy and resolution were investigated. The tests showed good results for all sensors. For example tilt-movements can be monitored with an accuracy of +/- 0,06° and a resolution of 0,1°. With the displacement transducer change in length of >0,1mm is possible. Apart from laboratory tests, field tests in South France and Germany were done to prove data stability and movement detection under real conditions. The results obtained were very satisfying, too. In the next step the combination of numerous sensors (sensor fusion) of the same type (redundancy) or different types (complementary) was researched. Different experiments showed that there is a high concordance between identical sensor-types. According to different sensor parameters (sensitivity, accuracy, resolution) some sensor-types can identify changes earlier. Taking this into consideration, good correlations between different kinds of sensors were achieved, too. Thus the experiments showed that combination of sensors is possible and this could improve the detection of movement and movement rate but also outliers. Based on this results various algorithms were setup that include different statistical methods (outlier tests, testing of hypotheses) and procedures from decision theories (Hurwicz-criteria). These calculation formulas will be implemented in the spatial data infrastructure (SDI) for the further data processing and validation. In comparison with today existing mainly punctually working monitoring systems, the application of wireless sensor networks in combination with low-cost, but precise micro-sensors provides an inexpensive and easy to set up monitoring system also in large areas. The correlation of same but also different sensor-types permits a good data control. Thus the sensor fusion is a promising tool

  9. Microsensor Hot-Film Anemometer

    NASA Technical Reports Server (NTRS)

    Mcginley, Catherine B.; Stephens, Ralph; Hopson, Purnell; Bartlett, James E.; Sheplak, Mark; Spina, Eric F.

    1995-01-01

    Improved hot-film anemometer developed for making high-bandwidth turbulence measurements in moderate-enthalpy supersonic and hypersonic flows (e.g., NASP inlets and control surfaces, HSCT jet exhaust). Features include low thermal inertia, ruggedness, and reduced perturbation of flow.

  10. Smart Integrated Microsensor System (SIMS)

    DTIC Science & Technology

    1992-11-01

    Real-Time Fatigue Life Algorithm Development ......................... 8 1.5.5 Packaging Design .................................................................. 10...337-01). The module then shifts data out of the IR transmitter (output LED) synchronous with the input clock. 1.5.5 Packaging Design Although the module

  11. Scanning tunneling microscopy of electrochemically activated platinum surfaces. A direct ex-situ determination of the electrode nanotopography

    SciTech Connect

    Vazquez, L.; Gomez, J.; Baro, A.M.; Garcia, N.; Marcos, M.L.; Velasco, J.G.; Vara, J.M.; Arvia, A.J.; Presa, J.; Garcia, A.; Aguilar, M.

    1987-03-18

    A direct scanning tunneling microscopy ex-situ determination on the nanometer scale of the topography of electrochemically highly activated platinum electrodes is presented. A correlation between catalytic activity and surface microtopography becomes evident. This result gives support to a structural model for the activated electrode surface. In the model, a volume with a pebble-like structure allows electrocatalytic processes to occur practically free of diffusion relaxation contributions under usual voltammetric conditions.

  12. A sensitive amplified sensor based on improved carbon paste electrode with 1-methyl-3-octylimidazolium tetrafluoroborate and ZnO/CNTs nanocomposite for differential pulse voltammetric analysis of raloxifene

    NASA Astrophysics Data System (ADS)

    Cheraghi, Somaye; Taher, Mohammad Ali; Karimi-Maleh, Hassan

    2017-10-01

    In this work, we suggested a carbon paste electrode improved with 1-methyl-3-octylimidazolium tetrafluoroborate (1-M-3-OITFB) and ZnO/CNTs nanocomposite (1-M-3-OITFB/ZnO/CNTs/CPE) for electrochemical determination of raloxifene (RXF) as a non-steroidal selective estrogen receptor regulator. The cyclic and differential pulse voltammetric methods were apply for investigation of RXF electrochemical response at a surface of 1-M-3-OITFB/ZnO/CNTs/CPE. Under the best experimental conditions, the 1-M-3-OITFB/ZnO/CNTs/CPE showed a wide linear dynamic range of 0.08 - 400.0 μM. We detected a detection limit of 0.04 μM for RXF analysis using differential pulse voltammetric method (DPV). The 1-M-3-OITFB/ZnO/CNTs/CPE showed high performance ability to RXF analysis in trace amounts on pharmaceutical and clinical preparations.

  13. Co-immobilization of glucose oxidase and xylose dehydrogenase displayed whole cell on multiwalled carbon nanotube nanocomposite films modified electrode for simultaneous voltammetric detection of D-glucose and D-xylose.

    PubMed

    Li, Liang; Liang, Bo; Li, Feng; Shi, Jianguo; Mascini, Marco; Lang, Qiaolin; Liu, Aihua

    2013-04-15

    In this paper, we first report the construction of Nafion/glucose oxidase (GOD)/xylose dehydrogenase displayed bacteria (XDH-bacteria)/multiwalled carbon nanotubes (MWNTs) modified electrode for simultaneous voltammetric determination of D-glucose and D-xylose. The optimal conditions for the immobilized enzymes were established. Both enzymes retained their good stability and activities. In the mixture solution of D-glucose and D-xylose containing coenzyme NAD⁺ (the oxidized form of nicotinamide adenine dinucleotide), the Nafion/GOD/XDH-bacteria/MWNTs modified electrode exhibited quasi-reversible oxidation-reduction peak at -0.5 V (vs. saturated calomel electrode, SCE) originating from the catalytic oxidation of D-glucose, and oxidation peak at +0.55 V(vs. SCE) responding to the oxidation of NADH (the reduced form of nicotinamide adenine dinucleotide) by the carbon nanotubes, where NADH is the resultant product of coenzyme NAD⁺ involved in the catalysis of D-xylose by XDH-displayed bacteria. For the proposed biosensor, cathodic peak current at -0.5 V was linear with the concentration of D-glucose within the range of 0.25-6 mM with a low detection limit of 0.1 mM D-glucose (S/N=3), and the anodic peak current at +0.55 V was linear with the concentration of d-xylose in the range of 0.25∼4 mM with a low detection limit of 0.1 mM D-xylose (S/N=3). Further, D-xylose and D-glucose did not interfere with each other. 300-fold excess saccharides including D-maltose, D-galactose, D-mannose, D-sucrose, D-fructose, D-cellobiose, and 60-fold excess L-arabinose, and common interfering substances (100-fold excess ascorbic acid, dopamine, uric acid) as well as 300-fold excess D-xylitol did not affect the detection of D-glucose and D-xylose (both 1 mM). Therefore, the proposed biosensor is stable, specific, reproducible, simple, rapid and cost-effective, which holds great potential in real applications.

  14. Differential pulse anodic stripping voltammetric determination of lead(II) with a 1,4-bis(prop-2'-enyloxy)-9,10-anthraquinone modified carbon paste electrode.

    PubMed

    Mousavi, M F; Rahmani, A; Golabi, S M; Shamsipur, M; Sharghi, H

    2001-08-30

    A sensitive and selective method for the determination of lead(II) with a 1,4-bis(prop-2'-enyloxy)-9,10-anthraquinone (AQ) modified carbon paste electrode has been developed. The method is based on non-electrolytic preconcentration via complex formation with modifier, followed by an accumulation period with a negative potential (-1.5 V), and then by a proper anodic stripping. The analytical performance was evaluated with respect to the quantity of modifier in the paste, concentration of electrolyte solution, preconcentration time, lead(II) concentration, and other variables. A linear calibration graph was obtained in the concentration range 2.00x10(-9)-1.06x10(-5) M Pb(II) (n=21, r=0.9999) with 30 s preconcentration time. The detection limit was found to be 1x10(-9) M. For eight preconcentration/determination cycles, the differential pulse voltammetric response was reproduced with 5.0 and 3.7% relative standard deviations at 2.00x10(-8) and 2.00x10(-6) M Pb(II), respectively. Rapid and convenient renewal of electrode surface allows the use of a single modified electrode surface in multiple analytical determinations over several weeks. Many coexisting metal ions had little or no effect on the determination of lead(II). The developed method was applied to lead determination in waste waters.

  15. Predominance-zone diagrams of Fe(III) and Fe(II) sulfate complexes in acidic media. Voltammetric and spectrophotometric studies.

    PubMed

    Gil, A F; Salgado, L; Galicia, L; González, I

    1995-03-01

    A thermodynamic study based on concepts of generalized species and equilibria, was used to understand the distribution of Fe(III) and Fe(II) species in the Fe(III)/Fe(II)/H(2)SO(4)/H(2)O system. The two-dimensional predominance zone diagrams (TDPZ) and Pourbaix type diagrams thus obtained permitted the selection of optimum experimental conditions, to differentiate the chemical species involved in this system. The existence of the different predominant chemical species for Fe(III): Fe(3+), FeSO(+)(4) and Fe(SO(4))(-)(2) was evidenced by spectrophotometrical studies for pSO'(4) values from 4 to 0 units in a buffered solution of pH 0.5. Additionally, voltammetric studies performed on Pt, Au and carbon paste electrodes confirmed that the electron exchange between Fe(III) Fe(II) in H(2)SO(4) media occurs by an inner Helmholtz layer mechanism. It was also possible to show that the representative couples at pSO'(4) = 0 (buffered) are: (a) for pH < 0 FeSO (+)(4)FeHSO (+)(4) and (b) for pH > 1.0: Fe(SO (4)) (-)(2)FeHSO (+)(4). The last couple presents a coupled chemical reaction in the electrochemical mechanism; this reaction is associated with the different coordination numbers of Fe(III) and Fe(II).

  16. A Fast Strategy for Determination of Vitamin B₉ in Food and Pharmaceutical Samples Using an Ionic Liquid-Modified Nanostructure Voltammetric Sensor.

    PubMed

    Khaleghi, Fatemeh; Irai, Abolfazl Elyasi; Sadeghi, Roya; Gupta, Vinod Kumar; Wen, Yangping

    2016-05-24

    Vitamin B₉ or folic acid is an important food supplement with wide clinical applications. Due to its importance and its side effects in pregnant women, fast determination of this vitamin is very important. In this study we present a new fast and sensitive voltammetric sensor for the analysis of trace levels of vitamin B₉ using a carbon paste electrode (CPE) modified with 1,3-dipropylimidazolium bromide (1,3-DIBr) as a binder and ZnO/CNTs nanocomposite as a mediator. The electro-oxidation signal of vitamin B₉ at the surface of the 1,3-DIBr/ZnO/CNTs/CPE electrode appeared at 800 mV, which was about 95 mV less positive compared to the corresponding unmodified CPE. The oxidation current of vitamin B₉ by square wave voltammetry (SWV) increased linearly with its concentration in the range of 0.08-650 μM. The detection limit for vitamin B₉ was 0.05 μM. Finally, the utility of the new 1,3-DIBr/ZnO/CNTs/CPE electrode was tested in the determination of vitamin B₉ in food and pharmaceutical samples.

  17. Modification of carbon paste electrode with Fe(III)-clinoptilolite nano-particles for simultaneous voltammetric determination of acetaminophen and ascorbic acid.

    PubMed

    Sharifian, Samira; Nezamzadeh-Ejhieh, Alireza

    2016-01-01

    A novel carbon paste electrode (CPE) modified with Fe(III)-exchanged clinoptilolite nano-particles (Fe(III)-NClino/CPE) was constructed and used for simultaneous voltammetric (CV, SqW and chronoamperometry) determination of ascorbic acid and acetaminophen. Raw and modified zeolites were characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM). The square wave peak current was linearly increased in the concentration ranges of 1.0 × 10(-9)-1.0 × 10(-2) mol L(-1) for ascorbic acid and 1.0 × 10(-10-)1.0 × 10(-2) mol L(-1) for acetaminophen with detection limits of 1.8 × 10(-9) mol L(-1) and 9.9 × 10(-10) mol L(-1), respectively. The detection limits of 2.4 × 10(-10) mol L(-1) and 2.5 × 10(-11) mol L(-1) were also obtained for AA and AC in chronoamperometric measurements, respectively. The diffusion coefficients of 7.5 × 10(-5) cm(2) s(-1) and 2.4 × 10(-5) cm(2) s(-1) were respectively calculated for the oxidation of AC and AA by chronoamperometry. The proposed electrode exhibited high sensitivity and good stability, and would be valuable for the clinical assay of ascorbic acid and acetaminophen. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. A Fast Strategy for Determination of Vitamin B9 in Food and Pharmaceutical Samples Using an Ionic Liquid-Modified Nanostructure Voltammetric Sensor

    PubMed Central

    Khaleghi, Fatemeh; Irai, Abolfazl Elyasi; Sadeghi, Roya; Gupta, Vinod Kumar; Wen, Yangping

    2016-01-01

    Vitamin B9 or folic acid is an important food supplement with wide clinical applications. Due to its importance and its side effects in pregnant women, fast determination of this vitamin is very important. In this study we present a new fast and sensitive voltammetric sensor for the analysis of trace levels of vitamin B9 using a carbon paste electrode (CPE) modified with 1,3-dipropylimidazolium bromide (1,3-DIBr) as a binder and ZnO/CNTs nanocomposite as a mediator. The electro-oxidation signal of vitamin B9 at the surface of the 1,3-DIBr/ZnO/CNTs/CPE electrode appeared at 800 mV, which was about 95 mV less positive compared to the corresponding unmodified CPE. The oxidation current of vitamin B9 by square wave voltammetry (SWV) increased linearly with its concentration in the range of 0.08–650 μM. The detection limit for vitamin B9 was 0.05 μM. Finally, the utility of the new 1,3-DIBr/ZnO/CNTs/CPE electrode was tested in the determination of vitamin B9 in food and pharmaceutical samples. PMID:27231909

  19. Biochar prepared from castor oil cake at different temperatures: A voltammetric study applied for Pb(2+), Cd(2+) and Cu(2+) ions preconcentration.

    PubMed

    Kalinke, Cristiane; Mangrich, Antonio Sálvio; Marcolino-Junior, Luiz H; Bergamini, Márcio F

    2016-11-15

    Biochar is a carbonaceous material similar produced by pyrolysis of biomass under oxygen-limited conditions. Pyrolysis temperature is an important parameter that can alters biochar characteristics (e.g. surface area, pore size distribution and surface functional groups) and affects it efficacy for adsorption of several probes. In this work, biochar samples have been prepared from castor oil cake using different temperatures of pyrolysis (200-600°C). For the first time, a voltammetric procedure based on carbon paste modified electrode (CPME) was used to investigate the effect of temperature of pyrolysis on the adsorptive characteristics of biochar for Pb(II), Cd(II) and Cu(II) ions. Besides the electrochemical techniques, several characterizations have been performed to evaluate the physicochemical properties of biochar in function of the increase of the pyrolysis temperature. Results suggest that biochar pyrolized at 400°C (BC400) showed a better potential for ions adsorption. The CPME modified with BC400 showed better relative current signal with adsorption affinity: Pb(II)>Cd(II)>Cu(II). Kinetic studies revealed that the pseudo-second order model describes more accurately the adsorption process suggesting that the surface reactions control the adsorption rate. Values found for amount adsorbed were 15.94±0.09; 4.29±0.13 and 2.38±0.39μgg(-1) for Pb(II), Cd(II) and Cu(II) ions, respectively.

  20. Aging time and brand determination of pasteurized milk using a multisensor e-nose combined with a voltammetric e-tongue.

    PubMed

    Bougrini, Madiha; Tahri, Khalid; Haddi, Zouhair; El Bari, Nezha; Llobet, Eduard; Jaffrezic-Renault, Nicole; Bouchikhi, Benachir

    2014-12-01

    A combined approach based on a multisensor system to get additional chemical information from liquid samples through the analysis of the solution and its headspace is illustrated and commented. In the present work, innovative analytical techniques, such as a hybrid e-nose and a voltammetric e-tongue were elaborated to differentiate between different pasteurized milk brands and for the exact recognition of their storage days through the data fusion technique of the combined system. The Principal Component Analysis (PCA) has shown an acceptable discrimination of the pasteurized milk brands on the first day of storage, when the two instruments were used independently. Contrariwise, PCA indicated that no clear storage day's discrimination can be drawn when the two instruments are applied separately. Mid-level of abstraction data fusion approach has demonstrated that results obtained by the data fusion approach outperformed the classification results of the e-nose and e-tongue taken individually. Furthermore, the Support Vector Machine (SVM) supervised method was applied to the new subset and confirmed that all storage days were correctly identified. This study can be generalized to several beverage and food products where their quality is based on the perception of odor and flavor. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Voltammetric sensor based on carbon paste electrode modified with molecular imprinted polymer for determination of sulfadiazine in milk and human serum.

    PubMed

    Sadeghi, Susan; Motaharian, Ali

    2013-12-01

    A new sensitive voltammetric sensor for determination of sulfadiazine is described. The developed sensor is based on carbon paste electrode modified with sulfadiazine imprinted polymer (MIP) as a recognition element. For comparison, a non-imprinted polymer (NIP) modified carbon paste electrode was prepared. Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods were performed to study the binding event and electrochemical behavior of sulfadiazine at the modified carbon paste electrodes. The determination of sulfadiazine after its extraction onto the electrode surface was carried out by DPV at 0.92 V vs. Ag/AgCl owing to oxidation of sulfadiazine. Under the optimized operational conditions, the peak current obtained at the MIP modified carbon paste electrode was proportional to the sulfadiazine concentration within the range of 2.0×10(-7)-1.0×10(-4) mol L(-1) with a detection limit and sensitivity of 1.4×10(-7) mol L(-1) and 4.2×10(5) μA L mol(-1), respectively. The reproducibility of the developed sensor in terms of relative standard deviation was 2.6%. The sensor was successfully applied for determination of sulfadiazine in spiked cow milk and human serum samples with recovery values in the range of 96.7-100.9%.

  2. Label-free voltammetric detection of MicroRNAs at multi-channel screen printed array of electrodes comparison to graphite sensors.

    PubMed

    Erdem, Arzum; Congur, Gulsah

    2014-01-01

    The multi-channel screen-printed array of electrodes (MUX-SPE16) was used in our study for the first time for electrochemical monitoring of nucleic acid hybridization related to different miRNA sequences (miRNA-16, miRNA-15a and miRNA-660, i.e, the biomarkers for Alzheimer disease). The MUX-SPE16 was also used for the first time herein for the label-free electrochemical detection of nucleic acid hybridization combined magnetic beads (MB) assay in comparison to the disposable pencil graphite electrode (PGE). Under the principle of the magnetic beads assay, the biotinylated inosine substituted DNA probe was firstly immobilized onto streptavidin coated MB, and then, the hybridization process between probe and its complementary miRNA sequence was performed at MB surface. The voltammetric transduction was performed using differential pulse voltammetry (DPV) technique in combination with the single-use graphite sensor technologies; PGE and MUX-SPE16 for miRNA detection by measuring the guanine oxidation signal without using any external indicator. The features of single-use sensor technologies, PGE and MUX-SPE16, were discussed concerning to their reproducibility, detection limit, and selectivity compared to the results in the earlier studies presenting the electrochemical miRNA detection related to different miRNA sequences.

  3. Voltammetric behavior of dopamine at a glassy carbon electrode modified with NiFe(2)O(4) magnetic nanoparticles decorated with multiwall carbon nanotubes.

    PubMed

    Ensafi, Ali A; Arashpour, B; Rezaei, B; Allafchian, Ali R

    2014-06-01

    Voltammetric behavior of dopamine was studied on a glassy carbon electrode (GCE) modified-NiFe(2)O(4) magnetic nanoparticles decorated with multiwall carbon nanotubes. Impedance spectroscopy and cyclic voltammetry were used to characterize the behavior of dopamine at the surface of modified-GCE. The modified electrode showed a synergic effect toward the oxidation of dopamine. The oxidation peak current is increased linearly with the dopamine concentration (at pH7.0) in wide dynamic ranges of 0.05-6.0 and 6.0-100μmolL(-1) with a detection limit of 0.02μmolL(-1), using differential pulse voltammetry. The selectivity of the method was studied and the results showed that the modified electrode is free from interference of organic compounds especially ascorbic acid, uric acid, cysteine and urea. Its applicability in the determination of dopamine in pharmaceutical, urine samples and human blood serum was also evaluated. The proposed electrochemical sensor has appropriate properties such as high selectivity, low detection limit and wide linear dynamic range when compared with that of the previous reported papers for dopamine detection. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Highly sensitive voltammetric sensor based on catechol-derivative-multiwall carbon nanotubes for the catalytic determination of captopril in patient human urine samples.

    PubMed

    Ensafi, A A; Karimi-Maleh, H; Mallakpour, S; Rezaei, B

    2011-10-15

    A new catechol-derivative compound, N-(3,4-dihydroxyphenethyl)-3,5-dinitrobenzamide, was synthesized and used to construct a modified-carbon nanotubes paste electrode. The electro-oxidation of captopril at the surface of the modified electrode was studied using cyclic voltammetry, chronoamperometry, and electrochemical impedance spectroscopy. Under the optimized conditions, the differential pulse voltammetric peak current of captopril increased linearly with captopril concentration in the ranges of 6.4×10(-8) to 3.2×10(-48) mol L(-1). The detection limit was 3.4×10(-8) mol L(-1) captopril. The diffusion coefficient and kinetic parameters (such as electron transfer coefficient and the heterogeneous rate constant) for captopril oxidation were also determined. The RSD% for 0.5 and 10.0 μmol L(-1) captopril were 2.1% and 1.6%, respectively. The proposed sensor was successfully applied for the determination of captopril in human patient urine and tablet samples.

  5. Simultaneous voltammetric determination of paracetamol and ascorbic acid using a boron-doped diamond electrode modified with Nafion and lead films.

    PubMed

    Tyszczuk-Rotko, Katarzyna; Bęczkowska, Ilona; Wójciak-Kosior, Magdalena; Sowa, Ireneusz

    2014-11-01

    The paper describes the fabrication and application of a novel sensor (a boron-doped diamond electrode modified with Nafion and lead films) for the simultaneous determination of paracetamol and ascorbic acid by differential pulse voltammetry. The main advantage of the lead film and polymer covered boron-doped diamond electrode is that the sensitivity of the stripping responses is increased and the separation of paracetamol and ascorbic acid signals is improved due to the modification of the boron-doped diamond surface by the lead layer. Additionally, the repeatability of paracetamol and ascorbic acid signals is improved by the application of the Nafion film coating. In the presence of oxygen, linear calibration curves were obtained in a wide concentration range from 5×10(-7) to 2×10(-4) mol L(-1) for paracetamol and from 1×10(-6) to 5×10(-4) mol L(-1) for ascorbic acid. The analytical utility of the differential pulse voltammetric method elaborated was tested in the assay of paracetamol and ascorbic acid in commercially available pharmaceutical formulations and the method was validated by high performance liquid chromatography coupled with diode array detector.

  6. Synthesis, crystal structure, Cu2+ doped EPR and voltammetric studies of bis[N-(2-hydroxyethyl)ethylenediamine]zinc(II) squarate monohydrate

    NASA Astrophysics Data System (ADS)

    Uçar, Ibrahim; Karabulut, Bünyamin; Bulut, Ahmet; Büyükgüngör, Orhan

    2007-01-01

    Crystal structure of [Zn(hydet-en)2]·C4O4·H2O (ZHES) (hydet-en is N-(2-hydroxyethyl)ethylenediamine) complex has been synthesized and characterized by analytical, spectroscopic (IR, UV/Vis) and voltammetric techniques. After doping Cu2+ ion, its magnetic environment has been identified by electron paramagnetic resonance (EPR) technique. The title complex crystalizes in monoclinic system with space group P21/c and with Z=4. Each hydet-en ligand acts as a tridentate ligand through the two N atoms and the hydroxyl O atom, resulting in a six coordinate Zn(II) ion. The EPR spectra were recorded in three perpendicular planes of Cu2+ doped ZHES single crystal. The calculated g and A values indicated that the paramagnetic center is rhombic symmetry with the Cu2+ ion having distorted octahedral environment. The molecular orbital bond coefficients of the Cu(II) ion in d9 state is also calculated by using EPR and optical absorption parameters. The dianion SQ2- is oxidized reversibly in two consecutive steps to the corresponding radical monoanion and neutral form.

  7. A novel voltammetric sensor for sensitive detection of mercury(II) ions using glassy carbon electrode modified with graphene-based ion imprinted polymer.

    PubMed

    Ghanei-Motlagh, Masoud; Taher, Mohammad Ali; Heydari, Abolfazl; Ghanei-Motlagh, Reza; Gupta, Vinod K

    2016-06-01

    In this paper, a novel strategy was proposed to prepare ion-imprinted polymer (IIP) on the surface of reduced graphene oxide (RGO). Polymerization was performed using methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, 2,2'-((9E,10E)-1,4-dihydroxyanthracene-9,10-diylidene) bis(hydrazine-1-carbothioamide) (DDBHCT) as the chelating agent and ammonium persulfate (APS) as initiator, via surface imprinted technique. The RGO-IIP was characterized by means of Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The electrochemical procedure was based on the accumulation of Hg(II) ions at the surface of a modified glassy carbon electrode (GCE) with RGO-IIP. The prepared RGO-IIP sensor has higher voltammetric response compared to the non-imprinted polymer (NIP), traditional IIP and RGO. The RGO-IIP modified electrode exhibited a linear relationship toward Hg(II) concentrations ranging from 0.07 to 80 μg L(-1). The limit of detection (LOD) was found to be 0.02 μg L(-1) (S/N=3), below the guideline value from the World Health Organization (WHO). The applicability of the proposed electrochemical sensor to determination of mercury(II) ions in different water samples was reported.

  8. Application of CdO nanoparticle ionic liquid modified carbon paste electrode as a high sensitive biosensor for square wave voltammetric determination of NADH.

    PubMed

    Pahlavan, Ali; Karimi-Maleh, Hassan; Karimi, Fatemeh; Amiri, Mohsen Aboukazempour; Khoshnama, Zahra; Shahmiri, Mandana Roodbari; Keyvanfard, Mohsen

    2014-12-01

    In this paper we report the synthesis and application of CdO nanoparticle (CdO/NPs) and 1,3-dipropylimidazolium bromide as high sensitive sensors for voltammetric determination of nicotinamide adenine dinucleotide (NADH) using carbon paste electrode. The cyclic voltammogram showed an irreversible oxidation peak at 0.68 V (vs. Ag/AgClsat), which corresponded to the oxidation of NADH. Compared to common carbon paste electrode, the electrochemical response was greatly improved for NADH electrooxidation at a surface of CdO/NP modified ionic liquid carbon paste electrode (IL/CdO/NP/CPE). The linear response range and detection limit were found to be 0.09-750 μmol L(-1) and 0.05 μmol L(-1), respectively. Result shows that other physiological species did not interfere in the determination of NADH at the surface of the proposed sensor in the optimum condition. The proposed sensor was successfully applied for the determination of NADH in tap water, urine and pharmaceutical serum samples.

  9. Development of a Nafion/MWCNT-SPCE-Based Portable Sensor for the Voltammetric Analysis of the Anti-Tuberculosis Drug Ethambutol

    PubMed Central

    Couto, Rosa A. S.; Quinaz, Maria Beatriz

    2016-01-01

    Herein we describe the development, characterization and application of an electrochemical sensor based on the use of Nafion/MWCNT-modified screen-printed carbon electrodes (SPCEs) for the voltammetric detection of the anti-tuberculosis (anti-TB) drug ethambutol (ETB). The electrochemical behaviour of the drug at the surface of the developed Nafion/MWCNT-SPCEs was studied through cyclic voltammetry (CV) and square wave voltammetry (SWV) techniques. Electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM) were employed to characterize the modified surface of the electrodes. Results showed that, compared to both unmodified and MWCNTs-modified SPCEs, negatively charged Nafion/MWCNT-SPCEs remarkably enhanced the electrochemical sensitivity and selectivity for ETB due to the synergistic effect of the electrostatic interaction between cationic ETB molecules and negatively charged Nafion polymer and the inherent electrocatalytic properties of both MWCNTs and Nafion. Nafion/MWCNT-SPCEs provided excellent biocompatibility, good electrical conductivity, low electrochemical interferences and a high signal-to-noise ratio, providing excellent performance towards ETB quantification in microvolumes of human urine and human blood serum samples. The outcomes of this paper confirm that the Nafion/MWCNT-SPCE-based device could be a potential candidate for the development of a low-cost, yet reliable and efficient electrochemical portable sensor for the low-level detection of this antimycobacterial drug in biological samples. PMID:27376291

  10. Development of a carbon paste electrode containing benzo-15-crown-5 for trace determination of the uranyl ion by using a voltammetric technique.

    PubMed

    Agrahari, Sunil K; Kumar, Sangita D; Srivastava, Ashwini K

    2009-01-01

    The interaction of macrocyclic compounds like crown ethers and UO2(2+) has been studied by electrochemical methods. A modified carbon paste electrode incorporating benzo-15-crown-5 (B15C5) was used to evaluate the electron transfer reaction of UO2(2+) by cyclic voltammetry, differential pulse voltammetry, and electrochemical impedance spectroscopy. Electrochemical impedance studies showed that charge transfer resistance was less for the B15C5-modified electrode than for the plain carbon paste electrode (PCPE). On the basis of these observations, a UO2(2+)-sensitive crown ether chemically modified electrode (CME) for trace analysis was fabricated and investigated in aqueous solutions. It was found that a 5% B15C5-CME for UO2(2+) showed a better voltammetric response than did the PCPE. UO2(2+) could be quantified at sub-microg/mL levels by differential pulse voltammetry with a detection limit of 0.03 microg/mL. By differential pulse adsorptive stripping voltammetry, UO2(2+) could be quantified in the working range of 0.002-0.2 microg/mL, with a detection limit of 1.1 microg/L. Simultaneous determination of UO2(2+), Pb(2+), and Cd(2+) was possible. The method was successfully applied to the determination of UO2(2+) in synthetic, as well as real, samples; the results were found to be comparable to those obtained by inductively coupled plasma-atomic emission spectroscopy.

  11. Modification of glassy carbon electrode with a bilayer of multiwalled carbon nanotube/tiron-doped polypyrrole: Application to sensitive voltammetric determination of acyclovir.

    PubMed

    Shahrokhian, Saeed; Azimzadeh, Mahnaz; Amini, Mohammad K

    2015-08-01

    A novel voltammetric sensor based on glassy carbon electrode (GCE) modified with a thin film of multi-walled carbon nanotubes (MWCNTs) coated with an electropolymerized layer of tiron-doped polypyrrole was developed and the resulting electrode was applied for the determination of acyclovir (ACV). The surface morphology and property of the modified electrode were characterized by field emission scanning electron microscopy and electrochemical impedance spectroscopy techniques. The electrochemical performance of the modified electrode was investigated by means of linear sweep voltammetry (LSV). The effect of several experimental variables, such as pH of the supporting electrolyte, drop size of the cast MWCNTssuspension, number of electropolymerization cycles and accumulation time was optimized by monitoring the LSV response of the modified electrode toward ACV. The best response was observed at pH7.0 after accumulation at open circuit for 160 s. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of ACV on the modified electrode surface relative to the bare GCE, resulting in a wide linear dynamic range (0.03-10.0μ M) and a low detection limit (10.0 nM) for ACV. Besides high sensitivity, the sensor represented high stability and good reproducibility for ACV analysis, and provided satisfactory results for the determination of this compound in pharmaceutical and clinical preparations. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Fabrication of electrochemical interface based on boronic acid-modified pyrroloquinoline quinine/reduced graphene oxide composites for voltammetric determination of glycated hemoglobin.

    PubMed

    Zhou, Yanli; Dong, Hui; Liu, Lantao; Hao, Yuanqiang; Chang, Zhu; Xu, Maotian

    2015-02-15

    A voltammetric sensor for determination of glycated hemoglobin (HbA1c) was developed based on the composites of phenylboronic acid-modified pyrroloquinoline quinine (PBA-PQQ) and reduced graphene oxide. After the electrodeposition of reduced graphene oxide (ERGO) on the glassy carbon (GC) electrode, PQQ multilayer was decorated on the surface of the ERGO/GC electrode via potential cycling. Further modification with PBA would lead to the formation of the working electrode, namely PBA-PQQ/ERGO/GC electrode. PQQ on the electrode exhibited a quasi-reversible electrode process with 2-electron transfer and 2-proton participation, and the electron transfer efficiency was further enhanced by the introduction of ERGO layer. The complexation of PBA with HbA1c through specific boronic acid-diol recognition could cause the change of the oxidation peak current of PQQ on the electrode, which was utilized for HbA1c detection. Under the optimized conditions, the PBA-PQQ/ERGO/GC electrode provided high selectivity and high sensitivity for HbA1c detection with a linear range of 9.4-65.8 μg mL(-1) and a low detection limit of 1.25 μg mL(-1). The fabricated sensor was also successfully applied to determine the percentages of HbA1c in whole blood of healthy individuals.

  13. Conductive Polymeric Ionic Liquid/Fe3O4 Nanocomposite as an Efficient Catalyst for the Voltammetric Determination of Amlodipine Besylate.

    PubMed

    Fathirad, Fariba; Mostafavi, Ali; Afzali, Daryoush

    2017-03-01

    A novel conductive polymeric ionic liquid (IL)-Fe3O4 nanocomposite (represented as PIL-Fe3O4) based on inorganic-organic hybrid material was synthesized using two different methods. Nuclear magnetic resonance, Fourier transform infrared, X-ray diffraction, and field emission scanning electron microscopy characterized the structures of IL, Fe3O4 nanoparticles, and PIL-Fe3O4. The electrochemical sensors based on PIL-Fe3O4-modified glassy carbon electrode were fabricated, and each of these nanocomposites was examined for the ability to determine amlodipine besylate (AMD). The electrochemical study of the modified electrodes, as well as its efficiency for the electro-oxidation of AMD, was described in 0.1 M phosphate-buffered solution (pH 7.0) using voltammetric methods. The results exhibit a linear dynamic range from 1 to 500 nM and a detection limit of 0.36 nM. Finally, the modified electrode was used for the determination of AMD in pharmaceutical and biological samples.

  14. Improving the voltammetric quantification of ill-defined peaks using second derivative signal transformation: example of the determination of platinum in water and sediments.

    PubMed

    Cobelo-García, Antonio; Santos-Echeandía, Juan; López-Sánchez, Daniel E; Almécija, Clara; Omanović, Dario

    2014-03-04

    The determination of trace elements using stripping voltammetry may be seriously affected by the presence of intensive matrix background or interfering peaks, leading to poorer detection limits and/or inaccurate quantitative results. In this work, we have tested the use of signal transformation (e.g., second derivative) in the analysis of platinum in seawater and sediment digests by means of catalytic adsorptive stripping voltammetry. In natural waters, the limit of detection of Pt is affected by a broad background wave due to the formazone complex used in the sample matrix for its determination, while in sediment digests, the Pt peak may be interfered with due to the presence of elevated concentrations of Zn, affecting the accuracy of the determination. Results applying second derivative signal transformation revealed a significant improvement (2-3-fold) of the detection limit in water due to the minimization of background effects, therefore allowing shorter accumulation times and faster determinations. In the presence of interfering peaks, the inaccuracy resulting from erroneous baseline selection in the original signal is eliminated when the second derivative is used. Signal processing should be considered as a useful tool for other voltammetric methodologies where more accurate or faster determinations are needed.

  15. A sensitive and selective voltammetric sensor based on multiwall carbon nanotubes decorated with MgCr₂O₄ for the determination of azithromycin.

    PubMed

    Ensafi, Ali A; Allafchian, Ali R; Rezaei, B

    2013-03-01

    In this report, we synthesized MgCr(2)O(4) nanoparticles and then multiwall carbon nanotubes were decorated with the MgCr(2)O(4) nanoparticles. The characteristics of the new materials were studied with different techniques such as transmission electron microscopy, Fourier transform infrared spectroscopy, atomic force microscopy and electrochemical impedance spectroscopy. The multiwall carbon nanotubes decorated with MgCr(2)O(4) nanoparticles were used as a new mediator for voltammetric determination of azithromycin. The oxidation peak of azithromycin was appeared at a potential of about 720 mV at a surface of the modified electrode. Differential pulse voltammetry exhibited two wide linear dynamic ranges of 0.25-4.0 and 4.0-10.0 μmol L(-1) azithromycin with a detection limit of 0.07 μmol L(-1) at pH 7.0. The influence of potential interfering compounds on the selectivity was studied. Finally, the modified electrode showed good sensitivity, selectivity and stability for the determination of azithromycin in real samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Poly(3-methylthiophene)/palladium sub-micro-modified sensor electrode. Part II: Voltammetric and EIS studies, and analysis of catecholamine neurotransmitters, ascorbic acid and acetaminophen.

    PubMed

    Atta, Nada F; El-Kady, Maher F

    2009-08-15

    Promising voltammetric sensors based on the modification of Pt and poly(3-methylthiophene) (PMT) electrodes with Pd nanoparticles were achieved for the determination of catecholamine neurotransmitters, ascorbic acid and acetaminophen. Electrochemistry of the indicated compounds was studied at these electrodes and interesting electrocatalytic effects were found. Furthermore, simple, easily prepared one electrochemical step Pd-modified Pt electrode (Pt/Pd) is reported for the first time. Cyclic voltammetry (CV) and chronocoulometry (CC) were used for the determination of the apparent diffusion coefficients in different electrolytes at these electrodes and the values are in the range from 10(-4) to 10(-5)cm(2)s(-1). Furthermore, it was found that the method of polymer formation had a substantial effect on the synergism between the polymer film and the loaded metal particles towards the oxidation of dopamine (DA) in different supporting electrolytes. This was confirmed by the CV, CC and EIS (electrochemical impedance spectroscopy) as well as SEM (Scanning Electron Microscopy) results. Pt and PMT electrodes modified with Pd nanoparticles showed excellent results for the simultaneous determination of tertiary and quaternary mixtures of the studied compounds.

  17. A novel nanostructured composite formed by interaction of copper octa(3-aminopropyl)octasilsesquioxane with azide ligands: Preparation, characterization and a voltammetric application

    SciTech Connect

    Ribeiro do Carmo, Devaney; Paim, Leonardo Lataro; Dias Filho, Newton Luiz; Stradiotto, Nelson Ramos

    2010-09-15

    This study presents the preparation, characterization and application of copper octa(3-aminopropyl)octasilsesquioxane following its subsequent reaction with azide ions (ASCA). The precursor (AC) and the novel compound (ASCA) were characterized by Fourier transform infrared spectra (FTIR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR), scanning electronic microscopy (SEM), X-ray diffraction (XRD), Thermogravimetric analyses and voltammetric technique. The cyclic voltammogram of the modified graphite paste electrode with ASCA (GPE-ASCA), showed one redox couple with formal potential (E{sub 1/2}{sup ox}) = 0.30 V and an irreversible process at 1.1 V (vs. Ag/AgCl; NaCl 1.0 M; v=20mVs{sup -1}). The material is very sensitive to nitrite concentrations. The modified graphite paste electrode (GPE-ASCA) gives a linear range from 1.0 x 10{sup -4} to 4.0 x 10{sup -3} mol L{sup -1} for the determination of nitrite, with a detection limit of 2.1 x 10{sup -4} mol L{sup -1} and the amperometric sensitivity of 8.04 mA/mol L{sup -1}.

  18. Nanogold-penetrated poly(amidoamine) dendrimer for enzyme-free electrochemical immunoassay of cardiac biomarker using cathodic stripping voltammetric method.

    PubMed

    Zhang, Bo; Zhang, Yi; Liang, Wenbin; Cui, Bin; Li, Jiabei; Yu, Xuejun; Huang, Lan

    2016-01-21

    Methods based on immunoassays have been developed for cardiac biomarkers, but most involve the low sensitivity and are unsuitable for early disease diagnosis. Herein we design an electrochemical immunoassay for sensitive detection of myoglobin (a cardiac biomarker for acute myocardial infarction) by using nanogold-penetrated poly(amidoamine) dendrimer (AuNP-PAMAM) for signal amplification without the need of natural enzymes. The assay was carried out on the monoclonal mouse anti-myoglobin (capture) antibody-anchored glassy carbon electrode using polyclonal rabbit anti-myoglobin (detection) antibody-labeled AuNP-PAMAM as the signal tag. In the presence of target myoglobin, the sandwiched immunocomplex could be formed between capture antibody and detection antibody. Accompanying AuNP-PAMAM, the carried gold nanoparticles could be directly determined via stripping voltammetric method under acidic conditions. Under optimal conditions, the detectable electrochemical signal increased with the increasing target myoglobin in the sample within a dynamic working range from 0.01 to 500 ng mL(-1) with a detection limit of 3.8 pg mL(-1). The electrochemical immunoassay also exhibited high specificity and good precision toward target myoglobin. Importantly, our strategy could be applied for quantitative monitoring of myoglobin in human serum specimens, giving well matched results with those obtained from commercialized enzyme-linked immunosorbent assay (ELISA) method.

  19. Amplified voltammetric detection of miRNA from serum samples of glioma patients via combination of conducting magnetic microbeads and ferrocene-capped gold nanoparticle/streptavidin conjugates.

    PubMed

    Lu, Zhixuan; Tang, Hailin; Wu, Daohong; Xia, Yonghong; Wu, Minghua; Yi, Xinyao; Li, Hengfeng; Wang, Jianxiu

    2016-12-15

    MicroRNA (miRNA) plays a key regulatory role in many biological processes, emerging as an important biomarker for a large variety of cancer diseases. Employing gold nanoparticle (AuNP)-coated magnetic microbeads (AuNP-MMBs) as an immobilization matrix for higher loading density of hairpin-structured DNA probes and then ferrocene (Fc)-capped gold nanoparticle/streptavidin conjugates, amplified electrochemical assay of miRNA has been performed. In the presence of target miRNA, a novel assembly was formed via linking biotinylated hairpin DNA probe-covered AuNP-MMBs with Fc-capped gold nanoparticle/streptavidin conjugates and then collected by magnetic electrodes for voltammetric detection. The enlarged surface area, good conductivity of AuNP-MMBs and the multiple Fc tags on the electrode surface ensure high sensitivity of the method. The oxidation peak current of Fc tags is proportional to the concentrations of miRNA ranging from 5 fM to 100 fM, and a detection limit of 0.14 fM was achieved. The proposed assay is highly selective and reproducible, serving as a viable alternative for the detection of miRNA-182 from serum samples of glioma patients.

  20. A validated stripping voltammetric procedure for quantification of the anti-hypertensive and benign prostatic hyperplasia drug terazosin in tablets and human serum.

    PubMed

    Ghoneim, M M; El Ries, M A; Hammam, E; Beltagi, A M

    2004-10-20

    The electrochemical behavior of terazosin at the hanging mercury drop electrode was studied in Britton-Robinson buffer (pH 2-11), acetate buffer (4.5-5.5), and in 0.1M solution of each of sodium sulfate, sodium nitrate, sodium perchlorate and potassium chloride as supporting electrolytes. The square-wave adsorptive cathodic stripping voltammogram of terazosin exhibited a single well-defined two-electron irreversible cathodic peak which may be attributed to the reduction of CO double bond of the drug molecule. A fully validated, simple, high sensitive, precise and inexpensive square-wave adsorptive cathodic stripping voltammetric procedure was described for determination of terazosin in bulk form, tablets and human serum. A mean recovery for 1x10(-8)M terazosin in bulk form, following preconcentration onto the hanging mercury drop electrode for 60s at a -1.0V (versus Ag/AgCl/KCl(s)), of 99+/-0.7% (n=5) was obtained. Limits of detection (LOD) and quantitation (LOQ) of 1.5x10(-11) and 5x10(-11)M bulk terazosin were achieved, respectively. The proposed procedure was successfully applied to determination of the drug in its Itrin((R)) tablets and human serum samples. The achieved LOD and LOQ of the drug in human serum samples were 5.3x10(-11) and 1.8x10(-10)M THD, respectively. The pharmacokinetic parameters of the drug in human plasma were estimated as: C(max)=77.5ngml(-1), t(max)=1.75h, AUC(0-t)=602.3nghml(-1), K(e)=0.088h(-1) and t(1/2)=11.32h) which are favorably compared with those reported in literature.

  1. Optimization of Stripping Voltammetric Sensor by a Back Propagation Artificial Neural Network for the Accurate Determination of Pb(II) in the Presence of Cd(II).

    PubMed

    Zhao, Guo; Wang, Hui; Liu, Gang; Wang, Zhiqiang

    2016-09-21

    An easy, but effective, method has been proposed to detect and quantify the Pb(II) in the presence of Cd(II) based on a Bi/glassy carbon electrode (Bi/GCE) with the combination of a back propagation artificial neural network (BP-ANN) and square wave anodic stripping voltammetry (SWASV) without further electrode modification. The effects of Cd(II) in different concentrations on stripping responses of Pb(II) was studied. The results indicate that the presence of Cd(II) will reduce the prediction precision of a direct calibration model. Therefore, a two-input and one-output BP-ANN was built for the optimization of a stripping voltammetric sensor, which considering the combined effects of Cd(II) and Pb(II) on the SWASV detection of Pb(II) and establishing the nonlinear relationship between the stripping peak currents of Pb(II) and Cd(II) and the concentration of Pb(II). The key parameters of the BP-ANN and the factors affecting the SWASV detection of Pb(II) were optimized. The prediction performance of direct calibration model and BP-ANN model were tested with regard to the mean absolute error (MAE), root mean square error (RMSE), average relative error (ARE), and correlation coefficient. The results proved that the BP-ANN model exhibited higher prediction accuracy than the direct calibration model. Finally, a real samples analysis was performed to determine trace Pb(II) in some soil specimens with satisfactory results.

  2. Development and validation of an adsorptive stripping voltammetric method for the quantification of vincamine in its formulations and human serum using a Nujol-based carbon paste electrode.

    PubMed

    Beltagi, Amr Mohamed

    2008-12-01

    An easy, rapid and selective adsorptive stripping voltammetry (AdSV) method for the determination of vincamine in its formulation and human serum was developed and validated. It was based on the oxidation of the drug onto a Nujol-based carbon paste electrode. The stripping step was carried out by using a square-wave (SW) potential-time voltammetric excitation signal. The optimal experimental variables as well as accumulation parameters were investigated as; frequency f=120 Hz, scan increment DeltaE(i)=10 mV, pulse-amplitude DeltaE(a)=25 mV and an accumulation potential E(acc) of 0.0 V using a Britton-Robinson (B-R) universal buffer of pH 5 as a supporting electrolyte. After validation of the described method, it was applied for determination of vincamine in its formulation and human serum. Mean recovery of 100.41+/-0.74 (n=5) was achieved for assay of vincamine in Oxybral capsules. Limits of detection and quantitation of 6.0 x 10(-9) M (2.20 ng ml(-1)) and 2 x 10(-8) M (7.33 ng ml(-1)) vincamine were achieved in human serum with a mean recovery of 99.5+/-1.79%, without prior extraction of the drug. No interferences were observed in formulation and/or human serum. Due to high sensitivity and specificity of the developed method, it was successfully applied for evaluating some pharmacokinetic parameters of two healthy volunteers after administration of a single oral Oxybral capsule.

  3. High selective SiO2-Al2O3 mixed-oxide modified carbon paste electrode for anodic stripping voltammetric determination of Pb(II).

    PubMed

    Ghiaci, M; Rezaei, B; Kalbasi, R J

    2007-08-15

    The main purpose of this study is to develop an inexpensive, simple, selective and especially highly selective modified mixed-oxide carbon paste electrode (CPE) for voltammetric determination of Pb(II). For the preliminary screening purpose, the catalyst was prepared by modification of SiO(2)-Al(2)O(3) mixed-oxide and characterized by TG, CHN elemental analysis and FTIR spectroscopy. Using cyclic voltammetry the electroanalytical characteristics of the catalyst have been determined, and consequently the modified mixed-oxide carbon paste electrode was constructed and applied for determination of Pb(II). The electroanalytical procedure for determination of the Pb(II) comprises two steps: the chemical accumulation of the analyte under open-circuit conditions followed by the electrochemical detection of the preconcentrated species using differential pulse anodic stripping voltammetry. During the preconcentration step, Pb(II) was accumulated on the surface of the modifier by the formation of a complex with the nitrogen atoms of the pyridyl groups in the modifier. The peak currents increases linearly with Pb(II) concentration over the range of 2.0 x 10(-9) to 5.2 x 10(-5)mol L(-1) (r(2)=0.9995). The detection limit (three times signal-to-noise) was found to be 1.07 x 10(-9)mol L(-1) Pb(II). The chemical and instrumental parameters have been optimized and the effect of the interferences has been determined. The Proposed method was used for determination of lead ion in the real samples.

  4. Stripping analysis of nanomolar perchlorate in drinking water with a voltammetric ion-selective electrode based on thin-layer liquid membrane.

    PubMed

    Kim, Yushin; Amemiya, Shigeru

    2008-08-01

    A highly sensitive analytical method is required for the assessment of nanomolar perchlorate contamination in drinking water as an emerging environmental problem. We developed the novel approach based on a voltammetric ion-selective electrode to enable the electrochemical detection of "redox-inactive" perchlorate at a nanomolar level without its electrolysis. The perchlorate-selective electrode is based on the submicrometer-thick plasticized poly(vinyl chloride) membrane spin-coated on the poly(3-octylthiophene)-modified gold electrode. The liquid membrane serves as the first thin-layer cell for ion-transfer stripping voltammetry to give low detection limits of 0.2-0.5 nM perchlorate in deionized water, commercial bottled water, and tap water under a rotating electrode configuration. The detection limits are not only much lower than the action limit (approximately 246 nM) set by the U.S. Environmental Protection Agency but also are comparable to the detection limits of the most sensitive analytical methods for detecting perchlorate, that is, ion chromatography coupled with a suppressed conductivity detector (0.55 nM) or electrospray ionization mass spectrometry (0.20-0.25 nM). The mass transfer of perchlorate in the thin-layer liquid membrane and aqueous sample as well as its transfer at the interface between the two phases were studied experimentally and theoretically to achieve the low detection limits. The advantages of ion-transfer stripping voltammetry with a thin-layer liquid membrane against traditional ion-selective potentiometry are demonstrated in terms of a detection limit, a response time, and selectivity.

  5. Development of a rotary disc voltammetric sensor system for semi-continuous and on-site measurements of Pb(II).

    PubMed

    Lee, Yong-Gu; Han, Jungyoup; Kwon, Soondong; Kang, Seoktae; Jang, Am

    2016-01-01

    Atomic absorption spectrometry and inductively coupled plasma-mass spectrometry are widely used for determination of heavy metals due to their low detection limits. However, they are not applicable to on-site measurements of heavy metals as bulky equipment, and highly skilled laboratory staffs are needed as well. In this study, a novel analytical method using a rotary disc voltammetric (RDV) sensor has been successfully designed, fabricated and characterized for semi-continuous and on-site measurements of trace levels of Pb(II) in non-deoxygenating solutions. The square wave anodic stripping voltammetry was used to improve the sensitivity of the Pb(II) detection level with less than 10nM (2μgL(-1)). The RDV sensor has 24-sensing holes to measure concentrations of Pb(II) semi-continuously at sampling sites. Each sensing hole consists of a silver working electrode, an integrated silver counter, and a quasi-reference electrode, which requires only a small amount of samples (<30μL) for measurement of Pb(II) without disturbing and/or clogging the sensing environment. In addition, the RDV sensor showed a correlation coefficient of 0.998 for the Pb(II) concentration range of 10nM-10μM at the deposition time of 180s and its low detection limit was 6.19nM (1.3μgL(-1)). These results indicated that the advanced monitoring technique using a RDV sensor might provide environmental engineers with a reliable way for semi-continuous and on-site measurements of Pb(II).

  6. Microfabricated three-electrode on-chip PDMS device with a vibration motor for stripping voltammetric detection of heavy metal ions.

    PubMed

    Zhang, Wen; Zhang, Han; Williams, Spencer E; Zhou, Anhong

    2015-01-01

    A microfabricated three-electrode on-chip device with a vibration motor for stripping voltammetric detection of Cd(2+) and Pb(2+) ions is introduced. Gold electrodes on a glass substrate are utilized as the counter electrode directly, as well as the working electrode with bismuth coating. The reference electrode is achieved by painting silver/silver chloride layer on the gold layer. Polydimethylsiloxane (PDMS) cover is bonded onto the glass substrate, organizing a compact module. A vibration motor in the device provides vibration as the alternate for stirring to improve detection limits and decrease deposition time. Cyclic voltammetry (CV) is performed with the on-chip reference electrode and a commercial liquid electrolyte Ag/AgCl electrode, showing that the potential shift is less than 20 mV. Differential pulse stripping voltammetry (DPSV) is used to detect Cd(2+) and Pb(2+) ions. Linearity is well defined from 10 µg/L to 80 µg/L for both ions. Detection limits for Cd(2+) and Pb(2+) ions are 0.7 µg/L and 1.2 µg/L, respectively, at 325 s deposition without vibration; the limits are 0.11 µg/L and 0.25 µg/L at 120 s deposition with vibration. The reliability is verified by detecting Cd(2+) and Pb(2+) concentrations of natural water samples and comparing with the results obtained from inductively coupled plasma mass spectrometry (ICP-MS). Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Salts purification and voltammetric study of the electroreduction of U(IV) to U(III) in molten LiF-ThF 4

    NASA Astrophysics Data System (ADS)

    Afonichkin, V.; Bovet, A.; Shishkin, V.

    2011-12-01

    Introduction of molten fluorides as reactor coolants and fuels (both as actinide burner and Th-U breeder) is one of the promising ways to sustainable development of these reactors. Special attention should be paid to the on-line control of the redox condition of the circulating molten fluorides mixtures, in particular, of the U(IV)/U(III) ratio by voltammetry. A "dry" technique for production and purification of metal fluorides, their mixtures, and fusion cakes without gaseous HF has been developed. The experimental studies confirmed that solid NH 4HF 2 can be efficiently used instead of the HF gas for conversion of UO 2 and ThO 2 to anhydrous tetrafluorides and for removal of oxygen-containing impurities from fluoride salts. The electrochemical behavior of UF 4 in a 77LiF-23ThF 4 (mole%) melt was studied by cyclic voltammetry at temperatures up to 800 °C. The studies have revealed that well reproducible voltammograms can only be obtained in partially reduced LiF-ThF 4-UF 4 melts containing UF 3, which are free from electropositive impurity ions. Processing of the experimental dependences shows that the basic calculated characteristics of the stage U(IV) electroreduction to U(III) considerably differ from the theoretical values corresponding to the one-electron process governed by a diffusion-controlled charge transfer. This points to quasi-reversibility of the electrode reaction studied. Since the Nernst equation can be used for processing voltammograms only reversible electroreduction U(IV), quasi-reversibility will lead to errors in voltammetric determination of the equilibrium relations U(IV)/U(III) in the melt studied. The results have to be considered as estimates or semiquantitative values.

  8. Optimization of Stripping Voltammetric Sensor by a Back Propagation Artificial Neural Network for the Accurate Determination of Pb(II) in the Presence of Cd(II)

    PubMed Central

    Zhao, Guo; Wang, Hui; Liu, Gang; Wang, Zhiqiang

    2016-01-01

    An easy, but effective, method has been proposed to detect and quantify the Pb(II) in the presence of Cd(II) based on a Bi/glassy carbon electrode (Bi/GCE) with the combination of a back propagation artificial neural network (BP-ANN) and square wave anodic stripping voltammetry (SWASV) without further electrode modification. The effects of Cd(II) in different concentrations on stripping responses of Pb(II) was studied. The results indicate that the presence of Cd(II) will reduce the prediction precision of a direct calibration model. Therefore, a two-input and one-output BP-ANN was built for the optimization of a stripping voltammetric sensor, which considering the combined effects of Cd(II) and Pb(II) on the SWASV detection of Pb(II) and establishing the nonlinear relationship between the stripping peak currents of Pb(II) and Cd(II) and the concentration of Pb(II). The key parameters of the BP-ANN and the factors affecting the SWASV detection of Pb(II) were optimized. The prediction performance of direct calibration model and BP-ANN model were tested with regard to the mean absolute error (MAE), root mean square error (RMSE), average relative error (ARE), and correlation coefficient. The results proved that the BP-ANN model exhibited higher prediction accuracy than the direct calibration model. Finally, a real samples analysis was performed to determine trace Pb(II) in some soil specimens with satisfactory results. PMID:27657083

  9. Analytical procedure for the simultaneous voltammetric determination of trace metals in food and environmental matrices. Critical comparison with atomic absorption spectroscopic measurements.

    PubMed

    Melucci, Dora; Torsi, Giancarlo; Locatelli, Clinio

    2007-01-01

    An analytical procedure fit for the simultaneous determination of copper (II), chromium(VI), thallium(I), lead(II), tin(II), antimony(III), and zinc(II) by square wave anodic stripping voltammetry (SWASV) in three interdependent environmental matrices involved in foods and food chain as meals, cereal plants and soils is described. The digestion of each matrix was carried out using a concentrated HCl-HNO3-H2SO4 (meals and cereal plants) and HCl-HNO3 (soils) acidic attack mixtures. 0.1 mol/L dibasic ammonium citrate pH 8.5 was employed as the supporting electrolyte. The voltammetric measurements were carried out using, as working electrode, a stationary hanging mercury drop electrode (HMDE) and a platinum electrode and an Ag/AgCl/KClsat electrode as auxiliary and reference electrodes, respectively. The analytical procedure was verified by the analyses of the standard reference materials: Wholemeal BCR-CRM 189, Tomato Leaves NIST-SRM 1573a and Montana Soil Moderately Elevated Traces NIST-SRM 2711. For all the elements in the certified matrix, the precision as repeatability, expressed as relative standard deviation (Sr %) was lower than 5%. The accuracy, expressed as percentage relative error (e %) was of the order of 3-7%, while the detection limits were in the range 0.015-0.103 microg/g. Once set up on the standard reference materials, the analytical procedure was transferred and applied to commercial meal samples, cereal plants and soils samples drawn in sites devoted to agricultural practice. A critical comparison with spectroscopic measurements is also discussed.

  10. Potential heating caused by intraparenchymal intracranial pressure transducers in a 3-tesla magnetic resonance imaging system using a body radiofrequency resonator: assessment of the Codman MicroSensor Transducer.

    PubMed

    Newcombe, Virginia F J; Hawkes, Robert C; Harding, Sally G; Willcox, Roslyn; Brock, Sarah; Hutchinson, Peter J; Menon, David K; Carpenter, T Adrian; Coles, Jonathan P

    2008-07-01

    Magnetic resonance imaging and spectroscopy may provide important clinical information in the acute stages of brain injury. For this to occur it must be ensured that intracranial pressure (ICP) monitoring devices are safe to bring into the MR imaging suite. The authors tested a Codman MicroSensor ICP Transducer (Codman & Shurtleff, Inc.) within a 3-T MR imaging system using the transmit body coil and receive-only coils and the transmit-and-receive head coil. Extreme and rapid heating of 64 degrees C was noted with the transducer wire in certain positions when using the transmit body coil and receive-only head coil. This is consistent with the phenomenon of resonance, and the probe was shown to have a distinct resonant response when coupled to HP 4195A Network Analyzer (Hewlett Packard). Coiling some of the transducer wire outside of the receive-only head coil reduced the generated current and so stopped the thermogenesis. This may be due to the introduction of a radiofrequency choke. The ICP transducer performed within clinically acceptable limits in both the static magnetic field and during imaging with high radiofrequency power when the excess wire was in this configuration. No heating was observed when a transmit-and-receive head coil was used. This study has shown when using a high-field magnet, the Codman ICP probe is MR conditional. That is, in the authors' system, it can be safely used with the transmit-and-receive head coil, but when using the transmit body coil the transducer wire must be coiled into concentric loops outside of the receive-only head coil.

  11. Theory and experiments for voltammetric and SECM investigations and application to ORR electrocatalysis at nanoelectrode ensembles of ultramicroelectrode dimensions.

    PubMed

    Fernández, José L; Wijesinghe, Manjula; Zoski, Cynthia G

    2015-01-20

    Theoretical and experimental approaches to characterizing nanoelectrode (NE) ensembles of ultramicroelectrode dimensions (UME-NEEs) as a function of fraction of active area and random NE distribution are described. UME-NEEs were fabricated by addressing microregions of a gold-filled polycarbonate membrane through the UMEs of an underlying microfabricated addressable array. Results of Comsol Multiphysics 3D simulations based on randomly spaced NEs of 15 nm radius on a UME disk geometry of radii up to 5 μm are shown for steady-state voltammetry (SSV) and scanning electrochemical microscopy (SECM) experiments. Analytical equations were developed to describe the diffusion-limited steady-state current and steady-state voltammogram at an UME-NEE. These equations are shown to be in good agreement with the simulations and enabled evaluation of experimental SSVs. Comparison of experimental and simulated SECM approach curves, images, and tip voltammograms enabled the fraction of active area and distribution of NEs to be visualized and determined for individual UME-NEEs. Gold UME-NEEs are shown to be unique platforms for electrodeposition in forming nanoparticle electrodes (UME-NPEs). Electrocatalysis results for the oxygen reduction reaction (ORR) on Pt UME-NPEs in 0.1 M H2SO4 are also shown.

  12. Voltammetric detection of the α-dicarbonyl compound: methylglyoxal as a flavoring agent in wine and beer.

    PubMed

    Chatterjee, Sanghamitra; Chen, Aicheng

    2012-11-02

    A simple, rapid and highly selective method for the determination of the most abundant α-dicarbonyl compound in wine and beer has been developed for the first time by employing square wave voltammetry. A novel electrochemical sensor, based on the electrodeposition of platinum nanoparticles onto single wall carbon nanotubes that were cast on a glassy carbon electrode (GCE) substrate, is presented in this paper. This modified electrode exhibited excellent catalytic activity in the electroreduction of methylglyoxal, showing much higher peak currents than those measured on an unmodified GCE. The effects of different experimental and instrumental parameters, such as solution pH and square wave frequency, were examined. The reduction peak current showed a linear range of from 0.1×10(-6) to 100×10(-6)M with a 0.9979 correlation coefficient; and a low detection limit of 2.8×10(-9)M was also obtained. The proposed methodology was successfully applied to the quantitative analysis of methylglyoxal in wine and beer samples. The developed sensor possesses advantageous properties such as a high active surface area, stability, and rapid electron transfer rate, which cumulatively demonstrate high performance toward the electrocatalytic reduction and detection of methylglyoxal.

  13. Electrochemical Oxidation of l-selenomethionine and Se-methylseleno-l-cysteine at a Thiol-Compound-Modified Gold Electrode: Its Application in a Flow-Through Voltammetric Sensor.

    PubMed

    Wang, Lai-Hao; Zhang, Yu-Han

    2017-02-16

    A flow-electrolytic cell that consists of a bare gold wire or of different thiol-compound-modified gold electrodes (such as 2,4-thiazolidinedione, 2-mercapto-5-thiazoline, 2-mercaptothiazoline, l-cysteine, thioglycolic acid) was designed to be used in a voltammetric detector to identify l-selenomethionine and Se-methylseleno-l-cysteine using high-performance liquid chromatography. Both l-selenomethionine and Se-methylseleno-l-cysteine are more efficiently electrochemically oxidized on a thiol/gold than on a bare gold electrode. For the DC mode, and for measurements with suitable experimental parameters, a linear concentration from 10 to 1600 ng·mL(-1) was found. The limits of quantification for l-selenomethionine and Se-methylseleno-l-cysteine were below 10 ng·mL(-1). The method can be applied to the quantitative determination of l-selenomethionine and Se-methylseleno-l-cysteine in commercial selenium-containing supplement products. Findings using high-performance liquid chromatography with a flow-through voltammetric detector and ultraviolet detector are comparable.

  14. Electrochemical Oxidation of l-selenomethionine and Se-methylseleno-l-cysteine at a Thiol-Compound-Modified Gold Electrode: Its Application in a Flow-Through Voltammetric Sensor

    PubMed Central

    Wang, Lai-Hao; Zhang, Yu-Han

    2017-01-01

    A flow-electrolytic cell that consists of a bare gold wire or of different thiol-compound-modified gold electrodes (such as 2,4-thiazolidinedione, 2-mercapto-5-thiazoline, 2-mercaptothiazoline, l-cysteine, thioglycolic acid) was designed to be used in a voltammetric detector to identify l-selenomethionine and Se-methylseleno-l-cysteine using high-performance liquid chromatography. Both l-selenomethionine and Se-methylseleno-l-cysteine are more efficiently electrochemically oxidized on a thiol/gold than on a bare gold electrode. For the DC mode, and for measurements with suitable experimental parameters, a linear concentration from 10 to 1600 ng·mL−1 was found. The limits of quantification for l-selenomethionine and Se-methylseleno-l-cysteine were below 10 ng·mL−1. The method can be applied to the quantitative determination of l-selenomethionine and Se-methylseleno-l-cysteine in commercial selenium-containing supplement products. Findings using high-performance liquid chromatography with a flow-through voltammetric detector and ultraviolet detector are comparable. PMID:28212326

  15. Direct quantification of microRNA at low picomolar level in sera of glioma patients using a competitive hybridization followed by amplified voltammetric detection.

    PubMed

    Wang, Jianxiu; Yi, Xinyao; Tang, Hailin; Han, Hongxing; Wu, Minghua; Zhou, Feimeng

    2012-08-07

    MicroRNAs (miRNAs), acting as oncogenes or tumor suppressors in humans, play a key role in regulating gene expression and are believed to be important for developing novel therapeutic treatments and clinical prognoses. Due to their short lengths (17-25 nucleotides) and extremely low concentrations (typically < picomolar) in biological samples, quantification of miRNAs has been challenging to conventional biochemical methods, such as Northern blotting, microarray, and quantitative polymerase chain reaction (qPCR). In this work, a biotinylated miRNA (biotin-miRNA) whose sequence is the same as that of a miRNA target is introduced into samples of interest and allowed to compete with the miRNA target for the oligonucleotide (ODN) probe preimmobilized onto an electrode. Voltammetric quantification of the miRNA target was accomplished after complexation of the biotin-miRNA with ferrocene (Fc)-capped gold nanoparticle/streptavidin conjugates. The Fc oxidation current was found to be inversely proportional to the concentration of target miRNA between 10 fM and 2.0 pM. The method is highly reproducible (relative standard deviation (RSD) < 5%), regenerable (at least 8 regeneration/assay cycles without discernible signal decrease), and selective (with sequence specificity down to a single nucleotide mismatch). The low detection levels (10 fM or 0.1 attomoles of miRNA in a 10 μL solution) allow the direct quantification of miRNA-182, a marker correlated to the progression of glioma in patients, to be performed in serum samples without sample pretreatment and RNA extraction and enrichment. The concentration of miRNA-182 in glioma patients was found to be 3.1 times as high as that in healthy persons, a conclusion in excellent agreement with a separate qPCR measurement of the expression level. The obviations of the requirement of an internal reference in qPCR, simplicity, and cost-effectiveness are other additional advantages of this method for detection of nucleic acids in

  16. Homogeneous solvation controlled photoreduction of cobalt(III) complexes in aqueous 2-methyl-2-propanol solutions. Linear solvation energy relationship and cyclic voltammetric analyses

    NASA Astrophysics Data System (ADS)

    Anbalagan, K.; Lydia, I. Sharmila

    2008-03-01

    The effect of solvent participation on the ligand-to-metal charge transfer (LMCT, L → Co III) reduction of the of Co III(en) 2Br(RC 6H 4NH 2) 2+ where R = m-OCH 3, p-F, H, m-CH 3, p-CH 3,p-OC 2H 5 and p-OCH 3 were examined in aqueous 2-methyl-2-propanol (Bu tOH) solutions. The change in the reduction behavior of Co III centre was also examined through cyclic voltammetric studies. The observed reduction in quantum yield due to LMCT excitation can mainly be accounted using linear solvation energy relationship (LSER) comprising model correlation equations. These consist of empirical parameters such as Grunwald-Winstein's solvent ionizing power, Y, Dimroth-Richardt's solvent micro-polarity parameter, ETN, Gutmann's donor number, DN N, along with Kamlet-Taft's solvatochromic parameters (hydrogen bond acceptor acidity/basicity α/ β and solvent dipolarity/polarizability, π*). The origin of solvent effect is found to be due to microscopic interaction between the solvent donor and the nitrogen-bound hydrogen of the ligand. Cyclic voltammograms show an irreversible reduction of Co III in DMF using Glassy Carbon Electrode, GCE, the redox peaks for the aniline complexes appear at -0.20 and 0.525 V. Irradiation of the complexes with UV light ( λ = 254 nm) in binary mixtures produce Co IIaq and the concentration of this species are highly dependent on xalc ( xalc = mole fraction of alcohol). The observed quantum yield (log ΦCo(II)) is found to be linearly related to mole fraction of organic co-solvent added in the mixture, therefore, log ΦCo(II) = 26.41 × 10 -2 when x2 = 0.0094 and 43.75 × 10 -2 when x2 = 0.076 for a typical complex Co III(en) 2Br( p-OCH 3C 6H 4NH 2) 2+ in aqueous 2-methyl-2-propanol at 300 K. Cyclic voltammetry and LSER analyses illustrate the variation of reduction property of Co(III) by the aryl ligand and homogeneous solvation of the excited state of the complex Co III(en) 2Br(RC 6H 4NH 2) 2+ in H 2O/Bu tOH mixtures.

  17. Square-wave anodic stripping voltammetric determination of thallium(I) at a Nafion/mercury film modified electrode.

    PubMed

    Lu, T H; Yang, H Y; Sun, I W

    1999-06-01

    A Nafion/mercury film electrode (NMFE) was used for the determination of trace thallium(I) in aqueous solutions. Thallium(I) was preconcentrated onto the NMFE from the sample solution containing 0.01 M ethylenediaminetetraacetate (EDTA), and determined by square-wave anodic stripping voltammetry (SWASV). Various factors influencing the determination of thallium(I) were thoroughly investigated. This modified electrode exhibits good resistance to interferences from surface-active compounds. The presence of EDTA effectively eliminated the interferences from metal ions, such as lead(II) and cadmium(II), which are generally considered as the major interferents in the determination of thallium at a mercury electrode. With 2-min preconcentration, linear calibration graphs were obtained over the range 0.05-100 ppb of thallium(I). An even lower detection limit, 0.01 ppb, were achieved with 5-min accumulation. The electrode is easy to prepare and can be readily renewed after each stripping experiment. Applicability of this procedure to various water samples is illustrated.

  18. A novel voltammetric sensor based on carbon nanotubes and nanoparticles of antimony tin oxide for the determination of ractopamine.

    PubMed

    Baytak, Aysegul Kutluay; Teker, Tugce; Duzmen, Sehriban; Aslanoglu, Mehmet

    2016-02-01

    An electrochemical sensor was prepared by the modification of a glassy carbon electrode (GCE) with carbon nanotubes (CNTs) and nanoparticles of antimony tin oxide (ATO). The surface layer was characterized by scanning electronmicroscopy (SEM), energy dispersive X-ray diffraction method (EDX) and ATR FT-IR spectroscopy. The proposed electrode was assessed in respect to the electro-oxidation of ractopamine. Compared with a bare GCE and a GCE electrode modified with CNTs, the ATONPs/CNTs/GCE exhibited a great catalytic activity towards the oxidation of ractopamine with a well-defined anodic peak at 600 mV. The current response was linear with the concentration of ractopamine over the range from 10 to 240 nM with a detection limit of 3.3 nM. The proposed electrode enabled the selective determination of ractopamine in the presence of high concentrations of ascorbic acid (AA), dopamine (DA) and uric acid (UA). The proposed electrode was successfully applied for the determination of ractopamine in feed and urine samples. The sensitive and selective determination of ractopamine makes the developed method of great interest for monitoring its therapeutic use and doping control purposes.

  19. A sensitive voltammetric detection of pramipexole based on 1,1,3,3-tetramethyldisilazanecarbon nanotube modified electrode.

    PubMed

    Amirighadi, Saeede; Raoof, Jahan Bakhsh; Chekin, Fereshteh; Ojani, Reza

    2017-06-01

    A simple low-cost method is proposed to fabricate a functionalized multi-wall carbon nanotube (MWCNT) with 1,1,3,3-tetramethyldisilazane (TMDS) molecule. The techniques of scanning electron microscope (SEM) with electron diffraction and energy dispersive X-ray (EDAX) analysis were applied to characterize the functionalized TMDS-MWCNT. The results showed that a MWCNT with high functionalization of TMDS can be obtained using this simple method. A new nanostructure sensor was constructed based on a glassy carbon electrode modified with TMDS-MWCNT (TMDS-MWCNT/GCE). It was found that the TMDS-MWCNT/GCE exhibits good catalytic activity toward oxidation of pramipexole (PPX) drug, leading to a concentration range of 0.8 to 600μM with a detection limit of 0.2μM at 3σ using the differential pulse voltammetry technique, a sensitivity of 0.084μAμM(-1), and a correlation coefficient of 0.991. Furthermore, the TMDS-MWCNT/GCE was used for PPX detection in tablets and human blood serum samples. The method showed no interference from tablet excipients; hence, it can be useful and fit for the quantification of PPX in bulk and tablet dosage forms. The proposed method was validated successfully as applied to the quantification of the drug in tablet dosage forms. The accuracy of detection results using the proposed method was evaluated as excellent comparing with those obtained by the reference method. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Voltammetric analysis apparatus and method

    DOEpatents

    Almon, A.C.

    1993-06-08

    An apparatus and method is described for electrochemical analysis of elements in solution. An auxiliary electrode, a reference electrode, and five working electrodes are positioned in a container containing a sample solution. The working electrodes are spaced apart evenly from each other and the auxiliary electrode to minimize any inter-electrode interference that may occur during analysis. An electric potential is applied between the auxiliary electrode and each of the working electrodes. Simultaneous measurements taken of the current flow through each of the working electrodes for each given potential in a potential range are used for identifying chemical elements present in the sample solution and their respective concentrations. Multiple working electrodes enable a more positive identification to be made by providing unique data characteristic of chemical elements present in the sample solution.