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Sample records for afm cyclic voltammetry

  1. Cyclic Voltammetry.

    ERIC Educational Resources Information Center

    Evans, Dennis H.; And Others

    1983-01-01

    Cyclic voltammetry is a simple experiment that has become popular in chemical research because it can provide useful information about redox reactions in a form which is easily obtained and interpreted. Discusses principles of the method and illustrates its use in the study of four electrode reactions. (Author/JN)

  2. Affordable Cyclic Voltammetry

    ERIC Educational Resources Information Center

    Stewart, Greg; Kuntzleman, Thomas S.; Amend, John R.; Collins, Michael J.

    2009-01-01

    Cyclic voltammetry is an important component of the undergraduate chemical curriculum. Unfortunately, undergraduate students rarely have the opportunity to conduct experiments in cyclic voltammetry owing to the high cost of potentiostats, which are required to control these experiments. By using MicroLab data acquisition interfaces in conjunction…

  3. Cyclic Voltammetry Experiment.

    ERIC Educational Resources Information Center

    Van Benschoten, James J.; And Others

    1983-01-01

    Describes a three-part experiment designed to introduce cyclic voltammetry to graduate/undergraduate students. Part 1 demonstrates formal reduction potential, redox electron transfer, diffusion coefficient, and electrochemical reversibility. Part 2 investigates electrochemical behavior of acetaminophen. Part 3 examines such experimental variables…

  4. A Cyclic Voltammetry Experiment for the Instrumental Analysis Laboratory.

    ERIC Educational Resources Information Center

    Baldwin, Richard P.; And Others

    1984-01-01

    Background information and procedures are provided for experiments that illustrate the nature of cyclic voltammetry and its application in the characterization of organic electrode processes. The experiments also demonstrate the concepts of electrochemical reversibility and diffusion-controlled mass transfer. (JN)

  5. Gas microsensors using cyclic voltammetry with a cermet electrochemical cell.

    SciTech Connect

    Shoemaker, E. L.; Vogt, M. C.; Dudek, F. J.; Turner, T.; Energy Systems

    1997-07-15

    The sensing characteristics of a cermet electrochemical cell, expressed as NiO|Pt|solid electrolyte|Pt were investigated by applying cyclic voltammetry to the Pt electrodes and measuring changes in ionic current through the solid electrolyte. Features of the current-voltage response (voltammograms) appear to depend uniquely on the type of gas exposed to the cell surface and the solid electrolyte material used. The novel sensors can selectively detect O{sub 2}, CO{sub 2}, and a variety of hydrocarbons. Performance characteristics such as selectivity, sensitivity, speed of response, and temperature dependence were also reported.

  6. Study of quinones reactions with wine nucleophiles by cyclic voltammetry.

    PubMed

    Oliveira, Carla M; Barros, António S; Ferreira, António C S; Silva, Artur M S

    2016-11-15

    Quinones are electrophilic species which can react with various nucleophiles, like wine antioxidants, such as sulfur dioxide or ascorbic acid, thiols, amino acids, and numerous polyphenols. These reactions are very important in wine aging because they mediate oxygen reactions during both production and bottle aging phases. In this work, the major challenge was to determine the interaction between ortho-quinones and wine nucleophiles (amino acids, thiols, and the antioxidants SO2 and ascorbic acid), by cyclic voltammetry. Wine-model solutions with gallic acid, caffeic acid, or (+)-catechin and nucleophilic compounds were used. To understand the effect of nucleophilic addition in wine, a white wine with the same added nucleophiles was also analysed. Cyclic voltammograms were taken with glassy carbon electrode or screen-printed carbon electrodes, respectively, for wine-model and white wines solutions, in the absence and in the presence of nucleophiles. A nucleophilic order profile related to the cathodic current intensity decrease was observed. PMID:27283600

  7. Cyclic voltammetry of aquocobalamin on clay-modified electrodes

    SciTech Connect

    Borek, V.; Morra, M.J.

    1998-07-15

    Halogenated synthetic compounds are widespread contaminants of the environment. Although corrinoids reductively dehalogenate synthetic contaminants in solution, the redox behavior of sorbed tetrapyrroles has received limited attention. Colloidal clay suspensions were prepared as Ca{sup 2+} forms of hectorite (SHCa-1), montmorillonite (SWy-1, Syn-1, and SAz-1), and vermiculite (VTx-1) and spin coated on platinum electrodes. Cyclic voltammetry was performed with the clay-modified electrodes immersed in buffered solutions containing 1.0 mM aquocobalamin. Aquocobalamin in the presence of vermiculite-coated electrodes displayed the same cathodic and anodic peak potentials as unmodified electrodes immersed in aquocobalamin solutions. All other clay-modified electrodes shifted cathodic peaks to more negative values, while anodic peak shifts varied with the clay. Hectorite caused the largest shift in formal redox potential as compared to aquocobalamin in solution. The redox behavior of aquocobalamin as modified by sorption to clay minerals potentially affects dehalogenation rates of synthetic organic compounds in the environment. Clays lowering the formal redox potential of the tetrapyrrole create a potentially more efficient catalyst for pollutant degradation. However, thermodynamic data as obtained using cyclic voltammetry cannot be used to make definitive predictions about the kinetics of contaminant dehalogenation. Reductive dehalogenation will be a function of altered electrochemical properties of the tetrapyrrole as well as rates of contaminant diffusion to the site of tetrapyrrole sorption.

  8. Nanoalloy electrocatalysis: Simulating cyclic voltammetry from configurational thermodynamics with adsorbates

    SciTech Connect

    Wang, Lin -Lin; Tan, Teck L.; Johnson, Duane D.

    2015-02-27

    We simulate the adsorption isotherms for alloyed nanoparticles (nanoalloys) with adsorbates to determine cyclic voltammetry (CV) during electrocatalysis. The effect of alloying on nanoparticle adsorption isotherms is provided by a hybrid-ensemble Monte Carlo simulation that uses the cluster expansion method extended to non-exchangeable coupled lattices for nanoalloys with adsorbates. Exemplified here for the hydrogen evolution reaction, a 2-dimensional CV is mapped for Pd–Pt nanoalloys as a function of both electrochemical potential and the global Pt composition, and shows a highly non-linear alloying effect on CV. Detailed features in CV arise from the interplay among the H-adsorption in multiple sites that is closely correlated with alloy configurations, which are in turn affected by the H-coverage. The origins of specific features in CV curves are assigned. As a result, the method provides a more complete means to design nanoalloys for electrocatalysis.

  9. Nanoalloy electrocatalysis: Simulating cyclic voltammetry from configurational thermodynamics with adsorbates

    DOE PAGESBeta

    Wang, Lin -Lin; Tan, Teck L.; Johnson, Duane D.

    2015-02-27

    We simulate the adsorption isotherms for alloyed nanoparticles (nanoalloys) with adsorbates to determine cyclic voltammetry (CV) during electrocatalysis. The effect of alloying on nanoparticle adsorption isotherms is provided by a hybrid-ensemble Monte Carlo simulation that uses the cluster expansion method extended to non-exchangeable coupled lattices for nanoalloys with adsorbates. Exemplified here for the hydrogen evolution reaction, a 2-dimensional CV is mapped for Pd–Pt nanoalloys as a function of both electrochemical potential and the global Pt composition, and shows a highly non-linear alloying effect on CV. Detailed features in CV arise from the interplay among the H-adsorption in multiple sites thatmore » is closely correlated with alloy configurations, which are in turn affected by the H-coverage. The origins of specific features in CV curves are assigned. As a result, the method provides a more complete means to design nanoalloys for electrocatalysis.« less

  10. Cyclic voltammetry of apple fruits: Memristors in vivo.

    PubMed

    Volkov, Alexander G; Nyasani, Eunice K; Tuckett, Clayton; Blockmon, Avery L; Reedus, Jada; Volkova, Maya I

    2016-12-01

    A memristor is a resistor with memory that exhibits a pinched hysteretic relationship in cyclic voltammetry. Recently, we have found memristors in the electrical circuitry of plants and seeds. There are no publications in literature about the possible existence of memristors and electrical differentiators in fruits. Here we found that the electrostimulation of Golden Delicious or Arkansas Black apple fruits by bipolar periodic waves induces hysteresis loops with pinched points in cyclic voltammograms at low frequencies between 0.1MHz and 1MHz. At high frequencies of 1kHz, the pinched hysteresis loop transforms to a non-pinched hysteresis loop instead of a single line I=V/R for ideal memristors because the amplitude of electrical current depends on capacitance of a fruit's tissue and electrodes, frequency and direction of scanning. Electrostimulation of electrical circuits in apple fruits by periodic voltage waves also induces electrotonic potential propagation due to cell-to-cell electrical coupling with electrical differentiators. A differentiator is an electrical circuit in which the output of the circuit is approximately directly proportional to the rate of change of the input. The information gained from electrostimulation can be used to elucidate and to observe electrochemical and electrophysiological properties of electrical circuits in fruits. PMID:27398978

  11. Fast Selective Detection of Pyocyanin Using Cyclic Voltammetry

    PubMed Central

    Alatraktchi, Fatima AlZahra’a; Breum Andersen, Sandra; Krogh Johansen, Helle; Molin, Søren; Svendsen, Winnie E.

    2016-01-01

    Pyocyanin is a virulence factor uniquely produced by the pathogen Pseudomonas aeruginosa. The fast and selective detection of pyocyanin in clinical samples can reveal important information about the presence of this microorganism in patients. Electrochemical sensing of the redox-active pyocyanin is a route to directly quantify pyocyanin in real time and in situ in hospitals and clinics. The selective quantification of pyocyanin is, however, limited by other redox-active compounds existing in human fluids and by other metabolites produced by pathogenic bacteria. Here we present a direct selective method to detect pyocyanin in a complex electroactive environment using commercially available electrodes. It is shown that cyclic voltammetry measurements between −1.0 V to 1.0 V reveal a potential detection window of pyocyanin of 0.58–0.82 V that is unaffected by other redox-active interferents. The linear quantification of pyocyanin has an R2 value of 0.991 across the clinically relevant concentration range of 2–100 µM. The proposed method was tested on human saliva showing a standard deviation of 2.5% ± 1% (n = 5) from the known added pyocyanin concentration to the samples. This inexpensive procedure is suggested for clinical use in monitoring the presence and state of P. aeruginosa infection in patients. PMID:27007376

  12. Fully printed flexible and disposable wireless cyclic voltammetry tag

    NASA Astrophysics Data System (ADS)

    Jung, Younsu; Park, Hyejin; Park, Jin-Ah; Noh, Jinsoo; Choi, Yunchang; Jung, Minhoon; Jung, Kyunghwan; Pyo, Myungho; Chen, Kevin; Javey, Ali; Cho, Gyoujin

    2015-01-01

    A disposable cyclic voltammetry (CV) tag is printed on a plastic film by integrating wireless power transmitter, polarized triangle wave generator, electrochemical cell and signage through a scalable gravure printing method. By proximity of 13.56 MHz RF reader, the printed CV tag generates 320 mHz of triangular sweep wave from +500 mV to -500 mV which enable to scan a printed electrochemical cell in the CV tag. By simply dropping any specimen solution on the electrochemical cell in the CV tag, the presence of solutes in the solution can be detected and shown on the signage of the CV tag in five sec. 10 mM of N,N,N',N'-tetramethyl-p-phenylenediamine (TMPD) was used as a standard solute to prove the working concept of fully printed disposable wireless CV tag. Within five seconds, we can wirelessly diagnose the presence of TMPD in the solution using the CV tag in the proximity of the 13.56 MHz RF reader. This fully printed and wirelessly operated flexible CV tag is the first of its kind and marks the path for the utilization of inexpensive and disposable wireless electrochemical sensor systems for initial diagnose hazardous chemicals and biological molecules to improve public hygiene and health.

  13. Fully printed flexible and disposable wireless cyclic voltammetry tag

    PubMed Central

    Jung, Younsu; Park, Hyejin; Park, Jin-Ah; Noh, Jinsoo; Choi, Yunchang; Jung, Minhoon; Jung, Kyunghwan; Pyo, Myungho; Chen, Kevin; Javey, Ali; Cho, Gyoujin

    2015-01-01

    A disposable cyclic voltammetry (CV) tag is printed on a plastic film by integrating wireless power transmitter, polarized triangle wave generator, electrochemical cell and signage through a scalable gravure printing method. By proximity of 13.56 MHz RF reader, the printed CV tag generates 320 mHz of triangular sweep wave from +500 mV to −500 mV which enable to scan a printed electrochemical cell in the CV tag. By simply dropping any specimen solution on the electrochemical cell in the CV tag, the presence of solutes in the solution can be detected and shown on the signage of the CV tag in five sec. 10 mM of N,N,N′,N′-tetramethyl-p-phenylenediamine (TMPD) was used as a standard solute to prove the working concept of fully printed disposable wireless CV tag. Within five seconds, we can wirelessly diagnose the presence of TMPD in the solution using the CV tag in the proximity of the 13.56 MHz RF reader. This fully printed and wirelessly operated flexible CV tag is the first of its kind and marks the path for the utilization of inexpensive and disposable wireless electrochemical sensor systems for initial diagnose hazardous chemicals and biological molecules to improve public hygiene and health. PMID:25630250

  14. Cyclic voltammetry and RBS study of paint components

    NASA Astrophysics Data System (ADS)

    Bowman, Lynn; Spencer, Dirk; Muntele, Claudiu; Muntele, Iulia; Ila, D.

    2007-08-01

    Heavy metals and metalloid ions are found in environmental matrices. The most toxic are lead, cadmium and mercury. These three heavy metals have no biological function and are toxic at all concentrations. Lead is one of the most insidious heavy metals and is introduced into the environment by many different means. It persists in both urban and rural settings, being found in paint chips, pottery, crystal and pharmaceutical and nutritional products. The analysis of heavy elements such as lead in soil is of particular importance [W.T. Sturges, R.M. Harrison, Sci. Total Environ. 44 (3) (1985) 225; M.L. Lepow, L. Bruckman, M. Gillette, S. Markowitz, R. Robino, J. Kapish, Environ. Res. 10 (3) (1975) 415; A.E. Daniels, J.R. Kominsky, P.J. Clark, J. Hazard. Mater. B 87 (2001) 117; G. Hutter, D. Moshman, J. Hazard. Mater. 40 (1995) 1]. In preparing the methods for lead detection in paint, we have used Rutherford backscattering spectrometry (RBS) in order to study the type and amount of heavy metal content in paint samples collected at various sites in the historic campus at A&M University (AAMU). We will show the results of our study with emphasis on comparison of what we learned about presence of lead in paints using our ion beam methods compared with the analysis of lead in paints using cyclic voltammetry.

  15. Development and Use of a Cyclic Voltammetry Simulator to Introduce Undergraduate Students to Electrochemical Simulations

    ERIC Educational Resources Information Center

    Brown, Jay H.

    2015-01-01

    Cyclic voltammetry (CV) is a popular technique for the study of electrochemical mechanisms because the method can provide useful information on the redox couple. The technique involves the application of a potential ramp on an unstirred solution while the current is monitored, and then the ramp is reversed for a return sweep. CV is sometimes…

  16. CYCLIC VOLTAMMETRY OF ORGANIC AND INORGANIC N-CHLORAMINES IN AQUEOUS SOLUTION

    EPA Science Inventory

    Aqueous solutions or organic and inorganic N-chloramines as well as hypochlorite were examined by cyclic voltammetry at DH 8 and in strong acid (pH<2) with platinum and glassy carbon electrodes. The inorganic N-chloramines were characterized in 1 M HC104. NHC12 is reduced at abou...

  17. Cyclic Voltammetry Simulations with DigiSim Software: An Upper-Level Undergraduate Experiment

    ERIC Educational Resources Information Center

    Messersmith, Stephania J.

    2014-01-01

    An upper-division undergraduate chemistry experiment is described which utilizes DigiSim software to simulate cyclic voltammetry (CV). Four mechanisms were studied: a reversible electron transfer with no subsequent or proceeding chemical reactions, a reversible electron transfer followed by a reversible chemical reaction, a reversible chemical…

  18. Hairy carbon electrodes studied by cyclic voltammetry and battery discharge testing

    NASA Technical Reports Server (NTRS)

    Chung, Deborah D. L.; Shui, Xiaoping; Frysz, Christine A.

    1993-01-01

    Hairy carbon is a new material developed by growing submicron carbon filaments on conventional carbon substrates. Typical substrate materials include carbon black, graphite powder, carbon fibers, and glassy carbon. A catalyst is used to initiate hair growth with carbonaceous gases serving as the carbon source. To study the electrochemical behavior of hairy carbons, cyclic voltammetry (CV) and discharge testing were conducted. In both cases, hairy carbon results surpassed those of the substrate material alone.

  19. Assessing principal component regression prediction of neurochemicals detected with fast-scan cyclic voltammetry.

    PubMed

    Keithley, Richard B; Wightman, R Mark

    2011-06-01

    Principal component regression is a multivariate data analysis approach routinely used to predict neurochemical concentrations from in vivo fast-scan cyclic voltammetry measurements. This mathematical procedure can rapidly be employed with present day computer programming languages. Here, we evaluate several methods that can be used to evaluate and improve multivariate concentration determination. The cyclic voltammetric representation of the calculated regression vector is shown to be a valuable tool in determining whether the calculated multivariate model is chemically appropriate. The use of Cook's distance successfully identified outliers contained within in vivo fast-scan cyclic voltammetry training sets. This work also presents the first direct interpretation of a residual color plot and demonstrated the effect of peak shifts on predicted dopamine concentrations. Finally, separate analyses of smaller increments of a single continuous measurement could not be concatenated without substantial error in the predicted neurochemical concentrations due to electrode drift. Taken together, these tools allow for the construction of more robust multivariate calibration models and provide the first approach to assess the predictive ability of a procedure that is inherently impossible to validate because of the lack of in vivo standards. PMID:21966586

  20. Oxidation management of white wines using cyclic voltammetry and multivariate process monitoring.

    PubMed

    Martins, Rui C; Oliveira, Raquel; Bento, Fatima; Geraldo, Dulce; Lopes, Vitor V; Guedes de Pinho, Paula; Oliveira, Carla M; Silva Ferreira, Antonio C

    2008-12-24

    The development of a fingerprinting strategy capable to evaluate the "oxidation status" of white wines based on cyclic voltammetry is proposed here. It is known that the levels of specific antioxidants and redox mechanisms may be evaluated by cyclic voltammetry. This electrochemical technique was applied on two sets of samples. One group was composed of normal aged white wines and a second group obtained from a white wine forced aging protocol with different oxygen, SO(2), pH, and temperature regimens. A study of antioxidant additions, namely ascorbic acid, was also made in order to establish a statistical link between voltammogram fingerprints and chemical antioxidant substances. It was observed that the oxidation curve presented typical features, which enables sample discrimination according to age, oxygen consumption, and antioxidant additions. In fact, it was possible to place the results into four significant orthogonal directions, compressing 99.8% of nonrandom features. Attempts were made to make voltammogram fingerprinting a tool for monitoring oxidation management. For this purpose, a supervised multivariate control chart was developed using a control sample as reference. When white wines are plotted onto the chart, it is possible to monitor the oxidation status and to diagnose the effects of oxygen regimes and antioxidant activity. Finally, quantification of substances implicated in the oxidation process as reagents (antioxidants) and products (off-flavors) was tried using a supervised algorithmic the partial least square regression analysis. Good correlations (r > 0.93) were observed for ascorbic acid, Folin-Ciocalteu index, total SO(2), methional, and phenylacetaldehyde. These results show that cyclic voltammetry fingerprinting can be used to monitor and diagnose the effects of wine oxidation. PMID:19053361

  1. Sampling phasic dopamine signaling with fast-scan cyclic voltammetry in awake behaving rats

    PubMed Central

    Fortin, SM; Cone, JJ; Ng-Evans, S; McCutcheon, JE; Roitman, MF

    2015-01-01

    Fast-scan cyclic voltammetry (FSCV) is an electrochemical technique which permits the in vivo measurement of extracellular fluctuations in multiple chemical species. The technique is frequently utilized to sample sub-second (phasic) concentration changes of the neurotransmitter dopamine in awake and behaving rats. Phasic dopamine signaling is implicated in reinforcement, goal-directed behavior, and locomotion and FSCV has been used to investigate how rapid changes in striatal dopamine concentration contribute to these and other behaviors. This unit describes the instrumentation and construction, implantation, and use of necessary components required to sample and analyze dopamine concentration changes in awake rats with FSCV. PMID:25559005

  2. A one-dimensional stochastic approach to the study of cyclic voltammetry with adsorption effects

    NASA Astrophysics Data System (ADS)

    Samin, Adib J.

    2016-05-01

    In this study, a one-dimensional stochastic model based on the random walk approach is used to simulate cyclic voltammetry. The model takes into account mass transport, kinetics of the redox reactions, adsorption effects and changes in the morphology of the electrode. The model is shown to display the expected behavior. Furthermore, the model shows consistent qualitative agreement with a finite difference solution. This approach allows for an understanding of phenomena on a microscopic level and may be useful for analyzing qualitative features observed in experimentally recorded signals.

  3. Microfluidic platform for neurotransmitter sensing based on cyclic voltammetry and dielectrophoresis for in vitro experiments.

    PubMed

    Mathault, Jessy; Zamprogno, Pauline; Greener, Jesse; Miled, Amine

    2015-08-01

    This paper presents a new microfluidic platform that can simultaneously measure and locally modulate neurotransmitter concentration in a neuron network. This work focuses on the development of a first prototype including a potentiostat and electrode functionalization to detect several neurotransmitter's simultaneously. We tested dopamine as proof of concept to validate functionality. The system is based on 320 bidirectional electrode array for dielectrophoretic manipulation and cyclic voltammetry. Each electrode is connected to a mechanical multiplexer in order to reduce noise interference and fully isolate the electrode. The multiplexing rate is 476 kHz and each electrode can drive a signal with an amplitude of 60 V pp for dielectrophoretic manipulation. PMID:26736720

  4. Dynamic Charge Storage in Ionic Liquids-Filled Nanopores: Insight from a Computational Cyclic Voltammetry Study.

    PubMed

    He, Yadong; Huang, Jingsong; Sumpter, Bobby G; Kornyshev, Alexei A; Qiao, Rui

    2015-01-01

    Understanding the dynamic charge storage in nanoporous electrodes with room-temperature ionic liquid electrolytes is essential for optimizing them to achieve supercapacitors with high energy and power densities. Herein, we report coarse-grained molecular dynamics simulations of the cyclic voltammetry of supercapacitors featuring subnanometer pores and model ionic liquids. We show that the cyclic charging and discharging of nanopores are governed by the interplay between the external field-driven ion transport and the sloshing dynamics of ions inside of the pore. The ion occupancy along the pore length depends strongly on the scan rate and varies cyclically during charging/discharging. Unlike that at equilibrium conditions or low scan rates, charge storage at high scan rates is dominated by counterions while the contribution by co-ions is marginal or negative. These observations help explain the perm-selective charge storage observed experimentally. We clarify the mechanisms underlying these dynamic phenomena and quantify their effects on the efficiency of the dynamic charge storage in nanopores. PMID:26263086

  5. Detection of Hypochlorous Acid Using Reduction Wave During Anodic Cyclic Voltammetry

    NASA Astrophysics Data System (ADS)

    Kodera, Fumihiro; Umeda, Minoru; Yamada, Akifumi

    2005-05-01

    A novel analysis method for detecting low free-chlorine concentrations using a reduction wave based on anodic cyclic voltammetry has been developed. The reduction wave has been observed at approximately 600 mV vs Ag/AgCl, which is dependent on the free-chlorine concentration and switching potential. The wave peak showed a maximum value for the switching potential at approximately 1350 mV vs Ag/AgCl, and a good linear relationship between the peak current and the concentrations in the range of 0.2-6.0 mg dm-3. The relative standard deviation (RSD) at each concentration was less than 2%. This method seems to be useful for the analysis of low free-chlorine concentrations.

  6. Application of N- and B-doped CVD diamond layers for cyclic voltammetry measurements

    NASA Astrophysics Data System (ADS)

    Torz-Piotrowska, R.; Wrzyszczyński, A.; Paprocki, K.; Staryga, E.

    2009-10-01

    Conductive polycrystalline diamond layers prepared by the CVD process have received attention from electrochemists owing to such superior electrochemical properties as the wide potential window, the very low background current, the stability of chemical and physical properties. In this paper, the cyclic voltammetry application using N- and B-doped diamond electrodes was studied. Diamond layers, doped with boron and nitrogen, were synthesized on a silicon substrate in a hot-filament CVD reactor. The obtained diamond layers were characterized using Raman spectroscopy and scanning electron microscopy (SEM). The electrochemical properties of diamond layers were measured in KCl and NaCl basic solutions to gain knowledge about their potential application as an electrode material. It was found that boron doped diamond electrodes showed potential windows up to about 7 V which were almost twice wider than those observed for conventional Pt electrodes.

  7. A Cyclic Voltammetry Experiment Illustrating Redox Potentials, Equilibrium Constants, and Substitution Reactions in Coordination Chemistry

    NASA Astrophysics Data System (ADS)

    Toma, Henrique E.; Araki, Koiti; Dovidauskas, Sergio

    2000-10-01

    We report a cyclic voltammetry experiment focusing on the [RuIII(EDTA)(H2O)]- complex and its equilibrium reaction with dimethyl sulfoxide (DMSO) in aqueous solution, yielding the [RuIII(EDTA)(kS-DMSO)]- complex. From the electrochemistry data, the formation constants for the [RuIII(EDTA)(kS-DMSO)]- and [RuII(EDTA)(kS-DMSO)]2- complexes were calculated as 2.0 mol-1 dm3 and 2.7 x 109 mol-1 dm3, respectively. The results illustrate the kinetic lability of the ruthenium(III)-EDTA complexes and the role of backbonding stabilization in ruthenium(II)-DMSO complexes. The experiment has been successfully performed in a Coordination Chemistry course, exploiting fundamental aspects of metal complexes and the applications of that important electrochemical technique.

  8. Cyclic voltammetry as a sensitive method for in situ probing of chemical transformations in quantum dots.

    PubMed

    Osipovich, Nikolai P; Poznyak, Sergei K; Lesnyak, Vladimir; Gaponik, Nikolai

    2016-04-21

    The application of electrochemical methods for the characterization of colloidal quantum dots (QDs) attracts considerable attention as these methods may allow for monitoring of some crucial parameters, such as energetic levels of conduction and valence bands as well as surface traps and ligands under real conditions of colloidal solution. In the present work we extend the applications of cyclic voltammetry (CV) to in situ monitoring of degradation processes of water-soluble CdTe QDs. This degradation occurs under lowering of pH to the values around 5, i.e. under conditions relevant to bioimaging applications of these QDs, and is accompanied by pronounced changes of their photoluminescence. Observed correlations between characteristic features of CV diagrams and the fluorescence spectra allowed us to propose mechanisms responsible for evolution of the photoluminescence properties as well as degradation pathway of CdTe QDs at low pH. PMID:27025663

  9. Chemical imaging with combined fast-scan cyclic voltammetry-scanning electrochemical microscopy.

    PubMed

    Schrock, Daniel S; Baur, John E

    2007-09-15

    Fast-scan cyclic voltammetry (FSCV) is applied to the tip of a scanning electrochemical microscope (SECM) for imaging the distribution of chemical species near a substrate. This approach was used to image the diffusion layer of both a large substrate electrode (3-mm-diameter glassy carbon) and a microelectrode substrate (10-microm-diameter Pt). Additionally, oxygen depletion near living cells was measured and correlated to respiratory activity. Finally, oxygen and hydrogen peroxide were simultaneously detected during the oxidative burst of a zymosan-stimulated macrophage cell. These results demonstrate the utility of FSCV-SECM for chemical imaging when conditions are chosen such that feedback interactions with the substrate are minimal. PMID:17705555

  10. Ascorbic Acid Determination in Commercial Fruit Juice Samples by Cyclic Voltammetry

    PubMed Central

    Pisoschi, Aurelia Magdalena; Danet, Andrei Florin; Kalinowski, Slawomir

    2008-01-01

    A method was developed for assessing ascorbic acid concentration in commercial fruit juice by cyclic voltammetry. The anodic oxidation peak for ascorbic acid occurs at about 490 mV on a Pt disc working electrode (versus SCE). The influence of the potential sweep speed on the peak height was studied. The obtained calibration graph shows a linear dependence between peak height and ascorbic acid concentration in the domain (0.1–10 mmol·L−1). The equation of the calibration graph was y = 6.391x + 0.1903 (where y represents the value of intensity measured for the anodic peak height, expressed as μA and x the analyte concentration, as mmol·L−1, r2 = 0.9995, r.s.d. = 1.14%, n = 10, Cascorbic acid = 2 mmol·L−1). The developed method was applied to ascorbic acid assessment in fruit juice. The ascorbic acid content determined ranged from 0.83 to 1.67 mmol·L−1 for orange juice, from 0.58 to 1.93 mmol·L−1 for lemon juice, and from 0.46 to 1.84 mmol·L−1 for grapefruit juice. Different ascorbic acid concentrations (from standard solutions) were added to the analysed samples, the degree of recovery being comprised between 94.35% and 104%. Ascorbic acid determination results obtained by cyclic voltammetry were compared with those obtained by the volumetric method with dichlorophenol indophenol. The results obtained by the two methods were in good agreement. PMID:19343183

  11. Electrode Calibration with a Microfluidic Flow Cell for Fast-scan Cyclic Voltammetry

    PubMed Central

    Sinkala, Elly; McCutcheon, James E.; Schuck, Matt; Schmidt, Eric; Roitman, Mitchell F.; Eddington, David T.

    2012-01-01

    Fast-scan cyclic voltammetry (FSCV) is a common analytical electrochemistry tool used to measure chemical species. It has recently been adapted for measurement of neurotransmitters such as dopamine in awake and behaving animals (in vivo). Electrode calibration is an essential step in FSCV to relate observed current to concentration of a chemical species. However, existing methods require multiple components, which reduce the ease of calibrations. To this end, a microfluidic flow cell (µFC) was developed as a simple device to switch between buffer and buffer with a known concentration of the analyte of interest – in this case dopamine - in a microfluidic Y-channel. The ability to quickly switch solutions yielded electrode calibrations with faster rise times and that were more stable at peak current values. The µFC reduced the number of external electrical components and produced linear calibrations over a range of concentrations. To demonstrate this, an electrode calibrated with the µFC was used in FSCV recordings from a rat during the delivery of food reward – a stimulus that reliably evokes a brief increase in current due to the oxidation of dopamine. Using the linear calibration, dopamine concentrations were determined from the current responses evoked during the behavioral task. The µFC is able to easily and quickly calibrate FSCV electrode responses to chemical species for both in vitro and in vivo experiments. PMID:22522908

  12. Simultaneous Measurement and Quantitation of 4-Hydroxyphenylacetic acid and Dopamine with Fast-Scan Cyclic Voltammetry

    PubMed Central

    Shin, Mimi; Kaplan, Sam V.; Raider, Kayla D.; Johnson, Michael A.

    2015-01-01

    Caged compounds have been used extensively to investigate neuronal function in a variety of preparations, including cell culture, ex vivo tissue samples, and in vivo. As a first step toward electrochemically measuring the extent of caged compound photoactivation while also measuring the release of the catecholamine neurotransmitter, dopamine, fast-scan cyclic voltammetry at carbon-fiber microelectrodes (FSCV) was used to electrochemically characterize 4-hydroxyphenylacetic acid (4HPAA) in the absence and presence of dopamine. 4HPAA is a by-product formed during the process of photoactivation of p-hydroxyphenylacyl-based caged compounds, such as p-hydroxyphenylglutamate (pHP-Glu). Our data suggest that the oxidation of 4HPAA occurs through the formation of a conjugated species. Moreover, we found that a triangular waveform of −0.4 V to +1.3 V to −0.4 V at 600 V/s, repeated every 100 ms, provided an oxidation current of 4HPAA that was enhanced with a limit of detection of 100 nM, while also allowing the detection and quantitation of dopamine within the same scan. Along with quantifying 4HPAA in biological preparations, the results from this work will allow the electrochemical measurement of photoactivation reactions that generate 4HPAA as a by-product as well as provide a framework for measuring the photorelease of electroactive by-products from caged compounds that incorporate other chromophores. PMID:25785694

  13. Evaluation of PEMFC System Contaminants on the Performance of Pt Catalyst via Cyclic Voltammetry: Preprint

    SciTech Connect

    Wang, H.; Macomber, C.; Dinh, H. N.

    2012-07-01

    Using electrochemical cyclic voltammetry as a quick ex-situ screening tool, the impact of the extracted solution and the individual leachable constituents from prospective BOP component materials on the performance and recoverability of the platinum catalyst were evaluated. Taking an extract from Zytel{trademark} HTN51G35HSLR (PPA) as an example, the major leachable organic components are caprolactam and 1,6 hexanediol. While these organic compounds by themselves do poison the Pt catalyst to some extent, such influence is mostly recoverable by means of potential holding and potential cycling. The extracted solution, however, shows a more drastic poisoning effect and it was not recoverable. Therefore the non-recoverable poisoning effect observed for the extracted solution is not from the two organic species studied. This demonstrates the complexity of such a contaminant study. Inorganic compounds that are known poisons like sulfur even in very low concentrations, may have a more dominant effect on the Pt catalyst and the recoverability.

  14. Failure of Standard Training Sets in the Analysis of Fast-Scan Cyclic Voltammetry Data.

    PubMed

    Johnson, Justin A; Rodeberg, Nathan T; Wightman, R Mark

    2016-03-16

    The use of principal component regression, a multivariate calibration method, in the analysis of in vivo fast-scan cyclic voltammetry data allows for separation of overlapping signal contributions, permitting evaluation of the temporal dynamics of multiple neurotransmitters simultaneously. To accomplish this, the technique relies on information about current-concentration relationships across the scan-potential window gained from analysis of training sets. The ability of the constructed models to resolve analytes depends critically on the quality of these data. Recently, the use of standard training sets obtained under conditions other than those of the experimental data collection (e.g., with different electrodes, animals, or equipment) has been reported. This study evaluates the analyte resolution capabilities of models constructed using this approach from both a theoretical and experimental viewpoint. A detailed discussion of the theory of principal component regression is provided to inform this discussion. The findings demonstrate that the use of standard training sets leads to misassignment of the current-concentration relationships across the scan-potential window. This directly results in poor analyte resolution and, consequently, inaccurate quantitation, which may lead to erroneous conclusions being drawn from experimental data. Thus, it is strongly advocated that training sets be obtained under the experimental conditions to allow for accurate data analysis. PMID:26758246

  15. Diamond microelectrodes and CMOS microelectronics for wireless transmission of fast-scan cyclic voltammetry.

    PubMed

    Roham, Masoud; Halpern, Jeffrey M; Martin, Heidi B; Chiel, Hillel J; Mohseni, Pedram

    2007-01-01

    This paper reports on technology development at the sensor and circuit levels for wireless transmission of fast-scan cyclic voltammetry (FSCV) in neurochemical detection. Heavily conductive, boron-doped diamond is selectively deposited onto the polished tip of a tungsten microelectrode to fabricate versatile, implantable, micro-needle microprobes capable of neurochemical sensing in the brain. In addition, an integrated circuit is fabricated in a 0.5-microm CMOS technology for processing and wireless transmission of the electrochemical signals corresponding to extracellular concentration changes of various neurotransmitters. The chip consists of a current-based, second-order, front-end SigmaDelta ADC and an on-chip, RF-FSK transmitter at the back-end. The ADC core and the transmitter consume 22microA and 400microA, respectively, from a 2.6-V power supply. Major electroactive neurotransmitters such as serotonin and dopamine in micromolar concentration have been wirelessly recorded at 433MHz using 300-V/s FSCV in flow injection analysis experiments. PMID:18003392

  16. Feedback Effects in Combined Fast-Scan Cyclic Voltammetry-Scanning Electrochemical Microscopy

    PubMed Central

    Schrock, Daniel S.; Wipf, David O.; Baur, John E.

    2008-01-01

    Fast-scan cyclic voltammetry at scan rates between 5 and 1000 Vs−1 was performed at the tip of a scanning electrochemical microscope immersed in a solution of redox mediator. The effect of conducting and insulating substrates on the voltammetric signal was investigated as a function of scan rate and tip-substrate distance. It was found that diffusional interactions between the tip and the substrate are greatest at lower scan rates and on the reverse sweep of the voltammogram. At the fastest scan rates used, the tip could be brought to with 1 μm of the substrate without appreciable perturbation of the voltammogram. By selecting scan rates and tip-substrate distances such that feedback effects were negligible, it was possible to image the diffusion layer of a 10 μm Pt substrate electrode. With the tip placed 1 μm above a biological cell, tip-substrate diffusional interactions were greatly diminished at a scan rate of 100 Vs−1, and absent at a scan rate of 1000 Vs−1. These results suggest conditions can be selected that allow chemical imaging of substrates without the feedback interactions typically encountered in scanning electrochemical microscopy. PMID:17550230

  17. Feedback effects in combined fast-scan cyclic voltammetry-scanning electrochemical microscopy.

    PubMed

    Schrock, Daniel S; Wipf, David O; Baur, John E

    2007-07-01

    Fast-scan cyclic voltammetry at scan rates between 5 and 1000 V s(-1) was performed at the tip of a scanning electrochemical microscope immersed in a solution of redox mediator. The effect of conducting and insulating substrates on the voltammetric signal was investigated as a function of scan rate and tip-substrate distance. It was found that diffusional interactions between the tip and the substrate are greatest at lower scan rates and on the reverse sweep of the voltammogram. At the fastest scan rates used, the tip could be brought to with 1 microm of the substrate without appreciable perturbation of the voltammogram. By selecting scan rates and tip-substrate distances such that feedback effects were negligible, it was possible to image the diffusion layer of a 10 microm Pt substrate electrode. With the tip placed 1 microm above a biological cell, tip-substrate diffusional interactions were greatly diminished at a scan rate of 100 V s(-1) and absent at a scan rate of 1000 V s(-1). These results suggest conditions can be selected that allow chemical imaging of substrates without the feedback interactions typically encountered in scanning electrochemical microscopy. PMID:17550230

  18. Fast-Scan Cyclic Voltammetry (FSCV) Detection of Endogenous Octopamine in Drosophila melanogaster Ventral Nerve Cord.

    PubMed

    Pyakurel, Poojan; Privman Champaloux, Eve; Venton, B Jill

    2016-08-17

    Octopamine is an endogenous biogenic amine neurotransmitter, neurohormone, and neuromodulator in invertebrates and has functional analogy with norepinephrine in vertebrates. Fast-scan cyclic voltammetry (FSCV) can detect rapid changes in neurotransmitters, but FSCV has not been optimized for octopamine detection in situ. The goal of this study was to characterize octopamine release in the ventral nerve cord of Drosophila larvae for the first time. A FSCV waveform was optimized so that the potential for octopamine oxidation would not be near the switching potential where interferences can occur. Endogenous octopamine release was stimulated by genetically inserting either the ATP sensitive channel, P2X2, or the red-light sensitive channelrhodopsin, CsChrimson, into cells expressing tyrosine decarboxylase (TDC), an octopamine synthesis enzyme. To ensure that release is due to octopamine and not the precursor tyramine, the octopamine synthesis inhibitor disulfiram was applied, and the signal decreased by 80%. Stimulated release was vesicular, and a 2 s continuous light stimulation of CsChrimson evoked 0.22 ± 0.03 μM of octopamine release in the larval ventral nerve cord. Repeated stimulations were stable with 2 or 5 min interstimulation times. With pulsed stimulations, the release was dependent on the frequency of applied light pulse. An octopamine transporter has not been identified, and blockers of the dopamine transporter and serotonin transporter had no significant effect on the clearance time of octopamine, suggesting that they do not take up octopamine. This study shows that octopamine can be monitored in Drosophila, facilitating future studies of how octopamine release functions in the insect brain. PMID:27326831

  19. Neurobiological model of stimulated dopamine neurotransmission to interpret fast-scan cyclic voltammetry data.

    PubMed

    Harun, Rashed; Grassi, Christine M; Munoz, Miranda J; Torres, Gonzalo E; Wagner, Amy K

    2015-03-01

    Fast-scan cyclic voltammetry (FSCV) is an electrochemical method that can assess real-time in vivo dopamine (DA) concentration changes to study the kinetics of DA neurotransmission. Electrical stimulation of dopaminergic (DAergic) pathways can elicit FSCV DA responses that largely reflect a balance of DA release and reuptake. Interpretation of these evoked DA responses requires a framework to discern the contribution of DA release and reuptake. The current, widely implemented interpretive framework for doing so is the Michaelis-Menten (M-M) model, which is grounded on two assumptions- (1) DA release rate is constant during stimulation, and (2) DA reuptake occurs through dopamine transporters (DAT) in a manner consistent with M-M enzyme kinetics. Though the M-M model can simulate evoked DA responses that rise convexly, response types that predominate in the ventral striatum, the M-M model cannot simulate dorsal striatal responses that rise concavely. Based on current neurotransmission principles and experimental FSCV data, we developed a novel, quantitative, neurobiological framework to interpret DA responses that assumes DA release decreases exponentially during stimulation and continues post-stimulation at a diminishing rate. Our model also incorporates dynamic M-M kinetics to describe DA reuptake as a process of decreasing reuptake efficiency. We demonstrate that this quantitative, neurobiological model is an extension of the traditional M-M model that can simulate heterogeneous regional DA responses following manipulation of stimulation duration, frequency, and DA pharmacology. The proposed model can advance our interpretive framework for future in vivo FSCV studies examining regional DA kinetics and their alteration by disease and DA pharmacology. PMID:25527399

  20. Detection and classification of gaseous sulfur compounds by solid electrolyte cyclic voltammetry of cermet sensor array.

    PubMed

    Kramer, Kirsten E; Rose-Pehrsson, Susan L; Hammond, Mark H; Tillett, Duane; Streckert, Holger H

    2007-02-12

    Electrochemical sensors composed of a ceramic-metallic (cermet) solid electrolyte are used for the detection of gaseous sulfur compounds SO(2), H(2)S, and CS(2) in a study involving 11 toxic industrial chemical (TIC) compounds. The study examines a sensor array containing four cermet sensors varying in electrode-electrolyte composition, designed to offer selectivity for multiple compounds. The sensors are driven by cyclic voltammetry to produce a current-voltage profile for each analyte. Raw voltammograms are processed by background subtraction of clean air, and the four sensor signals are concatenated to form one vector of points. The high-resolution signal is compressed by wavelet transformation and a probabilistic neural network is used for classification. In this study, training data from one sensor array was used to formulate models which were validated with data from a second sensor array. Of the 11 gases studied, 3 that contained sulfur produced the strongest responses and were successfully analyzed when the remaining compounds were treated as interferents. Analytes were measured from 10 to 200% of their threshold-limited value (TLV) according to the 8-h time weighted average (TWA) exposure limits defined by the National Institute of Occupational Safety and Health (NIOSH). True positive classification rates of 93.3, 96.7, and 76.7% for SO(2), H(2)S, and CS(2), respectively, were achieved for prediction of one sensor unit when a second sensor was used for modeling. True positive rates of 83.3, 90.0, and 90.0% for SO(2), H(2)S, and CS(2), respectively, were achieved for the second sensor unit when the first sensor unit was used for modeling. Most of the misclassifications were for low concentration levels (such 10-25% TLV) in which case the compound was classified as clean air. Between the two sensors, the false positive rates were 2.2% or lower for the three sulfur compounds, 0.9% or lower for the interferents (eight remaining analytes), and 5.8% or lower for

  1. Cyclic voltammetry deposition of copper nanostructure on MWCNTs modified pencil graphite electrode: An ultra-sensitive hydrazine sensor.

    PubMed

    Heydari, Hamid; Gholivand, Mohammad B; Abdolmaleki, Abbas

    2016-09-01

    In this study, Copper (Cu) nanostructures (CuNS) were electrochemically deposited on a film of multiwall carbon nanotubes (MWCNTs) modified pencil graphite electrode (MWCNTs/PGE) by cyclic voltammetry method to fabricate a CuNS-MWCNTs composite sensor (CuNS-MWCNT/PGE) for hydrazine detection. Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) were used for the characterization of CuNS on the MWCNTs matrix. The composite of CuNS-MWCNTs was characterized with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The preliminary studies showed that the proposed sensor have a synergistic electrocatalytic activity for the oxidation of hydrazine in phosphate buffer. The catalytic currents of square wave voltammetry had a linear correlation with the hydrazine concentration in the range of 0.1 to 800μM with a low detection limit of 70nM. Moreover, the amperometric oxidation current exhibited a linear correlation with hydrazine concentration in the concentration range of 50-800μM with the detection limit of 4.3μM. The proposed electrode was used for the determination of hydrazine in real samples and the results were promising. Empirical results also indicated that the sensor had good reproducibility, long-term stability, and the response of the sensor to hydrazine was free from interferences. Moreover, the proposed sensor benefits from simple preparation, low cost, outstanding sensitivity, selectivity, and reproducibility for hydrazine determination. PMID:27207034

  2. Instrumentation for fast-scan cyclic voltammetry combined with electrophysiology for behavioral experiments in freely moving animals

    NASA Astrophysics Data System (ADS)

    Takmakov, Pavel; McKinney, Collin J.; Carelli, Regina M.; Wightman, R. Mark

    2011-07-01

    Fast-scan cyclic voltammetry is a unique technique for sampling dopamine concentration in the brain of rodents in vivo in real time. The combination of in vivo voltammetry with single-unit electrophysiological recording from the same microelectrode has proved to be useful in studying the relationship between animal behavior, dopamine release and unit activity. The instrumentation for these experiments described here has two unique features. First, a 2-electrode arrangement implemented for voltammetric measurements with the grounded reference electrode allows compatibility with electrophysiological measurements, iontophoresis, and multielectrode measurements. Second, we use miniaturized electronic components in the design of a small headstage that can be fixed on the rat's head and used in freely moving animals.

  3. An experimental evaluation of cyclic voltammetry of multicharged species at macrodisk electrodes in the absence of added supporting electrolyte.

    PubMed

    Bond, A M; Coomber, D C; Feldberg, S W; Oldham, K B; Vu, T

    2001-01-15

    The reversible reduction of [S2Mo18O62]4- to [S2Mo18O62]5- and [S2Mo18O62]6- at a glassy carbon macrodisk electrode has been studied by cyclic voltammetry in acetonitrile as a function of the concentration of [(C6H13)4N]4[S2Mo18O62] in the absence and presence of [(C6H13)4N]ClO4 as the added supporting electrolyte. Consideration is given to the influence of scan rate, reference-working electrode distance, [(C6H13)4N]4[S2Mo18O62], and electrolyte concentrations. Experimental data confirm theoretical predictions that cyclic voltammetry at a macrodisk electrode is a viable technique for studies of multiply charged electroactive species without added electrolyte, provided the influence of enhanced complexities associated with effects of increased solution resistance, the mass transport contribution from migration, and convection arising from enhanced density gradients are considered. Enhanced density gradients present in the absence of added supporting electrolyte give rise to a more marked dependence of voltammograms on the angle of the electrode and hence lead to significant distortion of wave shapes at low scan rates. The summation of all these obstacles implies that quantitative evaluation of cyclic voltammograms of multiply charged species requires significantly greater care in the absence than in the presence of added supporting electrolyte. PMID:11199989

  4. Development and Characterization of Carbon-Fiber Microbiosensors for Fast-Scan Cyclic Voltammetry

    NASA Astrophysics Data System (ADS)

    Lugo-Morales, Leyda Zoraida

    Electrochemistry has been shown to be a robust tool in neuroscience. The use of carbon-fiber microelectrodes coupled with background-subtracted fast-scan cyclic voltammetry (FSCV) offers high sensitivity, selectivity, as well as the spatial and temporal resolution necessary for monitoring rapid fluctuations of electroactive molecules in live brain tissue. Dopamine (DA) is a neurotransmitter playing a key role in the regulation of reward and motivated behavior. FSCV has been used to understand DA dynamics and how these underlie discrete aspects of brain function. The methodological aspects of real-time DA detection at carbon-fiber microelectrodes using FSCV in anesthetized and awake animals are presented. Furthermore, the combination of FSCV with other neuroanalytical techniques is also explained. The advantages of FSCV and carbon-fiber microelectrodes can be expanded to the detection of non-electroactive analytes. This broadens the scope of FSCV such that it can be used to investigate how changes in non-electroactive chemicals underlie disease, cognition, and behavior. Carbon-fiber microelectrodes can be modified with an enzyme to monitor non-electroactive molecules, generating an electroactive product (usually hydrogen peroxide, H2O2). The first voltammetric detection of H2O 2 at bare carbon-fiber microelectrodes using FSCV has recently been reported. Thus, an avenue exists to utilize FSCV at enzyme-modified microelectrodes to voltammetrically identify and quantify non-electroactive analytes in real-time. Such an approach will overcome many limitations associated with the traditional amperometric detection scheme, which lacks electrochemical selectivity. Electrodeposition of the biopolymer chitosan with glucose oxidase (GOx) at the carbon surface yields a stable, sensitive, and selective glucose microbiosensor that has been utilized to detect glucose fluctuations in vivo with unprecedented speed. This new method has revealed the first rapid glucose fluctuations in

  5. Development and Characterization of Carbon-Fiber Microbiosensors for Fast-Scan Cyclic Voltammetry

    NASA Astrophysics Data System (ADS)

    Lugo-Morales, Leyda Zoraida

    Electrochemistry has been shown to be a robust tool in neuroscience. The use of carbon-fiber microelectrodes coupled with background-subtracted fast-scan cyclic voltammetry (FSCV) offers high sensitivity, selectivity, as well as the spatial and temporal resolution necessary for monitoring rapid fluctuations of electroactive molecules in live brain tissue. Dopamine (DA) is a neurotransmitter playing a key role in the regulation of reward and motivated behavior. FSCV has been used to understand DA dynamics and how these underlie discrete aspects of brain function. The methodological aspects of real-time DA detection at carbon-fiber microelectrodes using FSCV in anesthetized and awake animals are presented. Furthermore, the combination of FSCV with other neuroanalytical techniques is also explained. The advantages of FSCV and carbon-fiber microelectrodes can be expanded to the detection of non-electroactive analytes. This broadens the scope of FSCV such that it can be used to investigate how changes in non-electroactive chemicals underlie disease, cognition, and behavior. Carbon-fiber microelectrodes can be modified with an enzyme to monitor non-electroactive molecules, generating an electroactive product (usually hydrogen peroxide, H2O2). The first voltammetric detection of H2O 2 at bare carbon-fiber microelectrodes using FSCV has recently been reported. Thus, an avenue exists to utilize FSCV at enzyme-modified microelectrodes to voltammetrically identify and quantify non-electroactive analytes in real-time. Such an approach will overcome many limitations associated with the traditional amperometric detection scheme, which lacks electrochemical selectivity. Electrodeposition of the biopolymer chitosan with glucose oxidase (GOx) at the carbon surface yields a stable, sensitive, and selective glucose microbiosensor that has been utilized to detect glucose fluctuations in vivo with unprecedented speed. This new method has revealed the first rapid glucose fluctuations in

  6. Diagnostic Criteria for the Characterization of Electrode Reactions with Chemically Coupled Reactions Preceding the Electron Transfer by Cyclic Square Wave Voltammetry.

    PubMed

    Helfrick, John C; Mann, Megan A; Bottomley, Lawrence A

    2016-08-18

    Theory for cyclic square wave voltammetry of electrode reactions with chemical reactions preceding the electron transfer is presented. Theoretical voltammograms were calculated following systematic variation of empirical parameters to assess their impact on the shape of the voltammogram. From the trends obtained, diagnostic criteria for this mechanism were deduced. When properly applied, these criteria will enable non-experts in voltammetry to assign the electrode reaction mechanism and accurately measure reaction kinetics. PMID:27443581

  7. Cyclic voltammetry on sputter-deposited films of electrochromic Ni oxide: Power-law decay of the charge density exchange

    SciTech Connect

    Wen, Rui-Tao Granqvist, Claes G.; Niklasson, Gunnar A.

    2014-10-20

    Ni-oxide-based thin films were produced by reactive direct-current magnetron sputtering and were characterized by X-ray diffraction and Rutherford backscattering spectroscopy. Intercalation of Li{sup +} ions was accomplished by cyclic voltammetry (CV) in an electrolyte of LiClO{sub 4} in propylene carbonate, and electrochromism was documented by spectrophotometry. The charge density exchange, and hence the optical modulation span, decayed gradually upon repeated cycling. This phenomenon was accurately described by an empirical power law, which was valid for at least 10{sup 4} cycles when the applied voltage was limited to 4.1 V vs Li/Li{sup +}. Our results allow lifetime assessments for one of the essential components in an electrochromic device such as a “smart window” for energy-efficient buildings.

  8. Cyclic voltammetry on sputter-deposited films of electrochromic Ni oxide: Power-law decay of the charge density exchange

    NASA Astrophysics Data System (ADS)

    Wen, Rui-Tao; Granqvist, Claes G.; Niklasson, Gunnar A.

    2014-10-01

    Ni-oxide-based thin films were produced by reactive direct-current magnetron sputtering and were characterized by X-ray diffraction and Rutherford backscattering spectroscopy. Intercalation of Li+ ions was accomplished by cyclic voltammetry (CV) in an electrolyte of LiClO4 in propylene carbonate, and electrochromism was documented by spectrophotometry. The charge density exchange, and hence the optical modulation span, decayed gradually upon repeated cycling. This phenomenon was accurately described by an empirical power law, which was valid for at least 104 cycles when the applied voltage was limited to 4.1 V vs Li/Li+. Our results allow lifetime assessments for one of the essential components in an electrochromic device such as a "smart window" for energy-efficient buildings.

  9. Analytical solutions of the planar cyclic voltammetry process for two soluble species with equal diffusivities and fast electron transfer using the method of eigenfunction expansions

    NASA Astrophysics Data System (ADS)

    Samin, Adib; Lahti, Erik; Zhang, Jinsuo

    2015-08-01

    Cyclic voltammetry is a powerful tool that is used for characterizing electrochemical processes. Models of cyclic voltammetry take into account the mass transport of species and the kinetics at the electrode surface. Analytical solutions of these models are not well-known due to the complexity of the boundary conditions. In this study we present closed form analytical solutions of the planar voltammetry model for two soluble species with fast electron transfer and equal diffusivities using the eigenfunction expansion method. Our solution methodology does not incorporate Laplace transforms and yields good agreement with the numerical solution. This solution method can be extended to cases that are more general and may be useful for benchmarking purposes.

  10. Analytical solutions of the planar cyclic voltammetry process for two soluble species with equal diffusivities and fast electron transfer using the method of eigenfunction expansions

    SciTech Connect

    Samin, Adib; Lahti, Erik; Zhang, Jinsuo

    2015-08-15

    Cyclic voltammetry is a powerful tool that is used for characterizing electrochemical processes. Models of cyclic voltammetry take into account the mass transport of species and the kinetics at the electrode surface. Analytical solutions of these models are not well-known due to the complexity of the boundary conditions. In this study we present closed form analytical solutions of the planar voltammetry model for two soluble species with fast electron transfer and equal diffusivities using the eigenfunction expansion method. Our solution methodology does not incorporate Laplace transforms and yields good agreement with the numerical solution. This solution method can be extended to cases that are more general and may be useful for benchmarking purposes.

  11. Electrochemical behaviour of iron in a third-generation ionic liquid: cyclic voltammetry and micromachining investigations.

    PubMed

    Moustafa, Essam M; Mann, Olivier; Fürbeth, Wolfram; Schuster, Rolf

    2009-12-01

    The electrochemical behaviour of Fe in 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([Emim](+)Ntf2(-)) and mixtures with Cl(-) is studied with the aim of investigating the applicability of ionic liquids (IL) for the electrochemical machining of iron. Whereas in pure IL iron could not be significantly dissolved, the addition of Cl(-) enables the active dissolution with anodic current densities up to several mA cm(-2). Although several anodic peaks appear in the cyclic voltammograms (CV), the distinct assignment of those electrochemical processes remain difficult. In particular no proof for the formation of FeCl(x) (2-x) complexes during Fe dissolution are deduced from the CV, although such complexes are shown to be stable in the employed electrolyte. In addition, we present electrochemical drilling experiments with short potential pulses, which demonstrate that electrochemical machining of Fe is, in principle, possible in IL based electrolytes, even though hampered by slow machining speed. PMID:19760696

  12. Determination of nitroaromatic and nitramine type energetic materials in synthetic and real mixtures by cyclic voltammetry.

    PubMed

    Üzer, Ayşem; Sağlam, Sener; Tekdemir, Yasemin; Ustamehmetoğlu, Belkıs; Sezer, Esma; Erçağ, Erol; Apak, Reşat

    2013-10-15

    Nitro-explosives contain reducible aromatic -NO2 groups or cyclic >N-NO2 bonds that may undergo reductive cleavage. This work reports the development of a cyclic voltammetric (CV) assay for nitro-aromatics (trinitrotoluene (TNT), dinitrotoluene (DNT)) and nitramines (1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX)) using a glassy carbon electrode. This determination was first used for these energetic materials by resolving current responses of reduction potentials primarily due to one constituent but partly contributed by other constituents. Calibration curves of current intensity versus concentration were linear in the range of 30-120 mg L(-1) for RDX with a limit of detection (LOD) of 10.2 mg L(-1), 40-120 mg L(-1) for HMX (LOD=11.7 mg L(-1)), 40-120 mg L(-1) for TNT (LOD=11.2 mg L(-1)), and 40-140 mg L(-1) for DNT (LOD=10.8 mg L(-1)). Results showed that the CV method could provide a sensitive approach for the simultaneous determination of RDX and TNT in synthetic and real mixtures. Deconvolution of current contributions of mixtures at peak potentials of constituents was performed by multiple linear regression. The proposed method was successfully applied to the analysis of military explosives comp A5 and octol, and method validation was performed both against HPLC on a comp B (TNT+RDX) sample and against GC-MS on real post-blast residual samples containing both explosives. PMID:24054661

  13. Electrochemical characteristics of nanostructured platinum electrodes--a cyclic voltammetry study.

    PubMed

    Daubinger, P; Kieninger, J; Unmüssig, T; Urban, G A

    2014-05-14

    Platinum surfaces play a decisive role in catalysis in sensors, fuel cells, solar cells and other applications like neuronal stimulation and recording. Technical advances in nanotechnology contributed tremendously to the progress in these fields. A fundamental understanding of the chemical and physical interactions between the nanostructured surfaces and electrolytes is essential, but was barely investigated up to now. In this article, we present a wet-chemical process for the deposition of nanostructures on polycrystalline platinum surfaces. The electrochemically active surface area was increased by a factor of over 1000 times with respect to the geometrical surface. The influence of the nanostructures was examined in different acidic, alkaline, and neutral electrolytes. Comparing cyclic voltammograms of nanostructured and planar polycrystalline platinum revealed new insights into the microenvironment at the electrode-electrolyte interface. The characteristic features of the cyclic voltammograms were altered in their shape and strongly shifted with respect to the applied potential. In neutral buffered and unbuffered electrolytes the water window was expanded from 1.4 V to more than 2 V. The shifts were interpreted as local pH-changes and exhausted buffer capacity in direct proximity of the electrode surface due to the strong release and binding of protons, respectively. These polarized electrodes induce significant changes in the electrochemical potential of the electrolyte due to the high roughness of their surface. The electrochemical phenomena and the observed voltage shifts are crucial for the understanding of the basic mechanism at nanostructured electrodes and mandatory for designing fuel cells, sensors and many other devices. PMID:24664444

  14. Real-time monitoring of electrically evoked catecholamine signals in the songbird striatum using in vivo fast-scan cyclic voltammetry

    PubMed Central

    Smith, Amanda R.; Garris, Paul A.; Casto, Joseph M.

    2015-01-01

    Fast-scan cyclic voltammetry is a powerful technique for monitoring rapid changes in extracellular neurotransmitter levels in the brain. In vivo fast-scan cyclic voltammetry has been used extensively in mammalian models to characterize dopamine signals in both anesthetized and awake preparations, but has yet to be applied to a non-mammalian vertebrate. The goal of this study was to establish in vivo fast-scan cyclic voltammetry in a songbird, the European starling, to facilitate real-time measurements of extracellular catecholamine levels in the avian striatum. In urethane-anesthetized starlings, changes in catecholamine levels were evoked by electrical stimulation of the ventral tegmental area and measured at carbon-fiber microelectrodes positioned in the medial and lateral striata. Catecholamines were elicited by different stimulations, including trains related to phasic dopamine signaling in the rat, and were analyzed to quantify presynaptic mechanisms governing exocytotic release and neuronal uptake. Evoked extracellular catecholamine dynamics, maximal amplitude of the evoked catecholamine signal, and parameters for catecholamine release and uptake did not differ between striatal regions and were similar to those determined for dopamine in the rat dorsomedial striatum under similar conditions. Chemical identification of measured catecholamine by its voltammogram was consistent with the presence of both dopamine and norepinephrine in striatal tissue content. However, the high ratio of dopamine to norepinephrine in tissue content and the greater sensitivity of the carbon-fiber microelectrode to dopamine compared to norepinephrine favored the measurement of dopamine. Thus, converging evidence suggests that dopamine was the predominate analyte of the electrically evoked catecholamine signal measured in the striatum by fast-scan cyclic voltammetry. Overall, comparisons between the characteristics of these evoked signals suggested a similar presynaptic regulation of

  15. Real-time monitoring of electrically evoked catecholamine signals in the songbird striatum using in vivo fast-scan cyclic voltammetry.

    PubMed

    Smith, Amanda R; Garris, Paul A; Casto, Joseph M

    2015-01-01

    Fast-scan cyclic voltammetry is a powerful technique for monitoring rapid changes in extracellular neurotransmitter levels in the brain. In vivo fast-scan cyclic voltammetry has been used extensively in mammalian models to characterize dopamine signals in both anesthetized and awake preparations, but has yet to be applied to a non-mammalian vertebrate. The goal of this study was to establish in vivo fast-scan cyclic voltammetry in a songbird, the European starling, to facilitate real-time measurements of extracellular catecholamine levels in the avian striatum. In urethane-anesthetized starlings, changes in catecholamine levels were evoked by electrical stimulation of the ventral tegmental area and measured at carbon-fiber microelectrodes positioned in the medial and lateral striata. Catecholamines were elicited by different stimulations, including trains related to phasic dopamine signaling in the rat, and were analyzed to quantify presynaptic mechanisms governing exocytotic release and neuronal uptake. Evoked extracellular catecholamine dynamics, maximal amplitude of the evoked catecholamine signal, and parameters for catecholamine release and uptake did not differ between striatal regions and were similar to those determined for dopamine in the rat dorsomedial striatum under similar conditions. Chemical identification of measured catecholamine by its voltammogram was consistent with the presence of both dopamine and norepinephrine in striatal tissue content. However, the high ratio of dopamine to norepinephrine in tissue content and the greater sensitivity of the carbon-fiber microelectrode to dopamine compared to norepinephrine favored the measurement of dopamine. Thus, converging evidence suggests that dopamine was the predominate analyte of the electrically evoked catecholamine signal measured in the striatum by fast-scan cyclic voltammetry. Overall, comparisons between the characteristics of these evoked signals suggested a similar presynaptic regulation of

  16. Estimation of the composition of intermetallic compounds in LiCl-KCl molten salt by cyclic voltammetry.

    PubMed

    Liu, Ya L; Liu, Kui; Yuan, Li Y; Chai, Zhi F; Shi, Wei Q

    2016-08-15

    In this work, the compositions of Ce-Al, Er-Al and La-Bi intermetallic compounds were estimated by the cyclic voltammetry (CV) technique. At first, CV measurements were carried out at different reverse potentials to study the co-reduction processes of Ce-Al, Er-Al and La-Bi systems. The CV curves obtained were then re-plotted with the current as a function of time, and the coulomb number of each peak was calculated. By comparing the coulomb number of the related peaks, the compositions of the Ce-Al, Er-Al and La-Bi intermetallic compounds formed in the co-reduction process could be estimated. The results showed that Al11Ce3, Al3Ce, Al2Ce and AlCe could be formed by the co-reduction of Ce(iii) and Al(iii). For the co-reduction of Er(iii) and Al(iii), Al3Er2, Al2Er and AlEr were formed. In a La(iii) and Bi(iii) co-existing system in LiCl-KCl melts, LaBi2, LaBi and Li3Bi were the major products as a result of co-reduction. PMID:27203295

  17. Impulse radio ultra wideband wireless transmission of dopamine concentration levels recorded by fast-scan cyclic voltammetry.

    PubMed

    Ebrazeh, Ali; Bozorgzadeh, Bardia; Mohseni, Pedram

    2015-08-01

    This paper demonstrates the feasibility of utilizing impulse radio ultra wideband (IR-UWB) signaling technique for reliable, wireless transmission of dopamine concentration levels recorded by fast-scan cyclic voltammetry (FSCV) at a carbon-fiber microelectrode (CFM) to address the problem of elevated data rates in high-channel-count neurochemical monitoring. Utilizing an FSCV-sensing chip fabricated in AMS 0.35μm 2P/4M CMOS, a 3-5-GHz, IR-UWB transceiver (TRX) chip fabricated in TSMC 90nm 1P/9M RF CMOS, and two off-chip, miniature, UWB antennae, wireless transfer of pseudo-random binary sequence (PRBS) data at 50Mbps over a distance of <;1m is first shown with bit-error rates (BER) <; 10(-3). Further, IR-UWB wireless transmission of dopamine concentration levels prerecorded with FSCV at a CFM during flow injection analysis (FIA) is also demonstrated with transmitter (TX) power dissipation of only ~4.4μW from 1.2V, representing two orders of magnitude reduction in TX power consumption compared to that of a conventional frequency-shift-keyed (FSK) link operating at ~433MHz. PMID:26737929

  18. Photoinduced electron transfer occurs between 2-aminopurine and the DNA nucleic acid monophosphates: results from cyclic voltammetry and fluorescence quenching.

    PubMed

    Narayanan, Madhavan; Kodali, Goutham; Xing, Yangjun; Stanley, Robert J

    2010-08-19

    2-Aminopurine (2AP) is a fluorescent adenine analogue that is useful in part because its substantial fluorescence quantum yield is sensitive to base stacking with native bases in ss- and ds-DNA. However, the degree of quenching is sequence dependent and the mechanism of quenching is still a matter of some debate. Here we show that the most likely quenching mechanism in aqueous solution involves photoinduced electron transfer (PET), as revealed by cyclic voltammetry (CV) performed in aprotic organic solvents. These potentials were used with spectroscopic data to obtain excited-state reduction and oxidation potentials. Stern-Volmer (S-V) experiments using the native base monophosphate nucleotides (NMPs) rGMP, rAMP, rCMP, and dTMP were performed in aqueous solution to obtain quenching rate constants kq. The results suggest that 2AP* can act as either an electron donor or an electron acceptor depending on the particular NMP but that PET proceeds for all NMPs tested. PMID:20734496

  19. Enhanced Dopamine Release by Dopamine Transport Inhibitors Described by a Restricted Diffusion Model and Fast-Scan Cyclic Voltammetry.

    PubMed

    Hoffman, Alexander F; Spivak, Charles E; Lupica, Carl R

    2016-06-15

    Fast-scan cyclic voltammetry (FSCV) using carbon fiber electrodes is widely used to rapidly monitor changes in dopamine (DA) levels in vitro and in vivo. Current analytical approaches utilize parameters such as peak oxidation current amplitude and decay times to estimate release and uptake processes, respectively. However, peak amplitude changes are often observed with uptake inhibitors, thereby confounding the interpretation of these parameters. To overcome this limitation, we demonstrate that a simple five-parameter, two-compartment model mathematically describes DA signals as a balance of release (r/ke) and uptake (ku), summed with adsorption (kads and kdes) of DA to the carbon electrode surface. Using nonlinear regression, we demonstrate that our model precisely describes measured DA signals obtained in brain slice recordings. The parameters extracted from these curves were then validated using pharmacological manipulations that selectively alter vesicular release or DA transporter (DAT)-mediated uptake. Manipulation of DA release through altering the Ca(2+)/Mg(2+) ratio or adding tetrodotoxin reduced the release parameter with no effect on the uptake parameter. DAT inhibitors methylenedioxypyrovalerone, cocaine, and nomifensine significantly reduced uptake and increased vesicular DA release. In contrast, a low concentration of amphetamine reduced uptake but had no effect on DA release. Finally, the kappa opioid receptor agonist U50,488 significantly reduced vesicular DA release but had no effect on uptake. Together, these data demonstrate a novel analytical approach to distinguish the effects of manipulations on DA release or uptake that can be used to interpret FSCV data. PMID:27018734

  20. Interaction between reactive oxygen species and coenzyme Q10 in an aprotic medium: a cyclic voltammetry study.

    PubMed

    Ferri, E; Gattavecchia, E; Feroci, G; Battino, M

    1994-01-01

    The involvement of coenzyme Q (CoQ) as an antioxidant agent in several oxidative processes both in vitro and in vivo is nowadays pointed out by several biochemical and clinical studies, but the chemical mechanisms of this action are not yet unequivocally established. Electrochemistry provides very useful techniques for the analysis of the kinetics and thermodynamics, and mechanisms of chemical phenomena involving electron transfers, e.g. in the case of radical reactions. In the present study we used cyclic voltammetry to investigate the interactions between oxygen radicals and ubiquinone in aprotic medium, a condition similar to that existing in the biological membranes. The results obtained showed that ubiquinone is more easily reduced than oxygen, ruling out the possibility of an electron transfer from semiquinone to oxygen to produce superoxide radicals. On the contrary, it was demonstrated that fully reduced quinone is able to scavenge the superoxide radical, by reduction to peroxide ion, lowering actually the oxidative potential in the medium. PMID:7752848

  1. Wireless fast-scan cyclic voltammetry measurement of histamine using WINCS -- a proof-of-principle study

    PubMed Central

    Chang, Su-Youne; Jay, Taylor; Muñoz, Joel; Kim, Inyong; Lee, Kendall H.

    2012-01-01

    Histamine is among the most poorly understood biogenic amines, yet the histaminergic system spreads throughout the brain and has been implicated in functions as diverse as homeostasis and synaptic plasticity. Not surprisingly then, it has been linked to a number of conditions including minimally conscious state, persistent vegetative state, epilepsy, addiction, cluster headache, essential tremor, and Parkinson’s disease. We have previously reported that the Wireless Instantaneous Neurotransmitter Concentration Sensing (WINCS) system can monitor dopamine, serotonin, and adenosine using fast-scan cyclic voltammetry (FSCV). Here, we demonstrate the expanded capability of the WINCS system to measure histamine. The optimal FSCV waveform was determined to be a triangle wave scanned between −0.4 and +1.4 V at a rate of 400 V/s applied at 10 Hz. Using this optimized FSCV parameter, we found histamine release was induced by high frequency electrical stimulation at the tuberomammillary nucleus in rat brain slices. Our results suggest that the WINCS system can provide reliable, high fidelity measurements of histamine, consistently showing oxidative currents at +1.3 V, a finding that may have important clinical implications. PMID:22416270

  2. Electrochemical deposition of poly(trans-[RuCl2(4-vinylpyridine)4]) and its reductive desorption: cyclic voltammetry and electrochemical quartz crystal microbalance studies.

    PubMed

    Bandeira, Merlin C E; Crayston, Joe A; Franco, César V; Glidle, Andrew

    2007-02-28

    The electropolymerization of trans-[RuCl(2)(vpy)(4)](vpy = 4-vinylpyridine) on Au or Pt electrodes was studied by cyclic voltammetry and the electrochemical quartz crystal microbalance (EQCM) technique. Cyclic voltammetry of the monomer in DMSO on Au shows reductions at -2.0 and -2.2 V. Potential cycling over the first wave leads to polymer formation; however, scanning over the second wave leads to desorption of the polymer. These observations were confirmed by EQCM measurements which also revealed a high polymerization efficiency. Electrolysis, EQCM and XPS measurements showed that desorption was associated with substitution of chloride ligands by DMSO when the polymer was in a highly reduced state. The film also showed reversible mass changes due to the oxidation and accompanying ingress of charge-balancing anions and solvent into the film. Measurements on the dried films revealed that large quantities of solvent are trapped in the film during the electropolymerization process. PMID:17301891

  3. Expanding neurochemical investigations with multi-modal recording: simultaneous fast-scan cyclic voltammetry, iontophoresis, and patch clamp measurements.

    PubMed

    Kirkpatrick, D C; McKinney, C J; Manis, P B; Wightman, R M

    2016-08-01

    Multi-modal recording describes the simultaneous collection of information across distinct domains. Compared to isolated measurements, such studies can more easily determine relationships between varieties of phenomena. This is useful for neurochemical investigations which examine cellular activity in response to changes in the local chemical environment. In this study, we demonstrate a method to perform simultaneous patch clamp measurements with fast-scan cyclic voltammetry (FSCV) using optically isolated instrumentation. A model circuit simulating concurrent measurements was used to predict the electrical interference between instruments. No significant impact was anticipated between methods, and predictions were largely confirmed experimentally. One exception was due to capacitive coupling of the FSCV potential waveform into the patch clamp amplifier. However, capacitive transients measured in whole-cell current clamp recordings were well below the level of biological signals, which allowed the activity of cells to be easily determined. Next, the activity of medium spiny neurons (MSNs) was examined in the presence of an FSCV electrode to determine how the exogenous potential impacted nearby cells. The activities of both resting and active MSNs were unaffected by the FSCV waveform. Additionally, application of an iontophoretic current, used to locally deliver drugs and other neurochemicals, did not affect neighboring cells. Finally, MSN activity was monitored during iontophoretic delivery of glutamate, an excitatory neurotransmitter. Membrane depolarization and cell firing were observed concurrently with chemical changes around the cell resulting from delivery. In all, we show how combined electrophysiological and electrochemical measurements can relate information between domains and increase the power of neurochemical investigations. PMID:27314130

  4. Measurement of the ground-state distributions in bistable mechanically interlocked molecules using slow scan rate cyclic voltammetry

    PubMed Central

    Fahrenbach, Albert C.; Barnes, Jonathan C.; Li, Hao; Benítez, Diego; Basuray, Ashish N.; Fang, Lei; Sue, Chi-Hau; Barin, Gokhan; Dey, Sanjeev K.; Goddard, William A.; Stoddart, J. Fraser

    2011-01-01

    In donor–acceptor mechanically interlocked molecules that exhibit bistability, the relative populations of the translational isomers—present, for example, in a bistable [2]rotaxane, as well as in a couple of bistable [2]catenanes of the donor–acceptor vintage—can be elucidated by slow scan rate cyclic voltammetry. The practice of transitioning from a fast scan rate regime to a slow one permits the measurement of an intermediate redox couple that is a function of the equilibrium that exists between the two translational isomers in the case of all three mechanically interlocked molecules investigated. These intermediate redox potentials can be used to calculate the ground-state distribution constants, K. Whereas, (i) in the case of the bistable [2]rotaxane, composed of a dumbbell component containing π-electron-rich tetrathiafulvalene and dioxynaphthalene recognition sites for the ring component (namely, a tetracationic cyclophane, containing two π-electron-deficient bipyridinium units), a value for K of 10 ± 2 is calculated, (ii) in the case of the two bistable [2]catenanes—one containing a crown ether with tetrathiafulvalene and dioxynaphthalene recognition sites for the tetracationic cyclophane, and the other, tetrathiafulvalene and butadiyne recognition sites—the values for K are orders (one and three, respectively) of magnitude greater. This observation, which has also been probed by theoretical calculations, supports the hypothesis that the extra stability of one translational isomer over the other is because of the influence of the enforced side-on donor–acceptor interactions brought about by both π-electron-rich recognition sites being part of a macrocyclic polyether. PMID:22135467

  5. Redox intermediates of flavonoids and caffeic acid esters from propolis: an EPR spectroscopy and cyclic voltammetry study.

    PubMed

    Rapta, P; Misík, V; Stasko, A; Vrábel, I

    1995-05-01

    The redox properties of flavonoids: chrysin (1), tectochrysin (2), galangin (3), isalpinin (4), pinostrobin (5), pinobanksin (6), pinobanksin-3-acetate (7), and of caffeic acid ester (8) and diacetylcaffeic acid ester (9), all isolated from propolis, were investigated by cyclic voltammetry in acetonitrile. The choice of aprotic solvent lowered the reactivity of the radical intermediates and made possible to identify redox steps and intermediates not detected so far. The oxidation potentials (vs. saturated calomel electrode) of the investigated compounds were in the region of 1.5 V for 3 and 4; 1.9 V for 1, 2, and 5; 2.0 V for 6 and 7; 1.29 V for 8; and 2.3 V for 9. These oxidation potentials were mainly influenced by the presence of a double bond in 2,3-position and substituent R1 in position 3. Comparison with our earlier data revealed that flavonoids, 1-4, and caffeic acid ester 8 with lower oxidation potentials showed the maximal lipid antioxidant activity, whereas those with higher potentials (5, 6, 7, and 9) are less active. On reduction of 1-9 several one-electron-steps were typically observed in the potential regions: -1.5 V, -1.8 V, and -2 V. where in simultaneous EPR experiments anion radicals of 1 and 3 were observed with the center of unpaired spin density on ring A. Upon oxidation of flavonoids 1-4 carbonyl carbon-centered radicals, .C(O)R, were identified as consecutive products using the EPR spin trapping technique. PMID:7797098

  6. Simulations of Cyclic Voltammetry for Electric Double Layers in Asymmetric Electrolytes: A Generalized Modified Poisson-Nernst-Planck Model

    SciTech Connect

    Wang, Hainan; Thiele, Alexander; Pilon, Laurent

    2013-11-15

    This paper presents a generalized modified Poisson–Nernst–Planck (MPNP) model derived from first principles based on excess chemical potential and Langmuir activity coefficient to simulate electric double-layer dynamics in asymmetric electrolytes. The model accounts simultaneously for (1) asymmetric electrolytes with (2) multiple ion species, (3) finite ion sizes, and (4) Stern and diffuse layers along with Ohmic potential drop in the electrode. It was used to simulate cyclic voltammetry (CV) measurements for binary asymmetric electrolytes. The results demonstrated that the current density increased significantly with decreasing ion diameter and/or increasing valency |zi| of either ion species. By contrast, the ion diffusion coefficients affected the CV curves and capacitance only at large scan rates. Dimensional analysis was also performed, and 11 dimensionless numbers were identified to govern the CV measurements of the electric double layer in binary asymmetric electrolytes between two identical planar electrodes of finite thickness. A self-similar behavior was identified for the electric double-layer integral capacitance estimated from CV measurement simulations. Two regimes were identified by comparing the half cycle period τCV and the “RC time scale” τRC corresponding to the characteristic time of ions’ electrodiffusion. For τRC ← τCV, quasi-equilibrium conditions prevailed and the capacitance was diffusion-independent while for τRC → τCV, the capacitance was diffusion-limited. The effect of the electrode was captured by the dimensionless electrode electrical conductivity representing the ratio of characteristic times associated with charge transport in the electrolyte and that in the electrode. The model developed here will be useful for simulating and designing various practical electrochemical, colloidal, and biological systems for a wide range of applications.

  7. Structural transformation during Li/Na insertion and theoretical cyclic voltammetry of the δ-NH4V4O10 electrode: a first-principles study.

    PubMed

    Sarkar, Tanmay; Kumar, Parveen; Bharadwaj, Mridula Dixit; Waghmare, Umesh

    2016-04-14

    A double layer δ-NH4V4O10, due to its high energy storage capacity and excellent rate capability, is a very promising cathode material for Li-ion and Na-ion batteries for large-scale renewable energy storage in transportation and smart grids. While it possesses better stability, and higher ionic and electronic conductivity than the most widely explored V2O5, the mechanisms of its cyclability are yet to be understood. Here, we present a theoretical cyclic voltammetry as a tool based on first-principles calculations, and uncover structural transformations that occur during Li(+)/Na(+) insertion (x) into (Lix/Nax)NH4V4O10. Structural distortions associated with single-phase and multi-phase structural changes during the insertion of Li(+)/Na(+), identified through the analysis of voltage profile and theoretical cyclic voltammetry are in agreement with the reported experimental electrochemical measurements on δ-NH4V4O10. We obtain an insight into its electronic structure with a lower band gap that is responsible for the high rate capability of (Lix/Nax) δ-NH4V4O10. The scheme of theoretical cyclic voltammetry presented here will be useful for addressing issues of cyclability and energy rate in other electrode materials. PMID:26996324

  8. Development of the Wireless Instantaneous Neurotransmitter Concentration System for intraoperative neurochemical monitoring using fast-scan cyclic voltammetry

    PubMed Central

    Bledsoe, Jonathan M.; Kimble, Christopher J.; Covey, Daniel P.; Blaha, Charles D.; Agnesi, Filippo; Mohseni, Pedram; Whitlock, Sidney; Johnson, David M.; Horne, April; Bennet, Kevin E.; Lee, Kendall H.; Garris, Paul A.

    2009-01-01

    Object Emerging evidence supports the hypothesis that modulation of specific central neuronal systems contributes to the clinical efficacy of deep brain stimulation (DBS) and motor cortex stimulation (MCS). Real-time monitoring of the neurochemical output of targeted regions may therefore advance functional neurosurgery by, among other goals, providing a strategy for investigation of mechanisms, identification of new candidate neurotransmitters, and chemically guided placement of the stimulating electrode. The authors report the development of a device called the Wireless Instantaneous Neurotransmitter Concentration System (WINCS) for intraoperative neurochemical monitoring during functional neurosurgery. This device supports fast-scan cyclic voltammetry (FSCV) at a carbon-fiber microelectrode (CFM) for real-time, spatially and chemically resolved neurotransmitter measurements in the brain. Methods The FSCV study consisted of a triangle wave scanned between −0.4 and 1 V at a rate of 300 V/second and applied at 10 Hz. All voltages were compared with an Ag/AgCl reference electrode. The CFM was constructed by aspirating a single carbon fiber (r = 2.5 μm) into a glass capillary and pulling the capillary to a microscopic tip by using a pipette puller. The exposed carbon fiber (that is, the sensing region) extended beyond the glass insulation by ~ 100 μm. The neurotransmitter dopamine was selected as the analyte for most trials. Proof-of-principle tests included in vitro flow injection and noise analysis, and in vivo measurements in urethane-anesthetized rats by monitoring dopamine release in the striatum following high-frequency electrical stimulation of the medial forebrain bundle. Direct comparisons were made to a conventional hardwired system. Results The WINCS, designed in compliance with FDA-recognized consensus standards for medical electrical device safety, consisted of 4 modules: 1) front-end analog circuit for FSCV (that is, current-to-voltage transducer

  9. Cyclic voltammetry at TCNQ and TTF-TCNQ modified platinum electrodes: A study of the glucose oxidase/glucose and galactose oxidase/galactose systems

    SciTech Connect

    Hale, P.D.; Skotheim, T.A.

    1988-01-01

    Recent work has shown that the synthetic metal TTF-TCNQ can be used as an electrode material for the oxidation of enzymes containing the prosthetic group flavin adenine dinucleotide (FAD). This direct electron transfer (direct in the sense that oxygen is not a mediator) between reduced enzyme and electrode, a process which does not occur to any measurable extent at a typical metal electrode, is not very well understood. In the present work, electron transfer between reduced glucose oxidase and TTF-TCNQ is investigated using cyclic voltammetry, and it is also shown that TCNQ itself can mediate this electron transfer between the enzyme and a platinum electrode. In addition to the glucose oxidase studies, cyclic voltammetric experiments have been performed on the galactose oxidase system, which contains a copper redox center rather than FAD. The results of these experiments demonstrate that the catalytic ability of TTF-TCNQ in enzyme-based electrochemical sensors is quite general. 15 refs., 4 figs.

  10. Corrosion Cyclic Voltammetry of Two Types of Heat-Affected Zones (HAZs) of API-X100 Steel in Bicarbonate Solutions

    NASA Astrophysics Data System (ADS)

    Eliyan, Faysal Fayez; Alfantazi, Akram

    2014-12-01

    This paper examined the electrochemical corrosion behavior and corrosion products of two types of heat-affected HAZs made from API-X100 steel. Cyclic voltammetry, with different scan rates and potential ranges at 10 cycles, was applied to analyze the interdependent corrosion reactions of cathodic reduction, anodic dissolution, passivation, and transpassivation. The HAZ cooled at 60 K/s, from a peak temperature of 1470 K (1197 °C) that was held for 15 seconds, exhibited better passivation and lower cathodic activity than the HAZ cooled at 10 K/s. Increasing bicarbonate concentration, from 0.05 and 0.2 to 0.6 M, increases the anodic activity and cathodic reduction, but accordingly protects the active surfaces and enhances passivation.

  11. Enzyme-modified carbon-fiber microelectrode for the quantification of dynamic fluctuations of nonelectroactive analytes using fast-scan cyclic voltammetry.

    PubMed

    Lugo-Morales, Leyda Z; Loziuk, Philip L; Corder, Amanda K; Toups, J Vincent; Roberts, James G; McCaffrey, Katherine A; Sombers, Leslie A

    2013-09-17

    Neurotransmission occurs on a millisecond time scale, but conventional methods for monitoring nonelectroactive neurochemicals are limited by slow sampling rates. Despite a significant global market, a sensor capable of measuring the dynamics of rapidly fluctuating, nonelectroactive molecules at a single recording site with high sensitivity, electrochemical selectivity, and a subsecond response time is still lacking. To address this need, we have enabled the real-time detection of dynamic glucose fluctuations in live brain tissue using background-subtracted, fast-scan cyclic voltammetry. The novel microbiosensor consists of a simple carbon fiber surface modified with an electrodeposited chitosan hydrogel encapsulating glucose oxidase. The selectivity afforded by voltammetry enables quantitative and qualitative measurements of enzymatically generated H2O2 without the need for additional strategies to eliminate interfering agents. The microbiosensors possess a sensitivity and limit of detection for glucose of 19.4 ± 0.2 nA mM(-1) and 13.1 ± 0.7 μM, respectively. They are stable, even under deviations from physiological normoxic conditions, and show minimal interference from endogenous electroactive substances. Using this approach, we have quantitatively and selectively monitored pharmacologically evoked glucose fluctuations with unprecedented chemical and spatial resolution. Furthermore, this novel biosensing strategy is widely applicable to the immobilization of any H2O2 producing enzyme, enabling rapid monitoring of many nonelectroactive enzyme substrates. PMID:23919631

  12. Characterization of the polycrystalline n-CuInSe/sub 2/-indium oxide/polyiodide junction by electrolyte electroreflectance, cyclic voltammetry, and scanning electron microscopy

    SciTech Connect

    Razzini, G.; Bicelli, L.P.; Scrosati, B.; Pujadas, M.; Salvador, P.

    1988-05-01

    It is well known that stable and efficient liquid-junction photovoltaic solar cells based on n-CuInSe/sub 2/ photoanodes can be obtained by coating the semiconductor surface with an indium-oxide layer and by employing an aqueous polyiodide solution containing Cu/sup +/, In/sup 3+/, and H/sup +/ ions. In this work, the authors further investigated the polycrystalline n-CuInSe/sub 2/-indium oxide/polyiodide junction using electrolyte electroreflectance and cyclic voltammetry. The effect of the indium-oxide overcoat on the semiconductor flatband potential in solutions having different pH values was studied by monitoring the whole specimen surface and small surface areas. Indium is found to be preferentally electrodeposited at surface defects and at zones of high electrical conductivity, while insulating areas (low doped crystallites) remain uncovered. This explains the lack of homogeneity of the In-oxide layer generated by thermal oxidation of the electrodeposited In. The flatband potential of the surface areas covered with indium oxide is reasonably more affected by electrolyte rhoH changes than that of uncovered zones. Finally, the influence of rhoH on the electroreduction efficiency of dissolved anions was investigated on both etched and In-oxide covered CuInSe/sub 2/ electrodes by cyclic voltammetry. The experimental fact that at acidic media, the electroreduction kinetics of anions I/sub 3//sup -/ is enhanced, is consistent with the observed rhoH dependence of the flatband potential and explains the photostabilizing effect of indium-oxide overcoating in H/sup +/ containing electrolytes.

  13. Part I. Carbon and mercury-carbon optically transparent electrodes. Part II. Investigation of redox properties of technetium by cyclic voltammetry and thin layer spectroelectrochemistry

    SciTech Connect

    Hurst, R.W.

    1980-01-01

    A carbon optically transparent electrode (C OTE) has been prepared by vapor-deposithing a thin carbon film (150 to 310 A thick) on glass and quartz. Optical transparency is good throughout the ultraviolet-visible region. Electrochemical and spectroelectrochemical measurements were made with ferricyanide and o-tolidine respectively. The C OTE serves as a good substrate for deposition of a thin mercury film to form a mercury film transparent electrode (Hg-C OTE). The Hg-C OTE exhibits electrochemical properties of conventional mercury film electrodes as evidenced by Pb/sup 2 +/ cyclic voltammograms. The Hg-C OTE exhibits electrochemical properties of conventional mercury film electrodes as evidenced by Pb/sup 2 -/ cyclic VOHammograms. The Hg-C OTE enabled the spectrochemical characterization of cysteine oxidation, which was shown to involve the oxidation of mercury to form mercurous cysteinate. An 8080 based microcomputer has been interfaced with a Harrick oscillating mirror rapid scanning uv-visible spectrophotometer. Two different approaches are compared for controlling the galvanometer. The first utilizes the digital hardware on the Harrick processing module to derive the mirror drive waveform, while the second creates the waveform under direct software control. A potentiostat is also interfaced and the system is demonstrated by the spectroelectrochemical determination of the redox potential of o-tolidine. Redox potentials are also determined for a series of technetium complexes by the spectropotentiostatic technique. These include hexahalogens, ditertiary arsine, and 1,2-bis(diphenylphosphino) ethane complexes of technetium. Transient hexavalent technetium is produced, detected, and characterized in aqueous alkaline media by pulse radiolysis and very fast scan cyclic voltammetry. The lifetime is of the order of milliseconds. This species is potentially useful in the preparation of technetium radiopharmaceuticals.

  14. CZTS x Se1-x nanocrystals: Composition dependent method of preparation, morphological characterization and cyclic voltammetry data analysis.

    PubMed

    Jadhav, Yogesh A; Thakur, Pragati R; Haram, Santosh K

    2016-09-01

    In this article, synthesis procedures of preparation of copper zinc tin sulpho-selenide (CZTS x Se1-x ) alloy nanocrystals and the data acquired for the material characterization are presented. This data article is related to the research article doi: http://dx.doi.org/10.1016/j.solmat.2016.06.030 (Jadhav et al., 2016) [1]. FTIR data have been presented which helped in confirmation of adsorption of oleylamine on CZTS x Se1-x . Transmission electron microscopy (TEM), Field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) data have been presented which have been used to reveal the morphological details of the nanocrystals. The Energy dispersive X-ray analysis (EDAX) based elemental mapping data has been presented to confirm the elemental composition of nanocrystals. Procedure for the preparation of CZTS x Se1-x based working electrode for the CV measurements have been given. The summary table for the optical, electrochemical band gaps, valance and conduction band edges as a function of composition are listed for the ready reference. PMID:27508267

  15. Integrated wireless fast-scan cyclic voltammetry recording and electrical stimulation for reward-predictive learning in awake, freely moving rats

    NASA Astrophysics Data System (ADS)

    Li, Yu-Ting; Wickens, Jeffery R.; Huang, Yi-Ling; Pan, Wynn H. T.; Chen, Fu-Yu Beverly; Chen, Jia-Jin Jason

    2013-08-01

    Objective. Fast-scan cyclic voltammetry (FSCV) is commonly used to monitor phasic dopamine release, which is usually performed using tethered recording and for limited types of animal behavior. It is necessary to design a wireless dopamine sensing system for animal behavior experiments. Approach. This study integrates a wireless FSCV system for monitoring the dopamine signal in the ventral striatum with an electrical stimulator that induces biphasic current to excite dopaminergic neurons in awake freely moving rats. The measured dopamine signals are unidirectionally transmitted from the wireless FSCV module to the host unit. To reduce electrical artifacts, an optocoupler and a separate power are applied to isolate the FSCV system and electrical stimulator, which can be activated by an infrared controller. Main results. In the validation test, the wireless backpack system has similar performance in comparison with a conventional wired system and it does not significantly affect the locomotor activity of the rat. In the cocaine administration test, the maximum electrically elicited dopamine signals increased to around 230% of the initial value 20 min after the injection of 10 mg kg-1 cocaine. In a classical conditioning test, the dopamine signal in response to a cue increased to around 60 nM over 50 successive trials while the electrically evoked dopamine concentration decreased from about 90 to 50 nM in the maintenance phase. In contrast, the cue-evoked dopamine concentration progressively decreased and the electrically evoked dopamine was eliminated during the extinction phase. In the histological evaluation, there was little damage to brain tissue after five months chronic implantation of the stimulating electrode. Significance. We have developed an integrated wireless voltammetry system for measuring dopamine concentration and providing electrical stimulation. The developed wireless FSCV system is proven to be a useful experimental tool for the continuous

  16. Characterization of smart microwave window materials based on conducting polymer composites: coaxial line, waveguide, and cyclic voltammetry measurements

    NASA Astrophysics Data System (ADS)

    Barnes, Alan; Wright, Peter V.; Despotakis, Anthony; Lees, K.; Chambers, Barry

    1998-07-01

    Discs of polyaniline-silver-polymer electrolyte composites exhibit rapid and reversible changes in their microwave impedance when small electric fields are applied across then in a resonant coaxial line test set. The experimental data show that the initial conductivity of the materials is dependent on the concentration of silver metal and suggests that changes in resistance due to chemical switching take plane, at least in part, in the manufacture of the composites. The experimental data show that changes in the gradient of the cyclic voltammograms coincide with large changes in microwave reflectivity consistent with increasing conductivity of the composite when fields are applied. The reverse change occurs when the fields are removed. Measurements of the switching speed have shown that the composites are able to switch between the different states at in times of less than a second for more than one million switching operations with no depreciation of the material. Large area films have also been studied in the front of waveguide devices and measured in a microwave transmission mode. The results show that large changes in microwave impedance occur with the application of small electric fields (~ 15 V cm-1).

  17. Cyclic voltammetry in solutions of aluminum bromide and KBr in aromatic hydrocarbons; II: the behavior of Pb and Sn

    SciTech Connect

    Elam, M.; Gileadi, E.

    1983-03-01

    The electrochemical behavior of dilute solutions of SnBr/sub 2/ and PbBr/sub 2/ in a nonpolar solvent system consisting of solutions of 1.0M Al/sub 2/Br/sub 6/ and 0.80M KBr in ethylbenzene was studied. Cyclic voltammograms show well defined peaks for the deposition and dissolution of the divalent metal. Oxidation to the tetravalent state could not be detected in the available potential region. The diffusion coefficients were 1.1 X 10/sup -6/ cm/sup 2//sec for lead and 2.7 X 10/sup -6/ cm/sup 2//sec for tin. Lead ions inhibit the electrodeposition of aluminum while tin ions seem to have little or no effect. An overpotentia associated with initial nucleation on a platinum electrode is observed for both metals and electrodeposition does not star until /eta/ reaches a value of about 30-40 mV. Formation of a thermodynamically unstable Al/Pb alloy at sufficiently cathodic potentials in solutions containing PbBr/sub 2/ is indicated.

  18. A comparative study of CO adsorption on tetrahexahedral Pt nanocrystals and interrelated Pt single crystal electrodes by using cyclic voltammetry and in situ FTIR spectroscopy.

    PubMed

    Liu, Hai-Xia; Tian, Na; Ye, Jin-Yu; Lu, Bang-An; Ren, Jie; Huangfu, Zhi-Chao; Zhou, Zhi-You; Sun, Shi-Gang

    2014-01-01

    This study focuses on CO adsorption at tetrahexahedral Pt nanocrystals (THH Pt NCs) by using cyclic voltammetry and in situ FTIR spectroscopy. Since the electrochemically prepared THH Pt NCs in this study are enclosed by {730} facets which could be considered by a subfacet configuration of 2{210} + {310}, we have also studied CO adsorption on the interrelated Pt(310) and Pt(210) single crystal electrodes as a comparison. Cyclic voltammetry results demonstrated that CO adsorbs dominantly on the (100) sites of THH Pt NCs at low CO coverage (θ(CO)≤ 0.135), while on both (100) and (110) sites at higher CO coverage. On ordered Pt(310) and Pt(210), i.e. they were flame annealed and then cooled in H(2) + Ar, CO adsorption also illustrates relative priority on (100) sites at low CO coverage; while at high CO coverage or on oxygen-disordered Pt(310) and Pt(210) when they were cooled in air after flame annealing, the adsorption of CO presents a weak preference on (100) sites of Pt(310) and even no preference at all on (100) sites of Pt(210). In situ FTIR spectroscopic studies illustrated that CO adsorption on THH Pt NCs yields anomalous infrared effects (AIREs), which are depicted by the Fano-like IR feature on a dense distribution (60 μm(-2)) and the enhancement of abnormal IR absorption on a sparse distribution (22 μm(-2)) of THH Pt NCs on glassy carbon substrate. Systematic investigation of CO coverage dependence of IR features revealed that, on THH Pt NCs, the IR band center (ν(COL)) of linearly bonded CO (COL) is rapidly shifted to higher wavenumbers along with the increase of CO coverage to 0.184, yielding a fast linear increase rate with a high slope (dν(COL)/dθ(IR)(CO) = 219 cm(-1)); when θ > 0.184, the increase of ν(COL) with θCO slows down and deviates drastically from linearity. In contrast, the ν(COL) on the ordered Pt(310) electrode maintains a linear increase with θ(IR)(CO) for the whole range of θ(IR)(CO) variation, and gives a much smaller

  19. Measurement of nanomolar dopamine diffusion using low-noise perfluorinated ionomer coated carbon fiber microelectrodes and high-speed cyclic voltammetry.

    PubMed

    Rice, M E; Nicholson, C

    1989-09-01

    Several improvements in the fabrication and use of carbon fiber voltammetric microelectrodes (CFVMs) are described. These procedures did not involve oxidative treatment, but resulted in sensitivities and selectivities approaching those of treated CFVMs, without the inherent slow response times associated with the latter electrodes. To accomplish this we reduced CFVM noise by (1) improving the adhesive seal between the 8 microns o.d. carbon fiber and the glass insulation using vacuum, (2) snapping rather than cutting or beveling the fiber to be flush with the glass, and (3) using a concentrated electrolyte solution to make electrical contact with the fiber. System noise was reduced by digital smoothing and signal averaging. Selectivity of the CFVMs for dopamine over ascorbate was enhanced to better than 2000:1 by coating with Naflon, a perfluorinated cation exchange polymer, using a low (+0.5 V vs Ag/AgCl) electroplating potential. This low voltage also prevented electrode surface oxidation. To demonstrate the performance of our CFVMs, we used them in conjunction with high-speed cyclic voltammetry to accurately measure the diffusion coefficient of iontophoretically released dopamine at concentrations as low as 35 nM over distances of less than 200 microns in agarose gel. PMID:2802146

  20. Pulse Voltammetry.

    ERIC Educational Resources Information Center

    Osteryoung, Janet

    1983-01-01

    Discusses the nature of pulse voltammetry, indicating that its widespread use arises from good sensitivity and detection limits and from ease of application and low cost. Provides analytical and mechanistic applications of the procedure. (JN)

  1. Separation of Intrinsic and Electrostrictive Volume Effects in Redox Reaction Volumes of Metal Complexes Measured Using High-Pressure Cyclic Staircase Voltammetry.

    PubMed

    Sachinidis, John I.; Shalders, Richard D.; Tregloan, Peter A.

    1996-04-24

    Redox reaction volumes, obtained by high-pressure cyclic voltammetry, are reported for a selection tris(diimine), tris(diamine), hexaammine, and hexaaqua couples of Fe(III/II), Cr(III/II), Ru(III/II), and Co(III/II). Separation of the intrinsic and electrostrictive volume contributions for these couples has been achieved, some in both aqueous and acetonitrile solutions. For the Co(phen)(3)(3+/2+) system, the intrinsic volume change is estimated to be +15.3 +/- 2.1 cm(3) mol(-)(1) (based on measurements in water) and +16.5 +/- 2.0 cm(3) mol(-)(1) (in acetonitrile). For the Co(bipy)(3)(3+/2+) system, values are +12.7 +/- 1.4 cm(3) mol(-)(1) (in water) and +15.5 +/- 2.5 cm(3) mol(-)(1) (in acetonitrile). Using these experimentally determined intrinsic contributions, a simple structural model suggests that the intrinsic volume change for these reactions can be described using the change in effective volume of a sphere with radius close to that of the coordinating-atom-metal bond length. Electrostrictive volume changes for the 3+/2+ complex-ion couples are a function of solute size and coordinated ligands. For Ru(H(2)O)(6)(3+) and Fe(H(2)O)(6)(3+) reduction, volume behavior is significantly different from that of the other systems studied and can be rationalized in terms of possible H-bonding interactions with surrounding solvent which affect the electrostrictive volume changes but which are not available for the ammine and other complexes studied. PMID:11666462

  2. Insight into the template effect of vesicles on the laccase-catalyzed oligomerization of N-phenyl-1,4-phenylenediamine from Raman spectroscopy and cyclic voltammetry measurements

    PubMed Central

    Ležaić, Aleksandra Janoševic; Luginbühl, Sandra; Bajuk-Bogdanović, Danica; Pašti, Igor; Kissner, Reinhard; Rakvin, Boris; Walde, Peter; Ćirić-Marjanović, Gordana

    2016-01-01

    We report about the first Raman spectroscopy study of a vesicle-assisted enzyme-catalyzed oligomerization reaction. The aniline dimer N-phenyl-1,4-phenylenediamine (= p-aminodiphenylamine, PADPA) was oxidized and oligomerized with Trametes versicolor laccase and dissolved O2 in the presence of sodium bis(2-ethylhexyl)sulfosuccinate (AOT) vesicles (80–100 nm diameter) as templates. The conversion of PADPA into oligomeric products, poly(PADPA), was monitored during the reaction by in situ Raman spectroscopy. The results obtained are compared with UV/vis/NIR and EPR measurements. All three complementary methods indicate that at least some of the poly(PADPA) products, formed in the presence of AOT vesicles, resemble the conductive emeraldine salt form of polyaniline (PANI-ES). The Raman measurements also show that structural units different from those of “ordinary” PANI-ES are present too. Without vesicles PANI-ES-like products are not obtained. For the first time, the as-prepared stable poly(PADPA)-AOT vesicle suspension was used directly to coat electrodes (without product isolation) for investigating redox activities of poly(PADPA) by cyclic voltammetry (CV). CV showed that poly(PADPA) produced with vesicles is redox active not only at pH 1.1–as expected for PANI-ES–but also at pH 6.0, unlike PANI-ES and poly(PADPA) synthesized without vesicles. This extended pH range of the redox activity of poly(PADPA) is important for applications. PMID:27561552

  3. Insight into the template effect of vesicles on the laccase-catalyzed oligomerization of N-phenyl-1,4-phenylenediamine from Raman spectroscopy and cyclic voltammetry measurements.

    PubMed

    Ležaić, Aleksandra Janoševic; Luginbühl, Sandra; Bajuk-Bogdanović, Danica; Pašti, Igor; Kissner, Reinhard; Rakvin, Boris; Walde, Peter; Ćirić-Marjanović, Gordana

    2016-01-01

    We report about the first Raman spectroscopy study of a vesicle-assisted enzyme-catalyzed oligomerization reaction. The aniline dimer N-phenyl-1,4-phenylenediamine (= p-aminodiphenylamine, PADPA) was oxidized and oligomerized with Trametes versicolor laccase and dissolved O2 in the presence of sodium bis(2-ethylhexyl)sulfosuccinate (AOT) vesicles (80-100 nm diameter) as templates. The conversion of PADPA into oligomeric products, poly(PADPA), was monitored during the reaction by in situ Raman spectroscopy. The results obtained are compared with UV/vis/NIR and EPR measurements. All three complementary methods indicate that at least some of the poly(PADPA) products, formed in the presence of AOT vesicles, resemble the conductive emeraldine salt form of polyaniline (PANI-ES). The Raman measurements also show that structural units different from those of "ordinary" PANI-ES are present too. Without vesicles PANI-ES-like products are not obtained. For the first time, the as-prepared stable poly(PADPA)-AOT vesicle suspension was used directly to coat electrodes (without product isolation) for investigating redox activities of poly(PADPA) by cyclic voltammetry (CV). CV showed that poly(PADPA) produced with vesicles is redox active not only at pH 1.1-as expected for PANI-ES-but also at pH 6.0, unlike PANI-ES and poly(PADPA) synthesized without vesicles. This extended pH range of the redox activity of poly(PADPA) is important for applications. PMID:27561552

  4. Determination of the relative contribution of quercetin and its glucosides to the antioxidant capacity of onion by cyclic voltammetry and spectrophotometric methods.

    PubMed

    Zielinska, Danuta; Wiczkowski, Wieslaw; Piskula, Mariusz Konrad

    2008-05-28

    This paper describes the use of cyclic voltammetry (CV), spectrophotometric methods [Trolox equivalent antioxidant capacity (TEAC), peroxyl radical trapping capacity (PRTC), DPPH radical scavenging activity (RSA), and Folin-Ciocalteu reagent (FCR) reducing capacity], and photochemiluminescence (PCL) for the measurement of the antioxidant capacity of onion var. Sochaczewska and var. Szalotka. The antioxidant and reducing activity of the dominant onion flavonoids quercetin (Q), quercetin-3- O-beta-glucoside (Q3G), quercetin-4'- O-beta-glucoside (Q4'G), and quercetin-3,4'-di- O-beta-glucoside (Q3,4'G) were determined by spectrophotometric (TEAC and PRTC) and CV methods, respectively. The contribution of quercetin and its glucosides to the antioxidant capacity of onion was calculated in consequence of the qualitative and quantitative analysis of onion flavonoids by high-performance liquid chromatography-ultraviolet-mass spectrometry. The dominant forms of quercetin in the onion var. Sochaczewska and Szalotka included Q4'G (61 and 54%), Q3,4'G (37 and 44%), Q3G (1.4 and 1.1%), and free quercetin (1.1 and 0.7%), respectively. The CV experiment showed the highest reducing activity of Q while Q3G, Q4'G, and Q3,4'G exhibited about 68, 51, and 30% of the reducing power noted for Q. The order of the reducing activity of onion flavonoids was confirmed by their free radical scavenging activity and evaluated by TEAC and PRTC assays as follows: Q > Q3G > Q4'G > Q3,4'G. The Q4'G and Q3,4'G showed poor antioxidant activity under both applied spectrophotometric assays but still exhibited reducing activity based on CV experiments. The reducing capacity of onions determined by CV method was twice higher than the antioxidant capacity formed by water-soluble compounds (ACW) evaluated by PCL, and it was about 50% higher than PRTC and DPPH RSA results and the converted FCR reducing capacity. In contrast, the reducing capacity of onions determined by the CV method was 3-fold and about four

  5. AFM and TEM study of cyclic slip localization in fatigued ferritic X10CrAl24 stainless steel

    SciTech Connect

    Man, J. . E-mail: man@ipm.cz; Petrenec, M.; Obrtlik, K.; Polak, J.

    2004-11-08

    Atomic force microscopy and high resolution scanning electron microscopy were applied to the study of surface relief evolution at emerging persistent slip bands (PSBs) in individual grains of ferritic X10CrAl24 stainless steel cycled with constant plastic strain amplitude. Only the combination of both methods can reveal the true shape and fine details of extrusions and intrusions. Quantitative data on the changes of the surface topography of persistent slip markings and on the kinetics of extrusion growth during the fatigue life were obtained. Transmission electron microscopy of surface foils revealed PSBs with the typical, well-known ladder structure. Experimental data on cyclic slip localization in PSBs are compared with those in fcc metals and discussed in terms of vacancy models of surface relief evolution and fatigue crack initiation.

  6. Fabrication of cone-shaped boron doped diamond and gold nanoelectrodes for AFM-SECM.

    PubMed

    Avdic, A; Lugstein, A; Wu, M; Gollas, B; Pobelov, I; Wandlowski, T; Leonhardt, K; Denuault, G; Bertagnolli, E

    2011-04-01

    We demonstrate a reliable microfabrication process for a combined atomic force microscopy (AFM) and scanning electrochemical microscopy (SECM) measurement tool. Integrated cone-shaped sensors with boron doped diamond (BDD) or gold (Au) electrodes were fabricated from commercially available AFM probes. The sensor formation process is based on mature semiconductor processing techniques, including focused ion beam (FIB) machining, and highly selective reactive ion etching (RIE). The fabrication approach preserves the geometry of the original AFM tips resulting in well reproducible nanoscaled sensors. The feasibility and functionality of the fully featured tips are demonstrated by cyclic voltammetry, showing good agreement between the measured and calculated currents of the cone-shaped AFM-SECM electrodes. PMID:21368355

  7. Fabrication of cone-shaped boron doped diamond and gold nanoelectrodes for AFM-SECM

    NASA Astrophysics Data System (ADS)

    Avdic, A.; Lugstein, A.; Wu, M.; Gollas, B.; Pobelov, I.; Wandlowski, T.; Leonhardt, K.; Denuault, G.; Bertagnolli, E.

    2011-04-01

    We demonstrate a reliable microfabrication process for a combined atomic force microscopy (AFM) and scanning electrochemical microscopy (SECM) measurement tool. Integrated cone-shaped sensors with boron doped diamond (BDD) or gold (Au) electrodes were fabricated from commercially available AFM probes. The sensor formation process is based on mature semiconductor processing techniques, including focused ion beam (FIB) machining, and highly selective reactive ion etching (RIE). The fabrication approach preserves the geometry of the original AFM tips resulting in well reproducible nanoscaled sensors. The feasibility and functionality of the fully featured tips are demonstrated by cyclic voltammetry, showing good agreement between the measured and calculated currents of the cone-shaped AFM-SECM electrodes.

  8. Stripping Voltammetry

    NASA Astrophysics Data System (ADS)

    Lovrić, Milivoj

    Electrochemical stripping means the oxidative or reductive removal of atoms, ions, or compounds from an electrode surface (or from the electrode body, as in the case of liquid mercury electrodes with dissolved metals) [1-5]. In general, these atoms, ions, or compounds have been preliminarily immobilized on the surface of an inert electrode (or within it) as the result of a preconcentration step, while the products of the electrochemical stripping will dissolve in the electrolytic solution. Often the product of the electrochemical stripping is identical to the analyte before the preconcentration. However, there are exemptions to these rules. Electroanalytical stripping methods comprise two steps: first, the accumulation of a dissolved analyte onto, or in, the working electrode, and, second, the subsequent stripping of the accumulated substance by a voltammetric [3, 5], potentiometric [6, 7], or coulometric [8] technique. In stripping voltammetry, the condition is that there are two independent linear relationships: the first one between the activity of accumulated substance and the concentration of analyte in the sample, and the second between the maximum stripping current and the accumulated substance activity. Hence, a cumulative linear relationship between the maximum response and the analyte concentration exists. However, the electrode capacity for the analyte accumulation is limited and the condition of linearity is satisfied only well below the electrode saturation. For this reason, stripping voltammetry is used mainly in trace analysis. The limit of detection depends on the factor of proportionality between the activity of the accumulated substance and the bulk concentration of the analyte. This factor is a constant in the case of a chemical accumulation, but for electrochemical accumulation it depends on the electrode potential. The factor of proportionality between the maximum stripping current and the analyte concentration is rarely known exactly. In fact

  9. Estimation of key physical properties for LaCl3 in molten eutectic LiCl-KCl by fitting cyclic voltammetry data to a BET-based electrode reaction kinetics model

    NASA Astrophysics Data System (ADS)

    Samin, Adib; Wang, Zhonghang; Lahti, Erik; Simpson, Michael; Zhang, Jinsuo

    2016-07-01

    Understanding the electrochemical properties of rare earth elements is important for developing efficient techniques for separating rare earth elements from actinides recovered during the electrodeposition process. In this study the cyclic voltammetry for lanthanum in molten LiClKCl eutectic was recorded at 773 K for different scan rates and different bulk concentrations. A model accounting for mass transport, kinetics and adsorption was applied to analyze the experimental data via performing a nonlinear least squares fit. The results of the simulation are compared against the results of a conventional analysis of the cyclic voltammograms and against the existing literature. At the scan rates used, the reduction/oxidation process is quasi-reversible. The values of diffusivities derived from simulation were larger than the ones derived commonly using equations for diffusion-limited processes. However, those equations were derived based on an assumption of reversibility. This simulation-based approach may provide a more accurate option for analyzing systems that do not exhibit reversibility.

  10. Application of fast-scan cyclic voltammetry for the in vivo characterization of optically evoked dopamine in the olfactory tubercle of the rat brain.

    PubMed

    Wakabayashi, Ken T; Bruno, Michael J; Bass, Caroline E; Park, Jinwoo

    2016-06-21

    The olfactory tubercle (OT), as a component of the ventral striatum, serves as an important multisensory integration center for reward-related processes in the brain. Recent studies show that dense dopaminergic innervation from the ventral tegmental area (VTA) into the OT may play an outsized role in disorders such as psychostimulant addiction and disorders of motivation, increasing recent scientific interest in this brain region. However, due to its anatomical inaccessibility, relative small size, and proximity to other dopamine-rich structures, neurochemical assessments using conventional methods cannot be readily employed. Here, we investigated dopamine (DA) regulation in the OT of urethane-anesthetized rats using in vivo fast-scan voltammetry (FSCV) coupled with carbon-fiber microelectrodes, following optogenetic stimulation of the VTA. The results were compared with DA regulation in the nucleus accumbens (NAc), a structure located adjacent to the OT and which also receives dense DA innervation from the VTA. FSCV coupled with optically evoked release allowed us to investigate the spatial distribution of DA in the OT and characterize OT DA dynamics (release and clearance) with subsecond temporal and micrometer spatial resolution for the first time. In this study, we demonstrated that DA transporters play an important role in regulating DA in the OT. However, the control of extracellular DA by uptake in the OT was less than in the NAc. The difference in DA transmission in the terminal fields of the OT and NAc may be involved in region-specific responses to drugs of abuse and contrasting roles in mediating reward-related behavior. PMID:27063845

  11. Use of cyclic current reversal polarization voltammetry for investigating the relationship between corrosion resistance and heat-treatment induced variations in microstructures of 400 C martensitic stainless steels

    NASA Technical Reports Server (NTRS)

    Ambrose, John R.

    1992-01-01

    Software for running a cyclic current reversal polarization voltammagram has been developed for use with a EG&G Princeton Applied Research Model 273 potentiostat/galvanostat system. The program, which controls the magnitude, direction and duration of an impressed galvanostatic current, will produce data in ASCII spreadsheets (Lotus, Quattro) for graphical representation of CCRPV voltammograms. The program was used to determine differences in corrosion resistance of 440 C martenstic stainless steel produced as a result of changes in microstructure effected by tempering. It was determined that tempering at all temperatures above 400 F resulted in increased polarizability of the material, with the increased likelihood that pitting would be initiated upon exposure to marine environments. These results will be used in development of remedial procedures for lowering the susceptibility of these alloys toward the stress corrosion cracking experienced in bearings used in high pressure oxygen turbopumps used in the main engines of space shuttle orbiters.

  12. Design and fabrication of a low-cost flow-through cell for the determination of acetaminophen in pharmaceutical formulations by flow injection cyclic voltammetry.

    PubMed

    Masawat, Prinya; Liawruangrath, Saisunee; Vaneesorn, Yuthsak; Liawruangrath, Boonsom

    2002-12-01

    A low-cost electrochemical flow-through cell is designed and fabricated to use in conjunction with a flow injection (FI) system. This detector cell used a centrosymmetric radial flow thin-layer geometry with a stainless steel auxiliary electrode and a reference electrode (Ag/AgCl) without a salt bridge. The 5H pencil lead electrode used as a working electrode in the home-made cell is an extremely inexpensive electrode which performs as well as the expensive commercial glassy carbon electrode. Optimum conditions for determining acetaminophen using the proposed FI manifold was investigated. Appropriate volume of sample and/or standard solution containing acetaminophen in pH 2.2 Mcllvaine buffer solution was injected into the proposed FI system and mixed with the flowing stream of supporting electrolyte (pH 2.2 Mcllvaine buffer solution) at an optimum flow rate of 1 mlmin(-1). The cyclic voltammograms were recorded over the potential range from -0.5 to +2.0 V with a scan rate of 40 mVs(-1). Linear calibration curve over the range of 0.1-5 mM acetaminophen was established with the regression equation Y=3.68X+1.0157 (r(2)=0.9964). The recommended method has been applied to the determination of acetaminophen in 8 commercial pharmaceutical preparations. The percentage recoveries of the spiked acetaminophen in four tablet samples were ranging from 103 to 112 with the relative standard deviation in the range of 0.1-1.3%. PMID:18968860

  13. New group 6 metal carbonyl complexes with 4,5-dimethyl-N,N-bis(pyridine-2-yl-methylene)benzene-1,2-diimine Schiff base: synthesis, spectral, cyclic voltammetry and biological activity studies.

    PubMed

    Mohamed, Rania G; Elantabli, Fatma M; Helal, Nadia H; El-Medani, Samir M

    2015-04-15

    Thermal reaction of M(CO)6 (M=Cr, Mo or W) with a Schiff base (DMPA) derived from the condensation of 4,5-dimethyl-1,2-phenylenediamine and pyridine-2-carboxaldehyde in THF in absence and presence of a secondary ligand; 2-aminobenzimidazole (Abz), thiourea (Tu) or 2-(2'-pyridyl)benzimidazole (pybz) were studied. The reaction of Cr(CO)6 gave the four complexes Cr2(CO)2(DMPA)2; 1, Cr(DMPA)2(Abz)2; 2, Cr2(CO)4(DMPA)2(Tu)2; 3 and Cr(DMPA)2(Pybz); 4, while the thermal reaction of Mo(CO)6 resulted in the formation of the two complexes Mo2(O)6(DMPA)2; 5, and Mo2(O)2(CO)2(DMPA)2(Tu)2; 6. Thermal reaction of W(CO)6 and the Schiff base DMPA gave the complex W(O)2(DMPA)2; 7. The ligand DMPA and its metal complexes have been reported and characterized based on elemental analyses, IR, (1)H NMR, magnetic measurements, and thermal analysis. Cyclic voltammetry and biological activity were also investigated. PMID:25670089

  14. Ionic, XRD, dielectric and cyclic voltammetry studies on PVdF-co-HFP / MMT clay intercalated LiN(C2F5SO2)2 based composite electrolyte for Li-ion batteries

    NASA Astrophysics Data System (ADS)

    Vickraman, P.; Purushothaman, K.; SankaraSubramanian, N.

    2014-04-01

    The composition dependence of plasticizer, (EC/DMC)(70-x(wt%)) and LiBETIx(wt%) salt for fixed contents on PVdF-co-HFP(25wt%)/surface modified(SM)-octadecylamine MMT(ODA-MMT) nanoclay(5wt%) host matrix by varying its compositions x=1.5, 3.0, 4.5, 6.0 wt% prepared via solution casting technique has been investigated by A.C. Impedance, Dielectric, XRD, and cyclic voltammetry(CV) studies. The enhanced conductivity 2.1×10-5 S/cm at 300C is observed for (EC/DMC)(70-6)wt%/LiBETI(x=6)wt%. The XRD at 2θ=20.9° confirms β-phase formation, and CV studies on membranes show cyclability and reversibility. The dielectric studies show increase in dielectric constant and dielectric loss with decrease in frequency is attributed to high contribution of charge accumulation at the electrode-electrolyte interface.

  15. New group 6 metal carbonyl complexes with 4,5-dimethyl-N,N-bis(pyridine-2-yl-methylene)benzene-1,2-diimine Schiff base: Synthesis, spectral, cyclic voltammetry and biological activity studies

    NASA Astrophysics Data System (ADS)

    Mohamed, Rania G.; Elantabli, Fatma M.; Helal, Nadia H.; El-Medani, Samir M.

    2015-04-01

    Thermal reaction of M(CO)6 (M = Cr, Mo or W) with a Schiff base (DMPA) derived from the condensation of 4,5-dimethyl-1,2-phenylenediamine and pyridine-2-carboxaldehyde in THF in absence and presence of a secondary ligand; 2-aminobenzimidazole (Abz), thiourea (Tu) or 2-(2‧-pyridyl)benzimidazole (pybz) were studied. The reaction of Cr(CO)6 gave the four complexes Cr2(CO)2(DMPA)2; 1, Cr(DMPA)2(Abz)2; 2, Cr2(CO)4(DMPA)2(Tu)2; 3 and Cr(DMPA)2(Pybz); 4, while the thermal reaction of Mo(CO)6 resulted in the formation of the two complexes Mo2(O)6(DMPA)2; 5, and Mo2(O)2(CO)2(DMPA)2(Tu)2; 6. Thermal reaction of W(CO)6 and the Schiff base DMPA gave the complex W(O)2(DMPA)2; 7. The ligand DMPA and its metal complexes have been reported and characterized based on elemental analyses, IR, 1H NMR, magnetic measurements, and thermal analysis. Cyclic voltammetry and biological activity were also investigated.

  16. Recent Advances in Voltammetry.

    PubMed

    Batchelor-McAuley, Christopher; Kätelhön, Enno; Barnes, Edward O; Compton, Richard G; Laborda, Eduardo; Molina, Angela

    2015-06-01

    Recent progress in the theory and practice of voltammetry is surveyed and evaluated. The transformation over the last decade of the level of modelling and simulation of experiments has realised major advances such that electrochemical techniques can be fully developed and applied to real chemical problems of distinct complexity. This review focuses on the topic areas of: multistep electrochemical processes, voltammetry in ionic liquids, the development and interpretation of theories of electron transfer (Butler-Volmer and Marcus-Hush), advances in voltammetric pulse techniques, stochastic random walk models of diffusion, the influence of migration under conditions of low support, voltammetry at rough and porous electrodes, and nanoparticle electrochemistry. The review of the latter field encompasses both the study of nanoparticle-modified electrodes, including stripping voltammetry and the new technique of 'nano-impacts'. PMID:26246984

  17. Recent Advances in Voltammetry

    PubMed Central

    Batchelor-McAuley, Christopher; Kätelhön, Enno; Barnes, Edward O; Compton, Richard G; Laborda, Eduardo; Molina, Angela

    2015-01-01

    Recent progress in the theory and practice of voltammetry is surveyed and evaluated. The transformation over the last decade of the level of modelling and simulation of experiments has realised major advances such that electrochemical techniques can be fully developed and applied to real chemical problems of distinct complexity. This review focuses on the topic areas of: multistep electrochemical processes, voltammetry in ionic liquids, the development and interpretation of theories of electron transfer (Butler–Volmer and Marcus–Hush), advances in voltammetric pulse techniques, stochastic random walk models of diffusion, the influence of migration under conditions of low support, voltammetry at rough and porous electrodes, and nanoparticle electrochemistry. The review of the latter field encompasses both the study of nanoparticle-modified electrodes, including stripping voltammetry and the new technique of ‘nano-impacts’. PMID:26246984

  18. Stripping Voltammetry of Pb and Cu using a Microcantilever Electrode

    SciTech Connect

    Bange, Adam; Brown, Gilbert M; Senesac, Larry R; Thundat, Thomas George

    2009-01-01

    Microfabricated silicon microcantilevers coated with gold on one side have been used as working electrode in a three-electrode electrochemical arrangement. In addition to electrochemical current, cantilever bending has been used as a signal for monitoring electrode reactions on the cantilever surface. The microcantilever bending was measured by an optical beam deflection method as the surface potential was scanned and electrochemical reactions occurred on the surface. The microcantilever bending due to differential surface stress was used to sense Pb and Cu using cyclic voltammetry (CV) and linear sweep stripping voltammetry (LSSV).

  19. Determination of secnidazole in urine by adsorptive stripping voltammetry.

    PubMed

    Radi, A E; Hassanein, A

    2000-05-01

    Cyclic voltammetry was used to explore the adsorption behavior of secnidazole on a hanging mercury drop electrode (HMDE). The effects of various operational parameters on the accumulation behavior of the adsorbed species were tested. Thus, a sensitive stripping voltammetry procedure for the determination of secnidazole with an adsorptive accumulation on the surface of HMDE has been developed. Measurements were taken by differential-pulse voltammetry after determination of the optimum conditions. The linear concentration range was 1 x 10(-8)-1 x 10(-7) s when using a 120 s preconcentration at -0.1 V vs. Ag/AgCl in acetate buffer of pH 4.0. The detection limit of secnidazole was 5 x 10(-9) M. The precision, expressed by the coefficient of variation, was 2.5% (n = 10) at a concentration of 1 x 10(-7) m. The method was successfully applied to the analysis of secnidazole in urine. PMID:10823692

  20. Qplus AFM driven nanostencil.

    PubMed

    Grévin, B; Fakir, M; Hayton, J; Brun, M; Demadrille, R; Faure-Vincent, J

    2011-06-01

    We describe the development of a novel setup, in which large stencils with suspended silicon nitride membranes are combined with atomic force microscopy (AFM) regulation by using tuning forks. This system offers the possibility to perform separate AFM and nanostencil operations, as well as combined modes when using stencil chips with integrated tips. The flexibility and performances are demonstrated through a series of examples, including wide AFM scans in closed loop mode, probe positioning repeatability of a few tens of nanometer, simultaneous evaporation of large (several hundred of micron square) and nanoscopic metals and fullerene patterns in static, multistep, and dynamic modes. This approach paves the way for further developments, as it fully combines the advantages of conventional stenciling with the ones of an AFM driven shadow mask. PMID:21721701

  1. Differential thermal voltammetry for tracking of degradation in lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Wu, Billy; Yufit, Vladimir; Merla, Yu; Martinez-Botas, Ricardo F.; Brandon, Nigel P.; Offer, Gregory J.

    2015-01-01

    Monitoring of lithium-ion batteries is of critical importance in electric vehicle applications in order to manage the operational condition of the cells. Measurements on a vehicle often involve current, voltage and temperature which enable in-situ diagnostic techniques. This paper presents a novel diagnostic technique, termed differential thermal voltammetry, which is capable of monitoring the state of the battery using voltage and temperature measurements in galvanostatic operating modes. This tracks battery degradation through phase transitions, and the resulting entropic heat, occurring in the electrodes. Experiments to monitor battery degradation using the new technique are compared with a pseudo-2D cell model. Results show that the differential thermal voltammetry technique provides information comparable to that of slow rate cyclic voltammetry at shorter timescale and with load conditions easier to replicate in a vehicle.

  2. Anodic Stripping Voltammetry: An Instrumental Analysis Experiment.

    ERIC Educational Resources Information Center

    Wang, Joseph

    1983-01-01

    Describes an experiment designed to acquaint students with the theory and applications of anodic stripping voltammetry (ASV) as well as such ASV problems as contamination associated with trace analysis. The experimental procedure, instrumentation, and materials discussed are designed to minimize cost and keep procedures as simple as possible. (JM)

  3. PREFACE: Non-contact AFM Non-contact AFM

    NASA Astrophysics Data System (ADS)

    Giessibl, Franz J.; Morita, Seizo

    2012-02-01

    This special issue is focussed on high resolution non-contact atomic force microscopy (AFM). Non-contact atomic force microscopy was established approximately 15 years ago as a tool to image conducting and insulating surfaces with atomic resolution. Since 1998, an annual international conference has taken place, and although the proceedings of these conferences are a useful source of information, several key developments warrant devoting a special issue to this subject. In the theoretic field, the possibility of supplementing established techniques such as scanning tunneling microscopy (STM) and Kelvin probe microscopy with atomically resolved force micrsoscopy poses many challenges in the calculation of contrast and contrast reversal. The surface science of insulators, self-assembled monolayers and adsorbates on insulators is a fruitful field for the application of non-contact AFM: several articles in this issue are devoted to these subjects. Atomic imaging and manipulation have been pioneered using STM, but because AFM allows the measurement of forces, AFM has had a profound impact in this field as well. Three-dimensional force spectroscopy has allowed many important insights into surface science. In this issue a combined 3D tunneling and force microscopy is introduced. Non-contact AFM typically uses frequency modulation to measure force gradients and was initially used mainly in a vacuum. As can be seen in this issue, frequency modulation is now also used in ambient conditions, allowing better spatial and force resolution. We thank all of the contributors for their time and efforts in making this special issue possible. We are also very grateful to the staff of IOP Publishing for handling the administrative aspects and for steering the refereeing process. Non-contact AFM contents Relation between the chemical force and the tunnelling current in atomic point contacts: a simple model Pavel Jelínek, Martin Ondrácek and Fernando Flores Theoretical simulation of

  4. Experimental aspects of solid-state voltammetry

    SciTech Connect

    Wooster, T.T.; Longmire, M.L.; Zhang, H.

    1992-05-15

    This paper describes the properties of poly(ether) polymer electrolytes as solvent media for solid-state voltammetry. Experimental requirements for microelectrode voltammetry and results for the dependency of diffusive transport of electroactive solutes on polymer solvent molecular weight, structure, and temperature (and related phase state) are described for eight poly(ether)s: linear poly(ethylene oxides) MW = 400, 1000, 2000, and 600 000 (Me{sub 2}PEG-400, Me{sub 2}PEG-1000, Me{sub 2}PEG-2000, PEO-600 000), linear poly(propylene oxide) MW = 4000 (PPO-4000), the comb polymer poly(bis[(methoxyethoxy)ethoxy]phosphazine) (MEEP), the block copolymer poly(ether)-poly(urethane urea)(PEUU), and the cross-linked poly(ether) network PEO. 28 refs., 10 figs., 1 tab.

  5. Determination of Bosentan in Pharmaceutical Preparations by Linear Sweep, Square Wave and Differential Pulse Voltammetry Methods

    PubMed Central

    Atila, Alptug; Yilmaz, Bilal

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation. PMID:25901151

  6. Voltammetry as a Model for Teaching Chemical Instrumentation.

    ERIC Educational Resources Information Center

    Gunasingham, H.; Ang, K. P.

    1985-01-01

    Voltammetry is used as a model for teaching chemical instrumentation to chemistry undergraduates at the National University of Singapore. Lists six criteria used to select a successful teaching model and shows how voltammetry satisfies each criterion. (JN)

  7. Voltammetry at the Thin-Film Mercury Electrode (TFME).

    ERIC Educational Resources Information Center

    Pomeroy, R. S.; And Others

    1989-01-01

    Reviewed is the use of the Thin-Film Mercury Electrode for anodic stripping voltammetry, simple voltammetry of solution cations and cathodic stripping voltammetry for the determination of an environmentally important molecule, thiourea. The construction of a simple potentiostat and applications for student laboratory courses are included. (CW)

  8. Electrochemistry in Media of Exceptionally Low Polarity: Voltammetry with a Fluorous Solvent.

    PubMed

    Olson, Eric J; Boswell, Paul G; Givot, Bradley L; Yao, Letitia J; Bühlmann, Philippe

    2010-02-15

    This work demonstrates the first cyclic voltammetry in a perfluorocarbon solvent without use of a cosolvent. The novel electrolyte tetrabutylammonium tetrakis[3,5-bis(perfluorohexyl)phenyl]borate (NBu(4)BArF(104); 80 mM) allows for voltammetry of ferrocene in perfluoro(methylcyclohexane) by lowering the specific resistance to Ω268 k cm at 20.8 °C. Despite significant solution resistance, the resulting voltammograms can be fitted quantitatively without difficulty. The thus determined standard electron transfer rate constant, k°, for the oxidation of ferrocene in perfluoro(methylcyclohexane) is somewhat smaller than for many solvents commonly used in electrochemistry, but can be explained readily as the result of the viscosity and size of the solvent using Marcus theory. Dielectric dispersion spectroscopy verifies that addition of NBu(4)BArF(104) does not significantly raise the overall polarity of the solution over that of neat perfluoro(methylcyclohexane). PMID:20212920

  9. Voltammetric detection of glutathione: an adsorptive stripping voltammetry approach.

    PubMed

    Areias, Madalena C C; Shimizu, Kenichi; Compton, Richard G

    2016-05-10

    A simple, sensitive, and rapid detection of glutathione by cyclic voltammetry using a bare glassy carbon electrode is reported in which glutathione forms a 1 : 1 complex compound with copper(ii) ions. This complex compound is adsorbed onto the electrode surface and undergoes electrochemical oxidation at a characteristic oxidation potential of ca. -0.20 V vs. the standard mercury/mercurous sulphate reference electrode, which is used to detect the glutathione concentration. The linear dynamic range is obtained for a glutathione concentration from 1 μM to 12.5 μM, and the sensitivity is found to be 0.1 ± 0.002 μA μM(-1). A low limit of detection (n = 3) of 0.14 μM and a precision of 1.8% are achieved using a simple, unmodified electrode. The robustness of the present methodology is demonstrated by the successful quantitative analysis of glutathione in the presence of cysteine. PMID:27074944

  10. Voltammetry of redox analytes at trace concentrations with nanoelectrode ensembles.

    PubMed

    Moretto, Ligia Maria; Pepe, Niki; Ugo, Paolo

    2004-04-19

    Gold nanoelectrodes ensembles (NEEs) have been prepared by electroless plating of Au nanoelectrode elements within the pores of a microporous polycarbonate template membrane. Cyclic voltammograms recorded in (ferrocenylmethyl) trimethylammonium hexafluorophosphate (FA(+) PF(6)(-)) solutions showed that these NEEs operate in the "total-overlap" response regime, giving well resolved peak shaped voltammograms. Experimental results show that the faradaic/background currents ratios at the NEE are independent on the total geometric area of the ensemble, so that NEE can be enlarged or miniaturized at pleasure without influencing the very favorable signal/noise ratio. Differential pulse voltammetry (DPV) at the NEE is optimized for direct determinations at trace levels. DPV at NEE allowed the determination (with no preconcentration) of trace amounts of FA(+), with a detection limit of 0.02muM. The use of NEE and DPV in cytochrome c (cyt c) solutions showed the possibility to observe the direct electrochemistry of submicromolar concentration of the protein, even without the need of adding any promoter or mediator. PMID:18969398

  11. AFM study of the effects of laser surface remelting on the morphology of Al-Fe aerospace alloys

    SciTech Connect

    Pariona, Moises Meza; Teleginski, Viviane; Santos, Kelly dos; Leandro Ribeiro dos Santos, Everton; Aparecida de Oliveira Camargo de Lima, Angela; Riva, Rudimar

    2012-12-15

    Laser beam welding has recently been incorporated into the fabrication process of aircraft and automobile structures. Surface roughness is an important parameter of product quality that strongly affects the performance of mechanical parts, as well as production costs. This parameter influences the mechanical properties such as fatigue behavior, corrosion resistance, creep life, etc., and other functional characteristics such as friction, wear, light reflection, heat transmission, lubrification, electrical conductivity, etc. The effects of laser surface remelting (LSR) on the morphology of Al-Fe aerospace alloys were examined before and after surface treatments, using optical microscopy (OM), scanning electron microscopy (SEM), low-angle X-ray diffraction (LA-XRD), atomic force microscopy (AFM), microhardness measurements (Vickers hardness), and cyclic voltammetry. This analysis was performed on both laser-treated and untreated sanded surfaces, revealing significant differences. The LA-XRD analysis revealed the presence of alumina, simple metals and metastable intermetallic phases, which considerably improved the microhardness of laser-remelted surfaces. The morphology produced by laser surface remelting enhanced the microstructure of the Al-Fe alloys by reducing their roughness and increasing their hardness. The treated surfaces showed passivity and stability characteristics in the electrolytic medium employed in this study. - Highlights: Black-Right-Pointing-Pointer The samples laser-treated and untreated showed significant differences. Black-Right-Pointing-Pointer The La-XRD revealed the presence of alumina in Al-1.5 wt.% Fe. Black-Right-Pointing-Pointer The laser-treated reducing the roughness and increasing the hardness. Black-Right-Pointing-Pointer The laser-treated surfaces showed characteristic passive in the electrolytic medium. Black-Right-Pointing-Pointer The laser-treated is a promising technique for applications technological.

  12. Bismuth electrodes, an alternative in stripping voltammetry

    NASA Astrophysics Data System (ADS)

    Barón-Jaimez, J.; Joya, M. R.; Barba-Ortega, J.

    2013-11-01

    The heavy metals are known as highly toxic contaminants, the processes carried out in industry contribute that finally they remain dispersed in effluents and sewage, doing part of the food chain. The importance of controlling the levels of these heavy metals has become an international policy, so it has generated interest in developing new analytical methodologies for its determination [1, 2, 3, 4]. The stripping voltammetry has been considered as a family of electro-sensitive analytical techniques useful for the determination of trace levels of many metals in environmental, clinical and industrial samples [3, 4]. This work presents an overview of these bismuth-based electrodes which were introduced around 2000, which have interesting characteristics for detection of heavy metals and which represent an alternative to mercury electrodes.

  13. Toward an in situ phosphate sensor in seawater using Square Wave Voltammetry.

    PubMed

    Barus, C; Romanytsia, I; Striebig, N; Garçon, V

    2016-11-01

    A Square Wave Voltammetry electrochemical method is proposed to measure phosphate in seawater as pulse techniques offer a higher sensitivity as compared to classical cyclic voltammetry. Chronoamperometry cannot be either adapted for an in situ sensor since this method requires to have controlled convection which will be impossible in a miniaturised sensor. Tests and validation of Square Wave Voltammetry parameters have been performed using an open cell and for the first time with a small volume (<400µL) laboratory prototypes. Two designs of prototypes have been compared. Using high frequency (f=250Hz) allows to obtain a linear behaviour between 0.1 and 1µmolL(-1) with a very low limit of detection of 0.05 µmolL(-1) after 60min of complexation waiting time. In order to obtain a linear regression for a larger concentration range i.e. 0.25-4µmolL(-1), a lower frequency of 2.5Hz is needed. A limit of detection of 0.1µmolL(-1) is obtained in this case after 30min of complexation waiting time for the peak measured at E=0.12V. Changing the position of the molybdenum electrode for the complexation step and moving the detection into another electrochemical cell allow to decrease the reaction time down to 5min. PMID:27591632

  14. Microbial Biofilm Voltammetry: Direct Electrochemical Characterization of Catalytic Electrode-Attached Biofilms▿ †

    PubMed Central

    Marsili, Enrico; Rollefson, Janet B.; Baron, Daniel B.; Hozalski, Raymond M.; Bond, Daniel R.

    2008-01-01

    While electrochemical characterization of enzymes immobilized on electrodes has become common, there is still a need for reliable quantitative methods for study of electron transfer between living cells and conductive surfaces. This work describes growth of thin (<20 μm) Geobacter sulfurreducens biofilms on polished glassy carbon electrodes, using stirred three-electrode anaerobic bioreactors controlled by potentiostats and nondestructive voltammetry techniques for characterization of viable biofilms. Routine in vivo analysis of electron transfer between bacterial cells and electrodes was performed, providing insight into the main redox-active species participating in electron transfer to electrodes. At low scan rates, cyclic voltammetry revealed catalytic electron transfer between cells and the electrode, similar to what has been observed for pure enzymes attached to electrodes under continuous turnover conditions. Differential pulse voltammetry and electrochemical impedance spectroscopy also revealed features that were consistent with electron transfer being mediated by an adsorbed catalyst. Multiple redox-active species were detected, revealing complexity at the outer surfaces of this bacterium. These techniques provide the basis for cataloging quantifiable, defined electron transfer phenotypes as a function of potential, electrode material, growth phase, and culture conditions and provide a framework for comparisons with other species or communities. PMID:18849456

  15. Cyclic multiverses

    NASA Astrophysics Data System (ADS)

    Marosek, Konrad; Da¸browski, Mariusz P.; Balcerzak, Adam

    2016-09-01

    Using the idea of regularization of singularities due to the variability of the fundamental constants in cosmology we study the cyclic universe models. We find two models of oscillating and non-singular mass density and pressure (`non-singular' bounce) regularized by varying gravitational constant G despite the scale factor evolution is oscillating and having sharp turning points (`singular' bounce). Both violating (big-bang) and non-violating (phantom) null energy condition models appear. Then, we extend this idea on to the multiverse containing cyclic individual universes with either growing or decreasing entropy though leaving the net entropy constant. In order to get an insight into the key idea, we consider the doubleverse with the same geometrical evolution of the two `parallel' universes with their physical evolution [physical coupling constants c(t) and G(t)] being different. An interesting point is that there is a possibility to exchange the universes at the point of maximum expansion - the fact which was already noticed in quantum cosmology. Similar scenario is also possible within the framework of Brans-Dicke theory where varying G(t) is replaced by the dynamical Brans-Dicke field φ(t) though these theories are slightly different.

  16. Single ricin detection by AFM chemomechanical mapping

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This research reports a method of detecting ricin molecules immobilized on chemically modified gold (Au;111) surface by chemomechanically mapping the molecular interactions with a chemically modified Atomic Force Microscope (AFM) tip. AFM images resolved the different fold-up conformations of single...

  17. ezAFM: A low cost Atomic Force Microscope(AFM)

    NASA Astrophysics Data System (ADS)

    Celik, Umit; Celik, Kubra; Aslan, Husnu; Kehribar, Ihsan; Dede, Munir; Ozgur Ozer, H.; Oral, Ahmet

    2012-02-01

    A low cost AFM, ezAFM is developed for educational purposes as well as research. Optical beam deflection method is used to measure the deflection of cantilever. ezAFM scanner is built using voice coil motors (VCM) with ˜50x50x6 μm scan area. The microscope uses alignment free cantilevers, which minimizes setup times. FPGA based AFM feedback Control electronics is developed. FPGA technology allows us to drive all peripherals in parallel. ezAFM Controller is connected to PC by USB 2.0 interface as well as Wi-Fi. We have achieved <5nm lateral and ˜0.01nm vertical resolution. ezAFM can image single atomic steps in HOPG and mica. An optical microscope with <3 μm resolution is also integrated into the system. ezAFM supports different AFM operation modes such as dynamic mode, contact mode, lateral force microscopy. Advanced modes like magnetic force microscopy and electric force microscopy will be implemented later on. The new ezAFM system provides, short learning times for student labs, quick setup and easy to transport for portable applications with the best price/performance ratio. The cost of the system starts from 15,000, with system performance comparable with the traditional AFM systems.

  18. Discrimination of Inner- and Outer-Sphere Electrode Reactions by Cyclic Voltammetry Experiments

    ERIC Educational Resources Information Center

    Tanimoto, Sachiko; Ichimura, Akio

    2013-01-01

    A laboratory experiment for undergraduate students who are studying homogeneous and heterogeneous electron-transfer reactions is described. Heterogeneous or electrode reaction kinetics can be examined by using the electrochemical reduction of three Fe[superscript III]/Fe[superscript II] redox couples at platinum and glassy carbon disk electrodes.…

  19. A Simple and Inexpensive Function Generator and a Four-Electrode Cell for Cyclic Voltammetry.

    ERIC Educational Resources Information Center

    Albahadily, F. N.; Mottola, Horacio A.

    1986-01-01

    Describes construction and operation of an inexpensive signal generator and a four-electrode electrochemical cell for use in voltammetric experiments. Also describes construction and operation of a four-electrode electrochemical cell used to illustrate elimination (or minimization) of background currents due to electrochemical reactions by species…

  20. The Effect of Complex Formation upon the Redox Potentials of Metallic Ions. Cyclic Voltammetry Experiments.

    ERIC Educational Resources Information Center

    Ibanez, Jorge G.; And Others

    1988-01-01

    Describes experiments in which students prepare in situ soluble complexes of metal ions with different ligands and observe and estimate the change in formal potential that the ion undergoes upon complexation. Discusses student formation and analysis of soluble complexes of two different metal ions with the same ligand. (CW)

  1. Controlled Iontophoresis Coupled with Fast-Scan Cyclic Voltammetry/Electrophysiology in Awake, Freely Moving Animals

    PubMed Central

    2013-01-01

    Simultaneous electrochemical and electrophysiological data were recorded to evaluate the effects of controlled local application of dopaminergic agonists and antagonists in awake rats. Measurements were made with a probe consisting of a carbon-fiber microelectrode fused to three iontophoretic barrels used to introduce the drugs of interest. The probe and the manipulator used to position it in the brain of behaving animals were optimized to improve their performance. The effect of the dopamine autoreceptor on electrically stimulated release was demonstrated. Dopamine inhibited the release of endogenous dopamine whereas raclopride, a D2 antagonist, enhanced it, with similar responses in anesthetized and awake animals. We also examined changes in the firing rate of nucleus accumbens (NAc) neurons in awake animals during and after brief (15 s) iontophoretic ejections of SCH 23390 (D1 receptor antagonist) or raclopride. Changes in response to these antagonists were seen both immediately and on a prolonged time scale. Application of raclopride increased the firing rate in 40% of medium spiny neurons (MSNs), of which half responded immediately. Decreases in firing rate were observed in 46% of MSNs after SCH 23390 application. Only 11% of MSNs responded to both antagonists and one MSN (3%) showed no response to either drug. The same prolonged response in firing rate was seen for electrically stimulated and locally applied dopamine in 75% of MSNs. These results are in agreement with previously reported distributions for dopamine receptor subtypes on MSNs and probe the effects of dopamine on these cell populations. PMID:23480099

  2. Nano Mechanical Machining Using AFM Probe

    NASA Astrophysics Data System (ADS)

    Mostofa, Md. Golam

    Complex miniaturized components with high form accuracy will play key roles in the future development of many products, as they provide portability, disposability, lower material consumption in production, low power consumption during operation, lower sample requirements for testing, and higher heat transfer due to their very high surface-to-volume ratio. Given the high market demand for such micro and nano featured components, different manufacturing methods have been developed for their fabrication. Some of the common technologies in micro/nano fabrication are photolithography, electron beam lithography, X-ray lithography and other semiconductor processing techniques. Although these methods are capable of fabricating micro/nano structures with a resolution of less than a few nanometers, some of the shortcomings associated with these methods, such as high production costs for customized products, limited material choices, necessitate the development of other fabricating techniques. Micro/nano mechanical machining, such an atomic force microscope (AFM) probe based nano fabrication, has, therefore, been used to overcome some the major restrictions of the traditional processes. This technique removes material from the workpiece by engaging micro/nano size cutting tool (i.e. AFM probe) and is applicable on a wider range of materials compared to the photolithographic process. In spite of the unique benefits of nano mechanical machining, there are also some challenges with this technique, since the scale is reduced, such as size effects, burr formations, chip adhesions, fragility of tools and tool wear. Moreover, AFM based machining does not have any rotational movement, which makes fabrication of 3D features more difficult. Thus, vibration-assisted machining is introduced into AFM probe based nano mechanical machining to overcome the limitations associated with the conventional AFM probe based scratching method. Vibration-assisted machining reduced the cutting forces

  3. Stoichiometry and Formation Constant Determination by Linear Sweep Voltammetry.

    ERIC Educational Resources Information Center

    Schultz, Franklin A.

    1979-01-01

    In this paper an experiment is described in which the equilibrium constants necessary for determining the composition and distribution of lead (II)-oxalate species may be measured by linear sweep voltammetry. (Author/BB)

  4. Ultrafast Electron Diffractive Voltammetry:. General Formalism and Applications

    NASA Astrophysics Data System (ADS)

    Chang, Kiseok; Murdick, Ryan A.; Tao, Zhen-Sheng; Han, Tzong-Ru T.; Ruan, Chong-Yu

    We present a general formalism of ultrafast diffractive voltammetry approach as a contact-free tool to investigate the ultrafast surface charge dynamics in nanostructured interfaces. As case studies, the photoinduced surface charging processes in oxidized silicon surface and the hot electron dynamics in nanoparticle-decorated interface are examined based on the diffractive voltammetry framework. We identify that the charge redistribution processes appear on the surface, sub-surface, and vacuum levels when driven by intense femtosecond laser pulses. To elucidate the voltammetry contribution from different sources, we perform controlled experiments using shadow imaging techniques and N-particle simulations to aid the investigation of the photovoltage dynamics in the presence of photoemission. We show that voltammetry contribution associated with photoemission has a long decay tail and plays a more significant role in the nanosecond timescale, whereas the ultrafast voltammetry are dominated by local charge transfer, such as surface charging and molecular charge transport at nanostructured interfaces. We also discuss the general applicability of the diffractive voltammetry as an integral part of quantitative ultrafast electron diffraction methodology in researching different types of interfaces having distinctive surface diffraction and boundary conditions.

  5. Electrochemical characterization of gelatinized starch dispersions: voltammetry and electrochemical impedance spectroscopy on platinum surface.

    PubMed

    Hernandez-Jaimes, C; Lobato-Calleros, C; Sosa, E; Bello-Pérez, L A; Vernon-Carter, E J; Alvarez-Ramirez, J

    2015-06-25

    The electrochemical properties of gelatinized starch dispersions (GSD; 5% w/w) from different botanical sources were studied using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) tests over a platinum surface. The phenomenological modelling of EIS data using equivalent circuits indicated that after gelatinization the electrical resistance was determined mainly by the resistance of insoluble material (i.e., ghosts). Sonication of the GSD disrupted the ghost microstructure, and produced an increase in electrical conductivity by reducing the resistance of the insoluble material. The CV data showed three oxidation peaks at potentials where glucose solutions displayed oxidation waves. It is postulated that hydrolysis at the bulk and electrocatalyzed oxidation on the Pt-surface are reactions involved in the starch transformation. Starches peak intensity increased with the amylose content, suggesting that the amylose-rich matrix played an important role in the charge transfer in the electrolytic system. PMID:25839788

  6. Square wave voltammetry with multivariate calibration tools for determination of eugenol, carvacrol and thymol in honey.

    PubMed

    Tonello, Natalia; Moressi, Marcela Beatriz; Robledo, Sebastián Noel; D'Eramo, Fabiana; Marioli, Juan Miguel

    2016-09-01

    The simultaneous determination of eugenol (EU), thymol (Ty) and carvacrol (CA) in honey samples, employing square wave voltammetry (SWV) and chemometrics tools, is informed for the first time. For this purpose, a glassy carbon electrode (GCE) was used as working electrode. The operating conditions and influencing parameters (involving several chemical and instrumental parameters) were first optimized by cyclic voltammetry (CV). Thus, the effects of the scan rate, pH and analyte concentration on the electrochemical response of the above mentioned molecules were studied. The results show that the electrochemical responses of the three compounds are very similar and that the voltammetric traces present a high degree of overlap under all the experimental conditions used in this study. Therefore, two chemometric tools were tested to obtain the multivariate calibration model. One method was the partial least squares regression (PLS-1), which assumes a linear behaviour. The other nonlinear method was an artificial neural network (ANN). In this last case we used a supervised, feed-forward network with Levenberg-Marquardt back propagation training. From the accuracies and precisions analysis between nominal and estimated concentrations calculated by using both methods, it was inferred that the ANN method was a good model to quantify EU, Ty and CA in honey samples. Recovery percentages were between 87% and 104%, except for two samples whose values were 136% and 72%. The analytical methodology was simple, fast and accurate. PMID:27343610

  7. Hydration states of AFm cement phases

    SciTech Connect

    Baquerizo, Luis G.; Matschei, Thomas; Scrivener, Karen L.; Saeidpour, Mahsa; Wadsö, Lars

    2015-07-15

    The AFm phase, one of the main products formed during the hydration of Portland and calcium aluminate cement based systems, belongs to the layered double hydrate (LDH) family having positively charged layers and water plus charge-balancing anions in the interlayer. It is known that these phases present different hydration states (i.e. varying water content) depending on the relative humidity (RH), temperature and anion type, which might be linked to volume changes (swelling and shrinkage). Unfortunately the stability conditions of these phases are insufficiently reported. This paper presents novel experimental results on the different hydration states of the most important AFm phases: monocarboaluminate, hemicarboaluminate, strätlingite, hydroxy-AFm and monosulfoaluminate, and the thermodynamic properties associated with changes in their water content during absorption/desorption. This data opens the possibility to model the response of cementitious systems during drying and wetting and to engineer systems more resistant to harsh external conditions.

  8. AFM indentation study of breast cancer cells

    SciTech Connect

    Li, Q.S.; Lee, G.Y.H.; Ong, C.N.; Lim, C.T.

    2008-10-03

    Mechanical properties of individual living cells are known to be closely related to the health and function of the human body. Here, atomic force microscopy (AFM) indentation using a micro-sized spherical probe was carried out to characterize the elasticity of benign (MCF-10A) and cancerous (MCF-7) human breast epithelial cells. AFM imaging and confocal fluorescence imaging were also used to investigate their corresponding sub-membrane cytoskeletal structures. Malignant (MCF-7) breast cells were found to have an apparent Young's modulus significantly lower (1.4-1.8 times) than that of their non-malignant (MCF-10A) counterparts at physiological temperature (37 deg. C), and their apparent Young's modulus increase with loading rate. Both confocal and AFM images showed a significant difference in the organization of their sub-membrane actin structures which directly contribute to their difference in cell elasticity. This change may have facilitated easy migration and invasion of malignant cells during metastasis.

  9. Conductance of AFM Deformed Carbon Nanotubes

    NASA Technical Reports Server (NTRS)

    Svizhenko, Alexei; Maiti, Amitesh; Anatram, M. P.; Biegel, Bryan (Technical Monitor)

    2002-01-01

    This viewgraph presentation provides information on the electrical conductivity of carbon nanotubes upon deformation by atomic force microscopy (AFM). The density of states and conductance were computed using four orbital tight-binding method with various parameterizations. Different chiralities develop bandgap that varies with chirality.

  10. Contact nanomechanical measurements with the AFM

    NASA Astrophysics Data System (ADS)

    Geisse, Nicholas

    2013-03-01

    The atomic force microscope (AFM) has found broad use in the biological sciences largely due to its ability to make measurements on unfixed and unstained samples under liquid. In addition to imaging at multiple spatial scales ranging from micro- to nanometer, AFMs are commonly used as nanomechanical probes. This is pertinent for cell biology, as it has been demonstrated that the geometrical and mechanical properties of the extracellular microenvironment are important in such processes as cancer, cardiovascular disease, muscular dystrophy, and even the control of cell life and death. Indeed, the ability to control and quantify these external geometrical and mechanical parameters arises as a key issue in the field. Because AFM can quantitatively measure the mechanical properties of various biological samples, novel insights to cell function and to cell-substrate interactions are now possible. As the application of AFM to these types of problems is widened, it is important to understand the performance envelope of the technique and its associated data analyses. This talk will discuss the important issues that must be considered when mechanical models are applied to real-world data. Examples of the effect of different model assumptions on our understanding of the measured material properties will be shown. Furthermore, specific examples of the importance of mechanical stimuli and the micromechanical environment to the structure and function of biological materials will be presented.

  11. A Batch Fabricated SECM-AFM Probe

    NASA Astrophysics Data System (ADS)

    Dobson, P. S.; Macpherson, J. V.; Holder, M.; Weaver, J. M. R.

    2003-12-01

    A scheme for the fabrication of combined Scanning Electrochemical Microscopy — Atomic Force Microscopy (SECM-AFM) probes is presented for both silicon nitride and silicon cantilevers. The advantages over exsisting methods used for their production is explained. The process flow is described and initial results from electrodeposition of silver are presented.

  12. Square wave voltammetry at the dropping mercury electrode: Experimental

    USGS Publications Warehouse

    Turner, J.A.; Christie, J.H.; Vukovic, M.; Osteryoung, R.A.

    1977-01-01

    Experimental verification of earlier theoretical work for square wave voltammetry at the dropping mercury electrode is given. Experiments using ferric oxalate and cadmium(II) in HCl confirm excellent agreement with theory. Experimental peak heights and peak widths are found to be within 2% of calculated results. An example of trace analysis using square wave voltammetry at the DME is presented. The technique is shown to have the same order of sensitivity as differential pulse polarography but is much faster to perform. A detection limit for cadmium in 0.1 M HCl for the system used here was 7 ?? 10-8 M.

  13. Plant Cyclic Nucleotide Signalling

    PubMed Central

    Martinez-Atienza, Juliana; Van Ingelgem, Carl; Roef, Luc

    2007-01-01

    The presence of the cyclic nucleotides 3′,5′-cyclic adenyl monophosphate (cAMP) and 3′,5′-cyclic guanyl monophosphate (cGMP) in plants is now generally accepted. In addition, cAMP and cGMP have been implicated in the regulation of important plant processes such as stomatal functioning, monovalent and divalent cation fluxes, chloroplast development, gibberellic acid signalling, pathogen response and gene transcription. However, very little is known regarding the components of cyclic nucleotide signalling in plants. In this addendum, the evidence for specific mechanisms of plant cyclic nucleotide signalling is evaluated and discussed. PMID:19704553

  14. Square wave voltammetry at the dropping mercury electrode: Theory

    USGS Publications Warehouse

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

    1977-01-01

    The theoretical aspects of square wave voltammetry at the dropping mercury electrode are presented. The technique involves scanning the entire potential range of interest on a single drop of a DME. Asymmetries in the waveform as well as variations in current measurement parameters are discussed. Indications are that previous uses of the waveform may not have utilized all its capabilities.

  15. Detection of Pathogens Using AFM and SPR

    NASA Astrophysics Data System (ADS)

    Vaseashta, Ashok

    2005-03-01

    A priori detection of pathogens in food and water has become a subject of paramount importance. Several recent incidents have resulted in the government passing stringent regulations for tolerable amounts of contamination of food products. Identification and/or monitoring of bacterial contamination in food are critical. The conventional methods of pathogen detection require time-consuming steps to arrive disembark at meaningful measurement in a timely manner as the detection time exceeds the time in which perishable food recycles through the food chain distribution. The aim of this presentation is to outline surface plasmon resonance (SPR) and atomic force microscopy (AFM) as two methods for fast detect6ion of pathogens. Theoretical basis of SPR and experimental results of SPR and AFM on E. coli O157:H7 and prion are presented.

  16. Characterizing Cell Mechanics with AFM and Microfluidics

    NASA Astrophysics Data System (ADS)

    Walter, N.; Micoulet, A.; Suresh, S.; Spatz, J. P.

    2007-03-01

    Cell mechanical properties and functionality are mainly determined by the cytoskeleton, besides the cell membrane, the nucleus and the cytosol, and depend on various parameters e.g. surface chemistry and rigidity, surface area and time available for cell spreading, nutrients and drugs provided in the culture medium. Human epithelial pancreatic and mammary cancer cells and their keratin intermediate filaments are the main focus of our work. We use Atomic Force Microscopy (AFM) to study cells adhering to substrates and Microfluidic Channels to probe cells in suspension, respectively. Local and global properties are extracted by varying AFM probe tip size and the available adhesion area for cells. Depth-sensing, instrumented indentation tests with AFM show a clear difference in contact stiffness for cells that are spread of controlled substrates and those that are loosely attached. Microfluidic Channels are utilized in parallel to evaluate cell deformation and ``flow resistance'', which are dependent on channel cross section, flow rate, cell nucleus size and the mechanical properties of cytoskeleton and membrane. The results from the study are used to provide some broad and quantitative assessments of the connections between cellular/subcellular mechanics and biochemical origins of disease states.

  17. Saddle-Shaped Cyclic Indole Tetramers: 3D Electroactive Molecules.

    PubMed

    Ruiz, Constanza; Monge, Ángeles; Gutiérrez-Puebla, Enrique; Alkorta, Ibon; Elguero, José; Navarrete, Juan T López; Ruiz Delgado, M Carmen; Gómez-Lor, Berta

    2016-07-18

    We present a joint theoretical and experimental study of a series of cyclic indole tetramers aimed at understanding the fundamental electronic properties of this 3D platform and evaluating its potential in the construction of new semiconductors. To this end, we combined absorption and Raman spectroscopy, cyclic voltammetry, and spectroelectrochemistry with DFT calculations. Our results suggest that this platform can be easily and reversibly oxidized. Additionally, it has a HOMO that matches very well with the workfunction of gold, therefore charge injection from a gold electrode is expected to occur without significant barriers. Interestingly, the cyclic tetraindoles allow for good electron delocalization in spite of their saddle-shaped structures. The steric constraints introduced by N-substitution significantly inhibits ring inversion of the central cyclooctatetraene unit, whereas it only barely affects the optical and electrochemical properties (a slightly higher oxidation potential and a blueshifted absorption upon alkylation are observed). PMID:27320301

  18. Application of thin-shielded mercury microelectrodes in anodic stripping voltammetry.

    PubMed

    Daniele, Salvatore; Bragato, Carlo; Baldo, M Antonietta; Ciani, Ilenia

    2008-10-19

    The performance in anodic stripping voltammetry (ASV) of hemispherical mercury microelectrodes, fabricated by electrodeposition of liquid mercury on the surface of Pt microdisks which were surrounded by a rather thick or thin insulating shield, was compared. The Pt microdisks were produced by sealing a wire of 25 microm diameter into a glass capillary, and by coating the cylindrical length of the Pt wire with a cathodic electrophoretic paint. The ratio of the overall tip radius b, to the basal radius of the electrode a, so-called RG=b/a, was equal to 110+/-10 and 1.52+/-0.01 for the thick- and thin-shielded microdisk, respectively. The mercury microelectrodes were characterized by cyclic voltammetry at 1 mVs(-1), in 1mM Ru(NH(3))(6)(3+) aqueous solution. The steady-state voltammogram recorded with the thin-shielded mercury microelectrode displayed less hysteresis, while the steady-state current was about 30% higher than that of the thicker one. This was a consequence of the additional flux due to diffusion from behind the plane of the electrode. The flux enhancement, which was operative at the thin-shielded mercury microelectrode during the deposition step in the ASV experiments, allowed recording stripping peaks for Cd and Pb, which resulted about 32% larger than those recorded at the thicker shielded mercury microelectrode, under same experimental conditions. The usefulness of the thin-shielded mercury microelectrode for ASV measurements in real samples was verified by determining the content of heavy metal ions released in the pore water (pH 4.5) of a soil slurry. PMID:18804626

  19. Cyclic phosphonium ionic liquids

    PubMed Central

    Mukhlall, Joshua A; Romeo, Alicia R; Gohdo, Masao; Ramati, Sharon; Berman, Marc; Suarez, Sophia N

    2014-01-01

    Summary Ionic liquids (ILs) incorporating cyclic phosphonium cations are a novel category of materials. We report here on the synthesis and characterization of four new cyclic phosphonium bis(trifluoromethylsulfonyl)amide ILs with aliphatic and aromatic pendant groups. In addition to the syntheses of these novel materials, we report on a comparison of their properties with their ammonium congeners. These exemplars are slightly less conductive and have slightly smaller self-diffusion coefficients than their cyclic ammonium congeners. PMID:24605146

  20. BOREAS AFM-6 Surface Meteorological Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from the National Oceanic and Atmospheric Adminsitration/Environment Technology Laboratory (NOAA/ETL) collected surface meteorological data from 21 May to 20 Sep 1994 near the Southern Study Area-Old Jack Pine (SSA-OJP) tower site. The data are in tabular ASCII files. The surface meteorological data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  1. Are Math Grades Cyclical?

    ERIC Educational Resources Information Center

    Adams, Gerald J.; Dial, Micah

    1998-01-01

    The cyclical nature of mathematics grades was studied for a cohort of elementary school students from a large metropolitan school district in Texas over six years (average cohort size of 8495). The study used an autoregressive integrated moving average (ARIMA) model. Results indicate that grades do exhibit a significant cyclical pattern. (SLD)

  2. Genetics Home Reference: cyclic neutropenia

    MedlinePlus

    ... Understand Genetics Home Health Conditions cyclic neutropenia cyclic neutropenia Enable Javascript to view the expand/collapse boxes. Download PDF Open All Close All Description Cyclic neutropenia is a disorder that causes frequent infections and ...

  3. [AFM fishing of proteins under impulse electric field].

    PubMed

    Ivanov, Yu D; Pleshakova, T O; Malsagova, K A; Kaysheva, A L; Kopylov, A T; Izotov, A A; Tatur, V Yu; Vesnin, S G; Ivanova, N D; Ziborov, V S; Archakov, A I

    2016-05-01

    A combination of (atomic force microscopy)-based fishing (AFM-fishing) and mass spectrometry allows to capture protein molecules from solutions, concentrate and visualize them on an atomically flat surface of the AFM chip and identify by subsequent mass spectrometric analysis. In order to increase the AFM-fishing efficiency we have applied pulsed voltage with the rise time of the front of about 1 ns to the AFM chip. The AFM-chip was made using a conductive material, highly oriented pyrolytic graphite (HOPG). The increased efficiency of AFM-fishing has been demonstrated using detection of cytochrome b5 protein. Selection of the stimulating pulse with a rise time of 1 ns, corresponding to the GHz frequency range, by the effect of intrinsic emission from water observed in this frequency range during water injection into the cell. PMID:27562998

  4. BOREAS AFM-06 Mean Temperature Profile Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from the National Oceanic and Atmospheric Adminsitration/Environment Technology Laboratory (NOAA/ETL) operated a 915-MHz wind/Radio Acoustic Sounding System (RASS) profiler system in the Southern Study Area (SSA) near the Old Jack Pine (OJP) tower from 21 May 1994 to 20 Sep 1994. The data set provides temperature profiles at 15 heights, containing the variables of virtual temperature, vertical velocity, the speed of sound, and w-bar. The data are stored in tabular ASCII files. The mean temperature profile data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  5. BOREAS AFM-6 Boundary Layer Height Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from National Oceanic and Atmospheric Adminsitration/Environment Technology Laboratory (NOAA/ETL) operated a 915-MHz wind/Radio Acoustic Sounding System (RASS) profiler system in the Southern Study Area (SSA) near the Old Jack Pine (OJP) site. This data set provides boundary layer height information over the site. The data were collected from 21 May 1994 to 20 Sep 1994 and are stored in tabular ASCII files. The boundary layer height data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  6. BOREAS AFM-06 Mean Wind Profile Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from the National Oceanic and Atmospheric Administration/Environment Technology Laboratory (NOAA/ETL) operated a 915-MHz wind/Radio Acoustic Sounding System (RASS) profiler system in the Southern Study Area (SSA) near the Old Jack Pine (OJP) tower from 21 May 1994 to 20 Sep 1994. The data set provides wind profiles at 38 heights, containing the variables of wind speed; wind direction; and the u-, v-, and w-components of the total wind. The data are stored in tabular ASCII files. The mean wind profile data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  7. Plasmonic-based Imaging of Local Square Wave Voltammetry

    PubMed Central

    Shan, Xiaonan; Wang, Shaopeng; Wang, Wei; Tao, Nongjian

    2012-01-01

    Square wave voltammetry (SWV) is widely used in electrochemical analysis and sensors because of its high sensitivity and efficient rejection of background current, but SWV by conventional electrochemical detection method does not provide spatial resolution. We report here a plasmonic method to image local SWV, which opens the door for analyzing heterogeneous electrochemical reactions and for high throughput detections of microarrays. We describe the basic principle, validate the principle by comparing the plasmonic-based SWV with those obtained with the conventional method, and demonstrate imaging capability for local electrochemical analysis. PMID:21793508

  8. Cyclic control stick

    DOEpatents

    Whitaker, Charles N.; Zimmermann, Richard E.

    1989-01-01

    A cyclic control stick of the type used in helicopters for reducing the safety hazards associated with such a mechanism in the event of a crewman being thrown violently into contact with the cyclic control stick resulting from a crash or the like. The cyclic control stick is configured to break away upon the exertion of an impact force which exceeds a predetermined value and/or is exerted for more than a momentary time duration. The cyclic control stick is also configured to be adjustable so as to locate the grip thereof as far away from the crewman as possible for safety reasons without comprising the comfort of the crewman or the use of the control stick, and a crushable pad is provided on the top of the grip for impact energy absorbing purposes.

  9. Determination of oleuropein using multiwalled carbon nanotube modified glassy carbon electrode by adsorptive stripping square wave voltammetry.

    PubMed

    Cittan, Mustafa; Koçak, Süleyman; Çelik, Ali; Dost, Kenan

    2016-10-01

    A multi-walled carbon nanotube modified glassy carbon electrode was used to prepare an electrochemical sensing platform for the determination of oleuropein. Results showed that, the accumulation of oleuropein on the prepared electrode takes place with the adsorption process. Electrochemical behavior of oleuropein was studied by using cyclic voltammetry. Compared to the bare GCE, the oxidation peak current of oleuropein increased about 340 times at MWCNT/GCE. Voltammetric determination of oleuropein on the surface of prepared electrode was studied using square wave voltammetry where the oxidation peak current of oleuropein was measured as an analytical signal. A calibration curve of oleuropein was performed between 0.01 and 0.70µM and a good linearity was obtained with a correlation coefficient of 0.9984. Detection and quantification limits of the method were obtained as 2.73 and 9.09nM, respectively. In addition, intra-day and inter-day precision studies indicated that the voltammetric method was sufficiently repeatable. Finally, the proposed electrochemical sensor was successfully applied to the determination of oleuropein in an olive leaf extract. Microwave-assisted extraction of oleuropein had good recovery values between 92% and 98%. The results obtained with the proposed electrochemical sensor were compared with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. PMID:27474292

  10. Cyclic steps on ice

    NASA Astrophysics Data System (ADS)

    Yokokawa, M.; Izumi, N.; Naito, K.; Parker, G.; Yamada, T.; Greve, R.

    2016-05-01

    Boundary waves often form at the interface between ice and fluid flowing adjacent to it, such as ripples under river ice covers, and steps on the bed of supraglacial meltwater channels. They may also be formed by wind, such as the megadunes on the Antarctic ice sheet. Spiral troughs on the polar ice caps of Mars have been interpreted to be cyclic steps formed by katabatic wind blowing over ice. Cyclic steps are relatives of upstream-migrating antidunes. Cyclic step formation on ice is not only a mechanical but also a thermodynamic process. There have been very few studies on the formation of either cyclic steps or upstream-migrating antidunes on ice. In this study, we performed flume experiments to reproduce cyclic steps on ice by flowing water, and found that trains of steps form when the Froude number is larger than unity. The features of those steps allow them to be identified as ice-bed analogs of cyclic steps in alluvial and bedrock rivers. We performed a linear stability analysis and obtained a physical explanation of the formation of upstream-migrating antidunes, i.e., precursors of cyclic steps. We compared the results of experiments with the predictions of the analysis and found the observed steps fall in the range where the analysis predicts interfacial instability. We also found that short antidune-like undulations formed as a precursor to the appearance of well-defined steps. This fact suggests that such antidune-like undulations correspond to the instability predicted by the analysis and are precursors of cyclic steps.

  11. Cyclic polymers from alkynes.

    PubMed

    Roland, Christopher D; Li, Hong; Abboud, Khalil A; Wagener, Kenneth B; Veige, Adam S

    2016-08-01

    Cyclic polymers have dramatically different physical properties compared with those of their equivalent linear counterparts. However, the exploration of cyclic polymers is limited because of the inherent challenges associated with their synthesis. Conjugated linear polyacetylenes are important materials for electrical conductivity, paramagnetic susceptibility, optical nonlinearity, photoconductivity, gas permeability, liquid crystallinity and chain helicity. However, their cyclic analogues are unknown, and therefore the ability to examine how a cyclic topology influences their properties is currently not possible. We have solved this challenge and now report a tungsten catalyst supported by a tetraanionic pincer ligand that can rapidly polymerize alkynes to form conjugated macrocycles in high yield. The catalyst works by tethering the ends of the polymer to the metal centre to overcome the inherent entropic penalty of cyclization. Gel-permeation chromatography, dynamic and static light scattering, viscometry and chemical tests are all consistent with theoretical predictions and provide unambiguous confirmation of a cyclic topology. Access to a wide variety of new cyclic polymers is now possible by simply choosing the appropriate alkyne monomer. PMID:27442285

  12. Cyclic polymers from alkynes

    NASA Astrophysics Data System (ADS)

    Roland, Christopher D.; Li, Hong; Abboud, Khalil A.; Wagener, Kenneth B.; Veige, Adam S.

    2016-08-01

    Cyclic polymers have dramatically different physical properties compared with those of their equivalent linear counterparts. However, the exploration of cyclic polymers is limited because of the inherent challenges associated with their synthesis. Conjugated linear polyacetylenes are important materials for electrical conductivity, paramagnetic susceptibility, optical nonlinearity, photoconductivity, gas permeability, liquid crystallinity and chain helicity. However, their cyclic analogues are unknown, and therefore the ability to examine how a cyclic topology influences their properties is currently not possible. We have solved this challenge and now report a tungsten catalyst supported by a tetraanionic pincer ligand that can rapidly polymerize alkynes to form conjugated macrocycles in high yield. The catalyst works by tethering the ends of the polymer to the metal centre to overcome the inherent entropic penalty of cyclization. Gel-permeation chromatography, dynamic and static light scattering, viscometry and chemical tests are all consistent with theoretical predictions and provide unambiguous confirmation of a cyclic topology. Access to a wide variety of new cyclic polymers is now possible by simply choosing the appropriate alkyne monomer.

  13. Solid state voltammetry and sensors in solids and gases

    SciTech Connect

    Murray, R.W.

    1992-04-01

    This project explores the electrochemical reactivity of electron transfer donor/acceptors dissolved in and diffusing through solid and semi-solid, ionically conductive media. The emphasis is on developing voltammetric experiments that are quantitatively interpretable in terms of the mass transport and electron transfer rates and thermodynamic equilibria of the redox solutes, and to exploit such experiments to probe their chemical and electrochemical behavior in the solid media. Techniques for quantitative voltammetry in solids were essentially unknown prior to initiation of this DOE project. We mainly employ poly(ethers)s containing dissolved metal salts electrolytes ( polymer electrolytes''), as prototype solid and semi-solid solvents. During this award year we have (a) concluded a study of plasticization chemistry in poly (ether) polymer electrolytes, (b) made progress in devising techniques for measuring the rates of electron transfer reactions in solid and semi-solid poly (ether)s, (c) continued efforts to design and understand the behavior of microband electrodes of various widths (0.1 to 10 {mu}m) in voltammetry of redox solutes, and (d) initiated synthetic efforts to attach ethylene oxide chains of various lengths to redox solutes.

  14. Particle deformation induced by AFM tapping under different setpoint voltages

    NASA Astrophysics Data System (ADS)

    Wu, Chung-Lin; Farkas, Natalia; Dagata, John A.; He, Bo-Ching; Fu, Wei-En

    2014-09-01

    The measured height of polystyrene nanoparticles varies with setpoint voltage during atomic force microscopy (AFM) tapping-mode imaging. Nanoparticle height was strongly influenced by the magnitude of the deformation caused by the AFM tapping forces, which was determined by the setpoint voltage. This influence quantity was studied by controlling the operational AFM setpoint voltage. A test sample consisting of well-dispersed 60-nm polystyrene and gold nanoparticles co-adsorbed on poly-l-lysine-coated mica was studied in this research. Gold nanoparticles have not only better mechanical property than polystyrene nanoparticles, but also obvious facets in AFM phase image. By using this sample of mixed nanoparticles, it allows us to confirm that the deformation resulted from the effect of setpoint voltage, not noise. In tapping mode, the deformation of polystyrene nanoparticles increased with decreasing setpoint voltage. Similar behavior was observed with both open loop and closed loop AFM instruments.

  15. Microrheology using a custom-made AFM

    NASA Astrophysics Data System (ADS)

    Kosgodagan Acharige, Sebastien; Benzaquen, Michael; Steinberger, Audrey

    In the past few years, a new method was developed to measure local properties of liquids (X. Xiong et al., Phys. Rev. E 80, 2009). This method consists of gluing a micron-sized glass fiber at the tip of an AFM cantilever and probing the liquid with it. In ENS Lyon, this method was perfected (C. Devailly et al., EPL, 106 5, 2014) with the help of an interferometer developped in the same laboratory (L. Bellon et al., Opt. Commun. 207 49, 2002 and P. Paolino et al., Rev. Sci. Instrum. 84, 2013), which background noise can reach 10-14 m /√{ Hz } . This method allows us to measure a wide range of viscosities (1 mPa . s to 500 mPa . s) of transparent and opaque fluids using a small sample volume ( 5 mL). In this presentation, I will briefly describe the interferometer developped in ENS Lyon, then explain precisely the microrheology measurements and then compare the experimental results to a model developped by M. Benzaquen. This work is supported financially by the ANR project NANOFLUIDYN (Grant Number ANR-13-BS10-0009).

  16. Manufacturing process of nanofluidics using afm probe

    NASA Astrophysics Data System (ADS)

    Karingula, Varun Kumar

    A new process for fabricating a nano fluidic device that can be used in medical application is developed and demonstrated. Nano channels are fabricated using a nano tip in indentation mode on AFM (Atomic Force Microscopy). The nano channels are integrated between the micro channels and act as a filter to separate biomolecules. Nano channels of 4 to7 m in length, 80nm in width, and at varying depths from 100nm to 850 nm allow the resulting device to separate selected groups of lysosomes and other viruses. Sharply developed vertical micro channels are produced from a deep reaction ion etching followed by deposition of different materials, such as gold and polymers, on the top surface, allowing the study of alternative ways of manufacturing a nanofluidic device. PDMS (Polydimethylsiloxane) bonding is performed to close the top surface of the device. An experimental setup is used to test and validate the device by pouring fluid through the channels. A detailed cost evaluation is conducted to compare the economical merits of the proposed process. It is shown that there is a 47:7% manufacturing time savings and a 60:6% manufacturing cost savings.

  17. BOREAS AFM-07 SRC Surface Meteorological Data

    NASA Technical Reports Server (NTRS)

    Osborne, Heather; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Young, Kim; Wittrock, Virginia; Shewchuck, Stan; Smith, David E. (Technical Monitor)

    2000-01-01

    The Saskatchewan Research Council (SRC) collected surface meteorological and radiation data from December 1993 until December 1996. The data set comprises Suite A (meteorological and energy balance measurements) and Suite B (diffuse solar and longwave measurements) components. Suite A measurements were taken at each of ten sites, and Suite B measurements were made at five of the Suite A sites. The data cover an approximate area of 500 km (North-South) by 1000 km (East-West) (a large portion of northern Manitoba and northern Saskatchewan). The measurement network was designed to provide researchers with a sufficient record of near-surface meteorological and radiation measurements. The data are provided in tabular ASCII files, and were collected by Aircraft Flux and Meteorology (AFM)-7. The surface meteorological and radiation data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  18. [Cyclic enteral nutrition].

    PubMed

    Hébuterne, X; Rampal, P

    1996-02-10

    Cyclic enteral nutrition consists in continuous infusion of nutrients with a pump over a 12 to 14 hour period at night. Different reports have demonstrated that cyclic enteral nutrition is well tolerated in malnourished ambulatory patients. The incidence of pneumonia by inhalation in this type of patients is less than 2%. Excepting patients with major amputation of the small intestine and important functional consequences, the increased infusion rate required by cyclic enteral nutrition does not diminish digestive tract absorption making the technique as effective as continuous 24-hour infusion. The main advantages of the cyclic infusion are the preservation of physiological balance between fasting and feeding, improved physical activity during the day with its beneficial effect on protein-energy metabolism, compatibility with oral nutrition during the day in nutrition reeducation programs, and the psychological impact in patients who are free to move about, further improving tolerance. Finally, cyclic enteral nutrition is adapted to enteral nutrition programs conducted in the patient's homes. PMID:8729381

  19. Interactions between tetrathiafulvalene units in dimeric structures - the influence of cyclic cores.

    PubMed

    Jiang, Huixin; Mazzanti, Virginia; Parker, Christian R; Broman, Søren Lindbæk; Wallberg, Jens Heide; Lušpai, Karol; Brincko, Adam; Kjaergaard, Henrik G; Kadziola, Anders; Rapta, Peter; Hammerich, Ole; Nielsen, Mogens Brøndsted

    2015-01-01

    A selection of cyclic and acyclic acetylenic scaffolds bearing two tetrathiafulvalene (TTF) units was prepared by different metal-catalyzed coupling reactions. The bridge separating the two TTF units was systematically changed from linearly conjugated ethyne, butadiyne and tetraethynylethene (trans-substituted) units to a cross-conjugated tetraethynylethene unit, placed in either acyclic or cyclic arrangements. The cyclic structures correspond to so-called radiaannulenes having both endo- and exocyclic double bonds. Interactions between two redox-active TTF units in these molecules were investigated by cyclic voltammetry, UV-vis-NIR and EPR absorption spectroscopical methods of the electrochemically generated oxidized species. The electron-accepting properties of the acetylenic cores were also investigated electrochemically. PMID:26124895

  20. Cloud Point Extraction for Electroanalysis: Anodic Stripping Voltammetry of Cadmium

    PubMed Central

    Rusinek, Cory A.; Bange, Adam; Papautsky, Ian; Heineman, William R.

    2016-01-01

    Cloud point extraction (CPE) is a well-established technique for the pre-concentration of hydrophobic species from water without the use of organic solvents. Subsequent analysis is then typically performed via atomic absorption spectroscopy (AAS), UV-Vis spectroscopy, or high performance liquid chromatography (HPLC). However, the suitability of CPE for electroanalytical methods such as stripping voltammetry has not been reported. We demonstrate the use of CPE for electroanalysis using the determination of cadmium (Cd2+) by anodic stripping voltammetry (ASV) as a representative example. Rather than using the chelating agents which are commonly used in CPE to form a hydrophobic, extractable metal complex, we used iodide and sulfuric acid to neutralize the charge on Cd2+ to form an extractable ion pair. Triton X-114 was chosen as the surfactant for the extraction because its cloud point temperature is near room temperature (22–25° C). Bare glassy carbon (GC), bismuth-coated glassy carbon (Bi-GC), and mercury-coated glassy carbon (Hg-GC) electrodes were compared for the CPE-ASV. A detection limit for Cd2+ of 1.7 nM (0.2 ppb) was obtained with the Hg-GC electrode. Comparison of ASV analysis without CPE was also investigated and a 20x decrease (4.0 ppb) in the detection limit was observed. The suitability of this procedure for the analysis of tap and river water samples was also demonstrated. This simple, versatile, environmentally friendly and cost-effective extraction method is potentially applicable to a wide variety of transition metals and organic compounds that are amenable to detection by electroanalytical methods. PMID:25996561

  1. Cloud Point Extraction for Electroanalysis: Anodic Stripping Voltammetry of Cadmium.

    PubMed

    Rusinek, Cory A; Bange, Adam; Papautsky, Ian; Heineman, William R

    2015-06-16

    Cloud point extraction (CPE) is a well-established technique for the preconcentration of hydrophobic species from water without the use of organic solvents. Subsequent analysis is then typically performed via atomic absorption spectroscopy (AAS), UV-vis spectroscopy, or high performance liquid chromatography (HPLC). However, the suitability of CPE for electroanalytical methods such as stripping voltammetry has not been reported. We demonstrate the use of CPE for electroanalysis using the determination of cadmium (Cd(2+)) by anodic stripping voltammetry (ASV). Rather than using the chelating agents which are commonly used in CPE to form a hydrophobic, extractable metal complex, we used iodide and sulfuric acid to neutralize the charge on Cd(2+) to form an extractable ion pair. This offers good selectivity for Cd(2+) as no interferences were observed from other heavy metal ions. Triton X-114 was chosen as the surfactant for the extraction because its cloud point temperature is near room temperature (22-25 °C). Bare glassy carbon (GC), bismuth-coated glassy carbon (Bi-GC), and mercury-coated glassy carbon (Hg-GC) electrodes were compared for the CPE-ASV. A detection limit for Cd(2+) of 1.7 nM (0.2 ppb) was obtained with the Hg-GC electrode. ASV with CPE gave a 20x decrease (4.0 ppb) in the detection limit compared to ASV without CPE. The suitability of this procedure for the analysis of tap and river water samples was demonstrated. This simple, versatile, environmentally friendly, and cost-effective extraction method is potentially applicable to a wide variety of transition metals and organic compounds that are amenable to detection by electroanalytical methods. PMID:25996561

  2. Cyclic membrane separation process

    DOEpatents

    Bowser, John

    2004-04-13

    A cyclic process for controlling environmental emissions of volatile organic compounds (VOC) from vapor recovery in storage and dispensing operations of liquids maintains a vacuum in the storage tank ullage. In one of a two-part cyclic process ullage vapor is discharged through a vapor recovery system in which VOC are stripped from vented gas with a selectively gas permeable membrane. In the other part, the membrane is inoperative while gas pressure rises in the ullage. Ambient air is charged to the membrane separation unit during the latter part of the cycle.

  3. Flow in cyclic cosmology

    SciTech Connect

    Kinney, William H.; Dizgah, Azadeh Moradinezhad

    2010-10-15

    In this paper, we use a known duality between expanding and contracting cosmologies to construct a dual of the inflationary flow hierarchy applicable to contracting cosmologies such as ekpyrotic and cyclic models. We show that the inflationary flow equations are invariant under the duality and therefore apply equally well to inflation or to cyclic cosmology. We construct a self-consistent small-parameter approximation dual to the slow-roll approximation in inflation, and calculate the power spectrum of perturbations in this limit. We also recover the matter-dominated contracting solution of Wands, and the recently proposed adiabatic ekpyrosis solution.

  4. Cyclic membrane separation process

    DOEpatents

    Nemser, Stuart M.

    2005-05-03

    A cyclic process for controlling environmental emissions of volatile organic compounds (VOC) from vapor recovery in storage and dispensing operations of liquids maintains a vacuum in the storage tank ullage. In the first part of a two-part cyclic process ullage vapor is discharged through a vapor recovery system in which VOC are stripped from vented gas with a selectively gas permeable membrane. In the second part, the membrane is inoperative while gas pressure rises in the ullage. In one aspect of this invention, a vacuum is drawn in the membrane separation unit thus reducing overall VOC emissions.

  5. Segmental calibration for commercial AFM in vertical direction

    NASA Astrophysics Data System (ADS)

    Shi, Yushu; Gao, Sitian; Lu, Mingzhen; Li, Wei; Xu, Xuefang

    2013-01-01

    Atomic force microscopy (AFM) is most widely applied in scientific research and industrial production. AFM is a scanning probe imaging and measuring device, useful for physical and chemical studies. Depends on its basic structure, microscopic surface pattern can be measured and captured by mechanically scanning. Its vertical and horizon resolution can reach to 0.01nm and 0.1nm. Commonly the measurement values of commercial AFM are directly from scanning piezoelectric tube, so that it not a traceable value. In order to solve the problem of commercial AFM's traceability, step height standard references are applied to calibrate the piezoelectric ceramic housing in scanning tube. All of the serial of step height standard references, covering the commercial AFM vertical scale, are calibrated by Metrology AFM developed by National Institute of Metrology (NIM), China. Three interferometers have been assembled in its XYZ axis, therefore the measurement value can directly trace to laser wavelength. Because of nonlinear characteristic of PZT, the method of segmental calibration is proposed. The measurement scale can be divided into several subsections corresponding to the calibrated values of the series of step height standards references. By this method the accuracy of measurements can be ensured in each segment measurement scale and the calibration level of the whole instrument can be promoted. In order to get a standard step shape by commercial AFM, substrate removal method is applied to deal with the bow shape problem.

  6. Raman and AFM study of gamma irradiated plastic bottle sheets

    SciTech Connect

    Ali, Yasir; Kumar, Vijay; Dhaliwal, A. S.; Sonkawade, R. G.

    2013-02-05

    In this investigation, the effects of gamma irradiation on the structural properties of plastic bottle sheet are studied. The Plastic sheets were exposed with 1.25MeV {sup 60}Co gamma rays source at various dose levels within the range from 0-670 kGy. The induced modifications were followed by micro-Raman and atomic force microscopy (AFM). The Raman spectrum shows the decrease in Raman intensity and formation of unsaturated bonds with an increase in the gamma dose. AFM image displays rough surface morphology after irradiation. The detailed Raman analysis of plastic bottle sheets is presented here, and the results are correlated with the AFM observations.

  7. Dynamics of the nanoneedle probe in trolling mode AFM.

    PubMed

    Abdi, Ahmad; Pishkenari, Hossein Nejat; Keramati, Ramtin; Minary-Jolandan, Majid

    2015-05-22

    Atomic force microscopy (AFM), as an indispensable tool for nanoscale characterization, presents major drawbacks for operation in a liquid environment arising from the large hydrodynamic drag on the vibrating cantilever. The newly introduced 'Trolling mode' (TR-mode) AFM resolves this complication by using a specialized nanoneedle cantilever that keeps the cantilever outside of the liquid. Herein, a mechanical model with a lumped mass was developed to capture the dynamics of such a cantilever with a nanoneedle tip. This new developed model was applied to investigate the effects of the needle-liquid interface on the performance of the AFM, including the imaging capability in liquid. PMID:25915451

  8. AFM Studies of Conformational Changes in Proteins and Peptides

    NASA Astrophysics Data System (ADS)

    Ploscariu, Nicoleta; Sukthankar, Pinakin; Tomich, John; Szoszkiewicz, Robert

    2015-03-01

    Here, we present estimates of molecular stiffness and mechanical energy dissipation factors for some examples of proteins and peptides. The results are obtained from AFM force spectroscopy measurements. To determine molecular stiffness and mechanical energy dissipation factors we developed a model based on measuring several resonance frequencies of an AFM cantilever in contact with either single protein molecule or peptides adsorbed on arbitrary surface. We used compliant AFM cantilevers with a small aspect ratio - a ratio of length to width - in air and in liquid, including biologically relevant phosphate buffered saline medium. Department of Physics.

  9. Comparison of the simple cyclic voltammetry (CV) and DPPH assays for the determination of antioxidant capacity of active principles.

    PubMed

    Arteaga, Jesús F; Ruiz-Montoya, Mercedes; Palma, Alberto; Alonso-Garrido, Gema; Pintado, Sara; Rodríguez-Mellado, José M

    2012-01-01

    Antioxidant activity of a number of small (low molecular weight) natural compounds found in spices, condiments or drugs (gallic acid, sesamol, eugenol, thymol, carvacrol, vanillin, salicylaldehyde, limonene, geraniol, 4-hexylresorcinol, etc.) has been evaluated using electrochemical and DPPH• radical scavenging measurements. Structural analysis of the tested compound suggest a remarkable activity for phenol derivatives and the importance of the -R groups located on the phenolic ring in the molecule's ability to act as free radical scavenging as well as their influence in the electrochemical behavior. The voltammetric method can be used for the determination of the antioxidant capability in the same manner as the DPPH• radical scavenging because of the correlation found between oxidation potentials and anti-radical power (ARP = 1/EC₅₀). Such electrochemical determination is fast and cheap and allows making measurements under a variety of experimental conditions. The accuracy of the electrochemical measurements is the same for all the compounds, irrespective of their scavenging activity, the opposite of what occurs in the DPPH• test. PMID:22555300

  10. Ability of Lactobacillus rhamnosus GAF01 to remove AFM1 in vitro and to counteract AFM1 immunotoxicity in vivo.

    PubMed

    Abbès, Samir; Salah-Abbès, Jalila Ben; Sharafi, Hakimeh; Jebali, Rania; Noghabi, Kambiz Akbari; Oueslati, Ridha

    2013-01-01

    Aflatoxin M1 (AFM1) has been detected in many parts of the world both in raw milk and many dairy products, causing great economic losses and human disease. Unfortunately, there are few studies dealing with AFM1 immunotoxicity/interactions with lactic acid bacteria for potential application as a natural preventive agent. The aim of this study was to isolate (from dairy products) food-grade probiotic bacteria able to degrade/bind AFM1 in vitro and evaluate whether the same organism(s) could impart a protective role against AFM1-induced immunotoxicity in exposed Balb/c mice. Bacteria (Lactobacillus plantarum MON03 and L. rhamnosus GAF01) were isolated from Tunisian artisanal butter and then tested for abilities to eliminate AFM1 from phosphate-buffered saline (PBS) and reconstituted milk (containing 0.05, 0.10, and 0.20 µg AFM1/ml) after 0, 6, and 24 h at 37°C. Results showed that the selected bacteria could 'remove' AFM1 both in PBS and skimmed milk. The binding abilities of AFM1 by L. plantarum MON03 and L. rhamnosus GAF01 strains (at 10(8) CFU/ml) in PBS and reconstituted milk ranged, respectively, from 16.1-78.6% and 15.3-95.1%; overall, L. rhamnosus showed a better potential for removal than L. plantarum. 'Removal' appeared to be by simple binding; the bacteria/AFM1 complex was stable and only a very small proportion of mycotoxin was released back into the solution. L. rhamnosus GAF01 had the highest binding capacity and was selected for use in the in vivo study. Those results indicated that use of the organism prevented AFM1-induced effects on total white and red blood cells, and lymphocyte subtypes, after 15 days of host treatment. These studies clearly indicated that L. rhamnosus GAF01 was able to bind AFM1 in vitro and-by mechanisms that might also be related to a binding effect-counteract AFM1-induced immunotoxicity. Moreover, by itself, this bacterium was not toxic and could potentially be used as an additive in dairy products and in biotechnology for

  11. Atomic force microscopy combined with optical tweezers (AFM/OT)

    NASA Astrophysics Data System (ADS)

    Pierini, F.; Zembrzycki, K.; Nakielski, P.; Pawłowska, S.; Kowalewski, T. A.

    2016-02-01

    The role of mechanical properties is essential to understand molecular, biological materials, and nanostructures dynamics and interaction processes. Atomic force microscopy (AFM) is the most commonly used method of direct force evaluation, but due to its technical limitations this single probe technique is unable to detect forces with femtonewton resolution. In this paper we present the development of a combined atomic force microscopy and optical tweezers (AFM/OT) instrument. The focused laser beam, on which optical tweezers are based, provides us with the ability to manipulate small dielectric objects and to use it as a high spatial and temporal resolution displacement and force sensor in the same AFM scanning zone. We demonstrate the possibility to develop a combined instrument with high potential in nanomechanics, molecules manipulation and biological studies. AFM/OT equipment is described and characterized by studying the ability to trap dielectric objects and quantifying the detectable and applicable forces. Finally, optical tweezers calibration methods and instrument applications are given.

  12. Nanoscale structural features determined by AFM for single virus particles.

    PubMed

    Chen, Shu-wen W; Odorico, Michael; Meillan, Matthieu; Vellutini, Luc; Teulon, Jean-Marie; Parot, Pierre; Bennetau, Bernard; Pellequer, Jean-Luc

    2013-11-21

    In this work, we propose "single-image analysis", as opposed to multi-image averaging, for extracting valuable information from AFM images of single bio-particles. This approach allows us to study molecular systems imaged by AFM under general circumstances without restrictions on their structural forms. As feature exhibition is a resolution correlation, we have performed AFM imaging on surfaces of tobacco mosaic virus (TMV) to demonstrate variations of structural patterns with probing resolution. Two AFM images were acquired with the same tip at different probing resolutions in terms of pixel width, i.e., 1.95 and 0.49 nm per pixel. For assessment, we have constructed an in silico topograph based on the three-dimensional crystal structure of TMV as a reference. The prominent artifacts observed in the AFM-determined shape of TMV were attributed to tip convolutions. The width of TMV rod was systematically overestimated by ~10 nm at both probing resolutions of AFM. Nevertheless, the effects of tip convolution were less severe in vertical orientation so that the estimated height of TMV by AFM imaging was in close agreement with the in silico X-ray topograph. Using dedicated image processing algorithms, we found that at low resolution (i.e., 1.95 nm per pixel), the extracted surface features of TMV can be interpreted as a partial or full helical repeat (three complete turns with ~7.0 nm in length), while individual protein subunits (~2.5 nm) were perceivable only at high resolution. The present study shows that the scales of revealed structural features in AFM images are subject to both probing resolution and processing algorithms for image analysis. PMID:24056758

  13. The Conductance of Nanotubes Deformed by the AFM Tip

    NASA Technical Reports Server (NTRS)

    Svizhenko, Alexei; Maiti, Amitesh; Anantram, M. P.

    2003-01-01

    The conductance drop under AFM-tip deformation can be explained by stretching of the tube length. NT sensors can be built utilizing uniform stretching. Single sp3 bond cross section cannot block electrons, because another conducting path may exist. AFM tip which forms sp3 bonds with the tube will decrease conductance. In the "table experiment" a conductance drop of 2 orders of magnitude happened only after some bonds were broken.

  14. Characterization of the interaction between AFM tips and surface nanobubbles.

    PubMed

    Walczyk, Wiktoria; Schönherr, Holger

    2014-06-24

    While the presence of gaseous enclosures observed at various solid-water interfaces, the so-called "surface nanobubles", has been confirmed by many groups in recent years, their formation, properties, and stability have not been convincingly and exhaustively explained. Here we report on an atomic force microscopy (AFM) study of argon nanobubbles on highly oriented pyrolitic graphite (HOPG) in water to elucidate the properties of nanobubble surfaces and the mechanism of AFM tip-nanobubble interaction. In particular, the deformation of the nanobubble-water interface by the AFM tip and the question whether the AFM tip penetrates the nanobubble during scanning were addressed by this combined intermittent contact (tapping) mode and force volume AFM study. We found that the stiffness of nanobubbles was smaller than the cantilever spring constant and comparable with the surface tension of water. The interaction with the AFM tip resulted in severe quasi-linear deformation of the bubbles; however, in the case of tip-bubble attraction, the interface deformed toward the tip. We tested two models of tip-bubble interaction, namely, the capillary force and the dynamic interaction model, and found, depending on the tip properties, good agreement with experimental data. The results showed that the tip-bubble interaction strength and the magnitude of the bubble deformation depend strongly on tip and bubble geometry and on tip and substrate material, and are very sensitive to the presence of contaminations that alter the interfacial tension. In particular, nanobubbles interacted differently with hydrophilic and hydrophobic AFM tips, which resulted in qualitatively and quantitatively different force curves measured on the bubbles in the experiments. To minimize bubble deformation and obtain reliable AFM results, nanobubbles must be measured with a sharp hydrophilic tip and with a cantilever having a very low spring constant in a contamination-free system. PMID:24856074

  15. Modeling the Interaction between AFM Tips and Pinned Surface Nanobubbles.

    PubMed

    Guo, Zhenjiang; Liu, Yawei; Xiao, Qianxiang; Schönherr, Holger; Zhang, Xianren

    2016-01-26

    Although the morphology of surface nanobubbles has been studied widely with different AFM modes, AFM images may not reflect the real shapes of the nanobubbles due to AFM tip-nanobubble interactions. In addition, the interplay between surface nanobubble deformation and induced capillary force has not been well understood in this context. In our work we used constraint lattice density functional theory to investigate the interaction between AFM tips and pinned surface nanobubbles systematically, especially concentrating on the effects of tip hydrophilicity and shape. For a hydrophilic tip contacting a nanobubble, its hydrophilic nature facilitates its departure from the bubble surface, displaying a weak and intermediate-range attraction. However, when the tip squeezes the nanobubble during the approach process, the nanobubble shows an elastic effect that prevents the tip from penetrating the bubble, leading to a strong nanobubble deformation and repulsive interactions. On the contrary, a hydrophobic tip can easily pierce the vapor-liquid interface of the nanobubble during the approach process, leading to the disappearance of the repulsive force. In the retraction process, however, the adhesion between the tip and the nanobubble leads to a much stronger lengthening effect on nanobubble deformation and a strong long-range attractive force. The trends of force evolution from our simulations agree qualitatively well with recent experimental AFM observations. This favorable agreement demonstrates that our model catches the main intergradient of tip-nanobubble interactions for pinned surface nanobubbles and may therefore provide important insight into how to design minimally invasive AFM experiments. PMID:26751634

  16. Differential pulse anodic stripping voltammetry for detection of As (III) by Chitosan-Fe(OH)3 modified glassy carbon electrode: A new approach towards speciation of arsenic.

    PubMed

    Saha, Suparna; Sarkar, Priyabrata

    2016-09-01

    An efficient electrochemical sensor for As(III) was developed based on adsorption of arsenic on a specially modified electrodes at some applied potential and subsequent i) stripping at a fixed potential by anodic stripping voltammetry ii) analysis by generating surface plasmon resonance (SPR). The working glassy carbon electrode was modified by Chitosan-Fe(OH)3 composite and a reducing agent L-cysteine. The composite enhanced adsorption of As(III) and subsequent reduction to As(O) moieties and measurement by anodic stripping. The surface property of modified electrode was characterized by SEM, AFM, FTIR, XPS and electrochemistry was analyzed by impedance spectroscopy (EIS). Surface Plasmon resonance (SPR) was also employed to investigate the As(III) binding capability of polymer matrix. Several optimum voltammetric parameters e.g supporting electrolyte; 0.1M acetate buffer (pH 5.2) deposition potential, -0.9V; deposition time, 100s were established for anodic stripping voltammetry (ASV). A linear correlation was obtained in the range of 2-100ppb for ASV (R(2) 0.974) with limit of detection 0.072ppb. A variety of common coexistent ions such as Mn, Zn, Pb, Cu, Cd in water samples showed no interferences on the As (III) determination. The method was applied successfully to real samples collected from arsenic affected areas of West Bengal, India. PMID:27343601

  17. Single Nanoparticle Voltammetry: Contact Modulation of the Mediated Current.

    PubMed

    Li, Xiuting; Batchelor-McAuley, Christopher; Whitby, Samuel A I; Tschulik, Kristina; Shao, Lidong; Compton, Richard G

    2016-03-18

    The cyclic voltammetric responses of individual palladium-coated carbon nanotubes are reported. Upon impact-from the solution phase-with the electrified interface, the nanoparticles act as individual nanoelectrodes catalyzing the hydrogen-oxidation reaction. At high overpotentials the current is shown to reach a quasi-steady-state diffusion limit, allowing determination of the tube length. The electrochemical response of the individual nanotubes also reveals the system to be modulated by the electrical contact between the electrode and carbon nanotube. This modulation presents itself as fluctuations in the recorded Faradaic current. PMID:26515036

  18. Stripping voltammetry at micro-interface arrays: a review.

    PubMed

    Herzog, Grégoire; Beni, Valerio

    2013-03-26

    In this article, a comprehensive overview of the most recent developments in the field of stripping voltammetry at regular micro-interfaces (both solid-liquid and liquid-liquid interfaces) is presented. This review will report on the most conventional arrays of metallic micro-electrodes but also on the rapidly growing field of electrochemistry at arrays of micro-interfaces between two immiscible electrolyte solutions (μITIES). The main fabrication methods, together with some design considerations and diffusion phenomena at such interfaces are discussed. Main applications of micro-interface arrays are presented including heavy metals detection at micro-electrode arrays and detection of organic molecules (amino acids, vitamins, peptides and drugs) at the μITIES. Stripping analysis at micro-interface arrays is suitable for the detection of analytes in several real media including water, soil extracts and biological fluids (blood and saliva) with high specificity, sensitivity (detection limits of nM, ppb level) and reliability. Stripping analysis at μITIES and micro-electrode arrays are two complementary approaches that have the advantages of being cost effective, simple to use and easily adaptable to field measurement. PMID:23498116

  19. Disposable Copper-Based Electrochemical Sensor for Anodic Stripping Voltammetry

    PubMed Central

    2015-01-01

    In this work, we report the first copper-based point-of-care sensor for electrochemical measurements demonstrated by zinc determination in blood serum. Heavy metals require careful monitoring, yet current methods are too complex for a point-of-care system. Electrochemistry offers a simple approach to metal detection on the microscale, but traditional carbon, gold (Au), or platinum (Pt) electrodes are difficult or expensive to microfabricate, preventing widespread use. Our sensor features a new low-cost electrode material, copper, which offers simple fabrication and compatibility with microfabrication and PCB processing, while maintaining competitive performance in electrochemical detection. Anodic stripping voltammetry of zinc using our new copper-based sensors exhibited a 140 nM (9.0 ppb) limit of detection (calculated) and sensitivity greater than 1 μA/μM in the acetate buffer. The sensor was also able to determine zinc in a bovine serum extract, and the results were verified with independent sensor measurements. These results demonstrate the advantageous qualities of this lab-on-a-chip electrochemical sensor for clinical applications, which include a small sample volume (μL scale), reduced cost, short response time, and high accuracy at low concentrations of analyte. PMID:24773513

  20. Electrochemical Investigation of Coenzyme Q10 on Silver Electrode in Ethanol Aqueous Solution and Its Determination Using Differential Pulse Voltammetry.

    PubMed

    Li, Dan; Deng, Wei; Xu, Hu; Sun, Yinxing; Wang, Yuhong; Chen, Shouhui; Ding, Xianting

    2016-08-01

    The electrochemistry reduction of coenzyme Q10 (CoQ10) on silver electrodes has been investigated in mixed solvent containing 95 vol. % ethanol and 5 vol. % water. A combination of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) is employed to explore the mechanism of redox processes of CoQ10 in the presence and absence of oxygen, respectively. It has been proved that the redox reaction of CoQ10 is highly dependent on the oxygen in the solution compared with that of CoQ0, which may be attributed to the isoprenoid side chain effect of CoQ10 Moreover, the effects of experimental variables such as electrolyte component, pH, temperature, and sonication time on the amperometric and potentiometric responses of CoQ10 are presented. The differential pulse voltammetry method has been developed for the quantification of the CoQ10 in the complex samples. Under the optimum conditions, the method is linear over the concentration range of 1.00 × 10(-7) to 1.00 × 10(-3) mol/L (8.63 × 10(-2) to 8.63 × 10(2) mg/kg). The limit of detection (3σ/k) is 3.33 × 10(-8) mol/L (2.88 × 10(-2) mg/kg). The recoveries of the spiked samples are between 91% and 108%. The presented method can be applied to the analysis of CoQ10 in real samples without any pretreatment. PMID:27094091

  1. Demon voltammetry and analysis software: Analysis of cocaine-induced alterations in dopamine signaling using multiple kinetic measures

    PubMed Central

    Yorgason, Jordan T.; España, Rodrigo A.; Jones, Sara R.

    2011-01-01

    The fast sampling rates of fast scan cyclic voltammetry make it a favorable method for measuring changes in brain monoamine release and uptake kinetics in slice, anesthetized, and freely moving preparations. The most common analysis technique for evaluating changes in dopamine signaling uses well-established Michaelis-Menten kinetic methods that can accurately model dopamine release and uptake parameters across multiple experimental conditions. Nevertheless, over the years, many researchers have turned to other measures to estimate changes in dopamine release and uptake, yet to our knowledge no systematic comparison amongst these measures has been conducted. To address this lack of uniformity in kinetic analyses, we have created the Demon Voltammetry and Analysis software suite, which is freely available to academic and non-profit institutions. Here we present an explanation of the Demon Acquisition and Analysis features, and demonstrate its utility for acquiring voltammetric data under in vitro, in vivo anesthetized, and freely moving conditions. Additionally, the software was used to compare the sensitivity of multiple kinetic measures of release and uptake to cocaine-induced changes in electrically evoked dopamine efflux in nucleus accumbens core slices. Specifically, we examined and compared tau, full width at half height, half-life, T20, T80, slope, peak height, calibrated peak dopamine concentration, and area under the curve to the well-characterized Michaelis-Menten parameters, dopamine per pulse, maximal uptake rate, and apparent affinity. Based on observed results we recommend tau for measuring dopamine uptake and calibrated peak dopamine concentration for measuring dopamine release. PMID:21392532

  2. AFM investigation of Martian soil simulants on micromachined Si substrates.

    PubMed

    Vijendran, S; Sykulska, H; Pike, W T

    2007-09-01

    The micro and nanostructures of Martian soil simulants with particles in the micrometre-size range have been studied using a combination of optical and atomic force microscopy (AFM) in preparation for the 2007 NASA Phoenix Mars Lander mission. The operation of an atomic force microscope on samples of micrometre-sized soil particles is a poorly investigated area where the unwanted interaction between the scanning tip and loose particles results in poor image quality and tip contamination by the sample. In order to mitigate these effects, etched silicon substrates with a variety of features have been used to facilitate the sorting and gripping of particles. From these experiments, a number of patterns were identified that were particularly good at isolating and immobilizing particles for AFM imaging. This data was used to guide the design of micromachined substrates for the Phoenix AFM. Both individual particles as well as aggregates were successfully imaged, and information on sizes, shapes and surface morphologies were obtained. This study highlights both the strengths and weaknesses of AFM for the potential in situ investigation of Martian soil and dust. Also presented are more general findings of the limiting operational constraints that exist when attempting the AFM of high aspect ratio particles with current technology. The performance of the final designs of the substrates incorporated on Phoenix will be described in a later paper. PMID:17760618

  3. An Early Cyclic Universe

    NASA Astrophysics Data System (ADS)

    Duhe, William; Biswas, Tirthibir

    2014-03-01

    We provide a comprehensive numerical study of the Emergent Cyclic Inflation scenario. This is a scenario where instead of traditional monotonic slow roll inflation, the universe expands over numerous short asymmetric cycles due to the production of entropy via interactions among different species. This is one of the very few scenarios of inflation which provides a nonsingular geodesically complete space-time and does not require any ``reheating'' mechanism. A special thanks to Loyola University for an excellent community to help this project grow.

  4. Investigation of the reduction process of dopamine using paired pulse voltammetry

    PubMed Central

    Kim, Do Hyoung; Oh, Yoonbae; Shin, Hojin; Blaha, Charles D.; Bennet, Kevin E.; Lee, Kendall H.; Kim, In Young; Jang, Dong Pyo

    2014-01-01

    The oxidation of dopamine (DA) around +0.6V potential in anodic sweep and its reduction around −0.1V in cathodic sweep at a relatively fast scanning rate (300 V/s or greater) have been used for identification of DA oxidation in fast-scan cyclic voltammetry (FSCV). However, compared to the oxidation peak of DA, the reduction peak has not been fully examined in analytical studies, although it has been used as one of the representative features to identify DA. In this study, the reduction process of DA was investigated using paired pulse voltammetry (PPV), which consists of two identical triangle-shaped waveforms, separated by a short interval at the holding potential. Especially, the discrepancies between the magnitude of the oxidation and reduction peaks of DA were investigated based on three factors: (1) the instant desorption of the DA oxidation product (dopamine-o-quinone: DOQ) after production, (2) the effect of the holding potential on the reduction process, and (3) the rate-limited reduction process of DA. For the first test, the triangle waveform FSCV experiment was performed on DA with various scanrates (from 400 to 1000 V/s) and durations of switching potentials of the triangle waveform (from 0.0 to 6.0 ms) in order to vary the duration between the applied oxidation potential at +0.6V and the reduction potential at −0.2V. As a result, the ratio of reduction over oxidation peak current response decreased as the duration became longer. To evaluate the effect of holding potentials during the reduction process, FSCV experiments were conducted with holding potential from 0.0V to −0.8V. We found that more negative holding potentials lead to larger amount of reduction process. For evaluation of the rate-limited reduction process of DA, PPV with a 1Hz repetition rate and various delays (2, 8, 20, 40 and 80ms) between the paired scans were utilized to determine how much reduction process occurred during the holding potential (−0.4V). These tests showed that

  5. Charging C60 islands with the AFM tip.

    PubMed

    Hoff, Brice; Henry, Claude R; Barth, Clemens

    2016-01-01

    We show that electrons can be transferred on demand from an AFM tip into single bulk-like C60 islands, which are supported on the insulating NaCl(001) surface. We exemplify this by controlled charge-manipulation experiments conducted in ultrahigh vacuum by noncontact AFM (nc-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM). KPFM shows a homogeneous contrast at the islands, which is a signature for an equal distribution of the electrons in the T1u band. The charge dissipates during half a day due to an interaction of the charged C60 islands with defects in the near surface region of NaCl. Our results open the perspective in photo-voltaics to study charge attachment, stability and charge exchange with the environment of any C60 bulk-like system. PMID:26617348

  6. Liquid contact resonance AFM: analytical models, experiments, and limitations

    NASA Astrophysics Data System (ADS)

    Parlak, Zehra; Tu, Qing; Zauscher, Stefan

    2014-11-01

    Contact resonance AFM (CR-AFM) is a scanning probe microscopy technique that utilizes the contact resonances of the AFM cantilever for concurrent imaging of topography and surface stiffness. The technique has not been used in liquid until recently due to analytical and experimental difficulties, associated with viscous damping of cantilever vibrations and fluid loading effects. To address these difficulties, (i) an analytical approach for contact resonances in liquid is developed, and (ii) direct excitation of the contact resonances is demonstrated by actuating the cantilever directly in a magnetic field. By implementing the analytical approach and the direct actuation through magnetic particles, quantitative stiffness imaging on surfaces with a wide range of stiffness can be achieved in liquid with soft cantilevers and low contact forces.

  7. Imaging resolution of AFM with probes modified with FIB.

    PubMed

    Skibinski, J; Rebis, J; Wejrzanowski, T; Rozniatowski, K; Pressard, K; Kurzydlowski, K J

    2014-11-01

    This study concerns imaging of the structure of materials using AFM tapping (TM) and phase imaging (PI) mode, using probes modified with focused ion beam (FIB). Three kinds of modifications were applied - thinning of the cantilever, sharpening of the tip and combination of these two modifications. Probes shaped in that way were used for AFM investigations with Bruker AFM Nanoscope 8. As a testing material, titanium roughness standard supplied by Bruker was used. The results show that performed modifications influence the oscillation of the probes. In particular thinning of the cantilever enables one to acquire higher self-resonant frequencies, which can be advantageous for improving the quality of imaging in PI mode. It was found that sharpening the tip improves imaging resolution in tapping mode, which is consistent with existing knowledge, but lowered the quality of high frequency topography images. In this paper the Finite Element Method (FEM) was used to explain the results obtained experimentally. PMID:25080273

  8. AFM of biological complexes: what can we learn?

    PubMed Central

    Gaczynska, Maria; Osmulski, Pawel A.

    2009-01-01

    The term “biological complexes” broadly encompasses particles as diverse as multisubunit enzymes, viral capsids, transport cages, molecular nets, ribosomes, nucleosomes, biological membrane components and amyloids. The complexes represent a broad range of stability and composition. Atomic force microscopy offers a wealth of structural and functional data about such assemblies. For this review, we choose to comment on the significance of AFM to study various aspects of biology of selected nonmembrane protein assemblies. Such particles are large enough to reveal many structural details under the AFM probe. Importantly, the specific advantages of the method allow for gathering dynamic information about their formation, stability or allosteric structural changes critical for their function. Some of them have already found their way to nanomedical or nanotechnological applications. Here we present examples of studies where the AFM provided pioneering information about the biology of complexes, and examples of studies where the simplicity of the method is used toward the development of potential diagnostic applications. PMID:19802337

  9. Improvement in metrology on new 3D-AFM platform

    NASA Astrophysics Data System (ADS)

    Schmitz, Ingo; Osborn, Marc; Hand, Sean; Chen, Qi

    2008-10-01

    According to the 2007 edition of the ITRS roadmap, the requirement for CD uniformity of isolated lines on a binary or attenuated phase shift mask is 2.1nm (3σ) in 2008 and requires improvement to1.3 nm (3σ) in 2010. In order to meet the increasing demand for CD uniformity on photo masks, improved CD metrology is required. A next generation AFM, InSightTM 3DAFM, has been developed to meet these increased requirements for advanced photo mask metrology. The new system achieves 2X improvement in CD and depth precision on advanced photo masks features over the previous generation 3D-AFM. This paper provides measurement data including depth, CD, and sidewall angle metrology. In addition the unique capabilities of damage-free defect inspection and Nanoimprint characterization by 3D AFM are presented.

  10. Mounting of Escherichia coli spheroplasts for AFM imaging.

    SciTech Connect

    Sullivan, Claretta J; Morrell-Falvey, Jennifer L; Allison, David P; Doktycz, Mitchel John

    2005-11-01

    The cytoplasmic membrane of Escherichia coli (E. coli) is the location of numerous, chemically specific transporters and recognition elements. Investigation of this membrane in vivo by atomic force microscopy (AFM) requires removal of the cell wall and stable immobilization of the spheroplast. AFM images demonstrate that spheroplasts can be secured with warm gelatin applied to the mica substrate just before the addition of a spheroplast suspension. The resulting preparation can be repeatedly imaged by AFM over the course of several hours. Confocal fluorescence imaging confirms the association of the spheroplasts with the gelatin layer. Gelatin molecules are known to reorder into a network after heating. Entrapment within this gelatin network is believed to be responsible for the immobilization of spheroplasts on mica.

  11. Surface Morphological Studies on Nerve Cells by AFM

    NASA Astrophysics Data System (ADS)

    Durkaya, Goksel; Zhong, Lei; Rehder, Vincent; Dietz, Nikolaus

    2009-03-01

    Surface morphological properties of fixed and living nerve cells removed from the buccal ganglion of Helisoma trivolvis have been studied by using Atomic Force Microscopy (AFM). Identified, individual neurons were removed from the buccal ganglion of Helisoma trivolvis and plated into poly-L-lysine coated glass cover-slips. The growth of the nerve cells was stopped and fixed with 0.1% Glutaraldehyde and 4% Formaldehyde solution after extension of growth cones at the tip of the axons. Topography and softness of growth cone filopodia and overlying lamellopodium (veil) were probed by AFM. Information obtained from AFM's amplitude and phase channels have been used for determination of softness of the region probed. The results of structural studies on the cells are linked to their mechanical properties and internal molecular density distribution.

  12. Charging C60 islands with the AFM tip

    NASA Astrophysics Data System (ADS)

    Hoff, Brice; Henry, Claude R.; Barth, Clemens

    2015-12-01

    We show that electrons can be transferred on demand from an AFM tip into single bulk-like C60 islands, which are supported on the insulating NaCl(001) surface. We exemplify this by controlled charge-manipulation experiments conducted in ultrahigh vacuum by noncontact AFM (nc-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM). KPFM shows a homogeneous contrast at the islands, which is a signature for an equal distribution of the electrons in the T1u band. The charge dissipates during half a day due to an interaction of the charged C60 islands with defects in the near surface region of NaCl. Our results open the perspective in photo-voltaics to study charge attachment, stability and charge exchange with the environment of any C60 bulk-like system.We show that electrons can be transferred on demand from an AFM tip into single bulk-like C60 islands, which are supported on the insulating NaCl(001) surface. We exemplify this by controlled charge-manipulation experiments conducted in ultrahigh vacuum by noncontact AFM (nc-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM). KPFM shows a homogeneous contrast at the islands, which is a signature for an equal distribution of the electrons in the T1u band. The charge dissipates during half a day due to an interaction of the charged C60 islands with defects in the near surface region of NaCl. Our results open the perspective in photo-voltaics to study charge attachment, stability and charge exchange with the environment of any C60 bulk-like system. Electronic supplementary information (ESI) available. See DOI: 10.1039/C5NR04541J

  13. BOREAS AFM-04 Twin Otter Aircraft Flux Data

    NASA Technical Reports Server (NTRS)

    MacPherson, J. Ian; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Desjardins, Raymond L.; Smith, David E. (Technical Monitor)

    2000-01-01

    The BOREAS AFM-5 team collected and processed data from the numerous radiosonde flights during the project. The goals of the AFM-05 team were to provide large-scale definition of the atmosphere by supplementing the existing AES aerological network, both temporally and spatially. This data set includes basic upper-air parameters collected from the network of upper-air stations during the 1993, 1994, and 1996 field campaigns over the entire study region. The data are contained in tabular ASCII files. The data files are available on a CD-ROM (see document number 20010000884) or from the Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC).

  14. GPIM AF-M315E Propulsion System

    NASA Technical Reports Server (NTRS)

    Spores, Ronald A.; Masse, Robert; Kimbrel, Scott; McLean, Chris

    2014-01-01

    The NASA Space Technology mission Directorate's (STMD) Green Propellant Infusion Mission (GPIM) Technology Demonstration Mission (TDM) will demonstrate an operational AF-M315E green propellant propulsion system. Aerojet-Rocketdyne is responsible for the development of the propulsion system payload. This paper statuses the propulsion system module development, including thruster design and system design; Initial test results for the 1N engineering model thruster are presented. The culmination of this program will be high-performance, green AF-M315E propulsion system technology at TRL 7+, with components demonstrated to TRL 9, ready for direct infusion to a wide range of applications for the space user community.

  15. Solid-state linear sweep voltammetry. A probe of diffusion in thin films of polymer ion conductors on microdisk electrodes

    SciTech Connect

    Geng, L.; Reed, R.A.; Longmire, M.; Murray, R.W.

    1987-05-21

    Pt microdisk electrodes of diameter 10-70 ..mu..m sealed in glass, lying in the same plane with Ag pseudoreference and Pt auxiliary disk electrodes, and coated with a few micrometers of ionically conducting polymer film containing electroactive solutes provide a convenient experimental microcell format for solid-state linear sweep and cyclic voltammetry of the electroactive solutes. Transport rates of the solutes in the polymer depend on composition of the bathing (plasticizing) gas around the microcell, the temperature (polymer fluidity), and solute charge, size, and physical diffusion vs. electron self-exchange rates. Investigation of such transport phenomena requires theoretical analysis of the transport geometry of the microcell, which is the main subject of this paper. The preferred situations for measurements of transport rate are (i) polymer films thick in comparison to electrode diameter and transport rate, so that semi-infinite transport applies, and (ii) films thin in the same respects, so that currents are a summation of thin layer cell and microcylindrical geometries. Measured diffusion constants are confirmed with data from a four-electrode interdigitated array electrode experiment.

  16. AFM CHARACTERIZATION OF LASER INDUCED DAMAGE ON CDZNTE CRYSTAL SURFACES

    SciTech Connect

    Hawkins, S; Lucile Teague, L; Martine Duff, M; Eliel Villa-Aleman, E

    2008-06-10

    Semi-conducting CdZnTe (or CZT) crystals can be used in a variety of detector-type applications. CZT shows great promise for use as a gamma radiation spectrometer. However, its performance is adversely affected by point defects, structural and compositional heterogeneities within the crystals, such as twinning, pipes, grain boundaries (polycrystallinity), secondary phases and in some cases, damage caused by external forces. One example is damage that occurs during characterization of the surface by a laser during Raman spectroscopy. Even minimal laser power can cause Te enriched areas on the surface to appear. The Raman spectra resulting from measurements at moderate intensity laser power show large increases in peak intensity that is attributed to Te. Atomic Force Microscopy (AFM) was used to characterize the extent of damage to the CZT crystal surface following exposure to the Raman laser. AFM data reveal localized surface damage in the areas exposed to the Raman laser beam. The degree of surface damage to the crystal is dependent on the laser power, with the most observable damage occurring at high laser power. Moreover, intensity increases in the Te peaks of the Raman spectra are observed even at low laser power with little to no visible damage observed by AFM. AFM results also suggest that exposure to the same amount of laser power yields different amounts of surface damage depending on whether the exposed surface is the Te terminating face or the Cd terminating face of CZT.

  17. 3D Color Digital Elevation Map of AFM Sample

    NASA Technical Reports Server (NTRS)

    2008-01-01

    This color image is a three dimensional (3D) view of a digital elevation map of a sample collected by NASA's Phoenix Mars Lander's Atomic Force Microscope (AFM).

    The image shows four round pits, only 5 microns in depth, that were micromachined into the silicon substrate, which is the background plane shown in red. This image has been processed to reflect the levelness of the substrate.

    A Martian particle only one micrometer, or one millionth of a meter, across is held in the upper left pit.

    The rounded particle shown at the highest magnification ever seen from another world is a particle of the dust that cloaks Mars. Such dust particles color the Martian sky pink, feed storms that regularly envelop the planet and produce Mars' distinctive red soil.

    The particle was part of a sample informally called 'Sorceress' delivered to the AFM on the 38th Martian day, or sol, of the mission (July 2, 2008). The AFM is part of Phoenix's microscopic station called MECA, or the Microscopy, Electrochemistry, and Conductivity Analyzer.

    The AFM was developed by a Swiss-led consortium, with Imperial College London producing the silicon substrate that holds sampled particles.

    The Phoenix Mission is led by the University of Arizona, Tucson, on behalf of NASA. Project management of the mission is by NASA's Jet Propulsion Laboratory, Pasadena, Calif. Spacecraft development is by Lockheed Martin Space Systems, Denver.

  18. Structural investigations on native collagen type I fibrils using AFM

    SciTech Connect

    Strasser, Stefan; Zink, Albert; Janko, Marek; Heckl, Wolfgang M.; Thalhammer, Stefan . E-mail: stefan.thalhammer@gsf.de

    2007-03-02

    This study was carried out to determine the elastic properties of single collagen type I fibrils with the use of atomic force microscopy (AFM). Native collagen fibrils were formed by self-assembly in vitro characterized with the AFM. To confirm the inner assembly of the collagen fibrils, the AFM was used as a microdissection tool. Native collagen type I fibrils were dissected and the inner core uncovered. To determine the elastic properties of collagen fibrils the tip of the AFM was used as a nanoindentor by recording force-displacement curves. Measurements were done on the outer shell and in the core of the fibril. The structural investigations revealed the banding of the shell also in the core of native collagen fibrils. Nanoindentation experiments showed the same Young's modulus on the shell as well as in the core of the investigated native collagen fibrils. In addition, the measurements indicate a higher adhesion in the core of the collagen fibrils compared to the shell.

  19. Introduction to Atomic Force Microscopy (AFM) in Biology.

    PubMed

    Kreplak, Laurent

    2016-01-01

    The atomic force microscope (AFM) has the unique capability of imaging biological samples with molecular resolution in buffer solution over a wide range of time scales from milliseconds to hours. In addition to providing topographical images of surfaces with nanometer- to angstrom-scale resolution, forces between single molecules and mechanical properties of biological samples can be investigated from the nano-scale to the micro-scale. Importantly, the measurements are made in buffer solutions, allowing biological samples to "stay alive" within a physiological-like environment while temporal changes in structure are measured-e.g., before and after addition of chemical reagents. These qualities distinguish AFM from conventional imaging techniques of comparable resolution, e.g., electron microscopy (EM). This unit provides an introduction to AFM on biological systems and describes specific examples of AFM on proteins, cells, and tissues. The physical principles of the technique and methodological aspects of its practical use and applications are also described. © 2016 by John Wiley & Sons, Inc. PMID:27479503

  20. Hydrodynamic effects in fast AFM single-molecule force measurements.

    PubMed

    Janovjak, Harald; Struckmeier, Jens; Müller, Daniel J

    2005-02-01

    Atomic force microscopy (AFM) allows the critical forces that unfold single proteins and rupture individual receptor-ligand bonds to be measured. To derive the shape of the energy landscape, the dynamic strength of the system is probed at different force loading rates. This is usually achieved by varying the pulling speed between a few nm/s and a few microm/s, although for a more complete investigation of the kinetic properties higher speeds are desirable. Above 10 microm/s, the hydrodynamic drag force acting on the AFM cantilever reaches the same order of magnitude as the molecular forces. This has limited the maximum pulling speed in AFM single-molecule force spectroscopy experiments. Here, we present an approach for considering these hydrodynamic effects, thereby allowing a correct evaluation of AFM force measurements recorded over an extended range of pulling speeds (and thus loading rates). To support and illustrate our theoretical considerations, we experimentally evaluated the mechanical unfolding of a multi-domain protein recorded at 30 microm/s pulling speed. PMID:15257425

  1. AFM Structural Characterization of Drinking Water Biofilm under Physiological Conditions

    EPA Science Inventory

    Due to the complexity of mixed culture drinking water biofilm, direct visual observation under in situ conditions has been challenging. In this study, atomic force microscopy (AFM) revealed the three dimensional morphology and arrangement of drinking water relevant biofilm in air...

  2. Conductive supports for combined AFM SECM on biological membranes

    NASA Astrophysics Data System (ADS)

    Frederix, Patrick L. T. M.; Bosshart, Patrick D.; Akiyama, Terunobu; Chami, Mohamed; Gullo, Maurizio R.; Blackstock, Jason J.; Dooleweerdt, Karin; de Rooij, Nico F.; Staufer, Urs; Engel, Andreas

    2008-09-01

    Four different conductive supports are analysed regarding their suitability for combined atomic force and scanning electrochemical microscopy (AFM-SECM) on biological membranes. Highly oriented pyrolytic graphite (HOPG), MoS2, template stripped gold, and template stripped platinum are compared as supports for high resolution imaging of reconstituted membrane proteins or native membranes, and as electrodes for transferring electrons from or to a redox molecule. We demonstrate that high resolution topographs of the bacterial outer membrane protein F can be recorded by contact mode AFM on all four supports. Electrochemical feedback experiments with conductive cantilevers that feature nanometre-scale electrodes showed fast re-oxidation of the redox couple Ru(NH3)63+/2+ with the two metal supports after prolonged immersion in electrolyte. In contrast, the re-oxidation rates decayed quickly to unpractical levels with HOPG or MoS2 under physiological conditions. On HOPG we observed heterogeneity in the re-oxidation rate of the redox molecules with higher feedback currents at step edges. The latter results demonstrate the capability of conductive cantilevers with small electrodes to measure minor variations in an SECM signal and to relate them to nanometre-scale features in a simultaneously recorded AFM topography. Rapid decay of re-oxidation rate and surface heterogeneity make HOPG or MoS2 less attractive for combined AFM-SECM experiments on biological membranes than template stripped gold or platinum supports.

  3. Non-conductive nanomaterial enhanced electrochemical response in stripping voltammetry: The use of nanostructured magnesium silicate hollow spheres for heavy metal ions detection.

    PubMed

    Xu, Ren-Xia; Yu, Xin-Yao; Gao, Chao; Jiang, Yu-Jing; Han, Dong-Dong; Liu, Jin-Huai; Huang, Xing-Jiu

    2013-08-01

    Nanostructured magnesium silicate hollow spheres, one kind of non-conductive nanomaterials, were used in heavy metal ions (HMIs) detection with enhanced performance for the first time. The detailed study of the enhancing electrochemical response in stripping voltammetry for simultaneous detection of ultratrace Cd(2+), Pb(2+), Cu(2+) and Hg(2+) was described. Electrochemical properties of modified electrodes were characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The operational parameters which have influence on the deposition and stripping of metal ions, such as supporting electrolytes, pH value, and deposition time were carefully studied. The anodic stripping voltammetric performance toward HMIs was evaluated using square wave anodic stripping voltammetry (SWASV) analysis. The detection limits achieved (0.186nM, 0.247nM, 0.169nM and 0.375nM for Cd(2+), Pb(2+), Cu(2+) and Hg(2+)) are much lower than the guideline values in drinking water given by the World Health Organization (WHO). In addition, the interference and stability of the modified electrode were also investigated under the optimized conditions. An interesting phenomenon of mutual interference between different metal ions was observed. Most importantly, the sensitivity of Pb(2+) increased in the presence of certain concentrations of other metal ions, such as Cd(2+), Cu(2+) and Hg(2+) both individually and simultaneously. The proposed electrochemical sensing method is thus expected to open new opportunities to broaden the use of SWASV in analysis for detecting HMIs in the environment. PMID:23870406

  4. Novel Polymer Linkers for Single Molecule AFM Force Spectroscopy

    PubMed Central

    Tong, Zenghan; Mikheikin, Andrey; Krasnoslobodtsev, Alexey; Lv, Zhengjian; Lyubchenko, Yuri L.

    2013-01-01

    Flexible polymer linkers play an important role in various imaging and probing techniques that require surface immobilization, including atomic force microscopy (AFM). In AFM force spectroscopy, polymer linkers are necessary for the covalent attachment of molecules of interest to the AFM tip and the surface. The polymer linkers tether the molecules and provide their proper orientation in probing experiments. Additionally, the linkers separate specific interactions from nonspecific short-range adhesion and serve as a reference point for the quantitative analysis of single molecule probing events. In this report, we present our results on the synthesis and testing of a novel polymer linker and the identification of a number of potential applications for its use in AFM force spectroscopy experiments. The synthesis of the linker is based on the well-developed phosphoramidate (PA) chemistry that allows the routine synthesis of linkers with predetermined lengths and PA composition. These linkers are homogeneous in length and can be terminated with various functional groups. PA linkers with different functional groups were synthesized and tested in experimental systems utilizing different immobilization chemistries. We probed interactions between complementary DNA oligonucleotides; DNA and protein complexes formed by the site-specific binding protein SfiI; and interactions between amyloid peptide (Aβ42). The results of the AFM force spectroscopy experiments validated the feasibility of the proposed approach for the linker design and synthesis. Furthermore, the properties of the tether (length, functional groups) can be adjusted to meet the specific requirements for different force spectroscopy experiments and system characteristics, suggesting that it could be used for a large number of various applications. PMID:23624104

  5. MOS-based nanocapacitor using C-AFM

    NASA Astrophysics Data System (ADS)

    Hill, Daniel; Sadewasser, Sascha; Aymerich, Xavier

    2003-04-01

    This report details the attempts made to realise nanocapacitors for nanoscale MOS based integrated circuits by AFM anodic oxidation, and therefore isolation, of nano-sized squares of poly-silicon, titanium and aluminium on Si/SiO2. Conductive AFM (C-AFM) was used to perform topographical and electrical characterisation. The experiments were performed with contact mode C-AFM, in ambient air, using Pt-Ir, Co-Cr and Ti coated (20nm) n-type silicon cantilevers. Each sample consisted of a 3-5nm thick conductor deposited on 6nm of SiO2, which was thermally grown on Phosphorus doped (1019 cm-3) n-type Si(100) substrates. Standard cleaning and passivation processes were used. Poly-silicon was immediately found to be too rough to oxidise. Initial current-voltage measurements inside of the titanium-oxide squares suggest initial isolation followed by degradation through Fowler-Nordheim tunnelling. Measurement inconsistencies seen suggest charge storage on the surface or tip with the barrier height of the native titanium oxide thought to be responsible. Al has a thicker natural oxide. To overcome this we designed a series of structures consisting of a Ti finger on SiO2, that is connected to a Ti bond pad, allowing direct probing by a semiconductor parameter analyser. AFM anodic oxidation was performed upon these Ti fingers to reduce their in-plane dimensions towards the nanoscale. To confirm the existence of a nanocapacitor topographical and electrical measurements were then done on and around them.

  6. Amyloid-β peptides time-dependent structural modifications: AFM and voltammetric characterization.

    PubMed

    Enache, Teodor Adrian; Chiorcea-Paquim, Ana-Maria; Oliveira-Brett, Ana Maria

    2016-07-01

    The human amyloid beta (Aβ) peptides, Aβ1-40 and Aβ1-42, structural modifications, from soluble monomers to fully formed fibrils through intermediate structures, were investigated, and the results were compared with those obtained for the inverse Aβ40-1 and Aβ42-1, mutant Aβ1-40Phe(10) and Aβ1-40Nle(35), and rat Aβ1-40Rat peptide sequences. The aggregation was followed at a slow rate, in chloride free media and room temperature, and revealed to be a sequence-structure process, dependent on the physicochemical properties of each Aβ peptide isoforms, and occurring at different rates and by different pathways. The fibrilization process was investigated by atomic force microscopy (AFM), via changes in the adsorption morphology from: (i) initially random coiled structures of ∼0.6 nm height, corresponding to the Aβ peptide monomers in random coil or in α-helix conformations, to (ii) aggregates and protofibrils of 1.5-6.0 nm height and (iii) two types of fibrils, corresponding to the Aβ peptide in a β-sheet configuration. The reactivity of the carbon electrode surface was considered. The hydrophobic surface induced rapid changes of the Aβ peptide conformations, and differences between the adsorbed fibrils, formed at the carbon surface (beaded, thin, <2.0 nm height) or in solution (long, smooth, thick, >2.0 nm height), were detected. Differential pulse voltammetry showed that, according to their primary structure, the Aβ peptides undergo oxidation in one or two steps, the first step corresponding to the tyrosine amino acids oxidation, and the second one to the histidine and methionine amino acids oxidation. The fibrilization process was electrochemically detected via the decrease of the Aβ peptide oxidation peak currents that occurred in a time dependent manner. PMID:27216391

  7. Mercury(II) trace detection by a gold nanoparticle-modified glassy carbon electrode using square-wave anodic stripping voltammetry including a chloride desorption step.

    PubMed

    Laffont, Laure; Hezard, Teddy; Gros, Pierre; Heimbürger, Lars-Eric; Sonke, Jeroen E; Behra, Philippe; Evrard, David

    2015-08-15

    Gold nanoparticles (AuNPs) were deposited on a glassy carbon (GC) substrate by constant potential electrolysis and characterized by cyclic voltammetry in H2SO4 and field emission gun scanning electron microscopy (FEG-SEM). The modified AuNPs-GC electrode was used for low Hg(II) concentration detection using a Square Wave Anodic Stripping Voltammetry (SWASV) procedure which included a chloride desorption step. The comparison of the obtained results with our previous work in which no desorption step was used showed that this latter step significantly improved the analytical performances, providing a three time higher sensitivity and a limit of detection of 80pM for 300s preconcentration, as well as a lower average standard deviation. The influence of chloride concentration on the AuNPs-GC electrode response to Hg(II) trace amounts was also studied and its optimal value confirmed to be in the 10(-2)M range. Finally, the AuNPs-GC electrode was used for the determination of Hg(II) in a natural groundwater sample from south of France. By using a preconcentration time of 3000s, a Hg(II) concentration of 19±3pM was found, which compared well with the result obtained by cold vapor atomic fluorescence spectroscopy (22±2pM). PMID:25966376

  8. STM and AFM; Which is Better for Surface Structural Analysis? Non- contact AFM Studies on Ge/Si(105) Surface

    NASA Astrophysics Data System (ADS)

    Hasegawa, Yukio

    2006-03-01

    Scanning tunneling microscopy (STM) has been utilized to determine surface atomic structure with its highly resolved images. Probing surface electronic states near the Fermi energy (EF), STM images, however, do not necessarily represent the atomic structure of surfaces. It has been believed that atomic force microscopy (AFM) provides us surface topographic images without being disturbed by the electronic states. In order to prove the surpassing performance, we performed noncontact (nc) AFM on the Ge/Si(105) surface [1], which is a facet plane of the ?hut? clusters formed on Ge-deposited Si(001) surface. It is found that STM images taken on the surface, either filled- or empty-state images, do not show all surface atoms because of the electronic effect; some surface atoms have dangling bond states below EF and other surface atoms have states above EF. [2]. In a nc-AFM image, on the other hand, all surface atoms having a dangling bond are observed [3], directly representing an atomic structure of the surface. Electronic information can also be obtained in AFM by using a Kelvin-probe method. From atomically resolved potential profile we obtained, charge transfer among the dangling bond states is directly demonstrated. These results clearly demonstrate that highly-resolved nc-AFM with a Kelvin-probe method is an ideal tool for analysis of atomic structures and electronic properties of surfaces. This work was done in collaboration with T. Eguchi, K. Akiyama, T. An, and M. Ono, ISSP, Univ. Tokyo and JST, Y. Fujikawa and T. Sakurai, IMR. Tohoku Univ. T. Hashimoto, AIST, Y. Morikawa, ISIR, Osaka Univ. K. Terakura, Hokkaido Univ., and M.G. Lagally, University of Wisconsin-Madison. [1] T. Eguchi et al., Phys. Rev. Lett. 93, 266102 (2004). [2] Y. Fujikawa et al., Phys. Rev. Lett. 88, 176101 (2002). [3] T. Eguchi and Y. Hasegawa, Phys. Rev. Lett. 89, 256105 (2002)

  9. Ada and cyclic runtime scheduling

    NASA Technical Reports Server (NTRS)

    Hood, Philip E.

    1986-01-01

    An important issue that must be faced while introducing Ada into the real time world is efficient and prodictable runtime behavior. One of the most effective methods employed during the traditional design of a real time system is the cyclic executive. The role cyclic scheduling might play in an Ada application in terms of currently available implementations and in terms of implementations that might be developed especially to support real time system development is examined. The cyclic executive solves many of the problems faced by real time designers, resulting in a system for which it is relatively easy to achieve approporiate timing behavior. Unfortunately a cyclic executive carries with it a very high maintenance penalty over the lifetime of the software that is schedules. Additionally, these cyclic systems tend to be quite fragil when any aspect of the system changes. The findings are presented of an ongoing SofTech investigation into Ada methods for real time system development. The topics covered include a description of the costs involved in using cyclic schedulers, the sources of these costs, and measures for future systems to avoid these costs without giving up the runtime performance of a cyclic system.

  10. Cyclic AMP in prokaryotes.

    PubMed Central

    Botsford, J L; Harman, J G

    1992-01-01

    Cyclic AMP (cAMP) is found in a variety of prokaryotes including both eubacteria and archaebacteria. cAMP plays a role in regulating gene expression, not only for the classic inducible catabolic operons, but also for other categories. In the enteric coliforms, the effects of cAMP on gene expression are mediated through its interaction with and allosteric modification of a cAMP-binding protein (CRP). The CRP-cAMP complex subsequently binds specific DNA sequences and either activates or inhibits transcription depending upon the positioning of the complex relative to the promoter. Enteric coliforms have provided a model to explore the mechanisms involved in controlling adenylate cyclase activity, in regulating adenylate cyclase synthesis, and in performing detailed examinations of CRP-cAMP complex-regulated gene expression. This review summarizes recent work focused on elucidating the molecular mechanisms of CRP-cAMP complex-mediated processes. For other bacteria, less detail is known. cAMP has been implicated in regulating antibiotic production, phototrophic growth, and pathogenesis. A role for cAMP has been suggested in nitrogen fixation. Often the only data that support cAMP involvement in these processes includes cAMP measurement, detection of the enzymes involved in cAMP metabolism, or observed effects of high concentrations of the nucleotide on cell growth. PMID:1315922

  11. Cyclic Vomiting Syndrome

    PubMed Central

    2009-01-01

    Initially described in children, cyclic vomiting syndrome (CVS) is an idiopathic disorder that affects patients of all ages and is characterized by recurrent episodes of vomiting separated by symptom-free intervals or baseline health. Frequent misdiagnoses and delays in diagnosis often lead to years of recurrent vomiting. Similarities in the clinical features and symptoms of children and adults with CVS are often linked to migraines. Association with mitochondrial disorders and neuroendocrine dysfunction have been described in the pediatric CVS literature, whereas migraines, anxiety, and panic are common in adults with CVS. Various psychological, infectious, and physical stressors commonly precipitate episodes of CVS. Treatment is mostly empiric, with few controlled therapeutic studies conducted thus far. Associations with migraines have aided in developing pharmacologic treatment strategies for prophylaxis as well as abortive therapy during episodes, including the use of trip-tans. Most children outgrow CVS with time, though some children transition to migraine headaches or continue to have CVS as adults. Improved recognition of CVS in adults, along with the emergence of data in the use of anticonvulsants and antiemetics, may help further delineate pathophysiologic connections and therapeutic options for this debilitating disorder.

  12. Wedged AFM-cantilevers for parallel plate cell mechanics.

    PubMed

    Stewart, Martin P; Hodel, Adrian W; Spielhofer, Andreas; Cattin, Cedric J; Müller, Daniel J; Helenius, Jonne

    2013-04-01

    The combination of atomic force microscopy (AFM) and optical microscopy has gained popularity for mechanical analysis of living cells. In particular, recent AFM-based assays featuring tipless cantilevers and whole-cell deformation have yielded insights into cellular function, structure, and dynamics. However, in these assays the standard ≈10° tilt of the cantilever prevents uniaxial loading, which complicates assessment of cellular geometry and can cause cell sliding or loss of loosely adherent cells. Here, we describe an approach to modify tipless cantilevers with wedges and, thereby, achieve proper parallel plate mechanics. We provide guidance on material selection, the wedge production process, property and geometry assessment, and the calibration of wedged cantilevers. Furthermore, we demonstrate their ability to simplify the assessment of cell shape, prevent lateral displacement of round cells during compression, and improve the assessment of cell mechanical properties. PMID:23473778

  13. AFM-based mechanical characterization of single nanofibres.

    PubMed

    Neugirg, Benedikt R; Koebley, Sean R; Schniepp, Hannes C; Fery, Andreas

    2016-04-28

    Nanofibres are found in a broad variety of hierarchical biological systems as fundamental structural units, and nanofibrillar components are playing an increasing role in the development of advanced functional materials. Accurate determination of the mechanical properties of single nanofibres is thus of great interest, yet measurement of these properties is challenging due to the intricate specimen handling and the exceptional force and deformation resolution that is required. The atomic force microscope (AFM) has emerged as an effective, reliable tool in the investigation of nanofibrillar mechanics, with the three most popular approaches-AFM-based tensile testing, three-point deformation testing, and nanoindentation-proving preferable to conventional tensile testing in many (but not all) cases. Here, we review the capabilities and limitations of each of these methods and give a comprehensive overview of the recent advances in this field. PMID:27055900

  14. Insights into Epoxy Network Nanostructural Heterogeneity Using AFM-IR.

    PubMed

    Morsch, Suzanne; Liu, Yanwen; Lyon, Stuart B; Gibbon, Simon R

    2016-01-13

    The first direct observation of a chemically heterogeneous nanostructure within an epoxy resin is reported. Epoxy resins comprise the matrix component of many high performance composites, coatings and adhesives, yet the molecular network structure that underpins the performance of these industrially essential materials is not well understood. Internal nodular morphologies have repeatedly been reported for epoxy resins analyzed using SEM or AFM, yet the origin of these features remains a contentious subject, and epoxies are still commonly assumed to be chemically homogeneous. Uniquely, in this contribution we use the recently developed AFM-IR technique to eliminate previous differences in interpretation, and establish that nodule features correspond to heterogeneous network connectivity within an epoxy phenolic formulation. PMID:26694687

  15. Nano-Bio-Mechanics of Neuroblastoma Cells Using AFM

    NASA Astrophysics Data System (ADS)

    Bastatas, Lyndon; Matthews, James; Kang, Min; Park, Soyeun

    2011-10-01

    We have conducted an in vitro study to determine the elastic moduli of neurobalstoma cell lines using atomic force microscopy. Using a panel of cell lines established from neuroblastoma patients at different stages of disease progress and treatment, we have investigated the differences in elastic moduli during a course of cancer progression and chemotherapy. The cells were grown on the hard substrates that are chemically functionalized to enhance adhesion. We have performed the AFM indentation experiments with different applied forces from the AFM probe. For the purpose of the comparison between cell lines, the indentations were performed only on cell centers. The obtained force-distance curves were analyzed using the Hertz model in order to extract the elastic moduli. We have found that the elastic moduli of human neuroblastoma cells significantly varied during the disease progression. We postulate that the observed difference might be affected by the treatment and chemotherapy.

  16. AFM-based mechanical characterization of single nanofibres

    NASA Astrophysics Data System (ADS)

    Neugirg, Benedikt R.; Koebley, Sean R.; Schniepp, Hannes C.; Fery, Andreas

    2016-04-01

    Nanofibres are found in a broad variety of hierarchical biological systems as fundamental structural units, and nanofibrillar components are playing an increasing role in the development of advanced functional materials. Accurate determination of the mechanical properties of single nanofibres is thus of great interest, yet measurement of these properties is challenging due to the intricate specimen handling and the exceptional force and deformation resolution that is required. The atomic force microscope (AFM) has emerged as an effective, reliable tool in the investigation of nanofibrillar mechanics, with the three most popular approaches--AFM-based tensile testing, three-point deformation testing, and nanoindentation--proving preferable to conventional tensile testing in many (but not all) cases. Here, we review the capabilities and limitations of each of these methods and give a comprehensive overview of the recent advances in this field.

  17. Molecular modeling of enzyme attachment on AFM probes.

    PubMed

    Oliveira, Guedmiller S; Leite, Fabio L; Amarante, Adriano M; Franca, Eduardo F; Cunha, Richard A; Briggs, James M; Freitas, Luiz C G

    2013-09-01

    The immobilization of enzymes on atomic force microscope tip (AFM tip) surface is a crucial step in the development of nanobiosensors to be used in detection process. In this work, an atomistic modeling of the attachment of the acetyl coenzyme A carboxylase (ACC enzyme) on a functionalized AFM tip surface is proposed. Using electrostatic considerations, suitable enzyme-surface orientations with the active sites of the ACC enzyme available for interactions with bulk molecules were found. A 50 ns molecular dynamics trajectory in aqueous solution was obtained and surface contact area, hydrogen bonding and protein stability were analyzed. The enzyme-surface model proposed here with minor adjustment can be applied to study antigen-antibody interactions as well as enzyme immobilization on silica for chromatography applications. PMID:24029365

  18. AFM study of polymer lubricants on hard disk surfaces

    NASA Astrophysics Data System (ADS)

    Bao, G. W.; Troemel, M.; Li, S. F. Y.

    Thin liquid films of PFPE (perfluoropolyether) lubricants dip-coated on hard disk surfaces were imaged with non-contact mode AFM. Demnum lubricants with phosphazene additives exhibited strong interactions with a silicon tip due to the formation of liquid bridges between the lubricants and the tip, as indicated by a remarkable hysteresis loop between approach and retraction curves in force vs. distance measurements. Features resulting from capillary forces due to tip tapping to the lubricants were revealed, which demonstrated that the capillary forces could be used to lock the non-contacting tip at a certain separation from the substrate surface to obtain AFM images. Force vs. distance curves for Fomblin Z-dol lubricants showed negligible hysteresis effects and features corresponding to lateral distortion of the tip by the lubricants only were observed. In both cases, only when the tip was positioned far above the surfaces could the natural distributions of the lubricants be imaged.

  19. BOREAS AFM-5 Level-1 Upper Air Network Data

    NASA Technical Reports Server (NTRS)

    Barr, Alan; Hrynkiw, Charmaine; Newcomer, Jeffrey A. (Editor); Hall, Forrest G. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-5 team collected and processed data from the numerous radiosonde flights during the project. The goals of the AFM-05 team were to provide large-scale definition of the atmosphere by supplementing the existing Atmospheric Environment Service (AES) aerological network, both temporally and spatially. This data set includes basic upper-air parameters collected from the network of upper-air stations during the 1993, 1994, and 1996 field campaigns over the entire study region. The data are contained in tabular ASCII files. The level-1 upper-air network data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files also are available on a CD-ROM (see document number 20010000884).

  20. Adhesion forces in AFM of redox responsive polymer grafts: Effects of tip hydrophilicity

    NASA Astrophysics Data System (ADS)

    Feng, Xueling; Kieviet, Bernard D.; Song, Jing; Schön, Peter M.; Vancso, G. Julius

    2014-02-01

    The adherence between silicon nitride AFM tips and redox-active poly(ferrocenylsilanes) (PFS) grafts on gold was investigated by electrochemical AFM force spectroscopy. Before the adhesion measurements silicon nitride AFM probes were cleaned with organic solvents (acetone and ethanol) or piranha solution. Interestingly, these different AFM tip cleaning procedures drastically affected the observed adhesion forces. Water contact angle measurements on the corresponding AFM probe chips showed that piranha treatment resulted in a significant increase of AFM probe chip surface hydrophilicity compared to the organic solvent treatment. Obviously this hydrophilicity change caused drastic, even opposite changes in the tip-PFS adhesive force measurement upon electrode potential change to reversibly oxidize and reduce the PFS grafts. Our findings are of pivotal importance for AFM tip adhesion measurements utilizing standard silicon nitride AFM tips. Probe hydrophilicity must be carefully taken into consideration and controlled.

  1. LET Spectrum Measurements In CR-39 PNTD With AFM

    NASA Astrophysics Data System (ADS)

    Johnson, C. E.; DeWitt, J. M.; Benton, E. R.; Yasuda, N.; Benton, E. V.

    2011-06-01

    Energetic protons, neutrons, and heavy ions undergoing collisions with target nuclei of varying Z can produce residual heavy recoil fragments via intra-nuclear cascade/evaporation reactions. The particles produced in these non-elastic collisions generally have such extremely short range (˜<10 μm) that they cannot be directly observed by conventional detection methods including CR-39 plastic nuclear track detector (PNTD) that has been chemically etched for analysis by standard visible light microscopy. However, high-LET recoil fragments having range on the order of several cell diameters can be produced in tissue during radiotherapy using proton and carbon beams. We have developed a method to analyze short-range, high-LET tracks in CR-39 plastic nuclear track detector (PNTD) using short duration chemical etching (˜<1 μm) following by automated atomic force microscope (AFM) scanning. The post-scan data processing used in this work was based on semi-automated matrix analysis opposed to traditional grey-scale image analysis. This method takes advantage of the 3-D data obtained via AFM to achieve robust discrimination of nuclear tracks from other features inherently present in the post-etch detector surface. Through automation of AFM scanning, sufficient AFM scan frames were obtained to attain an LET spectrum spanning the LET range from 200-1500 keV/μm. In addition to our experiments, simulations were carried out with the Monte Carlo transport code, FLUKA. To demonstrate this method, CR-39 PNTD was exposed to the proton therapy beam at Loma Linda University Medical Center (LLUMC) at 60 and 230 MeV. Additionally, detectors were exposed to 1 GeV protons at the NASA Space Radiation Laboratory (NSRL) at Brookhaven National Laboratory (BNL). For these exposures CR-39 PNTD, Al and Cu target foils were used between detector layers.

  2. AFM and SThM Characterization of Graphene

    NASA Astrophysics Data System (ADS)

    Foy, Christopher; Sidorov, Anton; Chen, Xunchi; Ruan, Ming; Berger, Claire; de Heer, Walter; Jiang, Zhigang

    2012-03-01

    We report on detailed characterization of epitaxial grown graphene on SiC and chemical vapor deposition grown graphene on Cu foil using atomic force microscopy (AFM) and scanning thermal microscopy (SThM). We focus on the electronic and thermal properties of graphene grain boundaries, and thus providing valuable feedback to materials growth. Specifically, we perform thermal conductivity contrast mapping and surface potential mapping of graphene, and compare with that obtained on the Au electrodes and the substrate.

  3. Investigation of biopolymer networks by means of AFM

    NASA Astrophysics Data System (ADS)

    Keresztes, Z.; Rigó, T.; Telegdi, J.; Kálmán, E.

    Natural hydrogel alginate was investigated by means of atomic force microscopy (AFM) to gain microscale information on the morphological and rheological properties of the biopolymer network cross-linked by various cations. Local rheological properties of the gels measured by force spectroscopy gave correlation between increasing ion selectivity and increasing polymer elasticity. Adhesive forces acting between the surface of the gel and the probe, and also the intrinsic rheological properties of bulk polymers affect the microscopical image formation.

  4. LET Spectrum Measurements In CR-39 PNTD With AFM

    SciTech Connect

    Johnson, C. E.; DeWitt, J. M.; Benton, E. R.; Yasuda, N.; Benton, E. V.

    2011-06-01

    Energetic protons, neutrons, and heavy ions undergoing collisions with target nuclei of varying Z can produce residual heavy recoil fragments via intra-nuclear cascade/evaporation reactions. The particles produced in these non-elastic collisions generally have such extremely short range ({approx}<10 {mu}m) that they cannot be directly observed by conventional detection methods including CR-39 plastic nuclear track detector (PNTD) that has been chemically etched for analysis by standard visible light microscopy. However, high-LET recoil fragments having range on the order of several cell diameters can be produced in tissue during radiotherapy using proton and carbon beams. We have developed a method to analyze short-range, high-LET tracks in CR-39 plastic nuclear track detector (PNTD) using short duration chemical etching ({approx}<1 {mu}m) following by automated atomic force microscope (AFM) scanning. The post-scan data processing used in this work was based on semi-automated matrix analysis opposed to traditional grey-scale image analysis. This method takes advantage of the 3-D data obtained via AFM to achieve robust discrimination of nuclear tracks from other features inherently present in the post-etch detector surface. Through automation of AFM scanning, sufficient AFM scan frames were obtained to attain an LET spectrum spanning the LET range from 200-1500 keV/{mu}m. In addition to our experiments, simulations were carried out with the Monte Carlo transport code, FLUKA. To demonstrate this method, CR-39 PNTD was exposed to the proton therapy beam at Loma Linda University Medical Center (LLUMC) at 60 and 230 MeV. Additionally, detectors were exposed to 1 GeV protons at the NASA Space Radiation Laboratory (NSRL) at Brookhaven National Laboratory (BNL). For these exposures CR-39 PNTD, Al and Cu target foils were used between detector layers.

  5. Quantitative nano-mechanics of biological cells with AFM

    NASA Astrophysics Data System (ADS)

    Sokolov, Igor

    2013-03-01

    The importance of study of living cells is hard to overestimate. Cell mechanics is a relatively young, yet not a well-developed area. Besides just a fundamental interest, large practical need has emerged to measure cell mechanics quantitatively. Recent studies revealed a significant correlation between stiffness of biological cells and various human diseases, such as cancer, malaria, arthritis, and even aging. However, really quantitative studies of mechanics of biological cells are virtually absent. It is not even clear if the cell, being a complex and heterogeneous object, can be described by the elastic modulus at all. Atomic force microscopy (AFM) is a natural instrument to study properties of cells in their native environments. Here we will demonstrate that quantitative measurements of elastic modulus of cells with AFM are possible. Specifically, we will show that the ``cell body'' (cell without ``brush'' surface layer, a non-elastic layer surrounding cells) typically demonstrates the response of a homogeneous elastic medium up to the deformation of 10-20%, but if and only if a) the cellular brush layer is taken into account, b) rather dull AFM probes are used. This will be justified with the help of the strong condition of elastic behavior of material: the elastic modulus is shown to be independent on the indentation depth. We will also demonstrate that an attempt either to ignore the brush layer or to use sharp AFM probes will result in the violation of the strong condition, which implies impossibility to use the concept of the elastic modulus to describe cell mechanics in such experiments. Examples of quantitative measurements of the Young's modulus of the cell body and the cell brush parameters will be given for various cells. Address when submitting: Clarkson University, Potsdam, NY 13699

  6. LET spectrum measurements in Cr-39 PNTD with AFM

    SciTech Connect

    Johnson, Carl Edward; De Witt, Joel M; Benton, Eric R; Yasuda, Nakahiro; Benton, Eugene V

    2010-01-01

    Energetic protons, neutrons, and heavy ions undergoing collisions with target nuclei of varying Z can produce residual heavy recoil fragments via intra-nuclear cascade/evaporation reactions. The particles produced in these non-elastic collisions generally have such extremely short range ({approx}< 10 {mu}m) that they cannot be directly observed by conventional detection methods including CR-39 plastic nuclear track detector (PNTD) that has been chemically etched for analysis by standard visible light microscopy. However, high-LET recoil fragments having range on the order of several cell diameters can be produced in tissue during radiotherapy using proton and carbon beams. We have developed a method to analyze short-range, high-LET tracks in CR-39 plastic nuclear track detector (PNTD) using short duration chemical etching ({approx}< 1 {mu}m) followed by automated atomic force microscope (AFM) scanning. The post-scan data processing used in this work was based on semi-automated matrix analysis opposed to traditional grey-scale image analysis. This method takes advantage of the 3-D data obtained via AFM to achieve robust discrimination of nuclear tracks from other features. Through automation of AFM scanning, sufficient AFM scan frames were obtained to attain an LET spectrum spanning the LET range from 200-1500 keV/{mu}m. In addition to our experiments, simulations were carried out with the Monte Carlo transport code, FLUKA. To demonstrate this method, CR-39 PNTD was exposed to the proton therapy beam at Loma Linda University Medical Center (LLUMC) at 60 and 230 MeV. Additionally, detectors were exposed to I GeV protons at the NASA Space Radiation Laboratory (NSRL) at Brookhaven National Laboratory (BNL). For these exposures CR-39 PNTD, Al and Cu target foils were used between detector layers.

  7. Sequence-controlled RNA self-processing: computational design, biochemical analysis, and visualization by AFM

    PubMed Central

    Petkovic, Sonja; Badelt, Stefan; Flamm, Christoph; Delcea, Mihaela

    2015-01-01

    Reversible chemistry allowing for assembly and disassembly of molecular entities is important for biological self-organization. Thus, ribozymes that support both cleavage and formation of phosphodiester bonds may have contributed to the emergence of functional diversity and increasing complexity of regulatory RNAs in early life. We have previously engineered a variant of the hairpin ribozyme that shows how ribozymes may have circularized or extended their own length by forming concatemers. Using the Vienna RNA package, we now optimized this hairpin ribozyme variant and selected four different RNA sequences that were expected to circularize more efficiently or form longer concatemers upon transcription. (Two-dimensional) PAGE analysis confirms that (i) all four selected ribozymes are catalytically active and (ii) high yields of cyclic species are obtained. AFM imaging in combination with RNA structure prediction enabled us to calculate the distributions of monomers and self-concatenated dimers and trimers. Our results show that computationally optimized molecules do form reasonable amounts of trimers, which has not been observed for the original system so far, and we demonstrate that the combination of theoretical prediction, biochemical and physical analysis is a promising approach toward accurate prediction of ribozyme behavior and design of ribozymes with predefined functions. PMID:25999318

  8. Near-Field Spectroscopy with Nanoparticles Deposited by AFM

    NASA Technical Reports Server (NTRS)

    Anderson, Mark S.

    2008-01-01

    An alternative approach to apertureless near-field optical spectroscopy involving an atomic-force microscope (AFM) entails less complexity of equipment than does a prior approach. The alternative approach has been demonstrated to be applicable to apertureless near-field optical spectroscopy of the type using an AFM and surface enhanced Raman scattering (SERS), and is expected to be equally applicable in cases in which infrared or fluorescence spectroscopy is used. Apertureless near-field optical spectroscopy is a means of performing spatially resolved analyses of chemical compositions of surface regions of nanostructured materials. In apertureless near-field spectroscopy, it is common practice to utilize nanostructured probe tips or nanoparticles (usually of gold) having shapes and dimensions chosen to exploit plasmon resonances so as to increase spectroscopic-signal strengths. To implement the particular prior approach to which the present approach is an alternative, it is necessary to integrate a Raman spectrometer with an AFM and to utilize a special SERS-active probe tip. The resulting instrumentation system is complex, and the tasks of designing and constructing the system and using the system to acquire spectro-chemical information from nanometer-scale regions on a surface are correspondingly demanding.

  9. Tissue section AFM: In situ ultrastructural imaging of native biomolecules

    PubMed Central

    Graham, Helen K.; Hodson, Nigel W.; Hoyland, Judith A.; Millward-Sadler, Sarah J.; Garrod, David; Scothern, Anthea; Griffiths, Christopher E.M.; Watson, Rachel E.B.; Cox, Thomas R.; Erler, Janine T.; Trafford, Andrew W.; Sherratt, Michael J.

    2010-01-01

    Conventional approaches for ultrastructural high-resolution imaging of biological specimens induce profound changes in bio-molecular structures. By combining tissue cryo-sectioning with non-destructive atomic force microscopy (AFM) imaging we have developed a methodology that may be applied by the non-specialist to both preserve and visualize bio-molecular structures (in particular extracellular matrix assemblies) in situ. This tissue section AFM technique is capable of: i) resolving nm–µm scale features of intra- and extracellular structures in tissue cryo-sections; ii) imaging the same tissue region before and after experimental interventions; iii) combining ultrastructural imaging with complimentary microscopical and micromechanical methods. Here, we employ this technique to: i) visualize the macro-molecular structures of unstained and unfixed fibrillar collagens (in skin, cartilage and intervertebral disc), elastic fibres (in aorta and lung), desmosomes (in nasal epithelium) and mitochondria (in heart); ii) quantify the ultrastructural effects of sequential collagenase digestion on a single elastic fibre; iii) correlate optical (auto fluorescent) with ultrastructural (AFM) images of aortic elastic lamellae. PMID:20144712

  10. Nanoscale rippling on polymer surfaces induced by AFM manipulation

    PubMed Central

    2015-01-01

    Summary Nanoscale rippling induced by an atomic force microscope (AFM) tip can be observed after performing one or many scans over the same area on a range of materials, namely ionic salts, metals, and semiconductors. However, it is for the case of polymer films that this phenomenon has been widely explored and studied. Due to the possibility of varying and controlling various parameters, this phenomenon has recently gained a great interest for some technological applications. The advent of AFM cantilevers with integrated heaters has promoted further advances in the field. An alternative method to heating up the tip is based on solvent-assisted viscoplastic deformations, where the ripples develop upon the application of a relatively low force to a solvent-rich film. An ensemble of AFM-based procedures can thus produce nanoripples on polymeric surfaces quickly, efficiently, and with an unprecedented order and control. However, even if nanorippling has been observed in various distinct modes and many theoretical models have been since proposed, a full understanding of this phenomenon is still far from being achieved. This review aims at summarizing the current state of the art in the perspective of achieving control over the rippling process on polymers at a nanoscale level. PMID:26733086

  11. AFM imaging of functionalized carbon nanotubes on biological membranes

    NASA Astrophysics Data System (ADS)

    Lamprecht, C.; Liashkovich, I.; Neves, V.; Danzberger, J.; Heister, E.; Rangl, M.; Coley, H. M.; McFadden, J.; Flahaut, E.; Gruber, H. J.; Hinterdorfer, P.; Kienberger, F.; Ebner, A.

    2009-10-01

    Multifunctional carbon nanotubes are promising for biomedical applications as their nano-size, together with their physical stability, gives access into the cell and various cellular compartments including the nucleus. However, the direct and label-free detection of carbon nanotube uptake into cells is a challenging task. The atomic force microscope (AFM) is capable of resolving details of cellular surfaces at the nanometer scale and thus allows following of the docking of carbon nanotubes to biological membranes. Here we present topographical AFM images of non-covalently functionalized single walled (SWNT) and double walled carbon nanotubes (DWNT) immobilized on different biological membranes, such as plasma membranes and nuclear envelopes, as well as on a monolayer of avidin molecules. We were able to visualize DWNT on the nuclear membrane while at the same time resolving individual nuclear pore complexes. Furthermore, we succeeded in localizing individual SWNT at the border of incubated cells and in identifying bundles of DWNT on cell surfaces by AFM imaging.

  12. Investigation of the Mechanoelectrical Transduction at Single Stereocilia by Afm

    NASA Astrophysics Data System (ADS)

    Langer, M. G.; Fink, S.; Löffler, K.; Koitschev, A.; Zenner, H.-P.

    2003-02-01

    The transduction of sound into an electrical signal in the inner ear is closely related to the mechanical properties of the hair bundles cytoskeleton and cross-linkage. In this study the effect of lateral cross-links on hair bundle mechanics and the transduction current response is demonstrated on the level of individual stereocilia. For experiments stereocilia of outer hair cells of postnatal rats (P3 - P8) were scanned with a sharp AFM tip at nanometerscale. Transduction currents were simultaneously recorded in the whole-cell-recording mode with patch clamp. AFM was used as a nanotool for local mechanical stimulation and force measurement at stereocilia whereas patch clamp serves as a detector for the electrical response of the cell. In a first experiment force transmission between adjacent stereocilia of the V- and W- shaped hair bundles of outer hair cells was investigated. Results showed that a force exerted to a single stereocilium declined to 36 % at the nearest adjacent stereocilium of the same row. This result supposes AFM to be convenient for local displacement of single stereocilia. For control, the local response of transduction channels was measured at single stereocilia of the same hair bundle. Measured transduction current amplitudes ranged from 9 to 49 pA supposing an opening of one to five transduction channels. Both, weak force transmission by lateral cross-links and small transduction current amplitudes indicate a weak mechanical interaction between individual stereocilia of the tallest row of stereocilia of outer hair cells from postnatal rats.

  13. Oxide nanocrystal based nanocomposites for fabricating photoplastic AFM probes.

    PubMed

    Ingrosso, Chiara; Martin-Olmos, Cristina; Llobera, Andreu; Innocenti, Claudia; Sangregorio, Claudio; Striccoli, Marinella; Agostiano, Angela; Voigt, Anja; Gruetzner, Gabi; Brugger, Jürgen; Perez-Murano, Francesc; Curri, Maria Lucia

    2011-11-01

    We report on the synthesis, characterization and application of a novel nanocomposite made of a negative tone epoxy based photoresist modified with organic-capped Fe(2)O(3) nanocrystals (NCs). The mechanical properties of the nanocomposite drastically improve upon incorporation of a suitable concentration of NCs in the polymer, without deteriorating its photolithography performance. High aspect ratio 3D microstructures made of the nanocomposite have been fabricated with a uniform surface morphology and with a resolution down to few micrometres. The embedded organic-capped Fe(2)O(3) NCs drastically increase the stiffness and hardness of the epoxy based photoresist matrix, making the final material extremely interesting for manufacturing miniaturized polymer based mechanical devices and systems. In particular, the nanocomposite has been used as structural material for fabricating photoplastic Atomic Force Microscopy (AFM) probes with integrated tips showing outstanding mechanical response and high resolution imaging performance. The fabricated probes consist of straight cantilevers with low stress-gradient and high quality factors, incorporating sharp polymeric tips. They present considerably improved performance compared to pure epoxy based photoresist AFM probes, and to commercial silicon AFM probes. PMID:21858377

  14. Bioactive compounds immobilized on Ti and TiNbHf: AFM-based investigations of biofunctionalization efficiency and cell adhesion.

    PubMed

    Herranz-Diez, C; Li, Q; Lamprecht, C; Mas-Moruno, C; Neubauer, S; Kessler, H; Manero, J M; Guillem-Martí, J; Selhuber-Unkel, C

    2015-12-01

    Implant materials require optimal biointegration, including strong and stable cell-material interactions from the early stages of implantation. Ti-based alloys with low elastic modulus are attracting a lot of interest for avoiding stress shielding, but their osseointegration potential is still very low. In this study, we report on how cell adhesion is influenced by linear RGD, cyclic RGD, and recombinant fibronectin fragment III8-10 coated on titanium versus a novel low-modulus TiNbHf alloy. The bioactive molecules were either physisorbed or covalently coupled to the substrates and their conformation on the surfaces was investigated with atomic force microscopy (AFM). The influence of the different bioactive coatings on the adhesion of rat mesenchymal stem cells was evaluated using cell culture assays and quantitatively analyzed at the single cell level by AFM-based single-cell force spectroscopy. Our results show that bioactive moieties, particularly fibronectin fragment III8-10, improve cell adhesion on titanium and TiNbHf and that the covalent tethering of such molecules provides the most promising strategy to biofunctionalize these materials. Therefore, the use of recombinant protein fragments is of high importance for improving the osseointegration potential of implant materials. PMID:26513753

  15. Reinterpretation of reduction potential measurements done by linear sweep voltammetry in silicate melts

    NASA Technical Reports Server (NTRS)

    Colson, R. O.; Haskin, L. A.; Keedy, C. R.

    1991-01-01

    The equilibrium concentrations of Ni between silicate melt and Pt were determined experimentally as a function of oxygen fugacity. The results demonstrate that metallic species derived in linear sweep voltammetry experiments in silicate melts are diffusing into Pt electrodes and not into the melt, as was concluded by previoius studies. This requires reinterpretation of previous linear sweep voltammetry results and recalculation and correction of reported reduction potentials. This paper reports these corrected reduction potentials. Also reported are the activity coefficients for Ni in synthetic basalt and diopsidic melts and for Co in diopsidic melt.

  16. Cyclic performance tests of Sn/MWCNT composite lithium ion battery anodes at different temperatures

    NASA Astrophysics Data System (ADS)

    Tocoglu, U.; Cevher, O.; Akbulut, H.

    2016-04-01

    In this study tin-multi walled carbon nanotube (Sn-MWCNT) lithium ion battery anodes were produced and their electrochemical galvanostatic charge/discharge tests were conducted at various (25 °C, 35 °C, 50 °C) temperatures to determine the cyclic behaviors of anode at different temperatures. Anodes were produced via vacuum filtration and DC magnetron sputtering technique. Tin was sputtered onto buckypapers to form composite structure of anodes. SEM analysis was conducted to determine morphology of buckypapers and Sn-MWCNT composite anodes. Structural and phase analyses were conducted via X-ray diffraction and Raman Spectroscopy technique. CR2016 coin cells were assembled for electrochemical tests. Cyclic voltammetry test were carried out to determine the reversibility of reactions between anodes and reference electrode between 0.01-2.0 V potential window. Galvanostatic charge/discharge tests were performed to determine cycle performance of anodes at different temperatures.

  17. Adsorptive Stripping Voltammetry of Environmental Indicators: Determination of Zinc in Algae

    ERIC Educational Resources Information Center

    Collado-Sanchez, C.; Hernandez-Brito, J. J.; Perez-Pena, J.; Torres-Padron, M. E.; Gelado-Caballero, M. D.

    2005-01-01

    A method for sample preparation and for the determination of average zinc content in algae using adsorptive stripping voltammetry are described. The students gain important didactic advantages through metal determination in environmental matrices, which include carrying out clean protocols for sampling and handling, and digesting samples using…

  18. DETERMINATION OF ZINC, CADMIUM, LEAD, AND COPPER IN WATER BY ANODIC STRIPPING VOLTAMMETRY

    EPA Science Inventory

    The Tennessee Valley Authority developed a method of differential pulse anodic stripping voltammetry for determining total concentrations of cadmium and lead in water samples from ash ponds at steam-electric generating plants. After digestion of the sample and addition of reagent...

  19. The Rise of Voltammetry: From Polarography to the Scanning Electrochemical Microscope

    ERIC Educational Resources Information Center

    Bard, Allen J.

    2007-01-01

    The drooping mercury electrode (DME) was previously used to carry out electrochemical experiments but invention of polarography technique changed this. Voltammetry with DME was given the term polarography and are used in measurement of current as a function of potential at small electrodes.

  20. Lead-Testing Service to Elementary and Secondary Schools Using Anodic Stripping Voltammetry

    ERIC Educational Resources Information Center

    Goebel, Amanda; Vos, Tracy; Louwagie, Anne; Lundbohm, Laura; Brown, Jay H.

    2004-01-01

    The undergraduate chemistry club of the Southwest Minnesota State University offers assistance in lead-testing through the anodic stripping voltammetry (ASV) technique to elementary and secondary schools. Emphasis is given to this community service activity, which has increased club membership, and promoted discussion of water quality problems in…

  1. Solvent-mediated repair and patterning of surfaces by AFM

    SciTech Connect

    Elhadj, S; Chernov, A; De Yoreo, J

    2007-10-30

    A tip-based approach to shaping surfaces of soluble materials with nanometer-scale control is reported. The proposed method can be used, for example, to eliminate defects and inhomogeneities in surface shape, repair mechanical or laser-induced damage to surfaces, or perform 3D lithography on the length scale of an AFM tip. The phenomenon that enables smoothing and repair of surfaces is based on the transport of material from regions of high- to low-curvature within the solution meniscus formed in a solvent-containing atmosphere between the surface in question and an AFM tip scanned over the surface. Using in situ AFM measurements of the kinetics of surface remodeling on KDP (KH{sub 2}PO{sub 4}) crystals in humid air, we show that redistribution of solute material during relaxation of grooves and mounds is driven by a reduction in surface free energy as described by the Gibbs-Thomson law. We find that the perturbation from a flat interface evolves according to the diffusion equation where the effective diffusivity is determined by the product of the surface stiffness and the step kinetic coefficient. We also show that, surprisingly, if the tip is instead scanned over or kept stationary above an atomically flat area of the surface, a convex structure is formed with a diameter that is controlled by the dimensions of the meniscus, indicating that the presence of the tip and meniscus reduces the substrate chemical potential beneath that of the free surface. This allows one to create nanometer-scale 3D structures of arbitrary shape without the removal of substrate material or the use of extrinsic masks or chemical compounds. Potential applications of these tip-based phenomena are discussed.

  2. Applications of AFM for atomic manipulation and spectroscopy

    NASA Astrophysics Data System (ADS)

    Custance, Oscar

    2009-03-01

    Since the first demonstration of atom-by-atom assembly [1], atomic manipulation with scanning tunneling microscopy has yielded stunning realizations in nanoscience. A new exciting panorama has been recently opened with the possibility of manipulating atoms at surfaces using atomic force microscopy (AFM) [2-5]. In this talk, we will present two different approaches that enable patterning structures at semiconductor surfaces by manipulating individual atoms with AFM and at room temperature [2, 3]. We will discuss the physics behind each protocol through the analysis of the measured forces associated with these manipulations [3-5]. Another challenging issue in scanning probe microscopy is the ability to disclose the local chemical composition of a multi-element system at atomic level. Here, we will introduce a single-atom chemical identification method, which is based on detecting the forces between the outermost atom of the AFM tip and the atoms at a surface [6]. We demonstrate this identification procedure on a particularly challenging system, where any discrimination attempt based solely on topographic measurements would be impossible to achieve. [4pt] References: [0pt] [1] D. M. Eigler and E. K. Schweizer, Nature 344, 524 (1990); [0pt] [2] Y. Sugimoto, M. Abe, S. Hirayama, N. Oyabu, O. Custance and S. Morita, Nature Materials 4, 156 (2005); [0pt] [3] Y. Sugimoto, P. Pou, O. Custance, P. Jelinek, M. Abe, R. Perez and S. Morita, Science 322, 413 (2008); [0pt] [4] Y. Sugimoto, P. Jelinek, P. Pou, M. Abe, S. Morita, R. Perez and O. Custance, Phys. Rev. Lett. 98, 106104 (2007); [0pt] [5] M. Ternes, C. P. Lutz, C. F. Hirjibehedin, F. J. Giessibl and A. J. Heinrich, Science 319, 1066 (2008); [0pt] [6] Y. Sugimoto, P. Pou, M. Abe, P. Jelinek, R. Perez, S. Morita, and O. Custance, Nature 446, 64 (2007)

  3. An approach towards 3D sensitive AFM cantilevers

    NASA Astrophysics Data System (ADS)

    Koops, Richard; Fokkema, Vincent

    2014-04-01

    The atomic force microscope (AFM) tapping mode is a highly sensitive local probing technique that is very useful to study and measure surface properties down to the atomic scale. The tapping mode is mostly implemented using the resonance of the first bending mode of the cantilever and therefore provides sensitivity mainly along the direction of this oscillation. Driven by the semiconductor industry, there is an increasing need for accurate measurements of nanoscale structures for side wall characterization by AFM that requires additional sensitivity in the lateral direction. The conventional tapping mode has been augmented by various authors, for example by tilting the cantilever system (Cho et al 2011 Rev. Sci. Instrum. 82 023707) to access the sidewall or using a torsion mode (Dai et al 2011 Meas. Sci. Technol. 22 094009) of the cantilever to provide additional lateral sensitivity. These approaches however trade lateral sensitivity for vertical sensitivity or still lack sensitivity in the remaining lateral direction. We present an approach towards true 3D sensitivity for AFM cantilevers based on simultaneous excitation and optical detection of multiple cantilever resonance modes along three axes. Tuning the excitation of the cantilever to specific frequencies provides a mechanism to select only those cantilever modes that have the desired characteristics. Additionally, cantilever engineering has been used to design and create a substructure within the cantilever that has been optimized for specific resonance behavior around 4 MHz. In contrast to the conventional approach of using a piezo to actuate the cantilever modulation, we present results on photo-thermal excitation using an intensity modulated low-power laser source. By tightly focusing the excitation spot on the cantilever we were able to attain a deflection efficiency of 0.7 nm µW-1 for the first bending mode. The presented approach results in an efficient all optical excitation and deflection detection

  4. The Advancing State of AF-M315E Technology

    NASA Technical Reports Server (NTRS)

    Masse, Robert; Spores, Ronald A.; McLean, Chris

    2014-01-01

    The culmination of twenty years of applied research in hydroxyl ammonium nitrate (HAN)-based monopropellants, the NASA Space Technology mission Directorate's (STMD) Green Propellant Infusion Mission (GPIM) will achieve the first on-orbit demonstration of an operational AF-M315E green propellant propulsion system by the end of 2015. Following an contextual overview of the completed flight design of the GPIM propellant storage and feed system, results of first operation of a flight-representative heavyweight 20-N engineering model thruster (to be conducted in mid-2014) are presented with performance comparisons to prior lab model (heavyweight) test articles.

  5. Comparison of dynamic lever STM and noncontact AFM

    NASA Astrophysics Data System (ADS)

    Guggisberg, M.; Bammerlin, M.; Lüthi, R.; Loppacher, C.; Battiston, F.; Lü, J.; Baratoff, A.; Meyer, E.; Güntherodt, H.-J.

    We investigate interaction effects which occur in scanning tunneling microscopy (STM) by performing local force spectroscopy with an oscillating tip while imaging Si(111)7×7 terraces in the dynamic lever STM mode (constant time-averaged current). It is found that true atomic resolution is achieved close to the minimum of the resonance frequency vs. distance curve and even closer to the sample. On the other hand true atomic resolution in noncontact AFM (constant frequency shift) is expected several nm away from this minimum, in the range where the frequency shift becomes more negative with decreasing distance.

  6. On Improvements of Cyclic MUSIC

    NASA Astrophysics Data System (ADS)

    Yan, Huiqin; Fan, H. Howard

    2005-12-01

    Many man-made signals encountered in communications exhibit cyclostationarity. By exploiting cyclostationarity, cyclic MUSIC has been shown to be able to separate signals with different cycle frequencies, thus, to be able to perform signal selective direction of-arrival (DOA) estimation. However, as will be shown in this paper, the DOA estimation of cyclic MUSIC is actually biased. We show in this paper that by properly choosing the frequency for evaluating the steering vector, the bias of DOA estimation can be substantially reduced and the performance can be improved. Furthermore, we propose another algorithm exploiting cyclic conjugate correlation to further improve the performance of DOA estimation. Simulation results show the effectiveness of both of our methods.

  7. Physical properties of polyacrylamide gels probed by AFM and rheology

    NASA Astrophysics Data System (ADS)

    Abidine, Yara; Laurent, Valérie M.; Michel, Richard; Duperray, Alain; Iulian Palade, Liviu; Verdier, Claude

    2015-02-01

    Polymer gels have been shown to behave as viscoelastic materials but only a small amount of data is usually provided in the glass transition. In this paper, the dynamic moduli G\\prime and G\\prime\\prime of polyacrylamide hydrogels are investigated using both an AFM in contact force modulation mode and a classical rheometer. The validity is shown by the matching of the two techniques. Measurements are carried out on gels of increasing polymer concentration in a wide frequency range. A model based on fractional derivatives is successfully used, covering the whole frequency range. G\\text{N}0 , the plateau modulus, as well as several other parameters are obtained at low frequencies. The model also predicts the slope a of both moduli in the glass transition, and a transition frequency f\\text{T} is introduced to separate the gel-like behavior with the glassy state. Its variation with polymer content c gives a dependence f\\text{T}∼ c1.6 , in good agreement with previous theories. Therefore, the AFM data provides new information on the physics of polymer gels.

  8. Dual AFM probes alignment based on vision guidance

    NASA Astrophysics Data System (ADS)

    Zhang, Hua-kun; Gao, Si-tian; Lu, Ming-zhen; Wang, Long-long

    2013-10-01

    Atomic force microscope (AFM) with dual probes that operate together can measure both side walls excellently at the same time, which virtually eliminates the prevalent effect of probe width that contributes a large component of uncertainty in measurement results and finally obtains the critical dimension (CD)(e.g. the linewidth) through data synthesis. In calibration process, the dual probes must contact each other in advance, which realizes the alignment in the three dimensions, to establish a zero reference point and ensure the accuracy of measurement. Because nowadays the optical resolution of advanced lens have exceeded micrometer range, and the size of probes is within micro level, it is possible to acquire dual probes images in both horizontal and vertical directions, through which the movement of the probes can be controlled in time. In order to further enhance the alignment precision, sub-pixel edge detection method based on Zernike orthogonal moment is used to obtain relative position between these two probes, which helps the tips alignment attains sub-micron range. Piezoelectric nanopositioning stages calibrated by laser interferometer are used to implement fine movement of the probes to verify the accuracy of the experimental results. To simplify the system, novel self-sensing and self-actuating probe based on a quartz tuning fork combined with a micromachined cantilever is used for dynamic mode AFM. In this case, an external optical detection system is not needed, so the system is simple and small.

  9. Viscoelasticity of gelatin surfaces probed by AFM noise analysis.

    PubMed

    Benmouna, Farida; Johannsmann, Diethelm

    2004-01-01

    The viscoelastic properties of surfaces of swollen gelatin were investigated by analyzing the Brownian motion of an atomic force microscopy (AFM) cantilever in contact with the gel surface. A micron-sized glass sphere attached to the AFM cantilever is used as the dynamic probe. When the sphere approaches the gelatin surface, there is a static repulsive force without a jump into contact. The cantilever's Brownian movement is monitored in parallel, providing access to the dynamic sphere-surface interaction as quantified by the dynamic spring constant, kappa, and the drag coefficient, xi. Gelatin is used as a model substance for a variety of other soft surfaces, where the stiffness of the gel can be varied via the solvent quality, the bloom number, and the pH. The modulus derived from the static force-distance curve is in the kPa range, consistent with the literature. However, the dynamic spring constant as derived from the Brownian motion is much larger than the static differential spring constant dF/dz. On retraction, one observes a rather strong adhesion hysteresis. The strength of the bridge (as given by the dynamic spring constant and the drag coefficient) is very small. PMID:15745019

  10. Analysis of AFM cantilever dynamics close to sample surface

    NASA Astrophysics Data System (ADS)

    Habibnejad Korayem, A.; Habibnejad Korayem, Moharam; Ghaderi, Reza

    2013-07-01

    For imaging and manipulation of biological specimens application of atomic force microscopy (AFM) in liquid is necessary. In this paper, tapping-mode AFM cantilever dynamics in liquid close to sample surface is modeled and simulated by well defining the contact forces. The effect of cantilever tilting angle has been accounted carefully. Contact forces have some differences in liquid in comparison to air or vacuum in magnitude or formulation. Hydrodynamic forces are also applied on the cantilever due to the motion in liquid. A continuous beam model is used with its first mode and forward-time simulation method for simulation of its hybrid dynamics and the frequency response and amplitude versus separation diagrams are extracted. The simulation results show a good agreement with experimental results. The resonance frequency in liquid is so small in comparison to air due to additional mass and also additional damping due to the viscosity of the liquid around. The results show that the effect of separation on free vibration amplitude is great. Its effect on resonance frequency is considerable too.

  11. Iron oxide mineral-water interface reactions studied by AFM

    SciTech Connect

    Hawley, M.E.; Rogers, P.S.Z.

    1994-07-01

    Natural iron mineral surfaces have been examined in air by atomic force (AFM) and scanning tunneling (STM) microscopies. A number of different surface features were found to be characteristic of the native surface. Even surfaces freshly exposed by crushing larger crystals were found to have a pebbly surface texture caused by the presence of thin coatings of what might be surface precipitates. This finding is interpreted as evidence for previous exposure to water, probably through an extensive network of microfractures. Surface reactions on the goethite crystals were studied by AFM at size resolutions ranging from microns to atomic resolution before, during, and after reaction with distilled water and 0.lN HCl. Immediate and extensive surface reconfiguration occurred on contact with water. In one case, after equilibration with water for 3 days, surface reprecipitation, etching and pitting were observed. Atomic resolution images taken under water were found to be disordered. The result of surface reaction was generally to increase the surface area substantially through the extension of surface platelet arrays, present prior to reaction. This work is being done in support of the site characterization project at Yucca Mountain.

  12. Pathogen identification using peptide nanotube biosensors and impedance AFM

    NASA Astrophysics Data System (ADS)

    Maccuspie, Robert I.

    Pathogen identification at highly sensitive levels is crucial to meet urgent needs in fighting the spread of disease or detecting bioterrorism events. Toward that end, a new method for biosensing utilizing fluorescent antibody nanotubes is proposed. Fundamental studies on the self-assembly of these peptide nanotubes are performed, as are applications of aligning these nanotubes on surfaces. As biosensors, these nanotubes incorporate recognition units with antibodies at their ends and fluorescent signaling units at their sidewalls. When viral pathogens were mixed with these antibody nanotubes in solution, the nanotubes rapidly aggregated around the viruses. The size of the aggregates increased as the concentration of viruses increased, as detected by flow cytometry on the order of attomolar concentrations by changes in fluorescence and light scattering intensities. This enabled determination of the concentrations of viruses at trace levels (102 to 106 pfu/mL) within 30 minutes from the receipt of samples to the final quantitative data analysis, as demonstrated on Adenovirus, Herpes Simplex Virus, Influenza, and Vaccinia virus. As another separate approach, impedance AFM is used to study the electrical properties of individual viruses and nanoparticles used as model systems. The design, development, and implementation of the impedance AFM for an Asylum Research platform is described, as well as its application towards studying the impedance of individual nanoparticles as a model system for understanding the fundamental science of how the life cycle of a virus affects its electrical properties. In combination, these approaches fill a pressing need to quantify viruses both rapidly and sensitively.

  13. SU-8 hollow cantilevers for AFM cell adhesion studies

    NASA Astrophysics Data System (ADS)

    Martinez, Vincent; Behr, Pascal; Drechsler, Ute; Polesel-Maris, Jérôme; Potthoff, Eva; Vörös, Janos; Zambelli, Tomaso

    2016-05-01

    A novel fabrication method was established to produce flexible, transparent, and robust tipless hollow atomic force microscopy (AFM) cantilevers made entirely from SU-8. Channels of 3 μm thickness and several millimeters length were integrated into 12 μm thick and 40 μm wide cantilevers. Connected to a pressure controller, the devices showed high sealing performance with no leakage up to 6 bars. Changing the cantilever lengths from 100 μm to 500 μm among the same wafer allowed the targeting of various spring constants ranging from 0.5 to 80 N m‑1 within a single fabrication run. These hollow polymeric AFM cantilevers were operated in the optical beam deflection configuration. To demonstrate the performance of the device, single-cell force spectroscopy experiments were performed with a single probe detaching in a serial protocol more than 100 Saccharomyces cerevisiae yeast cells from plain glass and glass coated with polydopamine while measuring adhesion forces in the sub-nanoNewton range. SU-8 now offers a new alternative to conventional silicon-based hollow cantilevers with more flexibility in terms of complex geometric design and surface chemistry modification.

  14. Comparison of particle sizes determined with impactor, AFM and SEM

    NASA Astrophysics Data System (ADS)

    Gwaze, Patience; Annegarn, Harold J.; Huth, Joachim; Helas, Günter

    2007-11-01

    Particles size comparisons were made between conventional aerodynamic and mobility sizing techniques and physical geometric sizes measured by high resolution microscopes. Atmospheric particles were collected during the wet and dry seasons in the Amazonian ecosystems. Individual particles deposited on four stages of the MOUDI (Micro-Orifice Uniform Deposition Impactor) were characterised for particle volumes, projected surface diameters and morphologies with an Atomic Force Microscope (AFM) and a Scanning Electron Microscope (SEM). AFM and SEM size distributions were verified against distributions derived from response functions of individual MOUDI stages as specified by Winklmayr et al. [Winklmayr, W., Wang, H.-C., John, W., 1990. Adaptation of the Twomey algorithm to the inversion of cascade impactor data. Aerosol Science and Technology 13, 322-331.]. Particles indicated inherent discrepancies in sizing techniques. Particle volumes were systematically lower than expected by factors of up to 3.6. Differences were attributed to loss of mass, presumably water adsorbed on particles. Losses were high and could not be accounted for by measured humidity growth factors suggesting significant losses of other volatile compounds as well, particularly on particles that were collected during the wet season. Microscopy results showed that for hygroscopic particles, microscopy sizes depend on the relative humidity history of particles before and after sampling. Changes in relative humidity significantly altered particle morphologies. Depending on when changes occur, such losses will bias not only microscopy particle sizes but also impactor mass distributions and number concentrations derived from collected particles.

  15. AFM analysis of bleaching effects on dental enamel microtopography

    NASA Astrophysics Data System (ADS)

    Pedreira de Freitas, Ana Carolina; Espejo, Luciana Cardoso; Botta, Sergio Brossi; Teixeira, Fernanda de Sa; Luz, Maria Aparecida A. Cerqueira; Garone-Netto, Narciso; Matos, Adriana Bona; Salvadori, Maria Cecilia Barbosa da Silveira

    2010-02-01

    The purpose of this in vitro study was to test a new methodology to evaluate the effects of 35% hydrogen peroxide agent on the microtopography of sound enamel using an atomic force microscope (AFM). The buccal sound surfaces of three extracted human lower incisors were used, without polishing the surfaces to maintain them with natural morphology. These unpolished surfaces were subjected to bleaching procedure with 35% hydrogen peroxide that consisted of 4 applications of the bleaching agent on enamel surfaces for 10 min each application. Surface images were obtained in a 15 μm × 15 μm area using an AFM. The roughness (Ra and RMS) and the power spectral density (PSD) were obtained before and after the bleaching treatment. As results we could inquire that the PSD analyses were very suitable to identifying the morphological changes on the surfaces, while the Ra and RMS parameters were insufficient to represent the morphological alterations promoted by bleaching procedure on enamel. The morphological wavelength in the range of visible light spectrum (380-750 nm) was analyzed, showing a considerable increase of the PSD with the bleaching treatment.

  16. In situ microliter-droplet anodic stripping voltammetry of copper stained on the gold label after galvanic replacement reaction enlargement for ultrasensitive immunoassay of proteins.

    PubMed

    Qin, Xiaoli; Xu, Aigui; Wang, Linchun; Liu, Ling; Chao, Long; He, Fang; Tan, Yueming; Chen, Chao; Xie, Qingji

    2016-05-15

    We report a new protocol for ultrasensitive electrochemical sandwich-type immunosensing, on the basis of signal amplification by gold-label/copper-staining, galvanic replacement reactions (GRRs), and in situ microliter-droplet anodic stripping voltammetry (ASV) after an enhanced cathodic preconcentration of copper. First, a sandwich-type immuno-structure is appropriately assembled at a glassy carbon electrode. Second, copper is selectively stained on the catalytic surfaces of second antibody-conjugated Au nanoparticles through CuSO4-ascorbic acid redox reaction, and the GRRs between HAuCl4 and the stained copper are used to amplify the quantity of copper. Finally, the corresponding antigen is determined based on simultaneous chemical-dissolution/cathodic-preconcentration of copper for in-situ ASV analysis directly at the immunoelectrode. Cyclic voltammetry, electrochemical impedance spectroscopy, quartz crystal microbalance and scanning electron microscopy are used for film characterization and/or process monitoring. Under optimized conditions, ultrasensitive analyses of human immunoglobulin G (IgG) and human carbohydrate antigen 125 (CA125) are achieved. The limits of detection are 0.3 fg mL(-1) (equivalent to 7 IgG molecules in the 6 μL sample employed) for IgG (S/N=3) and 1.3 nU mL(-1) for CA125 (S/N=3), respectively, which are amongst the best reported to date for the two proteins. The theoretical feasibility of such a single-molecule-level amperometric immunoassay is also discussed based on the immunological reaction thermodynamics. PMID:26802573

  17. Three-dimensional voltammetry: a chemometrical analysis of electrochemical data for determination of dopamine in the presence of unexpected interference by a biosensor based on gold nanoparticles.

    PubMed

    Khoobi, Asma; Ghoreishi, Sayed Mehdi; Behpour, Mohsen; Masoum, Saeed

    2014-09-16

    Multivariate curve resolution by alternating least-squares (MCR-ALS) was used for voltammetric determination of dopamine (DA) in the presence of epinephrine (EP) at a gold nanoparticles chemically modified carbon paste electrode (AuNPs/CPE). Scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV) techniques were applied for characterization of the nanostructure modified electrode. Central composite rotatable design (CCRD) was employed to generate an experimental program to offer data to model the effects of different parameters on voltammetric responses. Response surface methodology (RSM) was applied to show the individual and interactive effects of chemical and instrumental variables at five levels, combined according to CCRD. For determination of DA in the presence of unexpected interference, three-way data were achieved from various pulse heights in differential pulse voltammetry (DPV) technique. This type of data construction, analyzed by MCR-ALS, makes it possible to exploit the so-called "second-order advantage". The second-order advantage provided unbiased results even in the presence of electroactive interferences with highly overlapped peaks. Also, an algorithm was applied to correct the detected potential shift in the voltammetric data. The voltammograms of the samples were then deposited in an augmented data matrix (column-wise) and subsequently analyzed by MCR-ALS. The effect of rotational ambiguity associated with a particular MCR-ALS solution under a set of constraints was also studied. The proposed method could be applied for the determination of DA and EP in the presence of each other in a wide concentration range of 0.1-205.0 μM, and the detection limit of DA has been found to be 35.5 nM. Finally, the technique has been used for the reliable analysis of DA in real samples. PMID:25191974

  18. Cyclical magnetic field flow fractionation

    NASA Astrophysics Data System (ADS)

    Tasci, T. O.; Johnson, W. P.; Gale, B. K.

    2012-04-01

    In this study, a new magnetic field flow fractionation (FFF) system was designed and modeled by using finite element simulations. Other than current magnetic FFF systems, which use static magnetic fields, our system uses cyclical magnetic fields. Results of the simulations show that our cyclical magnetic FFF system can be used effectively for the separation of magnetic nanoparticles. Cyclical magnetic FFF system is composed of a microfluidic channel (length = 5 cm, height = 30 μm) and 2 coils. Square wave currents of 1 Hz (with 90 deg of phase difference) were applied to the coils. By using Comsol Multiphysics 3.5a, magnetic field profile and corresponding magnetic force exerted on the magnetite nanoparticles were calculated. The magnetic force data were exported from Comsol to Matlab. In Matlab, a parabolic flow profile with maximum flow speed of 0.4 mL/h was defined. Particle trajectories were obtained by the calculation of the particle speeds resulted from both magnetic and hydrodynamic forces. Particle trajectories of the particles with sizes ranging from 10 to 50 nm were simulated and elution times of the particles were calculated. Results show that there is a significant difference between the elution times of the particles so that baseline separation of the particles can be obtained. In this work, it is shown that by the application of cyclical magnetic fields, the separation of magnetic nanoparticles can be done efficiently.

  19. Buffering in cyclic gene networks

    NASA Astrophysics Data System (ADS)

    Glyzin, S. D.; Kolesov, A. Yu.; Rozov, N. Kh.

    2016-06-01

    We consider cyclic chains of unidirectionally coupled delay differential-difference equations that are mathematical models of artificial oscillating gene networks. We establish that the buffering phenomenon is realized in these system for an appropriate choice of the parameters: any given finite number of stable periodic motions of a special type, the so-called traveling waves, coexist.

  20. Color visualization of cyclic magnitudes

    NASA Astrophysics Data System (ADS)

    Restrepo, Alfredo; Estupiñán, Viviana

    2014-02-01

    We exploit the perceptual, circular ordering of the hues in a technique for the visualization of cyclic variables. The hue is thus meaningfully used for the indication of variables such as the azimuth and the units of the measurement of time. The cyclic (or circular) variables may be both of the continuous type or the discrete type; among the first there is azimuth and among the last you find the musical notes and the days of the week. A correspondence between the values of a cyclic variable and the chromatic hues, where the natural circular ordering of the variable is respected, is called a color code for the variable. We base such a choice of hues on an assignment of of the unique hues red, yellow, green and blue, or one of the 8 even permutations of this ordered list, to 4 cardinal values of the cyclic variable, suitably ordered; color codes based on only 3 cardinal points are also possible. Color codes, being intuitive, are easy to remember. A possible low accuracy when reading instruments that use this technique is compensated by fast, ludic and intuitive readings; also, the use of a referential frame makes readings precise. An achromatic version of the technique, that can be used by dichromatic people, is proposed.

  1. The importance of correcting for variable probe-sample interactions in AFM-IR spectroscopy: AFM-IR of dried bacteria on a polyurethane film.

    PubMed

    Barlow, Daniel E; Biffinger, Justin C; Cockrell-Zugell, Allison L; Lo, Michael; Kjoller, Kevin; Cook, Debra; Lee, Woo Kyung; Pehrsson, Pehr E; Crookes-Goodson, Wendy J; Hung, Chia-Suei; Nadeau, Lloyd J; Russell, John N

    2016-08-01

    AFM-IR is a combined atomic force microscopy-infrared spectroscopy method that shows promise for nanoscale chemical characterization of biological-materials interactions. In an effort to apply this method to quantitatively probe mechanisms of microbiologically induced polyurethane degradation, we have investigated monolayer clusters of ∼200 nm thick Pseudomonas protegens Pf-5 bacteria (Pf) on a 300 nm thick polyether-polyurethane (PU) film. Here, the impact of the different biological and polymer mechanical properties on the thermomechanical AFM-IR detection mechanism was first assessed without the additional complication of polymer degradation. AFM-IR spectra of Pf and PU were compared with FTIR and showed good agreement. Local AFM-IR spectra of Pf on PU (Pf-PU) exhibited bands from both constituents, showing that AFM-IR is sensitive to chemical composition both at and below the surface. One distinct difference in local AFM-IR spectra on Pf-PU was an anomalous ∼4× increase in IR peak intensities for the probe in contact with Pf versus PU. This was attributed to differences in probe-sample interactions. In particular, significantly higher cantilever damping was observed for probe contact with PU, with a ∼10× smaller Q factor. AFM-IR chemical mapping at single wavelengths was also affected. We demonstrate ratioing of mapping data for chemical analysis as a simple method to cancel the extreme effects of the variable probe-sample interactions. PMID:27403761

  2. AFM CHARACTERIZATION OF RAMAN LASER INDUCED DAMAGE ON CDZNTECRYSTAL SURFACES

    SciTech Connect

    Teague, L.; Duff, M.

    2008-10-07

    High quality CdZnTe (or CZT) crystals have the potential for use in room temperature gamma-ray and X-ray spectrometers. Over the last decade, the methods for growing high quality CZT have improved the quality of the produced crystals however there are material features that can influence the performance of these materials as radiation detectors. The presence of structural heterogeneities within the crystals, such as twinning, pipes, grain boundaries (polycrystallinity), and secondary phases (SPs) can have an impact on the detector performance. There is considerable need for reliable and reproducible characterization methods for the measurement of crystal quality. With improvements in material characterization and synthesis, these crystals may become suitable for widespread use in gamma radiation detection. Characterization techniques currently utilized to test for quality and/or to predict performance of the crystal as a gamma-ray detector include infrared (IR) transmission imaging, synchrotron X-ray topography, photoluminescence spectroscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) and Raman spectroscopy. In some cases, damage caused by characterization methods can have deleterious effects on the crystal performance. The availability of non-destructive analysis techniques is essential to validate a crystal's quality and its ability to be used for either qualitative or quantitative gamma-ray or X-ray detection. The work presented herein discusses the damage that occurs during characterization of the CZT surface by a laser during Raman spectroscopy, even at minimal laser powers. Previous Raman studies have shown that the localized annealing from tightly focused, low powered lasers results in areas of higher Te concentration on the CZT surface. This type of laser damage on the surface resulted in decreased detector performance which was most likely due to increased leakage current caused by areas of higher Te concentration. In this study

  3. Device level 3D characterization using PeakForce AFM

    NASA Astrophysics Data System (ADS)

    Timoney, Padraig; Zhang, Xiaoxiao; Vaid, Alok; Hand, Sean; Osborne, Jason; Milligan, Eric; Feinstein, Adam

    2016-03-01

    Traditional metrology solutions face a range of challenges at the 1X node such as three dimensional (3D) measurement capabilities, shrinking overlay and critical dimension (CD) error budgets driven by multi-patterning and via in trench CD measurements. With advent of advanced technology nodes and 3D processing, an increasing need is emerging for in-die metrology including across-structure and structure-to-structure characterization. A myriad of work has emerged in the past few years intending to address these challenges from various aspects; in-die OCD with reduced spot size and tilt beam on traditional critical dimension scanning electron microscopy (CDSEM) for height measurements. This paper explores the latest capability offered by PeakForceTM Tapping Atomic Force Microscopy (PFT-AFM). The use of traditional harmonic tapping mode for scanning high aspect ratio, and complex "3D" wafer structures, results in limited depth probing capability as well as excessive tip wear. These limitations arise due to the large tip-sample interaction volume in such confined spaces. PeakForce Tapping eliminates these limitations through direct real time control of the tip-sample interaction contact force. The ability of PeakForce to measure, and respond directly to tip- sample interaction forces results in more detailed feature resolution, reduced tip wear, and improved depth capability. In this work, the PFT-AFM tool was applied for multiple applications, including the 14nm fin and replacement metal gate (RMG) applications outlined below. Results from DOE wafers, detailed measurement precision studies and correlation to reference metrology are presented for validation of this methodology. With the fin application, precision of 0.3nm is demonstrated by measuring 5 dies with 10 consecutive runs. Capability to resolve within-die and localized within-macro height variation is also demonstrated. Results obtained from the fin measurements support the increasing trend that measurements

  4. Effect of tip mass on frequency response and sensitivity of AFM cantilever in liquid.

    PubMed

    Farokh Payam, Amir; Fathipour, Morteza

    2015-03-01

    The effect of tip mass on the frequency response and sensitivity of atomic force microscope (AFM) cantilever in the liquid environment is investigated. For this purpose, using Euler-Bernoulli beam theory and considering tip mass and hydrodynamic functions in a liquid environment, an expression for the resonance frequencies of AFM cantilever in liquid is derived. Then, based on this expression, the effect of the surface contact stiffness on the flexural mode of a rectangular AFM cantilever in fluid is investigated and compared with the case where the AFM cantilever operates in the air. The results show that in contrast with an air environment, the tip mass has no significant impact on the resonance frequency and sensitivity of the AFM cantilever in the liquid. Hence, analysis of AFM behaviour in liquid environment by neglecting the tip mass is logical. PMID:25562584

  5. Pulse Voltammetry

    NASA Astrophysics Data System (ADS)

    Stojek, Zbigniew

    The idea of imposing potential pulses and measuring the currents at the end of each pulse was proposed by Barker in a little-known journal as early as in 1958 [1]. However, the first reliable trouble-free and affordable polarographs offering voltammetric pulse techniques appeared on the market only in the 1970s. This delay was due to some limitations on the electronic side. In the 1990s, again substantial progress in electrochemical pulse instrumentation took place. This was related to the introduction of microprocessors, computers, and advanced software.

  6. Anodic Stripping Voltammetry of Silver Nanoparticles: Aggregation Leads to Incomplete Stripping

    PubMed Central

    Cloake, Samantha J; Toh, Her Shuang; Lee, Patricia T; Salter, Chris; Johnston, Colin; Compton, Richard G

    2015-01-01

    The influence of nanoparticle aggregation on anodic stripping voltammetry is reported. Dopamine-capped silver nanoparticles were chosen as a model system, and melamine was used to induce aggregation in the nanoparticles. Through the anodic stripping of the silver nanoparticles that were aggregated to different extents, it was found that the peak area of the oxidative signal corresponding to the stripping of silver to silver(I) ions decreases with increasing aggregation. Aggregation causes incomplete stripping of the silver nanoparticles. Two possible mechanisms of ‘partial oxidation’ and ‘inactivation’ of the nanoparticles are proposed to account for this finding. Aggregation effects must be considered when anodic stripping voltammetry is used for nanoparticle detection and quantification. Hence, drop casting, which is known to lead to aggregation, is not encouraged for preparing electrodes for analytical purposes. PMID:25861566

  7. Detection of food additives by voltammetry at the liquid-liquid interface.

    PubMed

    Herzog, Grégoire; Kam, Victor; Berduque, Alfonso; Arrigan, Damien W M

    2008-06-25

    Electrochemistry at the liquid-liquid interface enables the detection of nonredoxactive species with electroanalytical techniques. In this work, the electrochemical behavior of two food additives, aspartame and acesulfame K, was investigated. Both ions were found to undergo ion-transfer voltammetry at the liquid-liquid interface. Differential pulse voltammetry was used for the preparation of calibration curves over the concentration range of 30-350 microM with a detection limit of 30 microM. The standard addition method was applied to the determination of their concentrations in food and beverage samples such as sweeteners and sugar-free beverages. Selective electrochemically modulated liquid-liquid extraction of these species in both laboratory solutions and in beverage samples was also demonstrated. These results indicate the suitability of liquid-liquid electrochemistry as an analytical approach in food analysis. PMID:18512937

  8. 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.

  9. AFM surface investigation of polyethylene modified by ion bombardment

    NASA Astrophysics Data System (ADS)

    Švorčík, V.; Arenholz, E.; Hnatowicz, V.; Rybka, V.; Öchsner, R.; Ryssel, H.

    1998-07-01

    Polyethylene (PE) was irradiated with 63 keV Ar + and 155 keV Xe + ions to fluences of 1 × 10 13 to 3 × 10 15 cm -2 with ion energies being chosen in order to achieve approximately the same penetration depth for both species. The PE surface morphology was examined by means of atomic force microscopy (AFM), whereas the concentration of free radicals and conjugated double bonds, both created by the ion irradiation, were determined using electron paramagnetic resonance (EPR) and UV-VIS spectroscopy, respectively. As expected, the degradation of PE was higher after irradiation with heavier Xe + ions but the changes in the PE surface morphology were more pronounced for Ar + ions. This newly observed effect can be explained by stronger compaction of the PE surface layer in the case of the Xe + irradiation, connected with a reduction of free volume available.

  10. FM-AFM crossover in vanadium oxide nanomaterials

    NASA Astrophysics Data System (ADS)

    Demishev, S. V.; Chernobrovkin, A. L.; Glushkov, V. V.; Grigorieva, A. V.; Goodilin, E. A.; Sluchanko, N. E.; Samarin, N. A.; Semeno, A. V.

    2010-01-01

    The magnetic properties of nanomaterials based on vanadium oxide (multiwall nanotubes, nanorods, and nanolayers) have been investigated in the temperature range of 1.8-220 K by high-frequency (60-GHz) EPR. A transition from a ferromagnetic temperature dependence to an antiferromagnetic temperature dependence has been observed in nanorods and nanotubes with a decrease in the temperature. The FM-AFM crossover observed near T C ˜ 110 K is accompanied by a low-temperature increase in the Curie constant by a factor of 2.7-7. The comparison of the experimental data for various VO x nanoparticles indicates that the most probable cause of the change in the type of magnetic interaction is a change in the concentration of V4+ magnetic ions.

  11. Adhesion forces between AFM tips and superficial dentin surfaces.

    PubMed

    Pelin, I M; Piednoir, A; Machon, D; Farge, P; Pirat, C; Ramos, S M M

    2012-06-15

    In this work, we study the adhesion forces between atomic force microscopy (AFM) tips and superficial dentin etched with phosphoric acid. Initially, we quantitatively analyze the effect of acid etching on the surface heterogeneity and the surface roughness, two parameters that play a key role in the adhesion phenomenon. From a statistical study of the force-distance curves, we determine the average adhesion forces on the processed substrates. Our results show that the average adhesion forces, measured in water, increase linearly with the acid exposure time. The highest values of such forces are ascribed to the high density of collagen fibers on the etched surfaces. The individual contribution of exposed collagen fibrils to the adhesion force is highlighted. We also discuss in this paper the influence of the environmental medium (water/air) in the adhesion measurements. We show that the weak forces involved require working in the aqueous medium. PMID:22472512

  12. BOREAS AFM-04 Twin Otter Aircraft Sounding Data

    NASA Technical Reports Server (NTRS)

    MacPherson, J. Ian; Desjardins, Raymond L.; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-4 team used the National Research Council, Canada (NRC) Twin Otter aircraft to make sounding measurements through the boundary layer. These measurements included concentrations of carbon dioxide and ozone, atmospheric pressure, dry bulb temperature, potential temperature, dewpoint temperature, calculated mixing ratio, and wind speed and direction. Aircraft position, heading, and altitude were also recorded. Data were collected at both the Northern Study Area (NSA) and the Southern Study Area (SSA) in 1994 and 1996. These data are stored in tabular ASCII files. The Twin Otter aircraft sounding data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files also are available on a CD-ROM (see document number 20010000884).

  13. Visualization of internal structure of banana starch granule through AFM.

    PubMed

    Peroni-Okita, Fernanda H G; Gunning, A Patrick; Kirby, Andrew; Simão, Renata A; Soares, Claudinéia A; Cordenunsi, Beatriz R

    2015-09-01

    Atomic force microscopy (AFM) is a high resolution technique for studying the external and internal structures of starch granules. For this purpose granules were isolated from bananas and embedded in a non-penetrating resin. To achieve image contrast of the ultrastructure, the face of the cut blocks were wetted in steam and force modulation mode imaging was used. Images of starch from green bananas showed large variation of height across the granule due to a locational specific absorption of water and swelling of amorphous regions; the data reveal that the center of the granules are structurally different and have different viscoelastic properties. Images of starches from ripe bananas showed an even greater different level of organization: absence of growth rings around the hilum; the central region of the granule is richer in amylose; very porous surface with round shaped dark structures; the size of blocklets are larger than the green fruits. PMID:26005137

  14. AFM of self-assembled lambda DNA-histone networks.

    PubMed

    Liu, YuYing; Guthold, Martin; Snyder, Matthew J; Lu, HongFeng

    2015-10-01

    Atomic force microscopy (AFM) was used to investigate the self-assembly behavior of λ-DNA and histones at varying histone:DNA ratios. Without histones and at the lowest histone:DNA ratio (less than one histone per 1000 base pairs of DNA), the DNA appeared as individual (uncomplexed), double-stranded DNA molecules. At increasing histone concentrations (one histone per 500, 250 and 167 base pairs of DNA), the DNA molecules started to form extensive polygonal networks of mostly pentagons and hexagons. The observed networks might be one of the naturally occurring, stable DNA-histone structures. The condensing effects of the divalent cations Mg(2+) and Ca(2+) on the DNA-histone complexes were also investigated. The networks persisted at high Mg(2+) concentration (20mM) and the highest histone concentration. At high Ca(2+) concentration and the highest histone concentration, the polygonal network disappeared and, instead, individual, tightly condensed aggregates were formed. PMID:26141439

  15. Mechanical Characterization of Photo-crosslinkable Hydrogels with AFM

    NASA Astrophysics Data System (ADS)

    McKenna, Alyssa; Byun, Myunghwan; Hayward, Ryan; Aidala, Katherine

    2012-02-01

    Stimuli-responsive hydrogel films formed from photo-crosslinkable polymers are versatile materials for controlled drug delivery devices, three-dimensional micro-assemblies, and components in microfluidic systems. For such applications, it is important to understand both the mechanical properties and the dynamics responses of these materials. We describe the use of atomic force microscope (AFM) based indentation experiments to characterize the properties of poly(N-isopropylacrylamide) copolymer films, crosslinked by activation of pendent benzophenone units using ultraviolet light. In particular, we study how the elastic modulus of the material, determined using the Johnson, Kendall, and Roberts model, depends on UV dose, and simultaneously investigate stress relaxation in these materials in the context of viscoelastic and poroelastic relaxation models.

  16. Purification of water by electrocoagulation with an alternating asymmetrical current for stripping voltammetry

    SciTech Connect

    Gorodovykh, V.E.; Kaplin, A.A.; Svishchenko, N.M.; Obraztsov, S.V.

    1987-11-20

    The influence of the flow velocity and the current density on the degree of purification of water by electrocoagulation with an alternating asymmetrical current has been studied. It has been demonstrated that under optimum conditions at pH/sub c/ 11.0-11.5 the residual metal content in the purified water drops to the level n x 10/sup -4/ g/ml; this allows its use in the practice of stripping voltammetry.

  17. Recent advances in exchange bias of layered magnetic FM/AFM systems

    NASA Astrophysics Data System (ADS)

    Liu, ZhongYuan

    2013-01-01

    The exchange bias (EB) has been investigated in magnetic materials with the ferromagnetic (FM)/antiferromagnetic (AFM) contacting interfaces for more than half a century. To date, the significant progress has been made in the layered magnetic FM/AFM thin film systems. EB mechanisms have shown substantive research advances. Here some of the new advances are introduced and discussed with the emphasis on the influence of AFM layer, the interlayer EB coupling across nonmagnetic spacer, and the interlayer coupling across AFM layer, as well as EB related to multiferrioc materials and electrical control.

  18. Modulators of cyclic AMP systems.

    PubMed

    Hess, S M; Chasin, M; Free, C A; Harris, D N

    1975-01-01

    On the basis of the data reported here, one may conclude that although many agents that act in the central nervous system are modulators of the action of cyclic AMP, it is difficult to establish a direct connection between the pharmacologic activity and the levels of cyclic AMP in the brain. This lack of interrelation applies to the benzodiazepines as well as to the pyrazolopyridines. The data for members of the latter group are somewhat frustrating in this regard, since an excellent correlation has been shown to exist between the potency of inhibition of PDE and activity in the antianxiety test. In measurements of steroidogenesis in the isolated adrenal cell, the correlation between activity in vito and the conflict assay is even better. The data presented here and reported elsewhere (Shimizu et al., 1974; Kelly et al., 1974; Mayer and King, 1974; King and Mayer, 1974) provide evidence that agents that act as inhibitors of PDE in cell-free systems exert their influence on cyclic AMP in tissue slices of the brain of guinea pigs by mechanisms that seem not to be related to an effect on PDE. Papaverine, and possibly chlordiazepoxide, may act by releasing agonists that, in turn, stimulate the accumulation of cyclic AMP. This activity is blocked bo other inhibitors of PDE, such as theophyline. Results obtained by the use of platelets are refreshingly clear. Inhibition of aggregation has been shown to occur when the level of cyclic AMP is raised, and a suggestive exists that the most potent inhibitors of platelet PDE are the best potentiators of the action of PGE1 in blocking aggregation. The study utilizing drugs collected from a large number of therapeutic classes makes clear that it is difficult to attribute the mechanism of action for any of the classes studied to modulation of cyclic AMP. An unexpected finding of this study, however, was the fact that pharmacologic agents include an unusually large number of inhibitors of PDE as compared with agents chosen at

  19. Voltammetry of naltrexone in commercial formulation and human body fluids: Quantification and pharmacokinetic studies.

    PubMed

    Ghoneim, Mohamed M; El-Desoky, Hanaa S; Abdel-Galeil, Mohamed M

    2011-06-01

    Naltrexone HCl (NAL.HCl) has been reduced at the mercury electrode in Britton-Robinson universal buffer of pH values 2-11 with a mechanism involving the quasi-reversible uptake of the first transferring electron followed by a rate-determining protonation step of its C=O double bond at position C-6. Simple, sensitive, selective and reliable linear-sweep and square-wave adsorptive cathodic stripping voltammetry methods have been described for trace quantitation of NAL.HCl in bulk form, commercial formulation and human body fluids without the necessity for sample pretreatment and/or time-consuming extraction steps prior to the analysis. Limits of quantitation of 6.0×10(-9)M and 8.0×10(-10)M NAL.HCl in bulk form or commercial formulation and of 9.0×10(-9) and 1.0×10(-9)M NAL.HCl in spiked human serum samples were achieved by the described linear and square-wave stripping voltammetry methods, respectively. Furthermore, pharmacokinetic parameters of the drug in human plasma samples of healthy volunteers following the administration of an oral single dose of 50mg NAL.HCl (one Revia(®) tablet) were estimated by means of the described square-wave stripping voltammetry method without interferences from the drug's metabolites and/or endogenous human plasma constituents. The estimated pharmacokinetic parameters were favorably compared with those reported in literature. PMID:21371948

  20. Copper-Based Electrochemical Sensor with Palladium Electrode for Cathodic Stripping Voltammetry of Manganese

    PubMed Central

    2015-01-01

    In this work, we report on the development of a palladium-based, microfabricated point-of-care electrochemical sensor for the determination of manganese using square wave cathodic stripping voltammetry. Heavy metals require careful monitoring, yet current methods are too complex for a point-of-care system. Voltammetry offers an attractive approach to metal detection on the microscale, but traditional carbon, gold, or platinum electrodes are difficult or expensive to microfabricate, preventing widespread use. Our sensor uses palladium working and auxiliary electrodes and integrates them with a copper-based reference electrode for simple fabrication and compatibility with microfabrication and printed circuit board processing, while maintaining competitive performance in electrochemical detection. Copper electrodes were prepared on glass substrate using a combination of microfabrication procedures followed by electrodeposition of palladium. The disposable sensor system was formed by bonding a poly(dimethylsiloxane) (PDMS) well to the glass substrate. Cathodic stripping voltammetry of manganese using our new disposable palladium-based sensors exhibited 334 nM (18.3 ppb) limit of detection in borate buffer. The sensor was used to demonstrate manganese determination in natural water samples from a pond in Burnet Woods, located in Cincinnati, OH, and the Ohio River. PMID:25476591

  1. Copper-based electrochemical sensor with palladium electrode for cathodic stripping voltammetry of manganese.

    PubMed

    Kang, Wenjing; Pei, Xing; Bange, Adam; Haynes, Erin N; Heineman, William R; Papautsky, Ian

    2014-12-16

    In this work, we report on the development of a palladium-based, microfabricated point-of-care electrochemical sensor for the determination of manganese using square wave cathodic stripping voltammetry. Heavy metals require careful monitoring, yet current methods are too complex for a point-of-care system. Voltammetry offers an attractive approach to metal detection on the microscale, but traditional carbon, gold, or platinum electrodes are difficult or expensive to microfabricate, preventing widespread use. Our sensor uses palladium working and auxiliary electrodes and integrates them with a copper-based reference electrode for simple fabrication and compatibility with microfabrication and printed circuit board processing, while maintaining competitive performance in electrochemical detection. Copper electrodes were prepared on glass substrate using a combination of microfabrication procedures followed by electrodeposition of palladium. The disposable sensor system was formed by bonding a poly(dimethylsiloxane) (PDMS) well to the glass substrate. Cathodic stripping voltammetry of manganese using our new disposable palladium-based sensors exhibited 334 nM (18.3 ppb) limit of detection in borate buffer. The sensor was used to demonstrate manganese determination in natural water samples from a pond in Burnet Woods, located in Cincinnati, OH, and the Ohio River. PMID:25476591

  2. Ferrocene‐Boronic Acid–Fructose Binding Based on Dual‐Plate Generator–Collector Voltammetry and Square‐Wave Voltammetry

    PubMed Central

    Li, Meng; Xu, Su‐Ying; Gross, Andrew J.; Hammond, Jules L.; Estrela, Pedro; Weber, James; Lacina, Karel; James, Tony D.

    2015-01-01

    Abstract The interaction of ferrocene‐boronic acid with fructose is investigated in aqueous 0.1 m phosphate buffer at pH 7, 8 and 9. Two voltammetric methods, based on 1) a dual‐plate generator–collector micro‐trench electrode (steady state) and 2) a square‐wave voltammetry (transient) method, are applied and compared in terms of mechanistic resolution. A combination of experimental data is employed to obtain new insights into the binding rates and the cumulative binding constants for both the reduced ferrocene‐boronic acid (pH dependent and weakly binding) and for the oxidised ferrocene‐boronic acid (pH independent and strongly binding). PMID:27525210

  3. Supramolecular nesting of cyclic polymers

    NASA Astrophysics Data System (ADS)

    Kondratuk, Dmitry V.; Perdigão, Luís M. A.; Esmail, Ayad M. S.; O'Shea, James N.; Beton, Peter H.; Anderson, Harry L.

    2015-04-01

    Advances in template-directed synthesis make it possible to create artificial molecules with protein-like dimensions, directly from simple components. These synthetic macromolecules have a proclivity for self-organization that is reminiscent of biopolymers. Here, we report the synthesis of monodisperse cyclic porphyrin polymers, with diameters of up to 21 nm (750 C-C bonds). The ratio of the intrinsic viscosities for cyclic and linear topologies is 0.72, indicating that these polymers behave as almost ideal flexible chains in solution. When deposited on gold surfaces, the cyclic polymers display a new mode of two-dimensional supramolecular organization, combining encapsulation and nesting; one nanoring adopts a near-circular conformation, thus allowing a second nanoring to be captured within its perimeter, in a tightly folded conformation. Scanning tunnelling microscopy reveals that nesting occurs in combination with stacking when nanorings are deposited under vacuum, whereas when they are deposited directly from solution under ambient conditions there is stacking or nesting, but not a combination of both.

  4. BOREAS AFM-12 1-km AVHRR Seasonal Land Cover Classification

    NASA Technical Reports Server (NTRS)

    Steyaert, Lou; Hall, Forrest G.; Newcomer, Jeffrey A. (Editor); Knapp, David E. (Editor); Loveland, Thomas R.; Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-12 team's efforts focused on regional scale Surface Vegetation and Atmosphere (SVAT) modeling to improve parameterization of the heterogeneous BOREAS landscape for use in larger scale Global Circulation Models (GCMs). This regional land cover data set was developed as part of a multitemporal one-kilometer Advanced Very High Resolution Radiometer (AVHRR) land cover analysis approach that was used as the basis for regional land cover mapping, fire disturbance-regeneration, and multiresolution land cover scaling studies in the boreal forest ecosystem of central Canada. This land cover classification was derived by using regional field observations from ground and low-level aircraft transits to analyze spectral-temporal clusters that were derived from an unsupervised cluster analysis of monthly Normalized Difference Vegetation Index (NDVI) image composites (April-September 1992). This regional data set was developed for use by BOREAS investigators, especially those involved in simulation modeling, remote sensing algorithm development, and aircraft flux studies. Based on regional field data verification, this multitemporal one-kilometer AVHRR land cover mapping approach was effective in characterizing the biome-level land cover structure, embedded spatially heterogeneous landscape patterns, and other types of key land cover information of interest to BOREAS modelers.The land cover mosaics in this classification include: (1) wet conifer mosaic (low, medium, and high tree stand density), (2) mixed coniferous-deciduous forest (80% coniferous, codominant, and 80% deciduous), (3) recent visible bum, vegetation regeneration, or rock outcrops-bare ground-sparsely vegetated slow regeneration bum (four classes), (4) open water and grassland marshes, and (5) general agricultural land use/ grasslands (three classes). This land cover mapping approach did not detect small subpixel-scale landscape

  5. Nano-Wilhelmy investigation of dynamic wetting properties of AFM tips through tip-nanobubble interaction.

    PubMed

    Wang, Yuliang; Wang, Huimin; Bi, Shusheng; Guo, Bin

    2016-01-01

    The dynamic wetting properties of atomic force microscopy (AFM) tips are of much concern in many AFM-related measurement, fabrication, and manipulation applications. In this study, the wetting properties of silicon and silicon nitride AFM tips are investigated through dynamic contact angle measurement using a nano-Wilhelmy balance based method. This is done by capillary force measurement during extension and retraction motion of AFM tips relative to interfacial nanobubbles. The working principle of the proposed method and mathematic models for dynamic contact angle measurement are presented. Geometric models of AFM tips were constructed using scanning electronic microscopy (SEM) images taken from different view directions. The detailed process of tip-nanobubble interaction was investigated using force-distance curves of AFM on nanobubbles. Several parameters including nanobubble height, adhesion and capillary force between tip and nanobubbles are extracted. The variation of these parameters was studied over nanobubble surfaces. The dynamic contact angles of the AFM tips were calculated from the capillary force measurements. The proposed method provides direct measurement of dynamic contact angles for AFM tips and can also be taken as a general approach for nanoscale dynamic wetting property investigation. PMID:27452115

  6. Nano-Wilhelmy investigation of dynamic wetting properties of AFM tips through tip-nanobubble interaction

    PubMed Central

    Wang, Yuliang; Wang, Huimin; Bi, Shusheng; Guo, Bin

    2016-01-01

    The dynamic wetting properties of atomic force microscopy (AFM) tips are of much concern in many AFM-related measurement, fabrication, and manipulation applications. In this study, the wetting properties of silicon and silicon nitride AFM tips are investigated through dynamic contact angle measurement using a nano-Wilhelmy balance based method. This is done by capillary force measurement during extension and retraction motion of AFM tips relative to interfacial nanobubbles. The working principle of the proposed method and mathematic models for dynamic contact angle measurement are presented. Geometric models of AFM tips were constructed using scanning electronic microscopy (SEM) images taken from different view directions. The detailed process of tip-nanobubble interaction was investigated using force-distance curves of AFM on nanobubbles. Several parameters including nanobubble height, adhesion and capillary force between tip and nanobubbles are extracted. The variation of these parameters was studied over nanobubble surfaces. The dynamic contact angles of the AFM tips were calculated from the capillary force measurements. The proposed method provides direct measurement of dynamic contact angles for AFM tips and can also be taken as a general approach for nanoscale dynamic wetting property investigation. PMID:27452115

  7. Beyond topography - enhanced imaging of cometary dust with the MIDAS AFM

    NASA Astrophysics Data System (ADS)

    Bentley, M. S.; Torkar, K.; Jeszenszky, H.; Romstedt, J.

    2013-09-01

    The MIDAS atomic force microscope (AFM) onboard the Rosetta spacecraft is primarily designed to return the 3D shape and structure of cometary dust particles collected at comet 67P/Churyumov-Gerasimenko [1]. Commercial AFMs have, however, been further developed to measure many other sample properties. The possibilities to make such measurements with MIDAS are explored here.

  8. Nano-Wilhelmy investigation of dynamic wetting properties of AFM tips through tip-nanobubble interaction

    NASA Astrophysics Data System (ADS)

    Wang, Yuliang; Wang, Huimin; Bi, Shusheng; Guo, Bin

    2016-07-01

    The dynamic wetting properties of atomic force microscopy (AFM) tips are of much concern in many AFM-related measurement, fabrication, and manipulation applications. In this study, the wetting properties of silicon and silicon nitride AFM tips are investigated through dynamic contact angle measurement using a nano-Wilhelmy balance based method. This is done by capillary force measurement during extension and retraction motion of AFM tips relative to interfacial nanobubbles. The working principle of the proposed method and mathematic models for dynamic contact angle measurement are presented. Geometric models of AFM tips were constructed using scanning electronic microscopy (SEM) images taken from different view directions. The detailed process of tip-nanobubble interaction was investigated using force-distance curves of AFM on nanobubbles. Several parameters including nanobubble height, adhesion and capillary force between tip and nanobubbles are extracted. The variation of these parameters was studied over nanobubble surfaces. The dynamic contact angles of the AFM tips were calculated from the capillary force measurements. The proposed method provides direct measurement of dynamic contact angles for AFM tips and can also be taken as a general approach for nanoscale dynamic wetting property investigation.

  9. High speed AFM studies of 193 nm immersion photoresists during TMAH development

    NASA Astrophysics Data System (ADS)

    Ngunjiri, Johnpeter; Meyers, Greg; Cameron, Jim; Suzuki, Yasuhiro; Jeon, Hyun; Lee, Dave; Choi, Kwang Mo; Kim, Jung Woo; Im, Kwang-Hwyi; Lim, Hae-Jin

    2016-03-01

    In this paper we report on our studies of the dynamic process of resist development in real time. Using High Speed - Atomic Force Microscopy (HS-AFM) in dilute developer solution, changes in morphology and nanomechanical properties of patterned resist were monitored. The Bruker Dimension FastScan AFMTM was applied to analyze 193 nm acrylic-based immersion resists in developer. HS-AFM operated in Peak Force mapping mode allowed for concurrent measurements of image topography resist stiffness, adhesion to AFM probe and deformation during development. In our studies we focused on HS-AFM topography data as it readily revealed detailed information about initial resist morphology, followed by a resist swelling process and eventual dissolution of the exposed resist areas. HS-AFM showed potential for tracking and understanding development of patterned resist films and can be useful in evaluating the dissolution properties of different resist designs.

  10. Determination of the depth profile distribution of guest species in microporous materials using the voltammetry of immobilized particles methodology: application to lapachol attachment to palygorskite and kaolinite.

    PubMed

    Doménech-Carbó, Antonio; Martini, Mariele; Valle-Algarra, Francisco Manuel

    2014-09-21

    A model for determining the in-depth profile distribution of electroactive species hosted in inorganic microporous matrixes using the voltammetry of immobilized particles methodology is described. The method, based on the analysis of cyclic voltammetric data at different potential scan rates, allows us to determine the in-depth profile variation of the concentration of electroactive guest species as well as the evaluation of the (oxidized form)/(reduced form) concentration ratio in cases where two oxidation states of the electroactive species coexist. The application to Maya blue-type materials prepared from lapachol, a naphtoquinonic dye, and palygorskite and kaolinite clays is reported. The determination of the in-depth distribution of guest molecules is not easy due to the heterogeneity of the clay particle size distribution and the appearance of cyclization and redox tuning reactions. Electrochemical data revealed differences in the in-depth distribution of the dye molecules in the grains of the channelled (palygorskite) and the laminar (kaolinite) clays that suggest that lapachol compounds can ingress into the channels of the palygorskite framework whereas remain externally adsorbed onto the kaolinite crystals. PMID:25093430

  11. (Solid state voltammetry and sensors in gases and other non-ionic media): Performance report, April 1, 1987--March 31, 1988

    SciTech Connect

    Murray, R.W.

    1988-01-01

    Progress is briefly described in the design and performance of an electrochemical microcell. This microcell contacts wire tips of 10..mu..m Pt working microelectrode and Ag reference and Pt auxiliary electrodes, sealed in glass and plastic, with a few micrometer thick film of an ionically conducting polymer /open quotes/solvent/close quotes/ containing dissolved electroactive monomers. The other side of the polymer film is contacted by a selected bathing gas from which other reagents can sorb into the polymer as reactants or as plasticizers. Using lithium triflate/poly(ethylene oxide), PEO LiCF/sub 3/SO/sub 3/, as the ionically conducting polymer solvent and species like ferrocene as electroactive solute, we demonstrated that quantitatively interpretable cyclic voltammetry could be carried out. We have recently completed work on a second and more elegant microcell design that defines the three electrodes of the cell microlithographically, with the working electrode being either a 11 /times/ 516 or 11 /times/ 256..mu..m microband or an 11 /times/ 11..mu..m square. Other work concerns electrochemical reactivity in PEO LiCF/sub 3/SO/sub 3/ and other polymer solvents. 5 refs.

  12. Study of temperature, air dew point temperature and reactant flow effects on proton exchange membrane fuel cell performances using electrochemical spectroscopy and voltammetry techniques

    NASA Astrophysics Data System (ADS)

    Wasterlain, S.; Candusso, D.; Hissel, D.; Harel, F.; Bergman, P.; Menard, P.; Anwar, M.

    A single PEMFC has been operated by varying the assembly temperature, the air dew point temperature and the anode/cathode stoichiometry rates with the aim to identify the parameters and combinations of factors affecting the cell performance. Some of the experiments were conducted with low humidified reactants (relative humidity of 12%). The FC characterizations tests have been conducted using in situ electrochemical methods based on load current and cell voltage signal analysis, namely: polarization curves, EIS measurements, cyclic and linear sweep voltammetries (CV and LSV). The impacts of the parameters on the global FC performances were observed using the polarization curves whereas EIS, CV and LSV test results were used to discriminate the different voltage loss sources. The test results suggest that some parameter sets allow maximal output voltages but can also induce material degradation. For instance, higher FC temperature and air flow values can induce significant electrical efficiency benefits, notably by increasing the reversible potential and the reaction kinetics. However, raising the cell temperature can also gradually dry the FC and increase the risk of membrane failure. LSV has also shown that elevated FC temperature and relative humidity can also accelerate the electrolyte degradation (i.e. slightly higher fuel crossover rate) and reduce the lifetime consequently.

  13. Electrochemical Characterization and Determination of Phenol and Chlorophenols by Voltammetry at Single Wall Carbon Nanotube/Poly(3,4-ethylenedioxythiophene) Modified Screen Printed Carbon Electrode

    PubMed Central

    Negash, Negussie; Alemu, Hailemichael; Tessema, Merid

    2015-01-01

    Screen printed carbon electrode (SPCE) has been modified with single wall carbon nanotube/poly(3,4-ethylenedioxythiophene) (SWCNT/PEDOT) composites for the determination of phenol and chlorophenols (phenol, 4-chlorophenol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol). The effect of the modifiers on the electrode characteristics was evaluated and the responses were optimized for the voltammetric determination of phenol and chlorophenols. The parameters affecting the responses such as pH, scan rate, and stability were studied. The analytical performance of the SWCNT/PEDOT/SPCE using cyclic voltammetry was tested and found to be impressive. Under these conditions, the designed electrode showed a good performance for the voltammetric measurements of the phenolic compounds. The modified SPCE, when it is compared with other enzymatic and nonenzymatic sensors, showed a wider dynamic range for the detection of the phenolic compounds. The modified SPCE was used for the quantification of phenol in water samples. The results suggest that the method is quite useful for analyzing and monitoring phenols and chlorophenols. PMID:27347519

  14. A potentiostat featuring an integrator transimpedance amplifier for the measurement of very low currents—Proof-of-principle application in microfluidic separations and voltammetry

    NASA Astrophysics Data System (ADS)

    Koutilellis, G. D.; Economou, A.; Efstathiou, C. E.

    2016-03-01

    This work reports the design and construction of a novel potentiostat which features an integrator transimpedance amplifier as a current-monitoring unit. The integration approach addresses the limitations of the feedback resistor approach used for current monitoring in conventional potentiostat designs. In the present design, measurement of the current is performed by a precision switched integrator transimpedance amplifier operated in the dual sampling mode which enables sub-pA resolution. The potentiostat is suitable for measuring very low currents (typical dynamic range: 5 pA-4.7 μA) with a 16 bit resolution, and it can support 2-, 3- and 4-electrode cell configurations. Its operation was assessed by using it as a detection module in a home-made capillary electrophoresis system for the separation and amperometric detection of paracetamol and p-aminophenol at a 3-electrode microfluidic chip. The potential and limitations of the proposed potentiostat to implement fast potential-scan voltammetric techniques were demonstrated for the case of cyclic voltammetry.

  15. BOREAS AFM-2 Wyoming King Air 1994 Aircraft Sounding Data

    NASA Technical Reports Server (NTRS)

    Kelly, Robert D.; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The BOREAS AFM-2 team used the University of Wyoming King Air aircraft during IFCs 1, 2, and 3 in 1994 to collected pass-by-pass fluxes (and many other statistics) for the large number of level (constant altitude), straight-line passes used in a variety of flight patterns over the SSA and NSA and areas along the transect between these study areas. The data described here form a second set, namely soundings that were incorporated into nearly every research flight by the King Air in 1994. These soundings generally went from near the surface to above the inversion layer. Most were flown immediately after takeoff or immediately after finishing the last flux pattern of that particular day's flights. The parameters that were measured include wind direction, wind speed, west wind component (u), south wind component (v), static pressure, air dry bulb temperature, potential temperature, dewpoint, temperature, water vapor mixing ratio, and CO2 concentration. Data on the aircraft's location, attitude, and altitude during data collection are also provided. These data are stored in tabular ASCH files. The data files are available on a CD-ROM (see document number 20010000884) or from the Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC).

  16. BOREAS AFM-03-NCAR Electra 1994 Aircraft Sounding Data

    NASA Technical Reports Server (NTRS)

    Lenschow, Donald H.; Oncley, Steven P.; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-3 team used the National Center for Atmospheric Research's (NCAR) Electra aircraft to make sounding measurements to study the planetary boundary layer using in situ and remote-sensing measurements. Measurements were made of wind speed and direction, air pressure and temperature, potential temperature, dewpoint, mixing ratio of H, O, CO, concentration, and ozone concentration. Twenty-five research missions were flown over the Northern Study Area (NSA), Southern Study Area (SSA), and the transect during BOREAS Intensive Field Campaigns (IFCs) 1, 2, and 3 during 1994. All missions had from four to ten soundings through the top of the planetary boundary layer. This sounding data set contains all of the in situ vertical profiles through the boundary layer top that were made (with the exception of 'porpoise' maneuvers). Data were recorded in one-second time intervals. These data are stored in tabular ASCII files. The NCAR Electra 1994 aircraft sounding data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  17. AFM-based force microsensor for a microrobot

    NASA Astrophysics Data System (ADS)

    Fatikow, Sergej; Fahlbusch, Stephan

    2001-10-01

    Microrobots are the result of increasing research activities at the border between microsystem technology and robotics. Today already, robots with dimensions of a few cubic- centimeters can be developed. Like conventional robots, microrobots represent a complex system that usually contains several different types of actuators and sensors. The measurement of gripping forces is the most important sensor application in micromanipulation besides visual servoing to protect the parts from too high surface pressures and thereby damage during the assembly process. Very small forces in the range of 200 (mu) N down to 0.1 (mu) N or even less have to be sensed. Thus, the aim of our current research activities is the development of a high-resolution integrated force microsensor for measuring gripping forces in a microhandling robot. On the one hand, the sensor should be a device for teleoperated manipulation tasks in a flexible microhandling station. On the other hand, typical microhandling operations should to a large extend be automated with the aid of computer-based signal processing of sensor information. The user should be provided with an interface for teleoperated manipulation and an interface for partially automated manipulation of microobjects. In this paper, a concept for the measurement of gripping forces in microrobotics using piezoresistive AFM (atomic force microscope) cantilevers is introduced. Further on, the concept of a microrobot-based SEM station and its applications are presented.

  18. AFM Investigation of Liquid-Filled Polymer Microcapsules Elasticity.

    PubMed

    Sarrazin, Baptiste; Tsapis, Nicolas; Mousnier, Ludivine; Taulier, Nicolas; Urbach, Wladimir; Guenoun, Patrick

    2016-05-10

    Elasticity of polymer microcapsules (MCs) filled with a liquid fluorinated core is studied by atomic force microscopy (AFM). Accurately characterized spherical tips are employed to obtain the Young's moduli of MCs having four different shell thicknesses. We show that those moduli are effective ones because the samples are composites. The strong decrease of the effective MC elasticity (from 3.0 to 0.1 GPa) as the shell thickness decreases (from 200 to 10 nm) is analyzed using a novel numerical approach. This model describes the evolution of the elasticity of a coated half-space according to the contact radius, the thickness of the film, and the elastic moduli of bulk materials. This numerical model is consistent with the experimental data and allows simulating the elastic behavior of MCs at high frequencies (5 MHz). While the quasi-static elasticity of the MCs is found to be very dependent on the shell thickness, the high frequency (5 MHz) elastic behavior of the core leads to a stable behavior of the MCs (from 2.5 to 3 GPa according to the shell thickness). Finally, the effect of thermal annealing on the MCs elasticity is investigated. The Young's modulus is found to decrease because of the reduction of the shell thickness due to the loss of the polymer. PMID:27058449

  19. Cyclic GMP and Cilia Motility

    PubMed Central

    Wyatt, Todd A.

    2015-01-01

    Motile cilia of the lungs respond to environmental challenges by increasing their ciliary beat frequency in order to enhance mucociliary clearance as a fundamental tenant of innate defense. One important second messenger in transducing the regulable nature of motile cilia is cyclic guanosine 3′,5′-monophosphate (cGMP). In this review, the history of cGMP action is presented and a survey of the existing data addressing cGMP action in ciliary motility is presented. Nitric oxide (NO)-mediated regulation of cGMP in ciliated cells is presented in the context of alcohol-induced cilia function and dysfunction. PMID:26264028

  20. Fitting curves to cyclic data

    USGS Publications Warehouse

    Langbein, W.B.

    1955-01-01

    A common problem in hydrology is to fit a smooth curve to cyclic or periodic data, either to define the most probable values of the data or to test some principle that one wishes to demonstrate.  This study treats of those problems where the length or period of the cycle is know beforehand - as a day, year, or meander length for example.  Curve-fitting can be made by free-hand drawing, and where the data are closely aligned this method offers the simplest and most direct course.  However, there are many problems where the best fit is far from obvious, and analytical methods may be necessary.

  1. How Do Structure and Charge Affect Metal-Complex Binding to DNA? An Upper-Division Integrated Laboratory Project Using Cyclic Voltammetry

    ERIC Educational Resources Information Center

    Kulczynska, Agnieszka; Johnson, Reed; Frost, Tony; Margerum, Lawrence D.

    2011-01-01

    An advanced undergraduate laboratory project is described that integrates inorganic, analytical, physical, and biochemical techniques to reveal differences in binding between cationic metal complexes and anionic DNA (herring testes). Students were guided to formulate testable hypotheses based on the title question and a list of different metal…

  2. Abrasive stripping square-wave voltammetry of blackberry, raspberry, strawberry, pomegranate, and sweet and blue potatoes.

    PubMed

    Komorsky-Lovrić, Šebojka; Novak, Ivana

    2011-08-01

    Electro-oxidation potentials of 7 fruits and vegetables were determined by abrasive stripping voltammetry. The responses were characterized by 2 peaks with maxima at 0.45 and 0.55 V compared with Ag/AgCl, respectively. Both electrode reactions appear reversible at a frequency of 8 Hz. They can be ascribed to anthocyanidins and ellagic acid as electroactive compounds. By this method, an antioxidative capacity of a certain plant can be quickly estimated without extraction of active components. PMID:22417490

  3. Linear-sweep voltammetry of a soluble redox couple in a cylindrical electrode

    NASA Technical Reports Server (NTRS)

    Weidner, John W.

    1991-01-01

    An approach is described for using the linear sweep voltammetry (LSV) technique to study the kinetics of flooded porous electrodes by assuming a porous electrode as a collection of identical noninterconnected cylindrical pores that are filled with electrolyte. This assumption makes possible to study the behavior of this ideal electrode as that of a single pore. Alternatively, for an electrode of a given pore-size distribution, it is possible to predict the performance of different pore sizes and then combine the performance values.

  4. Electrochemistry and analytical determination of lysergic acid diethylamide (LSD) via adsorptive stripping voltammetry.

    PubMed

    Merli, Daniele; Zamboni, Daniele; Protti, Stefano; Pesavento, Maria; Profumo, Antonella

    2014-12-01

    Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1-90 ng L(-1) for deposition times of 50s. LOD of 1.4 ng L(-1) and LOQ of 4.3 ng L(-1) were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane. PMID:25159435

  5. D.C. voltammetry of ionic liquid-based capacitors: effects of Faradaic reactions, electrolyte resistance and voltage scan speed investigated using an electrode of carbon nanotubes in EMIM-EtSO4.

    PubMed

    Zheng, J P; Pettit, C M; Goonetilleke, P C; Zenger, G M; Roy, D

    2009-05-15

    Carbon nanotube (CNT) electrodes in combination with ionic liquid (IL) electrolytes are potentially important for energy storage systems. We report electrochemical investigation of such a system involving a paper-electrode of multi-wall CNT (MWCNT) in the IL of 1-ethyl-3-methyl imidazolium ethylsulfate (EMIM-EtSO(4)). Our study concentrates on the analytical aspects of cyclic voltammetry (CV) to probe the double layer capacitance of these relatively unconventional systems (that involve rather large charge-discharge time constants). Both theoretical and experimental aspects of CV for such systems are discussed, focusing in particular, on the effects of Faradaic side-reactions, electrolyte resistance and voltage scan speeds. The results are analyzed using an electrode equivalent circuit (EEC) model, demonstrating a method to account for the typical artifacts expected in CV of CNT-IL interfaces. PMID:19269472

  6. Insights into How Cyclic Peptides Switch Conformations.

    PubMed

    McHugh, Sean M; Rogers, Julia R; Yu, Hongtao; Lin, Yu-Shan

    2016-05-10

    Cyclic peptides have recently emerged as promising modulators of protein-protein interactions. However, it is currently highly difficult to predict the structures of cyclic peptides owing to their rugged conformational free energy landscape, which prevents sampling of all thermodynamically relevant conformations. In this article, we first investigate how a relatively flexible cyclic hexapeptide switches conformations. It is found that, although the circular geometry of small cyclic peptides of size 6-8 may require rare, coherent dihedral changes to sample a new conformation, the changes are rather local, involving simultaneous changes of ϕi and ψi or ψi and ϕi+1. The understanding of how these cyclic peptides switch conformations enables the use of metadynamics simulations with reaction coordinates specifically targeting such coupled two-dihedral changes to effectively sample cyclic peptide conformational space. PMID:27031286

  7. Advances in targeting cyclic nucleotide phosphodiesterases

    PubMed Central

    Maurice, Donald H.; Ke, Hengming; Ahmad, Faiyaz; Wang, Yousheng; Chung, Jay; Manganiello, Vincent C.

    2014-01-01

    Cyclic nucleotide phosphodiesterases (PDEs) catalyse the hydrolysis of cyclic AMP and cyclic GMP, thereby regulating the intracellular concentrations of these cyclic nucleotides, their signalling pathways and, consequently, myriad biological responses in health and disease. Currently, a small number of PDE inhibitors are used clinically for treating the pathophysiological dysregulation of cyclic nucleotide signalling in several disorders, including erectile dysfunction, pulmonary hypertension, acute refractory cardiac failure, intermittent claudication and chronic obstructive pulmonary disease. However, pharmaceutical interest in PDEs has been reignited by the increasing understanding of the roles of individual PDEs in regulating the subcellular compartmentalization of specific cyclic nucleotide signalling pathways, by the structure-based design of novel specific inhibitors and by the development of more sophisticated strategies to target individual PDE variants. PMID:24687066

  8. Advances in targeting cyclic nucleotide phosphodiesterases.

    PubMed

    Maurice, Donald H; Ke, Hengming; Ahmad, Faiyaz; Wang, Yousheng; Chung, Jay; Manganiello, Vincent C

    2014-04-01

    Cyclic nucleotide phosphodiesterases (PDEs) catalyse the hydrolysis of cyclic AMP and cyclic GMP, thereby regulating the intracellular concentrations of these cyclic nucleotides, their signalling pathways and, consequently, myriad biological responses in health and disease. Currently, a small number of PDE inhibitors are used clinically for treating the pathophysiological dysregulation of cyclic nucleotide signalling in several disorders, including erectile dysfunction, pulmonary hypertension, acute refractory cardiac failure, intermittent claudication and chronic obstructive pulmonary disease. However, pharmaceutical interest in PDEs has been reignited by the increasing understanding of the roles of individual PDEs in regulating the subcellular compartmentalization of specific cyclic nucleotide signalling pathways, by the structure-based design of novel specific inhibitors and by the development of more sophisticated strategies to target individual PDE variants. PMID:24687066

  9. Cyclic Imide Dioxime: Formation and Hydrolytic Stability

    SciTech Connect

    Kang, S.O.; Vukovic, Sinisa; Custelcean, Radu; Hay, Benjamin

    2012-01-01

    Poly(acrylamidoximes) play an important role in the uranium extraction from seawater. The present work reports solution studies of simple analogs to address the formation and stability of two binding sites present in these polymers, open-chain amidoximes and cyclic imide dioximes, including: 1) conditions that maximize the formation of the cyclic form, 2) existence of a base-induced conversion from open-chain to cyclic form, and 3) degradation under acid and base conditions.

  10. XPS and AFM Study of GaAs Surface Treatment

    SciTech Connect

    Contreras-Guerrero, R.; Wallace, R. M.; Aguirre-Francisco, S.; Herrera-Gomez, A.; Lopez-Lopez, M.

    2008-11-13

    Obtaining smooth and atomically clean surfaces is an important step in the preparation of a surface for device manufacturing. In this work different processes are evaluated for cleaning a GaAs surface. A good surface cleaning treatment is that which provides a high level of uniformity and controllability of the surface. Different techniques are useful as cleaning treatments depending on the growth process to be used. The goal is to remove the oxygen and carbon contaminants and then form a thin oxide film to protect the surface, which is easy to remove later with thermal desorption mechanism like molecular beam epitaxy (MBE) with minimal impact to the surface. In this study, atomic force microscopy (AFM), x-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS) were used to characterize the structure of the surface, the composition, as well as detect oxygen and carbon contaminant on the GaAs surface. This study consists in two parts. The first part the surface was subjected to different chemical treatments. The chemical solutions were: (a)H{sub 2}SO{sub 4}:H{sub 2}O{sub 2}:H{sub 2}O(4:1:100), (b) HCl: H{sub 2}O(1:3), (c)NH{sub 4}OH 29%. The treatments (a) and (b) reduced the oxygen on the surface. Treatment (c) reduces carbon contamination. In the second part we made MOS devices on the surfaces treated. They were characterized by CV and IV electrical measurements. They show frequency dispersion.

  11. AFM nanoscale indentation in air of polymeric and hybrid materials with highly different stiffness

    NASA Astrophysics Data System (ADS)

    Suriano, Raffaella; Credi, Caterina; Levi, Marinella; Turri, Stefano

    2014-08-01

    In this study, nanomechanical properties of a variety of polymeric materials was investigated by means of AFM. In particular, selecting different AFM probes, poly(methyl methacrylate) (PMMA), polydimethylsiloxane (PDMS) bulk samples, sol-gel hybrid thin films and hydrated hyaluronic acid hydrogels were indented in air to determine the elastic modulus. The force-distance curves and the indentation data were found to be greatly affected by the cantilever stiffness and by tip geometry. AFM indentation tests show that the choice of the cantilever spring constant and of tip shape is crucially influenced by elastic properties of samples. When adhesion-dominated interactions occur between the tip and the surface of samples, force-displacement curves reveal that a suitable functionalization of AFM probes allows the control of such interactions and the extraction of Young' modulus from AFM curves that would be otherwise unfeasible. By applying different mathematical models depending on AFM probes and materials under investigation, the values of Young's modulus were obtained and compared to those measured by rheological and dynamic mechanical analysis or to literature data. Our results show that a wide range of elastic moduli (10 kPa-10 GPa) can be determined by AFM in good agreement with those measured by conventional macroscopic measurements.

  12. A simplified method for selecting a carbon-fiber electrode in pulse voltammetry.

    PubMed

    Liao, B Y; Lio, H P; Wang, C Y; Young, M S; Ho, M T; Lin, M T

    1993-12-01

    A method for selecting a usable carbon-fiber electrode using the equivalent resistance and capacitance is presented. This method uses an instrument with a PC-based look-up table for measuring the electrical characteristics of a carbon-fiber electrode in pulse voltammetry. Using this instrument, the equivalent resistance and capacitance of the carbon-fiber electrode in saturated sodium chloride solution can be obtained. This instrument includes a decade resistance box, a peak current detection and hold circuit, a half peak comparator and a decay duration counter. A look-up table is established by using RC circuits to emulate the electrochemical reaction of the carbon-fiber electrode in pulse voltammetry. The equivalent resistance is obtained from the decade resistance box according to Kirchhoff's law. Then the equivalent capacitance is determined from the decay duration counter reading and equivalent resistance with the look-up table via a PC interpolation program. After obtaining the equivalent resistance and capacitance of an electrode, the values are compared with the usable thresholds. This method provides an effective quality evaluation index of carbon-fiber electrode for the user in order to reduce electrode-induced experimental failure. The method is also available for other kinds of carbon-fiber electrodes as long as their look-up table and desired thresholds are established. PMID:8152240

  13. Solid state voltammetry and sensors in solids and gases. Performance report, April 1991--March 1992

    SciTech Connect

    Murray, R.W.

    1992-04-01

    This project explores the electrochemical reactivity of electron transfer donor/acceptors dissolved in and diffusing through solid and semi-solid, ionically conductive media. The emphasis is on developing voltammetric experiments that are quantitatively interpretable in terms of the mass transport and electron transfer rates and thermodynamic equilibria of the redox solutes, and to exploit such experiments to probe their chemical and electrochemical behavior in the solid media. Techniques for quantitative voltammetry in solids were essentially unknown prior to initiation of this DOE project. We mainly employ poly(ethers)s containing dissolved metal salts electrolytes (``polymer electrolytes``), as prototype solid and semi-solid solvents. During this award year we have (a) concluded a study of plasticization chemistry in poly (ether) polymer electrolytes, (b) made progress in devising techniques for measuring the rates of electron transfer reactions in solid and semi-solid poly (ether)s, (c) continued efforts to design and understand the behavior of microband electrodes of various widths (0.1 to 10 {mu}m) in voltammetry of redox solutes, and (d) initiated synthetic efforts to attach ethylene oxide chains of various lengths to redox solutes.

  14. Hydrodynamic Voltammetry as a Rapid and Simple Method for Evaluating Soil Enzyme Activities

    PubMed Central

    Sazawa, Kazuto; Kuramitz, Hideki

    2015-01-01

    Soil enzymes play essential roles in catalyzing reactions necessary for nutrient cycling in the biosphere. They are also sensitive indicators of ecosystem stress, therefore their evaluation is very important in assessing soil health and quality. The standard soil enzyme assay method based on spectroscopic detection is a complicated operation that requires the removal of soil particles. The purpose of this study was to develop a new soil enzyme assay based on hydrodynamic electrochemical detection using a rotating disk electrode in a microliter droplet. The activities of enzymes were determined by measuring the electrochemical oxidation of p-aminophenol (PAP), following the enzymatic conversion of substrate-conjugated PAP. The calibration curves of β-galactosidase (β-gal), β-glucosidase (β-glu) and acid phosphatase (AcP) showed good linear correlation after being spiked in soils using chronoamperometry. We also performed electrochemical detection using real soils. Hydrodynamic chronoamperometry can be used to assess the AcP in soils, with a detection time of only 90 s. Linear sweep voltammetry was used to measure the amount of PAP released from β-gal and β-glu by enzymatic reaction after 60 min. For the assessment of soil enzymes, the results of hydrodynamic voltammetry assay compared favorably to those using a standard assay procedure, but this new procedure is more user-friendly, rapid and simple. PMID:25746097

  15. Investigation of antioxidant capacity of the extracts of bilberry (VACCINUM MYRTILLIS L.) by voltammetry

    NASA Astrophysics Data System (ADS)

    Vtorushina, A. N.; Nikonova, E. D.

    2016-02-01

    This paper deals with the urgent issue of the search of new drugs based on plant raw materials that have an influence on various stages of oxidation processes occurring in the human body. The aim of this paper is to determine the antioxidant activity of the bilberry extracts that are used in the medicine practice by a cathodic voltammetry method. We consider the influence of water and alcohol bilberry extracts on the process of oxygen electroreduction. From these extracts the most activity relation to the process of cathodic oxygen reduction showed alcohol (40%) bilberry extract. It was also stated that the alcohol extract of bilberry has a greater antioxidant activity than other known antioxidants such as ascorbic acid, glucose, dihydroquercetin. Thus, after consideration of a number of plant objects, we showed the possibility of applying the method of cathodic voltammetry for the determination of total antioxidant activity of plant material and identifying and highlighting the most perspective sources of biologically active substances (BAS), as well as the ability of identifying extractants that fully extract BAS from plant raw materials. The activity data of extracts of plant raw materials gives an opportunity of establishing an effective yield phytopreparation based on bilberry that has an antioxidant effect.

  16. Cyclic voltammetric study of the redox system of glutathione using the disulfide bond reductant tris(2-carboxyethyl)phosphine.

    PubMed

    Kizek, René; Vacek, Jan; Trnková, Libuse; Jelen, Frantisek

    2004-06-01

    The stabilization of the reduction state of proteins and peptides is very important for the monitoring of protein-protein, protein-DNA and protein-xenobiotic interactions. The reductive state of protein or peptide is characterized by the reactive sulfhydryl group. Glutathione in the reduced (GSH) and oxidized (GSSG) forms was studied by cyclic voltammetry. Tris(2-carboxyethyl)phosphine (TCEP) as the disulfide bond reductant and/or hydrogen peroxide as the sulfhydryl group oxidant were used. Cyclic voltammetry measurements, following the redox state of glutathione, were performed on a hanging mercury drop electrode (HMDE) in borate buffer (pH 9.2). It was shown that in aqueous solutions TCEP was able to reduce disulfide groups smoothly and quantitatively. The TCEP response at -0.25 V vs. Ag/AgCl/3 M KCl did not disturb the signals of the thiol/disulfide redox couple. The origin of cathodic and anodic signals of GSH (at -0.44 and -0.37 V) and GSSG (at -0.69 and -0.40 V) glutathione forms is discussed. It was shown that the application of TCEP to the conservation of sulfhydryl groups in peptides and proteins can be useful instrument for the study of peptides and proteins redox behavior. PMID:15110242

  17. Tuning the resonance of a photonic crystal microcavity with an AFM probe.

    PubMed

    Märki, Iwan; Salt, Martin; Herzig, Hans Peter

    2006-04-01

    We present theoretical and experimental results on switching and tuning of a two-dimensional photonic crystal resonant microcavity by means of a silicon AFM tip, probing the highly localized optical field in the vicinity of the cavity. On-off switching and modulation of the transmission signal in the kHz range is achieved by bringing an AFM tip onto the center of the microcavity, inducing a damping effect on the transmission resonance. Tuning of the resonant wavelength in the order of several nanometers becomes possible by inserting the AFM tip into one of the holes of the Bragg mirror forming the microcavity in the propagation direction. PMID:19516436

  18. Development of portable experimental set-up for AFM to work at cryogenic temperature

    NASA Astrophysics Data System (ADS)

    Agarwal, D. H.; Bhatt, P. M.; Pathan, A. M.; Patel, Hitarthi; Joshi, U. S.

    2012-06-01

    We report on the designing aspects and fabrication of low temperature atomic force microscope (AFM) to study the surface structures of nanomaterials. Several key features of design including liquid nitrogen reservoir, vacuum chamber, vibration isolation table etc. have been presented. The whole set up was assembled in-house at a fairly low cost to be used with any commercial AFM system. The surface morphology of important oxide (In0.94Sn0.04)2O3 (ITO) thin film nanostructures has been investigated using the cryogenic AFM set up.

  19. The formation of liquid bridge in different operating modes of AFM

    NASA Astrophysics Data System (ADS)

    Wei, Zheng; Sun, Yan; Ding, WenXuan; Wang, ZaiRan

    2016-09-01

    The liquid bridge is one of the principal factors that cause artifacts in ambient-pressure atomic force microscope (AFM) images. Additionally, it is the main component of the adhesion force in ambient conditions. To understand the AFM imaging mechanism and the sample characteristics, it is essential to study the liquid bridge. This study interprets the physical mechanism involved in liquid bridge formation, which is composed of three different physical processes: the squeezing process, capillary condensation, and liquid film flow. We discuss the contributions of these three mechanisms to the volume and the capillary force of the liquid bridge in different AFM operation modes.

  20. MetaRep, an extended CMAS 3D program to visualize mafic (CMAS, ACF-S, ACF-N) and pelitic (AFM-K, AFM-S, AKF-S) projections

    NASA Astrophysics Data System (ADS)

    France, Lydéric; Nicollet, Christian

    2010-06-01

    MetaRep is a program based on our earlier program CMAS 3D. It is developed in MATLAB ® script. MetaRep objectives are to visualize and project major element compositions of mafic and pelitic rocks and their minerals in the pseudo-quaternary projections of the ACF-S, ACF-N, CMAS, AFM-K, AFM-S and AKF-S systems. These six systems are commonly used to describe metamorphic mineral assemblages and magmatic evolutions. Each system, made of four apices, can be represented in a tetrahedron that can be visualized in three dimensions with MetaRep; the four tetrahedron apices represent oxides or combination of oxides that define the composition of the projected rock or mineral. The three-dimensional representation allows one to obtain a better understanding of the topology of the relationships between the rocks and minerals and relations. From these systems, MetaRep can also project data in ternary plots (for example, the ACF, AFM and AKF ternary projections can be generated). A functional interface makes it easy to use and does not require any knowledge of MATLAB ® programming. To facilitate the use, MetaRep loads, from the main interface, data compiled in a Microsoft Excel ™ spreadsheet. Although useful for scientific research, the program is also a powerful tool for teaching. We propose an application example that, by using two combined systems (ACF-S and ACF-N), provides strong confirmation in the petrological interpretation.

  1. Nonlinear, nonbinary cyclic group codes

    NASA Technical Reports Server (NTRS)

    Solomon, G.

    1992-01-01

    New cyclic group codes of length 2(exp m) - 1 over (m - j)-bit symbols are introduced. These codes can be systematically encoded and decoded algebraically. The code rates are very close to Reed-Solomon (RS) codes and are much better than Bose-Chaudhuri-Hocquenghem (BCH) codes (a former alternative). The binary (m - j)-tuples are identified with a subgroup of the binary m-tuples which represents the field GF(2 exp m). Encoding is systematic and involves a two-stage procedure consisting of the usual linear feedback register (using the division or check polynomial) and a small table lookup. For low rates, a second shift-register encoding operation may be invoked. Decoding uses the RS error-correcting procedures for the m-tuple codes for m = 4, 5, and 6.

  2. Cyclic strength of hard metals

    SciTech Connect

    Sereda, N.N.; Gerikhanov, A.K.; Koval'chenko, M.S.; Pedanov, L.G.; Tsyban', V.A.

    1986-02-01

    The authors study the strength of hard-metal specimens and structural elements under conditions of cyclic loading since many elements of processing plants, equipment, and machines are made of hard metals. Fatigue tests were conducted on KTS-1N, KTSL-1, and KTNKh-70 materials, which are titanium carbide hard metals cemented with nickel-molybdenum, nickelcobalt-chromium, and nickel-chromium alloys, respectively. As a basis of comparison, the standard VK-15 (WC+15% Co) alloy was used. Some key physicomechanical characteristics of the materials investigated are presented. On time bases not exceeding 10/sup 6/ cycles, titanium carbide hard metals are comparable in fatigue resistance to the standard tungstencontaining hard metals.

  3. Cell reorientation under cyclic stretching.

    PubMed

    Livne, Ariel; Bouchbinder, Eran; Geiger, Benjamin

    2014-01-01

    Mechanical cues from the extracellular microenvironment play a central role in regulating the structure, function and fate of living cells. Nevertheless, the precise nature of the mechanisms and processes underlying this crucial cellular mechanosensitivity remains a fundamental open problem. Here we provide a novel framework for addressing cellular sensitivity and response to external forces by experimentally and theoretically studying one of its most striking manifestations--cell reorientation to a uniform angle in response to cyclic stretching of the underlying substrate. We first show that existing approaches are incompatible with our extensive measurements of cell reorientation. We then propose a fundamentally new theory that shows that dissipative relaxation of the cell's passively-stored, two-dimensional, elastic energy to its minimum actively drives the reorientation process. Our theory is in excellent quantitative agreement with the complete temporal reorientation dynamics of individual cells measured over a wide range of experimental conditions, thus elucidating a basic aspect of mechanosensitivity. PMID:24875391

  4. Cell reorientation under cyclic stretching

    NASA Astrophysics Data System (ADS)

    Livne, Ariel; Bouchbinder, Eran; Geiger, Benjamin

    2014-05-01

    Mechanical cues from the extracellular microenvironment play a central role in regulating the structure, function and fate of living cells. Nevertheless, the precise nature of the mechanisms and processes underlying this crucial cellular mechanosensitivity remains a fundamental open problem. Here we provide a novel framework for addressing cellular sensitivity and response to external forces by experimentally and theoretically studying one of its most striking manifestations—cell reorientation to a uniform angle in response to cyclic stretching of the underlying substrate. We first show that existing approaches are incompatible with our extensive measurements of cell reorientation. We then propose a fundamentally new theory that shows that dissipative relaxation of the cell’s passively-stored, two-dimensional, elastic energy to its minimum actively drives the reorientation process. Our theory is in excellent quantitative agreement with the complete temporal reorientation dynamics of individual cells measured over a wide range of experimental conditions, thus elucidating a basic aspect of mechanosensitivity.

  5. Rank estimation and the multivariate analysis of in vivo fast-scan cyclic voltammetric data

    PubMed Central

    Keithley, Richard B.; Carelli, Regina M.; Wightman, R. Mark

    2010-01-01

    Principal component regression has been used in the past to separate current contributions from different neuromodulators measured with in vivo fast-scan cyclic voltammetry. Traditionally, a percent cumulative variance approach has been used to determine the rank of the training set voltammetric matrix during model development, however this approach suffers from several disadvantages including the use of arbitrary percentages and the requirement of extreme precision of training sets. Here we propose that Malinowski’s F-test, a method based on a statistical analysis of the variance contained within the training set, can be used to improve factor selection for the analysis of in vivo fast-scan cyclic voltammetric data. These two methods of rank estimation were compared at all steps in the calibration protocol including the number of principal components retained, overall noise levels, model validation as determined using a residual analysis procedure, and predicted concentration information. By analyzing 119 training sets from two different laboratories amassed over several years, we were able to gain insight into the heterogeneity of in vivo fast-scan cyclic voltammetric data and study how differences in factor selection propagate throughout the entire principal component regression analysis procedure. Visualizing cyclic voltammetric representations of the data contained in the retained and discarded principal components showed that using Malinowski’s F-test for rank estimation of in vivo training sets allowed for noise to be more accurately removed. Malinowski’s F-test also improved the robustness of our criterion for judging multivariate model validity, even though signal-to-noise ratios of the data varied. In addition, pH change was the majority noise carrier of in vivo training sets while dopamine prediction was more sensitive to noise. PMID:20527815

  6. Cyclic Linearization and Island Repair in Sluicing

    ERIC Educational Resources Information Center

    Qiu, Chunan

    2009-01-01

    Cyclic Linearization is adopted to account for the island repair of Sluicing in English. The extraction of wh-phrase out of certain islands undergoes non-successive-cyclic movement, which yields conflicting ordering statements. The derivation can be rescued by deleting all ordering statements in IP, including those conflicting ones. Two arguments…

  7. Twisted Cyclic Cohomology and Modular Fredholm Modules

    NASA Astrophysics Data System (ADS)

    Rennie, Adam; Sitarz, Andrzej; Yamashita, Makoto

    2013-07-01

    Connes and Cuntz showed in [Comm. Math. Phys. 114 (1988), 515-526] that suitable cyclic cocycles can be represented as Chern characters of finitely summable semifinite Fredholm modules. We show an analogous result in twisted cyclic cohomology using Chern characters of modular Fredholm modules. We present examples of modular Fredholm modules arising from Podleś spheres and from SUq(2).

  8. Probing Cytoskeletal Structures by Coupling Optical Superresolution and AFM Techniques for a Correlative Approach

    PubMed Central

    Chacko, Jenu Varghese; Zanacchi, Francesca Cella; Diaspro, Alberto

    2013-01-01

    In this article, we describe and show the application of some of the most advanced fluorescence superresolution techniques, STED AFM and STORM AFM microscopy towards imaging of cytoskeletal structures, such as microtubule filaments. Mechanical and structural properties can play a relevant role in the investigation of cytoskeletal structures of interest, such as microtubules, that provide support to the cell structure. In fact, the mechanical properties, such as the local stiffness and the elasticity, can be investigated by AFM force spectroscopy with tens of nanometers resolution. Force curves can be analyzed in order to obtain the local elasticity (and the Young's modulus calculation by fitting the force curves from every pixel of interest), and the combination with STED/STORM microscopy integrates the measurement with high specificity and yields superresolution structural information. This hybrid modality of superresolution-AFM working is a clear example of correlative multimodal microscopy. PMID:24027190

  9. Hydrodynamic voltammetry at tubular electrodes-III Determination of traces of bismuth by differential-pulse anodic-stripping voltammetry at a glassy-carbon tubular electrode with in situ mercury plating.

    PubMed

    Zhen, W; Qiang, C

    1987-07-01

    An equation for the current in differential-pulse anodic-stripping voltammetry at tubular electrodes is derived. Application of a glassy-carbon tubular electrode to determination of traces of bismuth in environmental water samples by differential-pulse anodic-stripping voltammetry is described. In hydrochloric acid medium, the stripping peak current is proportional to the concentration of bismuth in the range 2-100 ng/ml, with a deposition time of 3-10 min. The detection limit is 0.5 ng/ml. PMID:18964381

  10. Phase behaviors of cyclic diblock copolymers.

    PubMed

    Zhang, Guojie; Fan, Zhongyong; Yang, Yuliang; Qiu, Feng

    2011-11-01

    A spectral method of self-consistent field theory has been applied to AB cyclic block copolymers. Phase behaviors of cyclic diblock copolymers, such as order-disorder transition, order-order transition, and domain spacing size, have been studied, showing good consistency with previous experimental and theoretical results. Compared to linear diblocks, cyclic diblocks are harder to phase separate due to the topological constraint of the ring structure. A direct disorder-to-cylinder transition window is observed in the phase diagram, which is significantly different from the mean field phase diagram of linear diblock copolymers. The domain spacing size ratio between cyclic and linear diblock copolymers is typically close to 0.707, indicating in segregation that the cyclic polymer can be considered to be made up of linear diblocks with half of the original chain length. PMID:22070321

  11. The dependence of Escherichia coli asparaginase II formation on cyclic AMP and cyclic AMP receptor protein.

    PubMed

    Russell, L; Yamazaki, H

    1978-05-01

    The amount of asparaginase II in an Escherichia coli wild-type strain (cya+, crp+) markedly increased upon a shift from aerobic to anaerobic growth. However, no such increase occurred in a mutant (cya) lacking cyclic AMP synthesis unless supplemented with exogenous cyclic AMP. Since a mutant (crp) deficient in cyclic AMP receptor protein also did not support the anaerobic formation of this enzyme, it is concluded that the formation of E. coli asparaginase II depends on both cyclic AMP and cyclic AMP receptor protein. PMID:207402

  12. Using XAFS, EDAX and AFM in comparative study of various natural and synthetic emeralds

    NASA Astrophysics Data System (ADS)

    Parikh, P.; Saini, N. L.; Dalela, S.; Bhardwaj, D. M.; Fernandes, S.; Gupta, R. P.; Garg, K. B.

    2003-01-01

    We have performed XAFS, EDAX and AFM studies on some natural and synthetic emeralds. While the XAFS results yield information on changes in the valence of the Cr ion and the n-n distance the AFM is used to determine the areal atomic density on surface of the crystals. It is a pilot study to explore if the three techniques can offer a possible way of distinguishing between the natural and synthetic emeralds and the results are promising.

  13. A Multifunctional Frontloading Approach for Repeated Recycling of a Pressure-Controlled AFM Micropipette.

    PubMed

    Roder, Phillip; Hille, Carsten

    2015-01-01

    Fluid force microscopy combines the positional accuracy and force sensitivity of an atomic force microscope (AFM) with nanofluidics via a microchanneled cantilever. However, adequate loading and cleaning procedures for such AFM micropipettes are required for various application situations. Here, a new frontloading procedure is described for an AFM micropipette functioning as a force- and pressure-controlled microscale liquid dispenser. This frontloading procedure seems especially attractive when using target substances featuring high costs or low available amounts. Here, the AFM micropipette could be filled from the tip side with liquid from a previously applied droplet with a volume of only a few μL using a short low-pressure pulse. The liquid-loaded AFM micropipettes could be then applied for experiments in air or liquid environments. AFM micropipette frontloading was evaluated with the well-known organic fluorescent dye rhodamine 6G and the AlexaFluor647-labeled antibody goat anti-rat IgG as an example of a larger biological compound. After micropipette usage, specific cleaning procedures were tested. Furthermore, a storage method is described, at which the AFM micropipettes could be stored for a few hours up to several days without drying out or clogging of the microchannel. In summary, the rapid, versatile and cost-efficient frontloading and cleaning procedure for the repeated usage of a single AFM micropipette is beneficial for various application situations from specific surface modifications through to local manipulation of living cells, and provides a simplified and faster handling for already known experiments with fluid force microscopy. PMID:26636981

  14. A Multifunctional Frontloading Approach for Repeated Recycling of a Pressure-Controlled AFM Micropipette

    PubMed Central

    Roder, Phillip; Hille, Carsten

    2015-01-01

    Fluid force microscopy combines the positional accuracy and force sensitivity of an atomic force microscope (AFM) with nanofluidics via a microchanneled cantilever. However, adequate loading and cleaning procedures for such AFM micropipettes are required for various application situations. Here, a new frontloading procedure is described for an AFM micropipette functioning as a force- and pressure-controlled microscale liquid dispenser. This frontloading procedure seems especially attractive when using target substances featuring high costs or low available amounts. Here, the AFM micropipette could be filled from the tip side with liquid from a previously applied droplet with a volume of only a few μL using a short low-pressure pulse. The liquid-loaded AFM micropipettes could be then applied for experiments in air or liquid environments. AFM micropipette frontloading was evaluated with the well-known organic fluorescent dye rhodamine 6G and the AlexaFluor647-labeled antibody goat anti-rat IgG as an example of a larger biological compound. After micropipette usage, specific cleaning procedures were tested. Furthermore, a storage method is described, at which the AFM micropipettes could be stored for a few hours up to several days without drying out or clogging of the microchannel. In summary, the rapid, versatile and cost-efficient frontloading and cleaning procedure for the repeated usage of a single AFM micropipette is beneficial for various application situations from specific surface modifications through to local manipulation of living cells, and provides a simplified and faster handling for already known experiments with fluid force microscopy. PMID:26636981

  15. Insight into mechanics of AFM tip-based nanomachining: bending of cantilevers and machined grooves.

    PubMed

    Al-Musawi, R S J; Brousseau, E B; Geng, Y; Borodich, F M

    2016-09-23

    Atomic force microscope (AFM) tip-based nanomachining is currently the object of intense research investigations. Values of the load applied to the tip at the free end of the AFM cantilever probe used for nanomachining are always large enough to induce plastic deformation on the specimen surface contrary to the small load values used for the conventional contact mode AFM imaging. This study describes an important phenomenon specific for AFM nanomachining in the forward direction: under certain processing conditions, the deformed shape of the cantilever probe may change from a convex to a concave orientation. The phenomenon can principally change the depth and width of grooves machined, e.g. the grooves machined on a single crystal copper specimen may increase by 50% on average following such a change in the deformed shape of the cantilever. It is argued that this phenomenon can take place even when the AFM-based tool is operated in the so-called force-controlled mode. The study involves the refined theoretical analysis of cantilever probe bending, the analysis of experimental signals monitored during the backward and forward AFM tip-based machining and the inspection of the topography of produced grooves. PMID:27532247

  16. AFM/CLSM data visualization and comparison using an open-source toolkit.

    PubMed

    Rajwa, Bartek; McNally, Helen A; Varadharajan, Padma; Sturgis, Jennifer; Robinson, J Paul

    2004-06-01

    There is a vast difference in the traditional presentation of AFM data and confocal data. AFM data are presented as surface contours while confocal data are usually visualized using either surface- or volume-rendering techniques. Finding a common meaningful visualization platform is not an easy task. AFM and CLSM technologies are complementary and are more frequently being used to image common biological systems. In order to provide a presentation method that would assist us in evaluating cellular morphology, we propose a simple visualization strategy that is comparative, intuitive, and operates within an open-source environment of ImageJ, SurfaceJ, and VolumeJ applications. In order to find some common ground for AFM-CLSM image comparison, we have developed a plug-in for ImageJ, which allows us to import proprietary image data sets into this application. We propose to represent both AFM and CLSM image data sets as shaded elevation maps with color-coded height. This simple technique utilizes the open source VolumeJ and SurfaceJ plug-ins. To provide an example of this visualization technique, we evaluated the three-dimensional architecture of living chick dorsal root ganglia and sympathetic ganglia measured independently with AFM and CLSM. PMID:15352089

  17. Probing ternary solvent effect in high Voc polymer solar cells using advanced AFM techniques

    DOE PAGESBeta

    Li, Chao; Soleman, Mikhael; Lorenzo, Josie; Dhasmana, Nitesh; Chantharasupawong, Panit; Ievlev, Anton; Gesquiere, Andre; Tetard, Laurene; Thomas, Jayan

    2016-01-25

    This work describes a simple method to develop a high Voc low band gap PSCs. In addition, two new atomic force microscopy (AFM)-based nanoscale characterization techniques to study the surface morphology and physical properties of the structured active layer are introduced. With the help of ternary solvent processing of the active layer and C60 buffer layer, a bulk heterojunction PSC with Voc more than 0.9 V and conversion efficiency 7.5% is developed. In order to understand the fundamental properties of the materials ruling the performance of the PSCs tested, AFM-based nanoscale characterization techniques including Pulsed-Force-Mode AFM (PFM-AFM) and Mode-Synthesizing AFMmore » (MSAFM) are introduced. Interestingly, MSAFM exhibits high sensitivity for direct visualization of the donor–acceptor phases in the active layer of the PSCs. Lastly, conductive-AFM (cAFM) studies reveal local variations in conductivity in the donor and acceptor phases as well as a significant increase in photocurrent in the PTB7:ICBA sample obtained with the ternary solvent processing.« less

  18. Membrane-based actuation for high-speed single molecule force spectroscopy studies using AFM.

    PubMed

    Sarangapani, Krishna; Torun, Hamdi; Finkler, Ofer; Zhu, Cheng; Degertekin, Levent

    2010-07-01

    Atomic force microscopy (AFM)-based dynamic force spectroscopy of single molecular interactions involves characterizing unbinding/unfolding force distributions over a range of pulling speeds. Owing to their size and stiffness, AFM cantilevers are adversely affected by hydrodynamic forces, especially at pulling speeds >10 microm/s, when the viscous drag becomes comparable to the unbinding/unfolding forces. To circumvent these adverse effects, we have fabricated polymer-based membranes capable of actuating commercial AFM cantilevers at speeds >or=100 microm/s with minimal viscous drag effects. We have used FLUENT, a computational fluid dynamics (CFD) software, to simulate high-speed pulling and fast actuation of AFM cantilevers and membranes in different experimental configurations. The simulation results support the experimental findings on a variety of commercial AFM cantilevers and predict significant reduction in drag forces when membrane actuators are used. Unbinding force experiments involving human antibodies using these membranes demonstrate that it is possible to achieve bond loading rates >or=10(6) pN/s, an order of magnitude greater than that reported with commercial AFM cantilevers and systems. PMID:20054686

  19. Anodic stripping voltammetry with graphite felt electrodes for the trace analysis of silver.

    PubMed

    Davies, Trevor J

    2016-08-01

    Graphite felt (GF) is a mass produced porous carbon electrode material commonly used in redox flow batteries. Previous studies have suggested GF may have valuable applications in electroanalysis as a low cost disposable carbon electrode material, although most GF sensors have used flow cell arrangements. In this work, an elegant wetting technique is employed that allows GF electrodes to be used in quiescent solution to detect trace levels of silver in water via anodic stripping voltammetry. GF electrodes display good repeatability and a limit of detection of 25 nM of Ag(+) in 0.1 M HNO3, with a linear range spanning two orders of magnitude. This compares to a value of around 140 nM when using conventional carbon electrodes. Combined with their low cost and disposable nature, the results suggest GF electrodes can make a valuable contribution to electroanalysis. PMID:27276994

  20. Square Wave Voltammetry: An Alternative Technique to Determinate Piroxicam Release Profiles from Nanostructured Lipid Carriers.

    PubMed

    Otarola, Jessica; Garrido, Mariano; Correa, N Mariano; Molina, Patricia G

    2016-08-01

    A new, simple, and fast electrochemical (EC) method has been developed to determine the release profile of piroxicam, a nonsteroidal anti-inflammatory drug, loaded in a drug delivery system based on nanostructured lipid carriers (NLCs). For the first time, the samples were analyzed by using square wave voltammetry, a sensitive EC technique. The piroxicam EC responses allow us to propose a model that explains the experimental results and to subsequently determine the amount of drug loaded into the NLCs formulation as a function of time. In vitro drug release studies showed prolonged drug release (up to 5 days), releasing 60 % of the incorporated drug. The proposed method is a promising and stable alternative for the study of different drug delivery systems. PMID:27128856

  1. Determination of antioxidant activity of spices and their active principles by differential pulse voltammetry.

    PubMed

    Palma, Alberto; Ruiz Montoya, Mercedes; Arteaga, Jesús F; Rodríguez Mellado, Jose M

    2014-01-22

    The anodic oxidation of mercury in the presence of hydrogen peroxide in differential pulse voltammetry (DPV) was used to determine the antioxidant (AO) character of radical scavengers. Hydroperoxide radical is formed at the potentials of the oxidation peak on mercury electrodes, such radical reacting with the antioxidants in different extension. The parameter C10 (antioxidant concentration at which the peak area decreases by 10%) is used to measure the scavenging activity of the individual antioxidants. To establish the scavenging activity of antioxidant mixtures as a whole, the parameter, μ10 as the reverse of V10, V10 being the volume necessary to decrease the peak area in DPV by 10%, was selected. Higher μ10 values correspond to higher scavenging activity. The studies have been extended to aqueous extracts of some species. The results may be useful in explaining the effect of spices in vitro and in vivo studies. PMID:25264569

  2. Signal stability of Nafion-coated thin mercury film electrodes for stripping voltammetry.

    PubMed

    Hoyer, B; Jensen, N

    1994-03-01

    The signal stability of the Nafion-coated thin mercury film electrode (NCTMFE) was studied by using cadmium and lead as test analytes and differential pulse anodic stripping voltammetry as detection method. In particular, the effect of the casting solvent and the curing procedure employed in the preparation of the polymer film was examined. Best results were obtained with N,N-dimethylacetamide as casting solvent and a two-step curing procedure in which the polymer was evaporated to dryness at 55 degrees and cured at 105 degrees with a hot-air gun. Mercury plating was performed ex situ. An NCTMFE prepared in this manner has a better signal stability than ex situ-plated as well as in situ-plated conventional mercury film electrodes. PMID:18965949

  3. Characterization of small noble metal electrodes by voltammetry and energy dispersive x ray analysis

    NASA Astrophysics Data System (ADS)

    Strein, Timothy G.; Ewing, Andrew G.

    1993-01-01

    Construction and characterization of platinum and gold electrodes with total structural diameters of 1-2 micrometers is described. These small voltammetric probes have been constructed by direct electroreduction of noble metals onto the tips of etched carbon fiber microdisk electrodes. Voltammetry, electron microscopy, energy-dispersive x-ray analysis, and pulsed amperometric detection have been used to characterize these electrodes. Dopamine concentrations have been determined over a range of 10(exp -4) to 10(exp -3) M in the biological buffer system which contains 25 mM glucose, a compound known to adsorb strongly to electrodes. Amperometric monitoring at a constant potential with these small results in signal decay of 20% to 40% in a ten minute experiment. Pulsed amperometric detection minimizes electrode fouling, resulting in 5% or less signal decay over the same ten minute period.

  4. Direct methods for the determination of lead in whole blood by anodic stripping voltammetry.

    PubMed

    Lee, S W; Méranger, J C

    1980-12-01

    Two methods for the direct determination of lead in whole blood by anodic stripping voltammetry (ASV) are described. The procedure in both methods involved the mixing of micro blood samples with a metal releasing reagent, Metexchange, and electrochemical analysis using carbon electrodes. A multiple Anodic Stripping Analyzer equipped with composite graphite mercury electrodes and a Charge Transfer Analyzer equipped with a mercury film electrode were employed. The standard addition method was used to minimize the matrix effects of whole blood. The ASV results correlated well with those obtained by flameless atomic absorption analysis. The methods are simple, reliable, and suitable for applications in the clinical field. The procedure using the Charge Transfer Analyzer is recommended because of its sensitivity and rapidity. PMID:7211939

  5. Dealloying NiCo and NiCoCu Alloy Thin Films Using Linear Sweep Voltammetry

    NASA Astrophysics Data System (ADS)

    Peecher, Benjamin; Hampton, Jennifer

    When electrodeposited into thin films, metals have well-known electrochemical potentials at which they will be removed from the film. These potential differences can be utilized to re-oxidize only certain metals in an alloy, altering the film's structure and composition. Here we discuss NiCo and NiCoCu thin films' response to linear sweep voltammetry (LSV) as a means of electrochemical dealloying. For each of four different metal ratios, films were dealloyed to various potentials in order to gain insight into the evolution of the film over the course of the LSV. Capacitance, topography, and composition were examined for each sample before and after linear sweep voltammetry was performed. For NiCo films with high percentages of Ni, dealloying resulted in almost no change in composition, but did result in an increased capacitance, with greater increases occurring at higher LSV potentials. Dealloying also resulted in the appearance of large (100-1000 nm) pores on the surface of the film. For NiCoCu films with high percentages of Ni, Cu was almost completely removed from the film at LSV potentials greater than 500 mV. The LSV first removed larger copper-rich dendrites from the film's surface before creating numerous nano-pores, resulting in a net increase in area. This work is supported by an Award to Hope College from the HHMI Undergraduate Science Education Program, the Hope College Department of Physics Frissel Research Fund, and the National Science Foundation under Grants RUI-DMR-1104725 and MRI-CHE-0959282.

  6. Direct recognition and quantification by voltammetry of thiol/thioamide mixes in seawater.

    PubMed

    Laglera, Luis M; Tovar-Sánchez, Antonio

    2012-01-30

    Thiols and thioamides form part of the pool of reduced sulfur substances (RSS) that modify the health of aquatic ecosystems acting as radical scavengers and heavy metal ligands. Their concentrations could be easily determined in seawater by cathodic stripping voltammetry (CSV) were it not be for the coalescence of their responses in a single peak. Here, we modified the traditional CSV method of RSS analysis to allow individual recognition and quantification in thiol/thioamide mixes. Glutathione, cysteine, thiourea and thioacetamide in UV digested seawater were repeatedly analyzed shifting the deposition potential (E(dep)) in the range +0.07 to -0.4V at high resolution. The representation of peak height (i(p)) and peak potential (E(p)) vs E(dep) resulted in different and distinctive profiles for each substance that allowed the selection of adequate E(dep) ranges for their separate quantification. Copper saturation modified thiol profiles and cancelled the response of thioamides. The vs E(dep) profiles explained the nature of the different thiols and thioamides present in the sample and permitted their individual quantification with excellent accuracy. The utility of the method was put to test with seawater modified with natural unknown RSS from pore waters and Posidonia oceanica exudates. Although both samples gave similar CSV signals, the vs E(dep) profiles unveiled completely different electrochemical behaviors incompatible with a similar nature. Based on those profiles we hypothesized that pore waters released a glutathione/thiourea mix and that one or several unidentified RSS formed part of P. oceanica exudates. The analytical scheme proposed here opens a new door to the use of direct voltammetry in the qualitative and quantitative determination of RSS in natural waters. PMID:22284523

  7. Bare and Polymer-Coated Indium Tin Oxide as Working Electrodes for Manganese Cathodic Stripping Voltammetry.

    PubMed

    Rusinek, Cory A; Bange, Adam; Warren, Mercedes; Kang, Wenjing; Nahan, Keaton; Papautsky, Ian; Heineman, William R

    2016-04-19

    Though an essential metal in the body, manganese (Mn) has a number of health implications when found in excess that are magnified by chronic exposure. These health complications include neurotoxicity, memory loss, infertility in males, and development of a neurologic psychiatric disorder, manganism. Thus, trace detection in environmental samples is increasingly important. Few electrode materials are able to reach the negative reductive potential of Mn required for anodic stripping voltammetry (ASV), so cathodic stripping voltammetry (CSV) has been shown to be a viable alternative. We demonstrate Mn CSV using an indium tin oxide (ITO) working electrode both bare and coated with a sulfonated charge selective polymer film, polystyrene-block-poly(ethylene-ran-butylene)-block-polystyrene-sulfonate (SSEBS). ITO itself proved to be an excellent electrode material for Mn CSV, achieving a calculated detection limit of 5 nM (0.3 ppb) with a deposition time of 3 min. Coating the ITO with the SSEBS polymer was found to increase the sensitivity and lower the detection limit to 1 nM (0.06 ppb). This polymer modified electrode offers excellent selectivity for Mn as no interferences were observed from other metal ions tested (Zn(2+), Cd(2+), Pb(2+), In(3+), Sb(3+), Al(3+), Ba(2+), Co(2+), Cu(2+), Ni(3+), Bi(3+), and Sn(2+)) except Fe(2+), which was found to interfere with the analytical signal for Mn(2+) at a ratio 20:1 (Fe(2+)/Mn(2+)). The applicability of this procedure to the analysis of tap, river, and pond water samples was demonstrated. This simple, sensitive analytical method using ITO and SSEBS-ITO could be applied to a number of electroactive transition metals detectable by CSV. PMID:26980322

  8. Electrochemical sensor with substitutional stripping voltammetry for highly sensitive endotoxin assay.

    PubMed

    Takano, Shinichiro; Inoue, Kumi Y; Takahashi, Satoko; Ino, Kosuke; Shiku, Hitoshi; Matsue, Tomokazu

    2014-10-01

    We have developed a novel method for detection of endotoxin with extra-high sensitivity by using substitutional stripping voltammetry (SSV). In this method, a p-aminophenol (pAP) conjugated peptide (Boc-Leu-Gly-Arg-pAP; LGR-pAP) was used as a substrate for a protease, which is activated at the last step of the endotoxin-induced Limulus amebocyte lysate (LAL) cascade reaction. Extra-highly sensitive detection of pAP liberated by the endotoxin-induced LAL reaction was successfully realized with SSV, based on the accumulation of an amperometric signal owing to exchange of the oxidation current of pAP generated at an electrode in a reaction cell with silver deposition on another electrode in a deposition cell. This reaction is driven by the difference in the redox potential between pAP/quinoneimine and silver/silver ion. The amount of the deposited silver is quantified by anodic stripping voltammetry (ASV). This SSV-based endotoxin assay was performed with a chip device comprising two cells, each of which was connected via a liquid junction made of Vycor® glass. The reaction cell and the deposition cell contained a standard endotoxin sample with LAL regents containing LGR-pAP and AgNO3 solution, respectively. After the cells were electrically connected for 60 min, ASV was conducted in the deposition cell to quantify the total electrical charge derived by the oxidation of free pAP in the reaction cell. The ASV signal increased with the increase of the endotoxin concentration in the sample solution in the range of 0.5-1000 EU L(-1). PMID:25096015

  9. Mixed Strategies in cyclic competition

    NASA Astrophysics Data System (ADS)

    Intoy, Ben; Pleimling, Michel

    2015-03-01

    Physicists have been using evolutionary game theory to model and simulate cyclically competing species, with applications to lizard mating strategies and competing bacterial strains. However these models assume that each agent plays the same strategy, which is called a pure strategy in game theory, until they are beaten by a better strategy which they immediately adopt. We relax this constraint of an agent playing a single strategy by instead letting the agent pick its strategy randomly from a probability distribution, which is called a mixed strategy in game theory. This scheme is very similar to multiple occupancy models seen in the literature, the major difference being that interactions happen between sites rather than within them. Choosing strategies out of a distribution also has applications to economic/social systems such as the public goods game. We simulate a model of mixed strategy and cylic competition on a one-dimensional lattice with three and four strategies and find interesting spatial and stability properties depending on how discretized the choice of strategy is for the agents. This work is supported by the US National Science Foundation through Grant DMR-1205309.

  10. Asymmetric cyclic evolution in polymerised cosmology

    SciTech Connect

    Hrycyna, Orest; Mielczarek, Jakub; Szydłowski, Marek E-mail: jakub.mielczarek@uj.edu.pl

    2009-12-01

    The dynamical systems methods are used to study evolution of the polymerised scalar field cosmologies with the cosmological constant. We have found all evolutional paths admissible for all initial conditions on the two-dimensional phase space. We have shown that the cyclic solutions are generic. The exact solution for polymerised cosmology is also obtained. Two basic cases are investigated, the polymerised scalar field and the polymerised gravitational and scalar field part. In the former the division on the cyclic and non-cyclic behaviour is established following the sign of the cosmological constant. The value of the cosmological constant is upper bounded purely from the dynamical setting.

  11. Processable Cyclic Peptide Nanotubes with Tunable Interiors

    SciTech Connect

    Hourani, Rami; Zhang, Chen; van der Weegen, Rob; Ruiz, Luis; Li, Changyi; Keten, Sinan; Helms, Brett A.; Xu, Ting

    2011-09-06

    A facile route to generate cyclic peptide nanotubes with tunable interiors is presented. By incorporating 3-amino-2-methylbenzoic acid in the d,l-alternating primary sequence of a cyclic peptide, a functional group can be presented in the interior of the nanotubes without compromising the formation of high aspect ratio nanotubes. The new design of such a cyclic peptide also enables one to modulate the nanotube growth process to be compatible with the polymer processing window without compromising the formation of high aspect ratio nanotubes, thus opening a viable approach toward molecularly defined porous membranes.

  12. Strength by atomic force microscopy (AFM): Molecular dynamics of water layer squeezing on magnesium oxide

    NASA Astrophysics Data System (ADS)

    Kendall, K.; Dhir, Aman; Yong, Chin W.

    2010-11-01

    Localised strength testing of materials is often carried out in an atomic force microscope (AFM), as foreseen by Kelly in his book Strong Solids (Clarendon Press, Oxford, 1966). During AFM indentation experiments, contamination can strongly influence the observed strength and theoretical interpretation of the results is a major problem. Here, we use molecular dynamics computer modelling to describe the contact of NaCl and MgO crystal probes onto surfaces, comparable to an AFM experiment. Clean NaCl gave elastic, brittle behaviour in contact simulations at 300 K, whereas MgO was more plastic, leading to increased toughness. This paper also considers the strength of an oxide substrate contaminated by water molecules and tested by indentation with a pyramidal probe of oxide crystal. Recent theory on the effect of liquid contaminant layers on surface strength has been mainly focussed on Lennard Jones (LJ) molecules with some studies on alcohols and water, described by molecular dynamics, which allows the molecules to be squeezed out as the crystal lattice is deformed. In this work, we have focused on water by studying the forces between a magnesium oxide (MgO) atomic force microscope (AFM) probe and an MgO slab. Force versus separation has been plotted as the AFM probe was moved towards and away from the substrate. Simulation results showed that the water layers could be removed in steps, giving up to four force peaks. The last monolayer of water could not be squeezed out, even at pressures where MgO deformed plastically. Interestingly, with water present, strength was reduced, but more in tensile than compressive measurements. In conclusion, water contaminating the oxide surface in AFM strength testing is structured. Water layer squeezing removal can be predicted by molecular modelling, which may be verified by AFM experiments to show that water can influence the strength of perfect crystals at the nanometre scale.

  13. A software tool for STED-AFM correlative super-resolution microscopy

    NASA Astrophysics Data System (ADS)

    Koho, Sami; Deguchi, Takahiro; Löhmus, Madis; Näreoja, Tuomas; Hänninen, Pekka E.

    2015-03-01

    Multi-modal correlative microscopy allows combining the strengths of several imaging techniques to provide unique contrast. However it is not always straightforward to setup instruments for such customized experiments, as most microscope manufacturers use their own proprietary software, with limited or no capability to interface with other instruments - this makes correlation of the multi-modal data extremely challenging. We introduce a new software tool for simultaneous use of a STimulated Emission Depletion (STED) microscope with an Atomic Force Microscope (AFM). In our experiments, a Leica TCS STED commercial super-resolution microscope, together with an Agilent 5500ilm AFM microscope was used. With our software, it is possible to synchronize the data acquisition between the STED and AFM instruments, as well as to perform automatic registration of the AFM images with the super-resolution STED images. The software was realized in LabVIEW; the registration part was also implemented as an ImageJ script. The synchronization was realized by controlling simple trigger signals, also available in the commercial STED microscope, with a low-cost National Instruments USB-6501 digital I/O card. The registration was based on detecting the positions of the AFM tip inside the STED fieldof-view, which were then used as registration landmarks. The registration should work on any STED and tip-scanning AFM microscope combination, at nanometer-scale precision. Our STED-AFM correlation method has been tested with a variety of nanoparticle and fixed cell samples. The software will be released under BSD open-source license.

  14. A rapid and automated relocation method of an AFM probe for high-resolution imaging.

    PubMed

    Zhou, Peilin; Yu, Haibo; Shi, Jialin; Jiao, Niandong; Wang, Zhidong; Wang, Yuechao; Liu, Lianqing

    2016-09-30

    The atomic force microscope (AFM) is one of the most powerful tools for high-resolution imaging and high-precision positioning for nanomanipulation. The selection of the scanning area of the AFM depends on the use of the optical microscope. However, the resolution of an optical microscope is generally no larger than 200 nm owing to wavelength limitations of visible light. Taking into consideration the two determinants of relocation-relative angular rotation and positional offset between the AFM probe and nano target-it is therefore extremely challenging to precisely relocate the AFM probe to the initial scan/manipulation area for the same nano target after the AFM probe has been replaced, or after the sample has been moved. In this paper, we investigate a rapid automated relocation method for the nano target of an AFM using a coordinate transformation. The relocation process is both simple and rapid; moreover, multiple nano targets can be relocated by only identifying a pair of reference points. It possesses a centimeter-scale location range and nano-scale precision. The main advantages of this method are that it overcomes the limitations associated with the resolution of optical microscopes, and that it is label-free on the target areas, which means that it does not require the use of special artificial markers on the target sample areas. Relocation experiments using nanospheres, DNA, SWCNTs, and nano patterns amply demonstrate the practicality and efficiency of the proposed method, which provides technical support for mass nanomanipulation and detection based on AFM for multiple nano targets that are widely distributed in a large area. PMID:27559679

  15. One-pot, template syntheses of a new class of metallomacrocycles with a tetraoxime cyclic skeleton.

    PubMed

    Tashiro, Shohei; Minoda, Ai; Yamada, Mihoko; Shionoya, Mitsuhiko

    2009-11-01

    Most common macrocycles such as crown ethers, porphyrins, and macrocyclic polyamines show versatile, excellent functions in a variety of research fields such as coordination chemistry, supramolecular chemistry, analytical chemistry, and material sciences. Thus, the rational design of a new class of readily synthesized macrocyclic metal ligands is a key to the development of a new category of functionalized macrocyclic metal complexes. Herein, we report one-pot, template syntheses of a new class of metallomacrocycles with a 16-membered tetraoxime cyclic skeleton from a dioxime in the presence of a template transition-metal ion such as Fe(2+), Ni(2+), Cu(2+), Co(2+), or Ag(+). These metal ions can be easily removed from the mononuclear metallomacrocycles, and, for example, the metal-free tetraoxime ligand was obtained in 90% yield when Fe(2+) was used as the template. It would appear that this one-pot, metal-template cyclization efficiently proceeds through continual metal-mediated oxime exchange reactions. Interestingly, Pd(2+), which does not afford any cyclized products, formed a 1:1 complex with the macrocyclic ligand. The molecular structures of the metal-free ligand, its 1:1 metal complexes with Fe(2+), Ni(2+), Cu(2+), Pd(2+), and Ag(+), and a dinuclear complex with Ag(+) were fully determined by single-crystal X-ray analyses. UV-visible absorption spectra and cyclic voltammetry measurements of these complexes are also reported. PMID:19852519

  16. Mapping Activity Variations for Ru2O3 in Lunar Volcanic Green Glass Analogs Using Differential Pulse Voltammetry

    NASA Technical Reports Server (NTRS)

    Malum, K. M.; Colson, R. O.; Sawarynski, M.

    2001-01-01

    Using differential pulse voltammetry, we are mapping variations in activities for NiO and Ru2O3 as a function of compositional variation for compositions centered around an Apollo 15 green glass analog. Additional information is contained in the original extended abstract.

  17. Cyclic resistive switching effect in plasma electrolytically oxidized mesoporous Pt/TiO2 structures

    NASA Astrophysics Data System (ADS)

    Fullam, S.; Ray, N. J.; Karpov, E. G.

    2015-06-01

    Understanding the resistive switching phenomenon in metal oxide semiconductors is necessary in producing reliable resistive random access memory and other variable resistance devices. An alternative technique for fabricating resistive switching elements is presented. Using plasma electrolytic oxidation, 10-11 μ m thick oxide layers were galvanostatically grown on Ti substrates in a 3 M H2SO4 electrolyte. Analysis of the TiO2 layer by SEM, AFM, and XRD found the mesoporous titania surface to have a high ratio of rutile to anatase phases. The samples demonstrated pinched I-V hysteresis attributed to the resistive switching effect, when subjected to cyclic loading (±2.5, 1.6, 0.7 V; 23-736 μ Hz) at room temperature. Ratio with magnitude of 6 is reported for the resistance switching effect during 1.6 V 368 μ Hz loads.

  18. Synchronization in chaotic oscillators by cyclic coupling

    NASA Astrophysics Data System (ADS)

    Olusola, O. I.; Njah, A. N.; Dana, S. K.

    2013-07-01

    We introduce a type of cyclic coupling to investigate synchronization of chaotic oscillators. We derive analytical solutions of the critical coupling for stable synchronization under the cyclic coupling for the Rössler system and the Lorenz oscillator as paradigmatic illustration. Based on the master stability function (MSF) approach, the analytical results on critical coupling are verified numerically. An enhancing effect in terms of lowering the critical coupling or enlarging the synchronization window in a critical coupling space is noticed. The cyclic coupling is also applied in other models, Hindmarsh-Rose model, Sprott system, Chen system and forced Duffing system to confirm the enhancing effect. The cyclic coupling allows tuning of two coupling constants in reverse directions when an optimal control of synchronization is feasible.

  19. AFM as an analysis tool for high-capacity sulfur cathodes for Li-S batteries.

    PubMed

    Hiesgen, Renate; Sörgel, Seniz; Costa, Rémi; Carlé, Linus; Galm, Ines; Cañas, Natalia; Pascucci, Brigitta; Friedrich, K Andreas

    2013-01-01

    In this work, material-sensitive atomic force microscopy (AFM) techniques were used to analyse the cathodes of lithium-sulfur batteries. A comparison of their nanoscale electrical, electrochemical, and morphological properties was performed with samples prepared by either suspension-spraying or doctor-blade coating with different binders. Morphological studies of the cathodes before and after the electrochemical tests were performed by using AFM and scanning electron microscopy (SEM). The cathodes that contained polyvinylidene fluoride (PVDF) and were prepared by spray-coating exhibited a superior stability of the morphology and the electric network associated with the capacity and cycling stability of these batteries. A reduction of the conductive area determined by conductive AFM was found to correlate to the battery capacity loss for all cathodes. X-ray diffraction (XRD) measurements of Li2S exposed to ambient air showed that insulating Li2S hydrolyses to insulating LiOH. This validates the significance of electrical ex-situ AFM analysis after cycling. Conductive tapping mode AFM indicated the existence of large carbon-coated sulfur particles. Based on the analytical findings, the first results of an optimized cathode showed a much improved discharge capacity of 800 mA·g(sulfur)(-1) after 43 cycles. PMID:24205455

  20. Sub-surface imaging of carbon nanotube-polymer composites using dynamic AFM methods.

    PubMed

    Cadena, Maria J; Misiego, Rocio; Smith, Kyle C; Avila, Alba; Pipes, Byron; Reifenberger, Ron; Raman, Arvind

    2013-04-01

    High-resolution sub-surface imaging of carbon nanotube (CNT) networks within polymer nanocomposites is demonstrated through electrical characterization techniques based on dynamic atomic force microscopy (AFM). We compare three techniques implemented in the single-pass configuration: DC-biased amplitude modulated AFM (AM-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM) in terms of the physics of sub-surface image formation and experimental robustness. The methods were applied to study the dispersion of sub-surface networks of single-walled nanotubes (SWNTs) in a polyimide (PI) matrix. We conclude that among these methods, the KPFM channel, which measures the capacitance gradient (∂C/∂d) at the second harmonic of electrical excitation, is the best channel to obtain high-contrast images of the CNT network embedded in the polymer matrix, without the influence of surface conditions. Additionally, we propose an analysis of the ∂C/∂d images as a tool to characterize the dispersion and connectivity of the CNTs. Through the analysis we demonstrate that these AFM-based sub-surface methods probe sufficiently deep within the SWNT composites, to resolve clustered networks that likely play a role in conductivity percolation. This opens up the possibility of dynamic AFM-based characterization of sub-surface dispersion and connectivity in nanostructured composites, two critical parameters for nanocomposite applications in sensors and energy storage devices. PMID:23478510

  1. Nanoscale crystallization of phase change Ge2Sb2Te5 film with AFM lithography.

    PubMed

    Kim, JunHo

    2010-01-01

    We have made nanoindents on Ge(2)Sb(2)Te(5)(GST) films using electric field-assisted atomic force microscope (AFM) lithography. GST shows increase of material density and electric conductivity as it changes from amorphous to crystalline phases. By applying electric field between AFM probe-tip and GST surface, nanoscale crystallization could be induced on tip contact area. As the crystallized GST exhibits increase of material density, that is to say depression of volume, nanoindented surface with crystallization is created on host amorphous GST (a-GST) film. For the AFM lithography, a highly conductive tip, which showed voltage-switching characteristics in current-voltage spectroscopy of GST film, was found to be very suitable for recording and sensing crystallized nanoindents on the GST film. By varying sample bias voltages, we performed nanoscale crystallization, and measured the nanostructured film in AFM conductance-image (C-image) mode and topography-image (T-image) mode, simultaneously. Two types of crystallized wires were fabricated on (a-GST) film. Type-I was sensed in only C-image, whereas Type-II was sensed in both C-image and T-image. These nanowires are discussed in terms of crystallization of GST and sensitivity of current (or topography) sensing. By repeated lithography, larger size of nanoindented wires were also produced, which indicates line-dimension controllability of AFM lithography. PMID:20853405

  2. AFM as an analysis tool for high-capacity sulfur cathodes for Li–S batteries

    PubMed Central

    Sörgel, Seniz; Costa, Rémi; Carlé, Linus; Galm, Ines; Cañas, Natalia; Pascucci, Brigitta; Friedrich, K Andreas

    2013-01-01

    Summary In this work, material-sensitive atomic force microscopy (AFM) techniques were used to analyse the cathodes of lithium–sulfur batteries. A comparison of their nanoscale electrical, electrochemical, and morphological properties was performed with samples prepared by either suspension-spraying or doctor-blade coating with different binders. Morphological studies of the cathodes before and after the electrochemical tests were performed by using AFM and scanning electron microscopy (SEM). The cathodes that contained polyvinylidene fluoride (PVDF) and were prepared by spray-coating exhibited a superior stability of the morphology and the electric network associated with the capacity and cycling stability of these batteries. A reduction of the conductive area determined by conductive AFM was found to correlate to the battery capacity loss for all cathodes. X-ray diffraction (XRD) measurements of Li2S exposed to ambient air showed that insulating Li2S hydrolyses to insulating LiOH. This validates the significance of electrical ex-situ AFM analysis after cycling. Conductive tapping mode AFM indicated the existence of large carbon-coated sulfur particles. Based on the analytical findings, the first results of an optimized cathode showed a much improved discharge capacity of 800 mA·g(sulfur)−1 after 43 cycles. PMID:24205455

  3. Enabling accurate gate profile control with inline 3D-AFM

    NASA Astrophysics Data System (ADS)

    Bao, Tianming; Lopez, Andrew; Dawson, Dean

    2009-05-01

    The logic and memory semiconductor device technology strives to follow the aggressive ITRS roadmap. The ITRS calls for increased 3D metrology to meet the demand for tighter process control at 45nm and 32nm nodes. In particular, gate engineering has advanced to a level where conventional metrology by CD-SEM and optical scatterometry (OCD) faces fundamental limitations without involvement of 3D atomic force microscope (3D-AFM or CD-AFM). This paper reports recent progress in 3D-AFM to address the metrology need to control gate dimension in MOSFET transistor formation. 3D-AFM metrology measures the gate electrode at post-etch with the lowest measurement uncertainty for critical gate geometry, including linewidth, sidewall profile, sidewall angle (SWA), line width roughness (LWR), and line edge roughness (LER). 3D-AFM enables accurate gate profile control in three types of metrology applications: reference metrology to validate CD-SEM and OCD, inline depth or 3D monitoring, or replacing TEM for 3D characterization for engineering analysis.

  4. Development of a new generation of active AFM tools for applications in liquids

    NASA Astrophysics Data System (ADS)

    Rollier, A.-S.; Jenkins, D.; Dogheche, E.; Legrand, B.; Faucher, M.; Buchaillot, L.

    2010-08-01

    Atomic force microscopy (AFM) is a powerful imaging tool with high-resolution imaging capability. AFM probes consist of a very sharp tip at the end of a silicon cantilever that can respond to surface artefacts to produce an image of the topography or surface features. They are intrinsically passive devices. For imaging soft biological samples, and also for samples in liquid, it is essential to control the AFM tip position, both statically and dynamically, and this is not possible using external actuators mounted on the AFM chip. AFM cantilevers have been fabricated using silicon micromachining to incorporate a piezoelectric thin film actuator for precise control. The piezoelectric thin films have been fully characterized to determine their actuation performance and to characterize the operation of the integrated device. Examples of the spatial and vertical response are presented to illustrate their imaging capability. For operation in a liquid environment, the dynamic behaviour has been modelled and verified experimentally. The optimal drive conditions for the cantilever, along with their dynamic response, including frequency and phase in air and water, are presented.

  5. Effect of AFM probe geometry on visco-hyperelastic characterization of soft materials.

    PubMed

    Boccaccio, Antonio; Lamberti, Luciano; Papi, Massimiliano; De Spirito, Marco; Pappalettere, Carmine

    2015-08-14

    Atomic force microscopy (AFM) nanoindentation is very suited for nano- and microscale mechanical characterization of soft materials. Although the structural response of polymeric networks that form soft matter depends on viscous effects caused by the relative slippage of polymeric chains, the usual assumption made in the AFM-based characterization is that the specimen behaves as a purely elastic material and viscous forces are negligible. However, for each geometric configuration of the AFM tip, there will be a limit indentation rate above which viscous effects must be taken into account to correctly determine mechanical properties. A parametric finite element study conducted on 12 geometric configurations of a blunt cone AFM tip (overall, the study included about 200 finite element analyses) allowed us to determine the limit indentation rate for each configuration. The selected tip dimensions cover commercially available products and account for changes in tip geometry caused by serial measurements. Nanoindentation rates cover typical experimental conditions set in AFM bio-measurements on soft matter. Viscous effects appear to be more significant in the case of sharper tips. This implies that, if quantitative data on sample viscosity are not available, using a rounded indenter and carrying out experiments below the limit indentation rate will allow errors in the determination of mechanical properties to be minimized. PMID:26201503

  6. AFM1 in Milk: Physical, Biological, and Prophylactic Methods to Mitigate Contamination

    PubMed Central

    Giovati, Laura; Magliani, Walter; Ciociola, Tecla; Santinoli, Claudia; Conti, Stefania; Polonelli, Luciano

    2015-01-01

    Aflatoxins (AFs) are toxic, carcinogenic, immunosuppressive secondary metabolites produced by some Aspergillus species which colonize crops, including many dietary staple foods and feed components. AFB1 is the prevalent and most toxic among AFs. In the liver, it is biotransformed into AFM1, which is then excreted into the milk of lactating mammals, including dairy animals. AFM1 has been shown to be cause of both acute and chronic toxicoses. The presence of AFM1 in milk and dairy products represents a worldwide concern since even small amounts of this metabolite may be of importance as long-term exposure is concerned. Contamination of milk may be mitigated either directly, decreasing the AFM1 content in contaminated milk, or indirectly, decreasing AFB1 contamination in the feed of dairy animals. Current strategies for AFM1 mitigation include good agricultural practices in pre-harvest and post-harvest management of feed crops (including storage) and physical or chemical decontamination of feed and milk. However, no single strategy offers a complete solution to the issue. PMID:26512694

  7. Antimicrobial Cyclic Peptides for Plant Disease Control

    PubMed Central

    Lee, Dong Wan; Kim, Beom Seok

    2015-01-01

    Antimicrobial cyclic peptides derived from microbes bind stably with target sites, have a tolerance to hydrolysis by proteases, and a favorable degradability under field conditions, which make them an attractive proposition for use as agricultural fungicides. Antimicrobial cyclic peptides are classified according to the types of bonds within the ring structure; homodetic, heterodetic, and complex cyclic peptides, which in turn reflect diverse physicochemical features. Most antimicrobial cyclic peptides affect the integrity of the cell envelope. This is achieved through direct interaction with the cell membrane or disturbance of the cell wall and membrane component biosynthesis such as chitin, glucan, and sphingolipid. These are specific and selective targets providing reliable activity and safety for non-target organisms. Synthetic cyclic peptides produced through combinatorial chemistry offer an alternative approach to develop antimicrobials for agricultural uses. Those synthesized so far have been studied for antibacterial activity, however, the recent advancements in powerful technologies now promise to provide novel antimicrobial cyclic peptides that are yet to be discovered from natural resources. PMID:25774105

  8. AFM-based force spectroscopy measurements of mature amyloid fibrils of the peptide glucagon

    NASA Astrophysics Data System (ADS)

    Dong, Mingdong; Bruun Hovgaard, Mads; Mamdouh, Wael; Xu, Sailong; Otzen, Daniel Erik; Besenbacher, Flemming

    2008-09-01

    We report on the mechanical characterization of individual mature amyloid fibrils by atomic force microscopy (AFM) and AFM-based single-molecule force spectroscopy (SMFS). These self-assembling materials, formed from the 29-residue amphiphatic peptide hormone glucagon, were found to display a reversible elastic behaviour. Based on AFM morphology and SMFS studies, we suggest that the observed elasticity is due to a force-induced conformational transition which is reversible due to the β-helical conformation of protofibrils, allowing a high degree of extension. The elastic properties of such mature fibrils contribute to their high stability, suggesting that the internal hydrophobic interactions of amyloid fibrils are likely to be of fundamental importance in the assembly of amyloid fibrils and therefore for the understanding of the progression of their associated pathogenic disorders. In addition, such biological amyloid fibril structures with highly stable mechanical properties can potentially be used to produce nanofibres (nanowires) that may be suitable for nanotechnological applications.

  9. AFM-assisted fabrication of thiol SAM pattern with alternating quantified surface potential

    PubMed Central

    2011-01-01

    Thiol self-assembled monolayers (SAMs) are widely used in many nano- and bio-technology applications. We report a new approach to create and characterize a thiol SAMs micropattern with alternating charges on a flat gold-coated substrate using atomic force microscopy (AFM) and Kelvin probe force microscopy (KPFM). We produced SAMs-patterns made of alternating positively charged, negatively charged, and hydrophobic-terminated thiols by an automated AFM-assisted manipulation, or nanografting. We show that these thiol patterns possess only small topographical differences as revealed by AFM, and distinguished differences in surface potential (20-50 mV), revealed by KPFM. The pattern can be helpful in the development of biosensor technologies, specifically for selective binding of biomolecules based on charge and hydrophobicity, and serve as a model for creating surfaces with quantified alternating surface potential distribution. PMID:21711703

  10. A sub-50 nm three-step height sample for AFM calibration

    NASA Astrophysics Data System (ADS)

    Yang, Shuming; Li, Changsheng; Wang, Chenying; Jiang, Zhuangde

    2014-12-01

    In this paper, a sub-50 nm three-step height sample was made for vertical calibration of atomic force microscopy (AFM) and a new step height evaluation algorithm based on polynomial fitting is discussed. The influences of AFM artefacts such as particles, image bow and high-order errors on step height were studied. The experimental results showed that the polynomial order p2 and threshold t were not critical factors. However, the increment Δh and the polynomial order p used in the calculation of optimal shifting distance were important and must be carefully considered. Δh = 0.1 nm and p ≥ 4 were determined to get a stable step height. The sample had small roughness and good uniformity. It has the potential to serve as a high quality step height standard sample for AFM calibration.

  11. Review and perspectives of AFM application on the study of deformable drop/bubble interactions.

    PubMed

    Wang, Wei; Li, Kai; Ma, Mengyu; Jin, Hang; Angeli, Panagiota; Gong, Jing

    2015-11-01

    The applications of Atomic Force Microscopy (AFM) on the study of dynamic interactions and film drainage between deformable bodies dispersed in aqueous solutions are reviewed in this article. Novel experimental designs and recent advances in experimental methodologies are presented, which show the advantage of using AFM as a tool for probing colloidal interactions. The effects of both DLVO and non-DLVO forces on the colloid stabilization mechanism are discussed. Good agreement is found between the force - drop/bubble deformation behaviour revealed by AFM measurements and the theoretical modeling of film drainage process, giving a convincing explanation of the occurrence of certain phenomenon. However, the behaviour and shape of deformable drops as they approach or retract is still not well resolved. In addition, when surfactants are present further research is needed on the absorption of surfactant molecules into the interfaces, their mobility and the effects on interfacial film properties. PMID:26344865

  12. Imaging and force measurement of LDL and HDL by AFM in air and liquid

    PubMed Central

    Gan, Chaoye; Ao, Meiying; Liu, Zhanghua; Chen, Yong

    2015-01-01

    The size and biomechanical properties of lipoproteins are tightly correlated with their structures/functions. While atomic force microscopy (AFM) has been used to image lipoproteins the force measurement of these nano-sized particles is missing. We detected that the sizes of LDL and HDL in liquid are close to the commonly known values. The Young’s modulus of LDL or HDL is ∼0.4 GPa which is similar to that of some viral capsids or nanovesicles but greatly larger than that of various liposomes. The adhesive force of LDL or HDL is small (∼200 pN). The comparison of AFM detection in air and liquid was also performed which is currently lacking. Our data may provide useful information for better understanding and AFM detection of lipoproteins. PMID:25893163

  13. Mapping site-specific endonuclease binding to DNA by direct imaging with AFM

    SciTech Connect

    Allison, D.P.; Thundat, T.; Doktycz, M.J.; Kerper, P.S.; Warmack, R.J.; Modrich, P.; Isfort, R.J.

    1995-12-31

    Physical mapping of DNA can be accomplished by direct AFM imaging of site specific proteins bound to DNA molecules. Using Gln-111, a mutant of EcoRI endonuclease with a specific affinity for EcoRI sites 1,000 times greater than wild type enzyme but with cleavage rate constants reduced by a factor of 10{sup 4}, the authors demonstrate site-specific mapping by direct AFM imaging. Images are presented showing specific-site binding of Gln-111 to plasmids having either one (pBS{sup +}) or two (pMP{sup 32}) EcoRI sites. Identification of the Gln-111/DNA complex is greatly enhanced by biotinylation of the complex followed by reaction with streptavidin gold prior to imaging. Image enhancement coupled with improvements in the preparation techniques for imaging large DNA molecules, such as lambda DNA (47 kb), has the potential to contribute to direct AFM restriction mapping of cosmid-sized genomic DNAs.

  14. Multiparametric high-resolution imaging of native proteins by force-distance curve-based AFM.

    PubMed

    Pfreundschuh, Moritz; Martinez-Martin, David; Mulvihill, Estefania; Wegmann, Susanne; Muller, Daniel J

    2014-05-01

    A current challenge in the life sciences is to understand how the properties of individual molecular machines adjust in order to meet the functional requirements of the cell. Recent developments in force-distance (FD) curve-based atomic force microscopy (FD-based AFM) enable researchers to combine sub-nanometer imaging with quantitative mapping of physical, chemical and biological properties. Here we present a protocol to apply FD-based AFM to the multiparametric imaging of native proteins under physiological conditions. We describe procedures for experimental FD-based AFM setup, high-resolution imaging of proteins in the native unperturbed state with simultaneous quantitative mapping of multiple parameters, and data interpretation and analysis. The protocol, which can be completed in 1-3 d, enables researchers to image proteins and protein complexes in the native unperturbed state and to simultaneously map their biophysical and biochemical properties at sub-nanometer resolution. PMID:24743419

  15. AFM characterization of nonwoven material functionalized by ZnO sputter coating

    SciTech Connect

    Deng Bingyao; Yan Xiong; Wei Qufu Gao Weidong

    2007-10-15

    Sputter coatings provide new approaches to the surface functionalization of textile materials. In this study, polyethylene terephthalate (PET) nonwoven material was used as a substrate for creating functional nanostructures on the fiber surfaces. A magnetron sputter coating was used to deposit functional zinc oxide (ZnO) nanostructures onto the nonwoven substrate. The evolution of the surface morphology of the fibers in the nonwoven web was examined using atomic force microscopy (AFM). The AFM observations revealed a significant difference in the morphology of the fibers before and after the sputter coating. The AFM images also indicated the effect of the sputtering conditions on the surface morphology of the fibers. The increase in the sputtering time led to the growth of the ZnO grains on the fiber surfaces. The higher pressure in the sputtering chamber could cause the formation of larger grains on the fiber surfaces. The higher power used also generated larger grains on the fiber surfaces.

  16. High precision attachment of silver nanoparticles on AFM tips by dielectrophoresis.

    PubMed

    Leiterer, Christian; Wünsche, Erik; Singh, Prabha; Albert, Jens; Köhler, Johann M; Deckert, Volker; Fritzsche, Wolfgang

    2016-05-01

    AFM tips are modified with silver nanoparticles using an AC electrical field. The used technique works with sub-micron precision and also does not require chemical modification of the tip. Based on the electrical parameters applied in the process, particle density and particle position on the apex of the tip can be adjusted. The feasibility of the method is proven by subsequent tip-enhanced Raman spectroscopy (TERS) measurements using the fabricated tips as a measurement probe. Since this modification process itself does not require any lithographic processing, the technique can be easily adapted to modify AFM tips with a variety of nanostructures with pre-defined properties, while being parallelizable for a potential commercial application. Graphical abstract Silver nanoparticles attached to AFM tips using dielectrophoresis. Comparing nanoparticles attached using 1 kHz (left) to 1 MHz (right), SEM and optical (inset) images. PMID:26968565

  17. Impact of Adsorption on Scanning Electrochemical Microscopy Voltammetry and Implications for Nanogap Measurements.

    PubMed

    Tan, Sze-yin; Zhang, Jie; Bond, Alan M; Macpherson, Julie V; Unwin, Patrick R

    2016-03-15

    Scanning electrochemical microscopy (SECM) is a powerful tool that enables quantitative measurements of fast electron transfer (ET) kinetics when coupled with modeling predictions from finite-element simulations. However, the advent of nanoscale and nanogap electrode geometries that have an intrinsically high surface area-to-solution volume ratio realizes the need for more rigorous data analysis procedures, as surface effects such as adsorption may play an important role. The oxidation of ferrocenylmethyl trimethylammonium (FcTMA(+)) at highly oriented pyrolytic graphite (HOPG) is used as a model system to demonstrate the effects of reversible reactant adsorption on the SECM response. Furthermore, the adsorption of FcTMA(2+) species onto glass, which is often used to encapsulate ultramicroelectrodes employed in SECM, is also found to be important and affects the voltammetric tip response in a nanogap geometry. If a researcher is unaware of such effects (which may not be readily apparent in slow to moderate scan voltammetry) and analyzes SECM data assuming simple ET kinetics at the substrate and an inert insulator support around the tip, the result is the incorrect assignment of tip-substrate heights, kinetics, and thermodynamic parameters. Thus, SECM kinetic measurements, particularly in a nanogap configuration where the ET kinetics are often very fast (only just distinguishable from reversible), require that such effects are fully characterized. This is possible by expanding the number of experimental variables, including the voltammetric scan rate and concentration of redox species, among others. PMID:26877069

  18. Determination of water in room temperature ionic liquids by cathodic stripping voltammetry at a gold electrode.

    PubMed

    Zhao, Chuan; Bond, Alan M; Lu, Xunyu

    2012-03-20

    An electrochemical method based on cathodic stripping voltammetry at a gold electrode has been developed for the determination of water in ionic liquids. The technique has been applied to two aprotic ionic liquids, (1-butyl-3-ethylimidazolium tetrafluoroborate and 1-butyl-3-methylimidazolium hexafluorophosphate), and two protic ionic liquids, (bis(2-hydroxyethyl)ammonium acetate and triethylammonium acetate). When water is present in an ionic liquid, electrooxidation of a gold electrode forms gold oxides. Thus, application of an anodic potential scan or holding the potential of the electrode at a very positive value leads to accumulation of an oxide film. On applying a cathodic potential scan, a sensitive stripping peak is produced as a result of the reduction of gold oxide back to gold. The magnitude of the peak current generated from the stripping process is a function of the water concentration in an ionic liquid. The method requires no addition of reagents and can be used for the sensitive and in situ determination of water present in small volumes of ionic liquids. Importantly, the method allows the determination of water in the carboxylic acid-based ionic liquids, such as acetate-based protic ionic liquids, where the widely used Karl Fischer titration method suffering from an esterification side reaction which generates water as a side product. PMID:22372467

  19. Integration of microfluidics/electrochemical system for trace metal analysis by stripping voltammetry

    NASA Astrophysics Data System (ADS)

    Lin, Yuehe; Zhao, Rui; Thrall, Karla D.; Timchalk, C. A.; Bennett, Wendy D.; Matson, Dean W.

    1999-08-01

    Microanalytical systems based on a microfluidics/electrochemical detection scheme were developed. Individual modules, such as microfabricated piezoelectrically actuated pumps and a microelectrochemical cell were integrated onto portable platforms. This allows rapid change-out and repair of individual components by incorporating `plug and play' concepts now standard in PC's. Two different integration schemes were used for construction of the microanalytical systems based on microfluidics/electrochemical detection. In first scheme, all individual modules were integrated in the surface of the standard microfluidic platform based on a plug-and-play design. Microelectrochemical flow cell which integrated three electrodes based on a wall-jet design was fabricated on polymer substrate. The microelectrochemical flow cell was then plugged directly into the microfluidic platform. Another integration scheme was based on a multilayer lamination method utilizing stacking modules with different functionality to achieve a compact microanalytical device. Application of the microanalytical system for detection of lead in river water and saliva samples using stripping voltammetry is described.

  20. Determination of humic substances in natural waters by cathodic stripping voltammetry of their complexes with iron.

    PubMed

    Laglera, Luis M; Battaglia, Gianluca; van den Berg, Constant M G

    2007-09-01

    A new voltammetric method is presented for the measurement of humic substances (HS) in natural waters. The method is based on catalytic cathodic stripping voltammetry (CSV) and makes use of adsorptive properties of iron-HS complexes on the mercury drop electrode at natural pH. A fulvic acid standard (IHSS) was used to confirm the voltammetric response (peak potential and sensitivity) for the HS for natural water samples. Optimized conditions included the linear-sweep mode, deposition at -0.1 V, pH buffered at 8 and a scan rate of 50 mV s(-1). At a deposition time of 240 s in the presence of 10 nM iron and 30 mM bromate, the detection limit was 5 microg L(-1) HS in seawater, which could be lowered further by an increase in the bromate concentration, or in the adsorption time. The method was used to determine HS in the Irish Sea which were found to occur at levels between 60 and 600 microg L(-1). The new method is sufficiently sensitive to detect the low HS content in oceanic samples and has implications to the study of iron speciation. PMID:17765064

  1. Sensitive quantitation of Ochratoxin A in cocoa beans using differential pulse voltammetry based aptasensor.

    PubMed

    Mishra, Rupesh K; Hayat, Akhtar; Catanante, Gaëlle; Istamboulie, Georges; Marty, Jean-Louis

    2016-02-01

    In this work, we propose for the first time a sensitive Ochratoxin A (OTA) detection in cocoa beans using competitive aptasensor by differential pulse voltammetry (DPV). In the proposed method, biotin labeled and free OTA competed to bind with immobilized aptamer onto the surface of a screen printed carbon electrode (SPCE), and percentage binding was calculated. The detection was performed after adding avidin-ALP to perform avidin-biotin reaction; the signal was generated through a suitable substrate 1-naphthyl phosphate (1-NP), for alkaline phosphatase (ALP). The cocoa samples were extracted and purified using molecular imprinted polymer (MIP) columns specifically designed for OTA. The developed aptasensor showed a good linearity in the range 0.15-5 ng/mL with the limit of detection (LOD) 0.07 ng/mL and 3.7% relative standard deviation (RSD). The aptasensor displayed good recovery values in the range 82.1-85% with 3.87% RSD, thus, demonstrated the efficiency of proposed aptasensor for such matrices. PMID:26304413

  2. Direct analysis of palladium in active pharmaceutical ingredients by anodic stripping voltammetry.

    PubMed

    Rosolina, Samuel M; Chambers, James Q; Xue, Zi-Ling

    2016-03-31

    Anodic stripping voltammetry, a classical electroanalytical method has been optimized to analyze trace Pd(II) in active pharmaceutical ingredient matrices. The electroanalytical approach with an unmodified glassy carbon electrode was performed in both aqueous and 95% DMSO/5% water (95/5 DMSO/H2O) solutions, without pretreatment such as acid digestion or dry ashing to remove the organics. Limits of detection (LODs) in the presence of caffeine and ketoprofen were determined to be 11 and 9.6 μg g(-1), with a relative standard deviation (RSD) of 5.7% and 2.3%, respectively. This method is simple, highly reproducible, sensitive, and robust. The instrumentation has the potential to be portable and the obviation of sample pretreatment makes it an ideal approach for determining lost catalytic metals in pharmaceutical-related industries. Furthermore, the simultaneous detection of Pd(II) with Cd(II) and Pb(II) in the low μg L(-1) range indicates that this system is capable of simultaneous multi-analyte analysis in a variety of matrices. PMID:26965326

  3. Aspartame decreases evoked extracellular dopamine levels in the rat brain: an in vivo voltammetry study.

    PubMed

    Bergstrom, Brian P; Cummings, Deirdre R; Skaggs, Tricia A

    2007-12-01

    Conflicting reports exist concerning the effect aspartame (APM, l-aspartyl-l-phenylalanine methyl ester) has upon brain biogenic amines. In the following study, in vivo voltammetry was utilized to measure evoked extracellular dopamine (DA) levels in the striatum of rats in order to assess APM's effect. Time-course experiments revealed a significant decline in evoked extracellular DA levels within 1h of a single systemic dose (500mg/kg i.p.) when compared to vehicle-injected controls. The effect was frequency dependent and showed a significant decrease utilizing high frequency stimulation parameters (50 and 60Hz). In order to further determine APM's potential to alter evoked extracellular DA levels, extended stimulation periods were employed to deplete releasable stores both before and after APM administration in intact and 6-OHDA partially lesioned animals. The extended stimulation periods were applied at 60Hz for 2,5,10 and 20s durations. APM decreased DA levels under these conditions in both intact and 6-OHDA partially lesioned animals by an average of 34% and 51%, respectively. Kinetic analysis performed on frequency series indicated that the diminished DA levels corresponded to a significant reduction in DA release. These findings suggest that APM has a relatively potent effect of decreasing evoked extracellular DA levels when administered systemically under the conditions specified. PMID:17976663

  4. Coulometric differential FFT admittance voltammetry determination of Amlodipine in pharmaceutical formulation by nano-composite electrode.

    PubMed

    Norouzi, Parviz; Gupta, Vinod Kumar; Larijani, Bagher; Rasoolipour, Solmaz; Faridbod, Farnoush; Ganjali, Mohammad R

    2015-01-01

    An electrochemical detection technique based on combination of was coulometric differential fast Fourier transformation admittance voltammetry (CDFFTAV) and nano-composite film modified glassy carbon electrode was successfully applied for sensitive determination of Amlodipine. The nano-composite film was made by a mixture of ionic liquid, 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIMBF4), multiwall carbon nanotube and Au nanoparticles as electrochemical mediators. Studies reveal that the irreversible oxidation of Amlodipine was highly facile on the electrode surface. The electrochemical response was established on calculation of the charge under the admittance peak, which was obtained by discrete integration of the admittance response in a selected potential range, obtained in a flow injection analysis. Once established the best operative optimum conditions, the resulting nano-composite film electrode showed a catalytic effect on the oxidation of the analyte. The response is linear in the Amlodipine concentration range of 1.0 × 10(-9) to 2.0 × 10(-7)M with a detection limit of 1.25 × 10(-10)M. Moreover, the proposed technique exhibited high sensitivity, fast response time (less than 6s) and long-term stability and reproducibility around 96%, and it was successfully used to the determination of Amlodipine content in the pharmaceutical formulation. PMID:25281143

  5. An advanced AFM sensor for high-aspect ratio pattern profile in-line measurement

    NASA Astrophysics Data System (ADS)

    Watanabe, Masahiro; Baba, Shuichi; Nakata, Toshihiko; Kurenuma, Toru; Kuroda, Hiroshi; Hiroki, Takenori

    2006-03-01

    Design rule shrinkage and the wider adoption of new device structures such as STI, copper damascene interconnects, and deep trench structures have increased the necessity of in-line process monitoring of step heights and profiles of device structures. For monitoring active device patterns, not test patterns as in OCD, AFM is the only non-destructive 3D monitoring tool. The barriers to using AFM in-line monitoring are its slow throughput and the accuracy degradation associated with probe tip wear and spike noise caused by unwanted oscillation on the steep slopes of high-aspect-ratio patterns. Our proprietary AFM scanning method, Step in mode®, is the method best suited to measuring high-aspect-ratio pattern profiles. Because the probe is not dragged on the sample surface as in conventional AFM, the profile trace fidelity across steep slopes is excellent. Because the probe does not oscillate and hit the sample at a high frequency as in AC scanning mode, this mode is free from unwanted spurious noises on steep sample slopes and incurs extremely little probe tip wear. To fully take advantage of the above properties, we have developed an AFM sensor optimized for in-line use, which produces accurate profile data at high speeds. The control scheme we have developed for the AFM sensor, which we call "Smart Step-in", elaborately analyses the contact force signal, enabling efficient probe tip scanning and a low and stable contact force. The mechanism of the AFM sensor has been optimized for the higher scanning rate and has improved the accuracy, such as the scanning planarity, position and height accuracy, and slope angle accuracy. Our prototype AFM sensor can scan high-aspect-ratio patterns while stabilizing the contact force at 3 nN. The step height measurement repeatability was 0.8 nm (3σ). A STI-like test pattern was scanned, and the steep sidewalls with angles of 84° were measured with high fidelity and without spurious noises.

  6. MEMS piezoresistive ring resonator for AFM imaging with pico-Newton force resolution

    NASA Astrophysics Data System (ADS)

    Xiong, Z.; Walter, B.; Mairiaux, E.; Faucher, M.; Buchaillot, L.; Legrand, B.

    2013-03-01

    A new concept of atomic force microscope (AFM) oscillating probes using electrostatic excitation and piezoresistive detection is presented. The probe is characterized by electrical methods in vacuum and by mechanical methods in air. A frequency-mixing measurement technique is developed to reduce the parasitic signal floor. The probe resonance frequencies are in the 1 MHz range and the quality factor is measured about 53 000 in vacuum and 3000 in air. The ring probe is mounted onto a commercial AFM set-up and topographic images of patterned sample surfaces are obtained. The force resolution deduced from the measurements is about 10 pN Hz-0.5.

  7. Studying post-etching silicon crystal defects on 300mm wafer by automatic defect review AFM

    NASA Astrophysics Data System (ADS)

    Zandiatashbar, Ardavan; Taylor, Patrick A.; Kim, Byong; Yoo, Young-kook; Lee, Keibock; Jo, Ahjin; Lee, Ju Suk; Cho, Sang-Joon; Park, Sang-il

    2016-03-01

    Single crystal silicon wafers are the fundamental elements of semiconductor manufacturing industry. The wafers produced by Czochralski (CZ) process are very high quality single crystalline materials with known defects that are formed during the crystal growth or modified by further processing. While defects can be unfavorable for yield for some manufactured electrical devices, a group of defects like oxide precipitates can have both positive and negative impacts on the final device. The spatial distribution of these defects may be found by scattering techniques. However, due to limitations of scattering (i.e. light wavelength), many crystal defects are either poorly classified or not detected. Therefore a high throughput and accurate characterization of their shape and dimension is essential for reviewing the defects and proper classification. While scanning electron microscopy (SEM) can provide high resolution twodimensional images, atomic force microscopy (AFM) is essential for obtaining three-dimensional information of the defects of interest (DOI) as it is known to provide the highest vertical resolution among all techniques [1]. However AFM's low throughput, limited tip life, and laborious efforts for locating the DOI have been the limitations of this technique for defect review for 300 mm wafers. To address these limitations of AFM, automatic defect review AFM has been introduced recently [2], and is utilized in this work for studying DOI on 300 mm silicon wafer. In this work, we carefully etched a 300 mm silicon wafer with a gaseous acid in a reducing atmosphere at a temperature and for a sufficient duration to decorate and grow the crystal defects to a size capable of being detected as light scattering defects [3]. The etched defects form a shallow structure and their distribution and relative size are inspected by laser light scattering (LLS). However, several groups of defects couldn't be properly sized by the LLS due to the very shallow depth and low

  8. Coexistence of orbital and CE-AFM orders in colossal magnetoresistance manganites: A symmetry perspective

    NASA Astrophysics Data System (ADS)

    Ribeiro, J. L.

    2016-07-01

    The complex interplay between order parameters of different nature that dominates the physics of colossal magnetoresistance manganites is analysed from a symmetry based perspective. Phenomenological energies are given for the different competing phases. It is shown that the general trends observed in different systems, such as the mutual exclusion of orbital order and A-AFM order and the related stabilization of the CE-AFM order, stem to large extend from the symmetry of the parameters involved. The possible stabilization of complex phases where charge and orbital order coexist with magnetic and ferroelectric states is also anticipated.

  9. FRAME (Force Review Automation Environment): MATLAB-based AFM data processor.

    PubMed

    Partola, Kostyantyn R; Lykotrafitis, George

    2016-05-01

    Data processing of force-displacement curves generated by atomic force microscopes (AFMs) for elastic moduli and unbinding event measurements is very time consuming and susceptible to user error or bias. There is an evident need for consistent, dependable, and easy-to-use AFM data processing software. We have developed an open-source software application, the force review automation environment (or FRAME), that provides users with an intuitive graphical user interface, automating data processing, and tools for expediting manual processing. We did not observe a significant difference between manually processed and automatically processed results from the same data sets. PMID:26972765

  10. Direct visualization of the trimeric structure of the ASIC1a channel, using AFM imaging

    SciTech Connect

    Carnally, Stewart M.; Dev, Harveer S.; Stewart, Andrew P.; Barrera, Nelson P.; Van Bemmelen, Miguel X.; Schild, Laurent; Henderson, Robert M.; Edwardson, J.Michael

    2008-08-08

    There has been confusion about the subunit stoichiometry of the degenerin family of ion channels. Recently, a crystal structure of acid-sensing ion channel (ASIC) 1a revealed that it assembles as a trimer. Here, we used atomic force microscopy (AFM) to image unprocessed ASIC1a bound to mica. We detected a mixture of subunit monomers, dimers and trimers. In some cases, triple-subunit clusters were clearly visible, confirming the trimeric structure of the channel, and indicating that the trimer sometimes disaggregated after adhesion to the mica surface. This AFM-based technique will now enable us to determine the subunit arrangement within heteromeric ASICs.

  11. Multiparametric imaging of biological systems by force-distance curve-based AFM.

    PubMed

    Dufrêne, Yves F; Martínez-Martín, David; Medalsy, Izhar; Alsteens, David; Müller, Daniel J

    2013-09-01

    A current challenge in the life sciences is to understand how biological systems change their structural, biophysical and chemical properties to adjust functionality. Addressing this issue has been severely hampered by the lack of methods capable of imaging biosystems at high resolution while simultaneously mapping their multiple properties. Recent developments in force-distance (FD) curve-based atomic force microscopy (AFM) now enable researchers to combine (sub)molecular imaging with quantitative mapping of physical, chemical and biological interactions. Here we discuss the principles and applications of advanced FD-based AFM tools for the quantitative multiparametric characterization of complex cellular and biomolecular systems under physiological conditions. PMID:23985731

  12. Probing the PEDOT:PSS/cell interface with conductive colloidal probe AFM-SECM

    NASA Astrophysics Data System (ADS)

    Knittel, P.; Zhang, H.; Kranz, C.; Wallace, G. G.; Higgins, M. J.

    2016-02-01

    Conductive colloidal probe Atomic Force-Scanning Electrochemical Microscopy (AFM-SECM) is a new approach, which employs electrically insulated AFM probes except for a gold-coated colloid located at the end of the cantilever. Hence, force measurements can be performed while biasing the conductive colloid under physiological conditions. Moreover, such colloids can be modified by electrochemical polymerization resulting, e.g. in conductive polymer-coated spheres, which in addition may be loaded with specific dopants. In contrast to other AFM-based single cell force spectroscopy measurements, these probes allow adhesion measurements at the cell-biomaterial interface on multiple cells in a rapid manner while the properties of the polymer can be changed by applying a bias. In addition, spatially resolved electrochemical information e.g., oxygen reduction can be obtained simultaneously. Conductive colloid AFM-SECM probes modified with poly(3,4-ethylenedioxythiophene) doped with polystyrene sulfonate (PEDOT:PSS) are used for single cell force measurements in mouse fibroblasts and single cell interactions are investigated as a function of the applied potential.Conductive colloidal probe Atomic Force-Scanning Electrochemical Microscopy (AFM-SECM) is a new approach, which employs electrically insulated AFM probes except for a gold-coated colloid located at the end of the cantilever. Hence, force measurements can be performed while biasing the conductive colloid under physiological conditions. Moreover, such colloids can be modified by electrochemical polymerization resulting, e.g. in conductive polymer-coated spheres, which in addition may be loaded with specific dopants. In contrast to other AFM-based single cell force spectroscopy measurements, these probes allow adhesion measurements at the cell-biomaterial interface on multiple cells in a rapid manner while the properties of the polymer can be changed by applying a bias. In addition, spatially resolved electrochemical

  13. AFM and XPA data on structural features and properties of films and powders based on naphthalocyanines

    NASA Astrophysics Data System (ADS)

    Ramonova, A. G.; Nakusov, A. T.; Sozanov, V. G.; Bliev, A. P.; Magkoev, T. T.

    2015-06-01

    The template synthesis is used to produce powders and films based on naphthalocyanines and the corresponding metal complexes (Pc, CuPc, and NiPc). The atomic-force microscopy (AFM) and X-ray phase analysis (XPA) are employed in the study of structure and phase of fine powders and nanostructured films. The AFM data are used to determine the orientation and density of primary particles packed in the film. The XPA method is used to study the chemical composition and crystal structure of the synthesized samples. The regularities related to the structural features that affect the electrophysical properties of the films under study are revealed.

  14. Measuring Cyclic Error in Laser Heterodyne Interferometers

    NASA Technical Reports Server (NTRS)

    Ryan, Daniel; Abramovici, Alexander; Zhao, Feng; Dekens, Frank; An, Xin; Azizi, Alireza; Chapsky, Jacob; Halverson, Peter

    2010-01-01

    An improved method and apparatus have been devised for measuring cyclic errors in the readouts of laser heterodyne interferometers that are configured and operated as displacement gauges. The cyclic errors arise as a consequence of mixing of spurious optical and electrical signals in beam launchers that are subsystems of such interferometers. The conventional approach to measurement of cyclic error involves phase measurements and yields values precise to within about 10 pm over air optical paths at laser wavelengths in the visible and near infrared. The present approach, which involves amplitude measurements instead of phase measurements, yields values precise to about .0.1 microns . about 100 times the precision of the conventional approach. In a displacement gauge of the type of interest here, the laser heterodyne interferometer is used to measure any change in distance along an optical axis between two corner-cube retroreflectors. One of the corner-cube retroreflectors is mounted on a piezoelectric transducer (see figure), which is used to introduce a low-frequency periodic displacement that can be measured by the gauges. The transducer is excited at a frequency of 9 Hz by a triangular waveform to generate a 9-Hz triangular-wave displacement having an amplitude of 25 microns. The displacement gives rise to both amplitude and phase modulation of the heterodyne signals in the gauges. The modulation includes cyclic error components, and the magnitude of the cyclic-error component of the phase modulation is what one needs to measure in order to determine the magnitude of the cyclic displacement error. The precision attainable in the conventional (phase measurement) approach to measuring cyclic error is limited because the phase measurements are af-

  15. Cyclic fatigue mechanisms in partially stabilized zirconia

    SciTech Connect

    Hoffman, M.J.; Wakayama, Shuichi; Kawahara, Masanori; Mai, Y.W.; Kishi, Teruo

    1995-12-31

    Cyclic fatigue crack growth rate and crack resistance curve testing were undertaken on 6 different grades of Mg-PSZ. The width of the transformation zone at the flanks of the cracks was determined using Raman spectroscopy and, combined with R-curve toughening values, used to ascertain the level of crack-tip shielding during cyclic fatigue crack growth and hence the crack-tip stress intensity factor amplitude. By normalizing the crack-tip stress intensity factor amplitude with the intrinsic toughness of the material, it was found that the cyclic fatigue threshold stress intensity factor was independent of the extent of crack-tip shielding and a function of the stress intensity factor at the crack tip. In situ SEM observations of cyclic fatigue revealed crack bridging by uncracked ligaments and the precipitate phase. Under cyclic loading the precipitate bridges were postulated to undergo frictional degradation at the precipitate/matrix interface with the degree of degradation determined by the cyclic amplitude. Acoustic emission testing revealed acoustic emissions at three distinct levels during the loading cycle: firstly, near the maximum applied stress intensity factor caused by crack propagation; secondly, at the mid-range of the applied stress intensity factor attributed to crack closure near the crack tip, presumably as a result of transformation induced dilation; and thirdly, intermittently near the base of the loading cycle as a result of fracture surface contact due to surface roughness at a significant distance behind the crack tip. Crack closure near the crack tip due to dilation is proposed to significantly reduce the crack tip stress intensity factor amplitude and hence the degree of cyclic fatigue.

  16. An Evaluation of the Impacts of AF-M315E Propulsion Systems for Varied Mission Applications

    NASA Technical Reports Server (NTRS)

    Deans, Matthew C.; Oleson, Steven R.; Fittje, James; Colozza, Anthony; Packard, Tom; Gyekenyesi, John; McLean, Christopher H.; Spores, Ronald A.

    2015-01-01

    The purpose of the AF-M315E COMPASS study is to identify near-term (3-5 years) and long term (5 years +) opportunities for infusion, specifically the thruster and associated component technologies being developed as part of the GPIM project. Develop design reference missions which show the advantages of the AF-M315E green propulsion system. Utilize a combination of past COMPASS designs and selected new designs to demonstrate AF-M315E advantages. Use the COMPASS process to show the puts and takes of using AF-M315E at the integrated system level.

  17. Novel pH-Sensitive Cyclic Peptides

    PubMed Central

    Weerakkody, Dhammika; Moshnikova, Anna; El-Sayed, Naglaa Salem; Adochite, Ramona-Cosmina; Slaybaugh, Gregory; Golijanin, Jovana; Tiwari, Rakesh K.; Andreev, Oleg A.; Parang, Keykavous; Reshetnyak, Yana K.

    2016-01-01

    A series of cyclic peptides containing a number of tryptophan (W) and glutamic acid (E) residues were synthesized and evaluated as pH-sensitive agents for targeting of acidic tissue and pH-dependent cytoplasmic delivery of molecules. Biophysical studies revealed the molecular mechanism of peptides action and localization within the lipid bilayer of the membrane at high and low pHs. The symmetric, c[(WE)4WC], and asymmetric, c[E4W5C], cyclic peptides translocated amanitin, a polar cargo molecule of similar size, across the lipid bilayer and induced cell death in a pH- and concentration-dependent manner. Fluorescently-labelled peptides were evaluated for targeting of acidic 4T1 mammary tumors in mice. The highest tumor to muscle ratio (5.6) was established for asymmetric cyclic peptide, c[E4W5C], at 24 hours after intravenous administration. pH-insensitive cyclic peptide c[R4W5C], where glutamic acid residues (E) were replaced by positively charged arginine residues (R), did not exhibit tumor targeting. We have introduced a novel class of cyclic peptides, which can be utilized as a new pH-sensitive tool in investigation or targeting of acidic tissue. PMID:27515582

  18. Cyclic depsipeptides as potential cancer therapeutics.

    PubMed

    Kitagaki, Jirouta; Shi, Genbin; Miyauchi, Shizuka; Murakami, Shinya; Yang, Yili

    2015-03-01

    Cyclic depsipeptides are polypeptides in which one or more amino acid is replaced by a hydroxy acid, resulting in the formation of at least one ester bond in the core ring structure. Many natural cyclic depsipeptides possessing intriguing structural and biological properties, including antitumor, antifungal, antiviral, antibacterial, anthelmintic, and anti-inflammatory activities, have been identified from fungi, plants, and marine organisms. In particular, the potent effects of cyclic depsipeptides on tumor cells have led to a number of clinical trials evaluating their potential as chemotherapeutic agents. Although many of the trials have not achieved the desired results, romidepsin (FK228), a bicyclic depsipeptide that inhibits histone deacetylase, has been shown to have clinical efficacy in patients with refractory cutaneous T-cell lymphoma and has received Food and Drug Administration approval for use in treatment. In this review, we discuss antitumor cyclic depsipeptides that have undergone clinical trials and focus on their structural features, mechanisms, potential applications in chemotherapy, and pharmacokinetic and toxicity data. The results of this study indicate that cyclic depsipeptides could be a rich source of new cancer therapeutics. PMID:25419631

  19. Cyclic transformation of orbital angular momentum modes

    NASA Astrophysics Data System (ADS)

    Schlederer, Florian; Krenn, Mario; Fickler, Robert; Malik, Mehul; Zeilinger, Anton

    2016-04-01

    The spatial modes of photons are one realization of a QuDit, a quantum system that is described in a D-dimensional Hilbert space. In order to perform quantum information tasks with QuDits, a general class of D-dimensional unitary transformations is needed. Among these, cyclic transformations are an important special case required in many high-dimensional quantum communication protocols. In this paper, we experimentally demonstrate a cyclic transformation in the high-dimensional space of photonic orbital angular momentum (OAM). Using simple linear optical components, we show a successful four-fold cyclic transformation of OAM modes. Interestingly, our experimental setup was found by a computer algorithm. In addition to the four-cyclic transformation, the algorithm also found extensions to higher-dimensional cycles in a hybrid space of OAM and polarization. Besides being useful for quantum cryptography with QuDits, cyclic transformations are key for the experimental production of high-dimensional maximally entangled Bell-states.

  20. Novel pH-Sensitive Cyclic Peptides.

    PubMed

    Weerakkody, Dhammika; Moshnikova, Anna; El-Sayed, Naglaa Salem; Adochite, Ramona-Cosmina; Slaybaugh, Gregory; Golijanin, Jovana; Tiwari, Rakesh K; Andreev, Oleg A; Parang, Keykavous; Reshetnyak, Yana K

    2016-01-01

    A series of cyclic peptides containing a number of tryptophan (W) and glutamic acid (E) residues were synthesized and evaluated as pH-sensitive agents for targeting of acidic tissue and pH-dependent cytoplasmic delivery of molecules. Biophysical studies revealed the molecular mechanism of peptides action and localization within the lipid bilayer of the membrane at high and low pHs. The symmetric, c[(WE)4WC], and asymmetric, c[E4W5C], cyclic peptides translocated amanitin, a polar cargo molecule of similar size, across the lipid bilayer and induced cell death in a pH- and concentration-dependent manner. Fluorescently-labelled peptides were evaluated for targeting of acidic 4T1 mammary tumors in mice. The highest tumor to muscle ratio (5.6) was established for asymmetric cyclic peptide, c[E4W5C], at 24 hours after intravenous administration. pH-insensitive cyclic peptide c[R4W5C], where glutamic acid residues (E) were replaced by positively charged arginine residues (R), did not exhibit tumor targeting. We have introduced a novel class of cyclic peptides, which can be utilized as a new pH-sensitive tool in investigation or targeting of acidic tissue. PMID:27515582

  1. Visualization of cyclic nucleotide dynamics in neurons

    PubMed Central

    Gorshkov, Kirill; Zhang, Jin

    2014-01-01

    The second messengers cyclic adenosine monophosphate (cAMP) and cyclic guanosine monophosphate (cGMP) transduce many neuromodulatory signals from hormones and neurotransmitters into specific functional outputs. Their production, degradation and signaling are spatiotemporally regulated to achieve high specificity in signal transduction. The development of genetically encodable fluorescent biosensors has provided researchers with useful tools to study these versatile second messengers and their downstream effectors with unparalleled spatial and temporal resolution in cultured cells and living animals. In this review, we introduce the general design of these fluorescent biosensors and describe several of them in more detail. Then we discuss a few examples of using cyclic nucleotide fluorescent biosensors to study regulation of neuronal function and finish with a discussion of advances in the field. Although there has been significant progress made in understanding how the specific signaling of cyclic nucleotide second messengers is achieved, the mechanistic details in complex cell types like neurons are only just beginning to surface. Current and future fluorescent protein reporters will be essential to elucidate the role of cyclic nucleotide signaling dynamics in the functions of individual neurons and their networks. PMID:25538560

  2. Further studies on cyclic erythropoiesis in mice

    SciTech Connect

    Gibson, C.M.; Gurney, C.W.; Simmons, E.L.; Gaston, E.O.

    1985-10-01

    When young adult female W/Wv mice are given 0.5 micro+Ci /sup 89/Sr/g body weight intravenously, their hematocrit values oscillate from nadirs of 26% to zeniths of 42% with a periodicity of 16 days. The response of the W/Wv mouse to an assortment of radioactive and hematologic stresses have been examined in an effort to understand better the pathophysiology of cyclic erythropoiesis. When the dose of /sup 89/Sr is increased, the amplitude of cycling increases as nadirs are lowered, but periodicity is unchanged. When the dose of /sup 89/Sr is lowered to 0.3 microCi or less, cyclic erythropoiesis of substantial amplitude is observed only after five or six microoscillations. A single hematopoietic insult of 80 rad x-irradiation coupled with phlebotomy produces a transient form of cyclic erythropoiesis, namely, a series of dampened oscillations prior to recovery. Finally, we report that Wv/Wv mice exhibit a form of cyclic erythropoiesis in response to 0.5 microCi /sup 89/Sr/g body weight, in which the hematocrit values of successive nadirs gradually increase, and stabilize at about 100 days. /sup 89/Sr does not induce cyclic erythropoiesis in the +/+, W/+, or W/v/+ mice, the Hertwig strain of anemic mice, or in normal BDF1 mice.

  3. Multiparameter Estimation in Voltammetry When an Electron Transfer Process Is Coupled to a Chemical Reaction.

    PubMed

    Simonov, Alexandr N; Morris, Graham P; Mashkina, Elena; Bethwaite, Blair; Gillow, Kathryn; Baker, Ruth E; Gavaghan, David J; Bond, Alan M

    2016-05-01

    Estimation of thermodynamic and kinetic parameters in electrochemical studies is usually undertaken via comparison of the experimental results with theory based on a model that mimics the experiment. The present study examines the credibility of transient d.c. and a.c. voltammetric theory-experiment comparisons for recovery of the parameters needed to model the ubiquitous mechanism when an electron transfer (E) reaction is followed by a chemical (C) step in the EC process ([Formula: see text]). The data analysis has been undertaken using optimization methods facilitated in some cases by grid computing. These techniques have been applied to the simulated (5% noise added) and experimental (reduction of trans-stilbene) voltammograms to assess the capabilities of parameter recovery of E(0) (reversible potential for the E step), k(0) (heterogeneous electron transfer rate constant at E(0)), α (charge transfer coefficient for the E step), and k(f) and k(b) (forward and backward rate constants for the C step) under different kinetic regimes. The advantages provided by the use of a.c. instead of d.c. voltammetry and data optimization methods over heuristic approaches to "experiment"-theory comparisons are discussed, as are the limitations in the efficient recovery of a unique set of parameters for the EC mechanism. In the particular experimental case examined herein, results for the protonation of the electrochemically generated stilbene dianion demonstrate that, notwithstanding significant advances in experiment and theory of voltammetric analysis, reliable recovery of the parameters for the EC mechanism with a fast chemical process remains a stiff problem. PMID:27041344

  4. Evaluation of seven cosubstrates in the quantification of horseradish peroxidase enzyme by square wave voltammetry.

    PubMed

    Kergaravat, Silvina V; Pividori, Maria Isabel; Hernandez, Silvia R

    2012-01-15

    The electrochemical detection for horseradish peroxidase-cosubstrate-H(2)O(2) systems was optimized. o-Phenilendiamine, phenol, hydroquinone, pyrocatechol, p-chlorophenol, p-aminophenol and 3,3'-5,5'-tetramethylbenzidine were evaluated as cosubstrates of horseradish peroxidase (HRP) enzyme. Therefore, the reaction time, the addition sequence of the substrates, the cosubstrate:H(2)O(2) ratio and the electrochemical techniques were elected by one-factor optimization assays while the buffer pH, the enzymatic activity and cosubstrate and H(2)O(2) concentrations for each system were selected simultaneously by response surface methodology. Then, the calibration curves for seven horseradish peroxidase-cosubstrate-H(2)O(2) systems were built and the analytic parameters were analyzed. o-Phenilendiamine was selected as the best cosubstrate for the HRP enzyme. For this system the reaction time of 60s, the phosphate buffer pH 6.0, and the concentrations of 2.5×10(-4)molL(-1) o-phenilendiamine and of 1.25×10(-4)molL(-1) H(2)O(2) were chosen as the optimal conditions. In these conditions, the calibration curve of horseradish peroxidase by square wave voltammetry showed a linearity range from 9.5×10(-11) to 1.9×10(-8)molL(-1) and the limit of detection of 3.8×10(-11)molL(-1) with RSD% of 0.03% (n=3). PMID:22265528

  5. Determination of tryptamine in foods using square wave adsorptive stripping voltammetry.

    PubMed

    Costa, Daniel J E; Martínez, Ana M; Ribeiro, Williame F; Bichinho, Kátia M; Di Nezio, María Susana; Pistonesi, Marcelo F; Araujo, Mario C U

    2016-07-01

    Tryptamine, a biogenic amine, is an indole derivative with an electrophilic substituent at the C3 position of the pyrrole ring of the indole moiety. The electrochemical oxidation of tryptamine was investigated using glassy carbon electrode (GCE), and focusing on trace level determination in food products by square wave adsorptive stripping voltammetry (SWAdSV). The electrochemical responses of tryptamine were evaluated using differing voltammetric techniques over a wide pH range, a quasi-reversible electron-transfer to redox system represented by coupled peaks P1-P3, and an irreversible reaction for peak P2 were demonstrated. The proton and electron counts associated with the oxidation reactions were estimated. The nature of the mass transfer process was predominantly diffusion-limited for the oxidation process of P1, the most selective and sensitive analytical response (acetate buffer solution pH 5.3), being used for the development of SWAdSV method, under optimum conditions. The excellent response allowed the development of an electroanalytical method with a linear response range of from 4.7-54.5)×10(-)(8)molL(-1), low detection limit (0.8×10(-)(9)molL(-)(1)), and quantification limit (2.7×10(-9)molL(-1)), and acceptable levels of repeatability (3.6%), and reproducibility (3.8%). Tryptamine content was determined in bananas, tomatoes, cheese (mozzarella and gorgonzola), and cold meats (chicken sausage and pepperoni sausage), yielding recoveries above 90%, with excellent analytical performance using simple and low cost instrumentation. PMID:27154658

  6. Determination of trace cobalt concentrations in human serum by adsorptive stripping voltammetry.

    PubMed

    Kajic, Petra; Milosev, Ingrid; Pihlar, Boris; Pisot, Venceslav

    2003-01-01

    The goal of our study was to develop an accurate and reliable method for determining trace cobalt concentrations in human serum. The method was used to determine cobalt in the sera of healthy persons and patients with orthopaedic implants containing cobalt - a possible source of systemic release of cobalt into the human body. This goal is of vital interest since cobalt and its compounds are classified by IARC as potentially carcinogenic to humans. We used an electrochemical method, adsorptive stripping voltammetry (AdSV), which made possible the low detection limit and high sensitivity needed for measurements in human serum. The serum was acid digested by a combination of H2SO4, HNO3 and H2O2 in a 10 mL Kjeldhal flask. The digested sample was then dissolved in 0.1 mol/L ammonia buffer, pH 9.0 +/- 0.2. The determination is based on the adsorptive collection of the complex of cobalt (II) with dimethylglyoxime on a hanging mercury drop electrode (HMDE). The optimum values of adsorption potential and time were determined to be -0.8 V and 60 s. The optimisation of the sample digestion protocol and measurement procedures ensured the reliable assessment of low cobalt concentrations, down to 0.03 microg/L. The mean concentration of serum cobalt in four healthy persons was 0.11 +/- 0.06 microg/L, and in four patients with total hip replacements 0.34 +/- 0.07 microg/L. This method will be used routinely for measuring serum cobalt levels in patients with total hip replacements. PMID:14968926

  7. Diamond-modified AFM probes: from diamond nanowires to atomic force microscopy-integrated boron-doped diamond electrodes.

    PubMed

    Smirnov, Waldemar; Kriele, Armin; Hoffmann, René; Sillero, Eugenio; Hees, Jakob; Williams, Oliver A; Yang, Nianjun; Kranz, Christine; Nebel, Christoph E

    2011-06-15

    In atomic force microscopy (AFM), sharp and wear-resistant tips are a critical issue. Regarding scanning electrochemical microscopy (SECM), electrodes are required to be mechanically and chemically stable. Diamond is the perfect candidate for both AFM probes as well as for electrode materials if doped, due to diamond's unrivaled mechanical, chemical, and electrochemical properties. In this study, standard AFM tips were overgrown with typically 300 nm thick nanocrystalline diamond (NCD) layers and modified to obtain ultra sharp diamond nanowire-based AFM probes and probes that were used for combined AFM-SECM measurements based on integrated boron-doped conductive diamond electrodes. Analysis of the resonance properties of the diamond overgrown AFM cantilevers showed increasing resonance frequencies with increasing diamond coating thicknesses (i.e., from 160 to 260 kHz). The measured data were compared to performed simulations and show excellent correlation. A strong enhancement of the quality factor upon overgrowth was also observed (120 to 710). AFM tips with integrated diamond nanowires are shown to have apex radii as small as 5 nm and where fabricated by selectively etching diamond in a plasma etching process using self-organized metal nanomasks. These scanning tips showed superior imaging performance as compared to standard Si-tips or commercially available diamond-coated tips. The high imaging resolution and low tip wear are demonstrated using tapping and contact mode AFM measurements by imaging ultra hard substrates and DNA. Furthermore, AFM probes were coated with conductive boron-doped and insulating diamond layers to achieve bifunctional AFM-SECM probes. For this, focused ion beam (FIB) technology was used to expose the boron-doped diamond as a recessed electrode near the apex of the scanning tip. Such a modified probe was used to perform proof-of-concept AFM-SECM measurements. The results show that high-quality diamond probes can be fabricated, which are

  8. Cyclic and low temperature effects on microcircuits

    NASA Technical Reports Server (NTRS)

    Weissflug, V. A.; Sisul, E. V.

    1977-01-01

    Cyclic temperature and low temperature operating life tests, and pre-/post-life device evaluations were used to determine the degrading effects of thermal environments on microcircuit reliability. Low power transistor-transistor-logic gates and linear devices were included in each test group. Device metallization systems included aluminum metallization/aluminum wire, aluminum metallization/gold wire, and gold metallization/gold wire. Fewer than 2% electrical failures were observed during the cyclic and low temperature life tests and the post-life evaluations revealed approximately 2% bond pull failures. Reconstruction of aluminum die metallization was observed in all devices and the severity of the reconstruction appeared to be directly related to the magnitude of the temperature excursion. All types of bonds except the gold/gold bonds were weakened by exposure to repeated cyclic temperature stress.

  9. The structure of high-methoxyl sugar acid gels of citrus pectin as determined by AFM

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Images of native high methoxyl sugar acid gels (HMSAG) were obtained by atomic force microscopy (AFM) in the Tapping ModeTM. Electronic thinning of the pectin strands to one pixel wide allowed the pectin network to be viewed in the absence of variable strand widths related to preferentially solvate...

  10. Nanomechanical probing of soft matter through hydrophobic AFM tips fabricated by two-photon polymerization

    NASA Astrophysics Data System (ADS)

    Suriano, Raffaella; Zandrini, Tommaso; De Marco, Carmela; Osellame, Roberto; Turri, Stefano; Bragheri, Francesca

    2016-04-01

    Atomic force microscopy (AFM) nanoindentation of soft materials is a powerful tool for probing mechanical properties of biomaterials. Though many results have been reported in this field over the last decade, adhesion forces between the tip and the sample hinder the elastic modulus measurement when hydrophilic soft samples are investigated. Here, two-photon polymerization (2PP) technology was used to fabricate hydrophobic perfluoropolyether-based AFM tips. The hydrophobic 2PP tips allowed us to overcome the limitations of commercial and functionalized tips as well as to successfully measure the elastic modulus of medically relevant soft materials in air. Our results obtained in the characterization of poly(dimethyl siloxane) and polyethylene glycol hydrogels showed lower adhesion forces over a larger measurement range when compared to measurements performed with commercial tips. The elastic moduli measured by means of hydrophobic 2PP AFM tips were also found to be comparable to those obtained using conventional techniques for macroscopic samples. We successfully showed that the hydrophobic AFM tips developed by this highly versatile technology enable the study of mechanical properties of soft matter, benefiting from reduced sample-tip interactions, and a custom-made shape and dimension of the tips.

  11. AFM tip characterization by using FFT filtered images of step structures.

    PubMed

    Yan, Yongda; Xue, Bo; Hu, Zhenjiang; Zhao, Xuesen

    2016-01-01

    The measurement resolution of an atomic force microscope (AFM) is largely dependent on the radius of the tip. Meanwhile, when using AFM to study nanoscale surface properties, the value of the tip radius is needed in calculations. As such, estimation of the tip radius is important for analyzing results taken using an AFM. In this study, a geometrical model created by scanning a step structure with an AFM tip was developed. The tip was assumed to have a hemispherical cone shape. Profiles simulated by tips with different scanning radii were calculated by fast Fourier transform (FFT). By analyzing the influence of tip radius variation on the spectra of simulated profiles, it was found that low-frequency harmonics were more susceptible, and that the relationship between the tip radius and the low-frequency harmonic amplitude of the step structure varied monotonically. Based on this regularity, we developed a new method to characterize the radius of the hemispherical tip. The tip radii estimated with this approach were comparable to the results obtained using scanning electron microscope imaging and blind reconstruction methods. PMID:26517548

  12. Tapping and contact mode imaging of native chromosomes and extraction of genomic DNA using AFM tips

    NASA Astrophysics Data System (ADS)

    Sun, Yingchun; Arakawa, Hideo; Osada, Toshiya; Ikai, Atsushi

    2002-03-01

    It is very important both in medicine and biology to clarify the chromosomal structure to understand its functions. In a standard cytogenetic procedure, chromosomes are often fixed in a mixture of acetic acid and methanol. This process most likely changes the mechanical property of chromosomes. We adopted a method to prepare native and unfixed chromosomes from mouse 3T3 cells and used tapping and contact mode atomic force microscopy (AFM) to image and manipulate them. Modified AFM tips were used to image chromosomes in contact mode in air, and then the chromosome samples were immobilized on a substrate and placed in a buffer solution to pull out DNA-histone complexes from them after they were optimally treated with trypsin. From the AFM images, we could see several bands and granular structures on chromosomes. We obtained force curves indicating long fiber extensions from native chromosomes both with low (in high concentration of NaCl) and high forces (physiological conditions). The result suggested that the degree of chromosome condensation decreased in high concentration of salt. It agrees with the known fact of histone H1 dissociation in a high concentration of salt. We intend to pull out DNA-histone complexes from chromosomes for later molecular operations on them using an AFM.

  13. Evaluation of shooting distance by AFM and FTIR/ATR analysis of GSR.

    PubMed

    Mou, Yongyan; Lakadwar, Jyoti; Rabalais, J Wayne

    2008-11-01

    The techniques of atomic force microscopy (AFM) and Fourier transform infrared attenuated total reflectance (FTIR/ATR) spectroscopy are applied to the analysis of gun-shot residue (GSR) to test their ability to determine shooting distance and discrimination of the powder manufacturers. AFM is a nondestructive technique that is capable of characterizing the shapes and size distributions of GSR particles with resolution down to less than a nanometer. This may be useful for estimation of the shooting distance. Our AFM images of GSR show that the size distribution of the particles is inversely proportional to the shooting distance. Discrimination of powder manufacturers is tested by FTIR/ATR investigation of GSR. Identifying the specific compounds in the GSR by FTIR/ATR was not possible because it is a mixture of the debris of several compounds that compose the residue. However, it is shown that the GSR from different cartridges has characteristic FTIR/ATR bands that may be useful in differentiating the powder manufacturers. It appears promising that the development of AFM and FTIR/ATR databases for various powder manufacturers may be useful in analysis and identification of GSR. PMID:18761553

  14. Fracture Mechanics Testing of Titanium 6AL-4V in AF-M315E

    NASA Technical Reports Server (NTRS)

    Sampson, J. W.; Martinez, J.; McLean, C.

    2016-01-01

    The Green Propellant Infusion Mission (GPIM) will demonstrate the performance of AF-M315E monopropellant on orbit. Flight certification requires a safe-life analysis of the titanium alloy fuel tank to ensure inherent processing flaws will not cause failure during the design life of the tank. Material property inputs for this analysis require testing to determine the stress intensity factor for environment-assisted cracking (KEAC) of Ti 6Al-4V in combination with the AF-M315E monopropellant. Testing of single-edge notched, or SE(B), specimens representing the bulk tank membrane and weld material were performed in accordance with ASTM E1681. Specimens with fatigue pre-cracks were loaded into test fixtures so that the crack tips were exposed to AF-M315E at 50 C for a duration of 1,000 hours. Specimens that did not fail during exposure were opened to inspect the crack surfaces for evidence of crack growth. The threshold stress intensity value, KEAC, is the highest applied stress intensity that produced neither a failure of the specimen during the exposure nor showed evidence of crack growth. The threshold stress intensity factor for environment-assisted cracking of the Ti 6Al-4V forged tank material was found to be at least 22 ksivin and at least 31 ksivin for the weld material when exposed to AF-M315E monopropellant.

  15. Nanomechanical probing of soft matter through hydrophobic AFM tips fabricated by two-photon polymerization.

    PubMed

    Suriano, Raffaella; Zandrini, Tommaso; De Marco, Carmela; Osellame, Roberto; Turri, Stefano; Bragheri, Francesca

    2016-04-15

    Atomic force microscopy (AFM) nanoindentation of soft materials is a powerful tool for probing mechanical properties of biomaterials. Though many results have been reported in this field over the last decade, adhesion forces between the tip and the sample hinder the elastic modulus measurement when hydrophilic soft samples are investigated. Here, two-photon polymerization (2PP) technology was used to fabricate hydrophobic perfluoropolyether-based AFM tips. The hydrophobic 2PP tips allowed us to overcome the limitations of commercial and functionalized tips as well as to successfully measure the elastic modulus of medically relevant soft materials in air. Our results obtained in the characterization of poly(dimethyl siloxane) and polyethylene glycol hydrogels showed lower adhesion forces over a larger measurement range when compared to measurements performed with commercial tips. The elastic moduli measured by means of hydrophobic 2PP AFM tips were also found to be comparable to those obtained using conventional techniques for macroscopic samples. We successfully showed that the hydrophobic AFM tips developed by this highly versatile technology enable the study of mechanical properties of soft matter, benefiting from reduced sample-tip interactions, and a custom-made shape and dimension of the tips. PMID:26926558

  16. Charge Measurement of Atoms and Atomic Resolution of Molecules with Noncontact AFM

    NASA Astrophysics Data System (ADS)

    Gross, Leo

    2010-03-01

    Individual gold and silver adatoms [1] and pentacene molecules [2] on ultrathin NaCl films on Cu(111) were investigated using a qPlus tuning fork atomic force microscope (AFM) operated at 5 Kelvin with oscillation amplitudes in the sub-ångstrom regime. Charging a gold adatom by one electron charge increased the force on the AFM tip by a few piconewtons. Employing Kelvin probe force microscopy (KPFM) we also measured the local contact potential difference (LCPD). We observed that the LCPD is shifted depending on the sign of the charge and allows the discrimination of positively charged, neutral, and negatively charged atoms. To image pentacene molecules we modified AFM tips by means of vertical manipulation techniques, i.e. deliberately picking up known atoms and molecules, such as Au, Ag, Cl, CO, and pentacene. Using a CO terminated tip we resolved all individual atoms and bonds within a pentacene molecule. Three dimensional force maps showing the site specific distance dependence above the molecule were extracted. We compared our experimental results with density functional theory (DFT) calculations to gain insight on the physical origin of AFM contrast formation. We found that atomic resolution is only obtained due to repulsive force contributions originating from the Pauli exclusion principle. [4pt] [1] L. Gross, F. Mohn, P. Liljeroth, J. Repp, F. J. Giessibl, G. Meyer, Science 324, 1428 (2009). [0pt] [2] L. Gross, F. Mohn, N. Moll, P. Liljeroth, G. Meyer, Science 325, 1110 (2009).

  17. Analysis of grating inscribed micro-cantilever for high resolution AFM probe

    NASA Astrophysics Data System (ADS)

    Balajee, N.; Mahapatra, D. R.; Hegde, G. M.

    2013-06-01

    We present a mathematical modelling and analysis of reflection grating etched Si AFM cantilever deflections under different loading conditions. A simple analysis of the effect of grating structures on cantilever deflection is carried out with emphasis on optimizing the beam and gratings such that maximum amount of diffracted light remains within the detector area.

  18. Relationship between model bacterial peptidoglycan network structures and AFM force-distance curves

    NASA Astrophysics Data System (ADS)

    Brown, Aidan; Wickham, Robert; Touhami, Ahmed; Dutcher, John

    2010-03-01

    Recent atomic force microscopy (AFM) measurements have involved pulling on Gram-negative bacterial sacculi with the AFM tip as a means of distinguishing between different proposed structures of the peptidoglycan network. The goal of the present study is to provide the theoretical connection between a given network structure and its response to the pulling force. We model the glycan strands as hinged rods, and the peptide cross-links as wormlike chains. Using Monte Carlo simulation to equilibrate the three-dimensional network, subject to a fixed AFM tip-to-substrate distance, we can compute the force exerted by the network on the AFM tip. The effects of adhesion of the sacculi to the substrate and enzymatic action on the network are included. We have modeled both the layered and the scaffold model for the peptidoglycan network structure. We have compared our theoretical force-distance curves for each network structure with experimental curves to determine which structure provides the best agreement with experiment.

  19. Controlled AFM detachments and movement of nanoparticles: gold clusters on HOPG at different temperatures

    NASA Astrophysics Data System (ADS)

    Tripathi, Manoj; Paolicelli, Guido; D'Addato, Sergio; Valeri, Sergio

    2012-06-01

    The effect of temperature on the onset of movement of gold nanoclusters (diameter 27 nm) deposited on highly oriented pyrolytic graphite (HOPG) has been studied by atomic force microscopy (AFM) techniques. Using the AFM with amplitude modulation (tapping mode AFM) we have stimulated and controlled the movement of individual clusters. We show how, at room temperature, controlled detachments and smooth movements can be obtained for clusters having dimensions comparable to or smaller than the tip radius. Displacement is practically visible in real time and it can be started and stopped easily by adjusting only one parameter, the tip amplitude oscillation. Analysing the energy dissipation signal at the onset of nanocluster sliding we evaluated a detachment threshold energy as a function of temperature in the range 300-413 K. We also analysed single cluster thermal induced displacement and combining this delicate procedure with AFM forced movement behaviour we conclude that detachment threshold energy is directly related to the activation energy of nanocluster diffusion and it scales linearly with temperature as expected for a single-particle thermally activated process.

  20. Accurate Calibration and Uncertainty Estimation of the Normal Spring Constant of Various AFM Cantilevers

    PubMed Central

    Song, Yunpeng; Wu, Sen; Xu, Linyan; Fu, Xing

    2015-01-01

    Measurement of force on a micro- or nano-Newton scale is important when exploring the mechanical properties of materials in the biophysics and nanomechanical fields. The atomic force microscope (AFM) is widely used in microforce measurement. The cantilever probe works as an AFM force sensor, and the spring constant of the cantilever is of great significance to the accuracy of the measurement results. This paper presents a normal spring constant calibration method with the combined use of an electromagnetic balance and a homemade AFM head. When the cantilever presses the balance, its deflection is detected through an optical lever integrated in the AFM head. Meanwhile, the corresponding bending force is recorded by the balance. Then the spring constant can be simply calculated using Hooke’s law. During the calibration, a feedback loop is applied to control the deflection of the cantilever. Errors that may affect the stability of the cantilever could be compensated rapidly. Five types of commercial cantilevers with different shapes, stiffness, and operating modes were chosen to evaluate the performance of our system. Based on the uncertainty analysis, the expanded relative standard uncertainties of the normal spring constant of most measured cantilevers are believed to be better than 2%. PMID:25763650

  1. [AFM-based technologies as the way towards the reverse Avogadro number].

    PubMed

    Pleshakova, T O; Shumov, I D; Ivanov, Yu D; Malsagova, K A; Kaysheva, A L; Archakov, A I

    2015-01-01

    Achievement of the concentration detection limit for proteins at the level of the reverse Avogadro number determines the modern development of proteomics. In this review, the possibility of approximating the reverse Avogadro number by using nanotechnological methods (AFM-based fishing with mechanical and electrical stimulation, nanowire detectors, and other methods) are discussed. The ability of AFM to detect, count, visualize and characterize physico-chemical properties of proteins at concentrations up to 10(-17)-10(-18) M is demonstrated. The combination of AFM-fishing with mass-spectrometry allows the identification of proteins not only in pure solutions, but also in multi-component biological fluids (serum). The possibilities to improve the biospecific fishing efficiency by use of SOMAmers in both AFM and nanowire systems are discussed. The paper also provides criteria for evaluation of the sensitivity of fishing-based detection systems. The fishing efficiency depending on the detection system parameters is estimated. The practical implementation of protein fishing depending on the ratio of the sample solution volume and the surface of the detection system is discussed. The advantages and disadvantages of today's promising nanotechnological protein detection methods implemented on the basis of these schemes. PMID:25978390

  2. Afm Measrurements of Martian Soil Particles Using Mems Technology - Results from the PHOENIX Mission

    NASA Astrophysics Data System (ADS)

    Gautsch, S.; Parrat, D.; de Rooij, N. F.; Staufer, U.; Morookian, J. M.; Hecht, M. H.; Vijendran, S.; Sykulska, H.; Pike, W. T.

    2011-12-01

    Light scattering experiments conducted on Mars indicated that soil particles have dimensions around 1 μm. Particles in that range play an important role in the gas exchange between sub-surface water ice and the atmosphere. Their shape can help tracing the geological history and may indicate past presence of liquid water. NASA's Phoenix mission therefore decided to analyze soil and dust particles in the sub-micrometer to a few micrometer range using an atomic force microscope (AFM) for the first time on another planet. The co-axially mounted AFM was capable of resolving particles with 10nm lateral resolution. A MEMS approach combined with mechatronic concepts for the scanner was selected for implementing the AFM. For redundancy, the sensor chip featured eight silicon cantilevers each with a 7 to 8 μm high tip. The cantilevers could be cleaved off if contaminated. During NASA's Phoenix Mission, which operated on the red planet from May to October 2008, we could demonstrate successful AFM operations. The instrument has executed 85 experiments of which 26 were needed for calibration. Of the remaining experiments about half (28) returned images where signatures of particles could be discerned.

  3. Single-Molecule Studies of Integrins by AFM-Based Force Spectroscopy on Living Cells

    NASA Astrophysics Data System (ADS)

    Eibl, Robert H.

    The characterization of cell adhesion between two living cells at the single-molecule level, i.e., between one adhesion receptor and its counter-receptor, appears to be an experimental challenge. Atomic force microscopy (AFM) can be used in its force spectroscopy mode to determine unbinding forces of a single pair of adhesion receptors, even with a living cell as a probe. This chapter provides an overview of AFM force measurements of the integrin family of cell adhesion receptors and their ligands. A focus is given to major integrins expressed on leukocytes, such as lymphocyte function-associated antigen 1 (LFA-1) and very late antigen 4 (VLA-4). These receptors are crucial for leukocyte trafficking in health and disease. LFA-1 and VLA-1 can be activated within the bloodstream from a low-affinity to a high-affinity receptor by chemokines in order to adhere strongly to the vessel wall before the receptor-bearing leukocytes extravasate. The experimental considerations needed to provide near-physiological conditions for a living cell and to be able to measure adequate forces at the single-molecule level are discussed in detail. AFM technology has been developed into a modern and extremely sensitive tool in biomedical research. It appears now that AFM force spectroscopy could enter, within a few years, medical applications in diagnosis and therapy of cancer and autoimmune diseases.

  4. Effective AFM cantilever tip size: methods for in-situ determination

    NASA Astrophysics Data System (ADS)

    Maragliano, Carlo; Glia, Ayoub; Stefancich, Marco; Chiesa, Matteo

    2015-01-01

    In atomic force microscopy (AFM) investigations, knowledge of the cantilever tip radius R is essential for the quantitative interpretation of experimental observables. Here we propose two techniques to rapidly quantify in-situ the effective tip radius of AFM probes. The first method is based on the strong dependency of the minimum value of the free amplitude required to observe a sharp transition from attractive to repulsive force regimes on the AFM probe radius. Specifically, the sharper the tip, the smaller the value of free amplitude required to observe such a transition. The key trait of the second method is to treat the tip-sample system as a capacitor. Provided with an analytical model that takes into account the geometry of the tip-sample’s capacitance, one can quantify the effective size of the tip apex fitting the experimental capacitance versus distance curve. Flowchart-like algorithms, easily implementable on any hardware, are provided for both methods, giving a guideline to AFM practitioners. The methods’ robustness is assessed over a wide range of probes of different tip radii R (i.e. 4 < R < 50 nm) and geometries. Results obtained from both methods are compared with the nominal values given by manufacturers and verified by acquiring scanning electron microscopy images. Our observations show that while both methods are reliable and robust over the range of tip sizes tested, the critical amplitude method is more accurate for relatively sharp tips (4 nm < R < 10 nm).

  5. First-principles AFM image simulation with frozen density embedding theory

    NASA Astrophysics Data System (ADS)

    Sakai, Yuki; Lee, Alex J.; Chelikowsky, James R.

    We present efficient first-principles method of non-contact atomic force microscopy (nc-AFM). Ordinary nc-AFM simulations based on density functional theory (DFT) require exhaustive computational cost because it involves thousands of total energy calculations. Regarding the sample as a fixed external potential can reduce the computational cost, and we adopt frozen density embedding theory (FDET) for this purpose. Simulated nc-AFM images with FDET using a carbon monoxide tip well reproduces the full DFT images of benzene, pentacene, and graphene, although optimized tip-sample distances and interaction energies in FDET are underestimated and overestimated, respectively. The FDET-based simulation method is promising for AFM image simulation of surfaces and two-dimensional materials. This work was supported by U.S. DOE under Grant No. DE-FG02-06ER46286 and Award No. DE-SC0008877, and by Welch Foundation under Grant F-1837. Computational resources are provided by NERSC and TACC.

  6. CDSEM AFM hybrid metrology for the characterization of gate-all-around silicon nano wires

    NASA Astrophysics Data System (ADS)

    Levi, Shimon; Schwarzband, Ishai; Weinberg, Yakov; Cornell, Roger; Adan, Ofer; Cohen, Guy M.; Gignac, Lynne; Bangsaruntip, Sarunya; Hand, Sean; Osborne, Jason; Feinstein, Adam

    2014-04-01

    In an ongoing study of the physical characterization of Gate-All-Around Silicon Nano Wires (GAASiNW), we found that the thin, suspended wires are prone to buckling as a function of their length and diameter. This buckling takes place between the fixed source and drain regions of the suspended wire, and can affect the device performance and therefore must be studied and controlled. For cylindrical SiNW, theory predicts that buckling has no directional preference. However, 3D CDSEM measurement results indicated that cylindrical wires prefer to buckle towards the wafer. To validate these results and to determine if the electron beam or charging is affecting our observations, we used 3D-AFM measurements to evaluate the buckling. To assure that the CDSEM and 3D-AFM measure the exact same locations, we developed a design based recipe generation approach to match the 3D-AFM and CDSEM coordinate systems. Measuring the exact same sites enables us to compare results and use 3D-AFM data to optimize CDSEM models. In this paper we will present a hybrid metrology approach to the characterization of GAASiNW for sub-nanometer variations, validating experimental results, and proposing methods to improve metrology capabilities.

  7. Use of anodic stripping voltammetry to determine zinc(II), lead(II), and copper(II) in foods

    SciTech Connect

    Maksimkina, L.M.; Gus'kova, V.P.

    1988-01-20

    The existing standard procedure for the polarographic determination of Zn, Pb, and Cu, based on the cathodic polarization of a dropping mercury electrode, is laborious and time-consuming and allows one to determine the above-mentioned trace elements only when they are separated beforehand. We consider the possibility of using anodic stripping voltammetry with a mercury film electrode for the simultaneous determination of Zn(II), Pb(II), and Cu(II) in foods.

  8. Implications of the contact radius to line step (CRLS) ratio in AFM for nanotribology measurements.

    PubMed

    Helt, James M; Batteas, James D

    2006-07-01

    Investigating the mechanisms of defect generation and growth at surfaces on the nanometer scale typically requires high-resolution tools such as the atomic force microscope (AFM). To accurately assess the kinetics and activation parameters of defect production over a wide range of loads (F(z)), the AFM data should be properly conditioned. Generally, AFM wear trials are performed over an area defined by the length of the slow (L(sscan)) and fast scan axes. The ratio of L(sscan) to image resolution (res, lines per image) becomes an important experimental parameter in AFM wear trials because it defines the magnitude of the line step (LS = L(sscan)/res), the distance the AFM tip steps along the slow scan axis. Comparing the contact radius (a) to the line step (LS) indicates that the overlap of successive scans will result unless the contact radius-line step ratio (CRLS) is < or =(1)/(2). If this relationship is not considered, then the scan history (e.g., contact frequency) associated with a single scan is not equivalent at different loads owing to the scaling of contact radius with load (a proportional variant F(z)(1/3)). Here, we present a model in conjunction with empirical wear tests on muscovite mica to evaluate the effects of scan overlap on surface wear. Using the Hertz contact mechanics definition of a, the CRLS model shows that scan overlap pervades AFM wear trials even under low loads. Such findings indicate that simply counting the number of scans (N(scans)) in an experiment underestimates the full history conveyed to the surface by the tip and translates into an error in the actual extent to which a region on the surface is contacted. Utilizing the CRLS method described here provides an approach to account for image scan history accurately and to predict the extent of surface wear. This general model also has implications for any AFM measurement where one wishes to correlate scan-dependent history to image properties as well as feature resolution in scanned

  9. Characterization of Local Mechanical Properties of Polymer Thin Films and Polymer Nanocomposites via AFM indentations

    NASA Astrophysics Data System (ADS)

    Cheng, Xu

    AFM indentation has become a tool with great potential in the characterization of nano-mechanical properties of materials. Thanks to the nanometer sized probes, AFM indentation is capable of capturing the changes of multiple properties within the range of tens of nanometers, such task would otherwise be difficult by using other experiment instruments. Despite the great potentials of AFM indentation, it operates based on a simple mechanism: driving the delicate AFM probe to indent the sample surface, and recording the force-displacement response. With limited information provided by AFM indentation, efforts are still required for any practice to successfully extract the desired nano-scale properties from specific materials. In this thesis, we focus on the mechanical properties of interphase between polymer and inorganic materials. It is known that in nanocomposites, a region of polymer exist around nanoparticles with altered molecular structures and improved properties, which is named as interphase polymer. The system with polymer thin films and inorganic material substrates is widely used to simulate the interphase effect in nanocomposites. In this thesis, we developed an efficient and reliable method to process film/substrate samples and characterize the changes of local mechanical properties inside the interphase region with ultra-high resolution AFM mechanical mapping technique. Applying this newly developed method, the interphase of several film/substrate pairs were examined and compared. The local mechanical properties on the other side of the polymer thin film, the free surface side, was also investigated using AFM indentation equipped with surface modified probes. In order to extract the full spectrum of local elastic modulus inside the surface region in the range of only tens of nanometers, the different contact mechanics models were studied and compared, and a Finite Element model was also established. Though the film/substrate system has been wide used as

  10. Femtomolar Detection of Silver Nanoparticles by Flow-Enhanced Direct-Impact Voltammetry at a Microelectrode Array

    PubMed Central

    2016-01-01

    We report the femtomolar detection of silver (Ag) nanoparticles by direct-impact voltammetry. This is achieved through the use of a random array of microelectrodes (RAM) integrated into a purpose-built flow cell, allowing combined diffusion and convection to the electrode surface. A coupled RAM-flow cell system is implemented and is shown to give reproducible wall-jet type flow characteristics, using potassium ferrocyanide as a molecular redox species. The calibrated flow system is then used to detect and quantitatively size Ag nanoparticles at femtomolar concentrations. Under flow conditions, it is found the nanoparticle impact frequency increases linearly with the volumetric flow rate. The resulting limit of detection is more than 2 orders of magnitude smaller than the previous detection limit for direct-impact voltammetry (900 fM) [J. Ellison et al. Sens. Actuators, B2014, 200, 47], and is more than 30 times smaller than the previous detection limit for mediated-impact voltammetry (83 fM) [T. M. Alligrant et al. Langmuir2014, 30, 13462]. PMID:27494652

  11. Femtomolar Detection of Silver Nanoparticles by Flow-Enhanced Direct-Impact Voltammetry at a Microelectrode Array.

    PubMed

    Sokolov, Stanislav V; Bartlett, Thomas R; Fair, Peter; Fletcher, Stephen; Compton, Richard G

    2016-09-01

    We report the femtomolar detection of silver (Ag) nanoparticles by direct-impact voltammetry. This is achieved through the use of a random array of microelectrodes (RAM) integrated into a purpose-built flow cell, allowing combined diffusion and convection to the electrode surface. A coupled RAM-flow cell system is implemented and is shown to give reproducible wall-jet type flow characteristics, using potassium ferrocyanide as a molecular redox species. The calibrated flow system is then used to detect and quantitatively size Ag nanoparticles at femtomolar concentrations. Under flow conditions, it is found the nanoparticle impact frequency increases linearly with the volumetric flow rate. The resulting limit of detection is more than 2 orders of magnitude smaller than the previous detection limit for direct-impact voltammetry (900 fM) [J. Ellison et al. Sens. Actuators, B 2014, 200, 47], and is more than 30 times smaller than the previous detection limit for mediated-impact voltammetry (83 fM) [T. M. Alligrant et al. Langmuir 2014, 30, 13462]. PMID:27494652

  12. Quasi-steady-state voltammetry of rapid electron transfer reactions at the macroscopic substrate of the scanning electrochemical microscope.

    PubMed

    Nioradze, Nikoloz; Kim, Jiyeon; Amemiya, Shigeru

    2011-02-01

    We report on a novel theory and experiment for scanning electrochemical microscopy (SECM) to enable quasi-steady-state voltammetry of rapid electron transfer (ET) reactions at macroscopic substrates. With this powerful approach, the substrate potential is cycled widely across the formal potential of a redox couple while the reactant or product of a substrate reaction is amperometrically detected at the tip in the feedback or substrate generation/tip collection mode, respectively. The plot of tip current versus substrate potential features the retraceable sigmoidal shape of a quasi-steady-state voltammogram although a transient voltammogram is obtained at the macroscopic substrate. Finite element simulations reveal that a short tip-substrate distance and a reversible substrate reaction (except under the tip) are required for quasi-steady-state voltammetry. Advantageously, a pair of quasi-steady-state voltammograms is obtained by employing both operation modes to reliably determine all transport, thermodynamic, and kinetic parameters as confirmed experimentally for rapid ET reactions of ferrocenemethanol and 7,7,8,8-tetracyanoquinodimethane at a Pt substrate with ∼0.5 μm-radius Pt tips positioned at 90 nm-1 μm distances. Standard ET rate constants of ∼7 cm/s were obtained for the latter mediator as the largest determined for a substrate reaction by SECM. Various potential applications of quasi-steady-state voltammetry are also proposed. PMID:21175129

  13. Quasi-Steady-State Voltammetry of Rapid Electron Transfer Reactions at the Macroscopic Substrate of the Scanning Electrochemical Microscope

    PubMed Central

    Nioradze, Nikoloz; Kim, Jiyeon; Amemiya, Shigeru

    2011-01-01

    We report on novel theory and experiment for scanning electrochemical microscopy (SECM) to enable quasi-steady-state voltammetry of rapid electron transfer (ET) reactions at macroscopic substrates. With this powerful approach, substrate potential is cycled widely across the formal potential of a redox couple while the reactant or product of a substrate reaction is amperometrically detected at the tip in the feedback or substrate generation/tip collection mode, respectively. The plot of tip current versus substrate potential features the retraceable sigmoidal shape of a quasi-steady-state voltammogram although a transient voltammogram is obtained at the macroscopic substrate. Finite element simulations reveal that a short tip–substrate distance and a reversible substrate reaction (except under the tip) are required for quasi-steady-state voltammetry. Advantageously, a pair of quasi-steady-state voltammograms is obtained by employing both operation modes to reliably determine all transport, thermodynamic, and kinetic parameters as confirmed experimentally for rapid ET reactions of ferrocenemethanol and 7,7,8,8-tetracyanoquinodimethane at a Pt substrate with ∼0.5-μm-radius Pt tips positioned at 90 nm–1 μm distances. Standard ET rate constants of ∼7 cm/s were obtained for the latter mediator as the largest determined for a substrate reaction by SECM. The various potential applications of quasi-steady-state voltammetry are also proposed. PMID:21175129

  14. Asymmetric catalytic aziridination of cyclic enones.

    PubMed

    De Vincentiis, Francesco; Bencivenni, Giorgio; Pesciaioli, Fabio; Mazzanti, Andrea; Bartoli, Giuseppe; Galzerano, Patrizia; Melchiorre, Paolo

    2010-07-01

    The first catalytic method for the asymmetric aziridination of cyclic enones is described. The presented organocatalytic strategy is based on the use of an easily available organocatalyst that is able to convert a wide range of cyclic enones into the desired aziridines with very high enantiomeric purity and good chemical yield. Such a method may very well open up new opportunities to stereoselectively prepare complex chiral molecules that possess an indane moiety, a framework that is found in a large number of bioactive and pharmaceutically important molecules. PMID:20512797

  15. Perturbations in bouncing and cyclic models

    NASA Astrophysics Data System (ADS)

    Biswas, Tirthabir; Mayes, Riley; Lattyak, Colleen

    2016-03-01

    Being able to reliably track perturbations across bounces and turnarounds in cyclic and bouncing cosmology lies at the heart of being able to compare the predictions of these models with the cosmic microwave background observations. This has been a challenging task due to the unknown nature of the physics involved during the bounce as well as the technical challenge of matching perturbations precisely between the expansion and contraction phases. In this paper, we present some general techniques (analytical and numerical) that can be applied to understand the physics of the fluctuations, especially those with "long" wavelengths, and apply our techniques to nonsingular cosmological models such as the bounce inflation and cyclic inflation.

  16. Vasopressin treatment for cyclic antidepressant overdose.

    PubMed

    Barry, James David; Durkovich, David W; Williams, Saralyn R

    2006-07-01

    Due to neurotransmitter reuptake inhibition, peripheral alpha receptor blocking effects, and sodium channel blockade, severe cyclic antidepressant poisoning may lead to intractable hypotension. We report a case of severe amitriptyline toxicity, with hypotension unresponsive to direct alpha receptor agonists after pH manipulation, but improved with intravenous vasopressin. Vasopressin use in the setting of cyclic antidepressant toxicity has not been previously reported. Vasopressin may be a beneficial agent in the treatment of recalcitrant hypotension associated with poisoning or overdose. The anecdotal nature of this report must be emphasized and the use of vasopressin requires further research to define efficacy, dose, and potential side effects. PMID:16798158

  17. Generalized Coefficients for Hopf Cyclic Cohomology

    NASA Astrophysics Data System (ADS)

    Hassanzadeh, Mohammad; Kucerovsky, Dan; Rangipour, Bahram

    2014-09-01

    A category of coefficients for Hopf cyclic cohomology is defined. It is shown that this category has two proper subcategories of which the smallest one is the known category of stable anti Yetter-Drinfeld modules. The middle subcategory is comprised of those coefficients which satisfy a generalized SAYD condition depending on both the Hopf algebra and the (co)algebra in question. Some examples are introduced to show that these three categories are different. It is shown that all components of Hopf cyclic cohomology work well with the new coefficients we have defined.

  18. Cyclical rectal bleeding in colorectal endometriosis.

    PubMed

    Levitt, M D; Hodby, K J; van Merwyk, A J; Glancy, R J

    1989-12-01

    Three case reports of cyclical rectal bleeding in endometriosis affecting rectum and sigmoid colon emphasize the close relationship between such cyclical bleeding and intestinal endometriosis. The cause of bleeding, however, is still unclear. The predilection of endometriotic deposits for the outer layers of the bowel wall suggests that mucosal involvement is not a prerequisite for rectal bleeding. The frequent absence of identifiable intramural haemorrhage casts doubt on the premise that intestinal endometriotic deposits 'menstruate'. The cause may simply be a transient tear in normal mucosa due to swelling of an underlying endometriotic deposit at the time of menstruation. PMID:2597100

  19. Calibration of AFM cantilever stiffness: a microfabricated array of reflective springs.

    PubMed

    Cumpson, P J Peter J; Zhdan, Peter; Hedley, John

    2004-08-01

    Calibration of the spring constant of atomic force microscope (AFM) cantilevers is necessary for the measurement of nanonewton and piconewton forces, which are critical to analytical applications of AFM in the analysis of polymer surfaces, biological structures and organic molecules. We have developed a compact and easy-to-use reference standard for this calibration. The new artifact consists of an array of 12 dual spiral-cantilever springs, each supporting a mirrored polycrystalline silicon disc of 160 microm in diameter. These devices were fabricated by a three-layer polysilicon surface micromachining method, including a reflective layer of gold on chromium. We call such an array a Microfabricated Array of Reference Springs (MARS). These devices have a number of advantages. Cantilever calibration using this device is straightforward and rapid. The devices have very small inertia, and are therefore resistant to shock and vibration. This means they need no careful treatment except reasonably clean laboratory conditions. The array spans the range of spring constant from around 0.16 to 11 N/m important in AFM, allowing almost all contact-mode AFM cantilevers to be calibrated easily and rapidly. Each device incorporates its own discrete gold mirror to improve reflectivity. The incorporation of a gold mirror both simplifies calibration of the devices themselves (via Doppler velocimetry) and allows interferometric calibration of the AFM z-axis using the apparent periodicity in the force-distance curve before contact. Therefore, from a single force-distance curve, taking about one second to acquire, one can calibrate the cantilever spring constant and, optionally, the z-axis scale. These are all the data one needs to make accurate and reliable force measurements. PMID:15231316

  20. Enhancing the Electrochemical Behavior of Pure Copper by Cyclic Potentiodynamic Passivation: A Comparison between Coarse- and Nano-Grained Pure Copper

    NASA Astrophysics Data System (ADS)

    Fattah-alhosseini, Arash; Imantalab, Omid; Attarzadeh, Farid Reza

    2016-07-01

    Electrochemical behavior of coarse- and nano-grained pure copper were modified and improved to a large extent by the application of cyclic potentiodynamic passivation. The efficacy of this method was evaluated on the basis of grain size which is of great importance in corrosion studies. In this study, the eight passes of accumulative roll bonding process at room temperature were successfully performed to produce nano-grained pure copper. Transmission electron microscopy image indicated that the average grain size reached below 100 nm after eight passes. On the basis of cyclic voltammetry and also the electrochemical tests performed after that, it was revealed that cyclic potentiodynamic passivation had a significant improving effect on the passive behavior of both coarse- and nano-grained samples. In addition, a superior behavior of nano-grained sample in comparison to coarse-grained one was distinguished by its smaller cyclic voltammogram loops, nobler free potentials, larger capacitive arcs in the Nyquist plots, and less charge carrier densities within the passive film.

  1. High throughput nanofabrication of silicon nanowire and carbon nanotube tips on AFM probes by stencil-deposited catalysts.

    PubMed

    Engstrom, Daniel S; Savu, Veronica; Zhu, Xueni; Bu, Ian Y Y; Milne, William I; Brugger, Juergen; Boggild, Peter

    2011-04-13

    A new and versatile technique for the wafer scale nanofabrication of silicon nanowire (SiNW) and multiwalled carbon nanotube (MWNT) tips on atomic force microscope (AFM) probes is presented. Catalyst material for the SiNW and MWNT growth was deposited on prefabricated AFM probes using aligned wafer scale nanostencil lithography. Individual vertical SiNWs were grown epitaxially by a catalytic vapor-liquid-solid (VLS) process and MWNTs were grown by a plasma-enhanced chemical vapor (PECVD) process on the AFM probes. The AFM probes were tested for imaging micrometers-deep trenches, where they demonstrated a significantly better performance than commercial high aspect ratio tips. Our method demonstrates a reliable and cost-efficient route toward wafer scale manufacturing of SiNW and MWNT AFM probes. PMID:21446752

  2. Characterization of single 1.8-nm Au nanoparticle attachments on AFM tips for single sub-4-nm object pickup

    PubMed Central

    2013-01-01

    This paper presents a novel method for the attachment of a 1.8-nm Au nanoparticle (Au-NP) to the tip of an atomic force microscopy (AFM) probe through the application of a current-limited bias voltage. The resulting probe is capable of picking up individual objects at the sub-4-nm scale. We also discuss the mechanisms involved in the attachment of the Au-NP to the very apex of an AFM probe tip. The Au-NP-modified AFM tips were used to pick up individual 4-nm quantum dots (QDs) using a chemically functionalized method. Single QD blinking was reduced considerably on the Au-NP-modified AFM tip. The resulting AFM tips present an excellent platform for the manipulation of single protein molecules in the study of single protein-protein interactions. PMID:24237663

  3. Cyclic unequal error protection codes constructed from cyclic codes of composite length

    NASA Technical Reports Server (NTRS)

    Lin, Shu

    1987-01-01

    The distance structure of cyclic codes of composite length was investigated. A lower bound on the minimum distance for this class of codes is derived. In many cases, the lower bound gives the true minimum distance of a code. Then the distance structure of the direct sum of two cyclic codes of composite length were investigated. It was shown that, under certain conditions, the direct-sum code provides two levels of error correcting capability, and hence is a two-level unequal error protection (UEP) code. Finally, a class of two-level UEP cyclic direct-sum codes and a decoding algorithm for a subclass of these codes are presented.

  4. An Experimental Test of Phonemic Cyclicity.

    ERIC Educational Resources Information Center

    Gierut, Judith A.

    1996-01-01

    Evaluates the principle of laryngeal-supralaryngeal cyclicity by manipulating the domain cycle and phase relationship of the cycle as independent variables and by monitoring longitudinally the order of emergent phonemic distinctions in the sound systems of seven children with phonological delays as the dependent variable. Findings are discussed.…

  5. One pot solution synthesis of cyclic oligodeoxyribonucleotides.

    PubMed Central

    Capobianco, M L; Carcuro, A; Tondelli, L; Garbesi, A; Bonora, G M

    1990-01-01

    Several cyclic oligodeoxynucleotides with different base composition and size have been prepared from 5',3'-unprotected linear precursors, using a bifunctional phosphorylating reagent. The final deprotected oligomers have been characterized by 1H- and 31P-NMR. The present procedure is particularly useful for millimolar scale syntheses. PMID:2339055

  6. One pot solution synthesis of cyclic oligodeoxyribonucleotides.

    PubMed

    Capobianco, M L; Carcuro, A; Tondelli, L; Garbesi, A; Bonora, G M

    1990-05-11

    Several cyclic oligodeoxynucleotides with different base composition and size have been prepared from 5',3'-unprotected linear precursors, using a bifunctional phosphorylating reagent. The final deprotected oligomers have been characterized by 1H- and 31P-NMR. The present procedure is particularly useful for millimolar scale syntheses. PMID:2339055

  7. Scale invariant density perturbations from cyclic cosmology

    NASA Astrophysics Data System (ADS)

    Frampton, Paul Howard

    2016-04-01

    It is shown how quantum fluctuations of the radiation during the contraction era of a comes back empty (CBE) cyclic cosmology can provide density fluctuations which re-enter the horizon during the subsequent expansion era and at lowest order are scale invariant, in a Harrison-Zel’dovich-Peebles sense. It is necessary to be consistent with observations of large scale structure.

  8. Cyclic Cratonic Carbonates and Phanerozoic Calcite Seas.

    ERIC Educational Resources Information Center

    Wilkinson, Bruce H.

    1982-01-01

    Discusses causes of cyclicity in cratonic carbonate sequences and evidence for and potential significance of postulated primary calcite sediment components in past Paleozoic seas, outlining problems, focusing on models explaining existing data, and identifying background. Future sedimentary geologists will need to address these and related areas…

  9. Determination of molybdenum in steel by adsorptive stripping voltammetry in a homogeneous ternary solvent system.

    PubMed

    de Andrade, J C; de Almeida, A M; Coscione, A R; Aleixo, L M

    2001-06-01

    A new alternative approach for the determination of molybdenum in steel is proposed, using adsorptive stripping voltammetry (AdSV). The determinations are performed in a homogeneous ternary solvent system (HTSS) composed of N,N-dimethylformamide, ethanol and water, with alpha-benzoinoxime (alpha BO) as the complexing agent and a sodium acetate-acetic acid buffer as the support electrolyte. The HTSS composition was optimized by mixture design modelling. The AdSV measurements were performed in the differential pulse mode using an accumulation potential of -1050 mV. Under these optimized experimental conditions, the Mo(VI)-alpha BO reduction current peak potential is observed at potentials near -1250 mV, much lower than those usually reported, and the calibration plot follows the polynomial equation I = 0.359 + 0.265 [CMo(VI)] - 0.015 [CMo(IV)]2 (r2 = 0.997), for Mo concentrations up to 10.0 micrograms L-1. There is a linear range in this calibration plot for Mo(VI) concentrations up to 0.20 microgram L-1, defined by the equation I = 0.353 + 0.385 [CMo(VI)] (r2 = 0.980). In both cases, I is the absolute value for the current in microA and CMo(VI) is the concentration of Mo in microgram L-1. The detection limit for this linear concentration range was estimated as 20 pg L-1. A RSD of 0.43% is associated with the signals at a Mo(VI) level of 0.72 microgram L-1. From the common method-interfering species tested, only iron at Fe/Mo(VI) ratios above 500 and vanadium and tungsten at M/Mo(VI) ratios above 100 appear to affect the analytical response significantly. Phosphorous may also reduce the analytical signal at P/Mo(VI) ratios above 100, due to the formation of the competitive P-Mo complex. The suggested routine procedure was tested by analyzing four stainless steel samples and the results compared well with the ICP-AES measurements. The higher sensitivity of this method permits direct determination of Mo(VI) in steels, eliminating the need of analyte concentration or

  10. Electrochemical Genotoxicity Assay Based on a SOS/umu Test Using Hydrodynamic Voltammetry in a Droplet

    PubMed Central

    Kuramitz, Hideki; Sazawa, Kazuto; Nanayama, Yasuaki; Hata, Noriko; Taguchi, Shigeru; Sugawara, Kazuharu; Fukushima, Masami

    2012-01-01

    The SOS/umu genotoxicity assay evaluates the primary DNA damage caused by chemicals from the β-galactosidase activity of S. typhimurium. One of the weaknesses of the common umu test system based on spectrophotometric detection is that it is unable to measure samples containing a high concentration of colored dissolved organic matters, sediment, and suspended solids. However, umu tests with electrochemical detection techniques prove to be a better strategy because it causes less interference, enables the analysis of turbid samples and allows detection even in small volumes without loss of sensitivity. Based on this understanding, we aim to develop a new umu test system with hydrodynamic chronoamperometry using a rotating disk electrode (RDE) in a microliter droplet. PAPG when used as a substrate is not electroactive at the potential at which PAP is oxidized to p-quinone imine (PQI), so the current response of chronoamperometry resulting from the oxidation of PAP to PQI is directly proportional to the enzymatic activity of S. typhimurium. This was achieved by performing genotoxicity tests for 2-(2-furyl)-3-(5-nitro-2-furyl)-acrylamide (AF-2) and 2-aminoanthracene (2-AA) as model genotoxic compounds. The results obtained in this study indicated that the signal detection in the genotoxicity assay based on hydrodynamic voltammetry was less influenced by the presence of colored components and sediment particles in the samples when compared to the usual colorimetric signal detection. The influence caused by the presence of humic acids (HAs) and artificial sediment on the genotoxic property of selected model compounds such as 4-nitroquinoline-N-oxide (4-NQO), 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX), 1,8-dinitropyrene (1,8-DNP) and 1-nitropyrene (1-NP) were also investigated. The results showed that the genotoxicity of 1-NP and MX changed in the presence of 10 mg·L−1 HAs. The genotoxicity of tested chemicals with a high hydrophobicity such as 1,8-DNP

  11. Nanoscopic polypyrrole AFM-SECM probes enabling force measurements under potential control

    NASA Astrophysics Data System (ADS)

    Knittel, P.; Higgins, M. J.; Kranz, C.

    2014-01-01

    Conductive polymers, and in particular polypyrrole, are frequently used as biomimetic interfaces facilitating growth and/or differentiation of cells and tissues. Hence, studying forces and local interactions between such polymer interfaces and cells at the nanoscale is of particular interest. Frequently, such force interactions are not directly accessible with high spatial resolution. Consequently, we have developed nanoscopic polypyrrole electrodes, which are integrated in AFM-SECM probes. Bifunctional AFM-SECM probes were modified via ion beam-induced deposition resulting in pyramidal conductive Pt-C composite electrodes. These nanoscopic electrodes then enabled localized polypyrrole deposition, thus resulting in polymer-modified AFM probes with a well-defined geometry. Furthermore, such probes may be reversibly switched from an insulating to a conductive state. In addition, the hydrophilicity of such polymer tips is dependent on the dopant, and hence, on the oxidation state. Force studies applying different tip potentials were performed at plasma-treated glass surfaces providing localized information on the associated force interactions, which are dependent on the applied potential and the dopant.Conductive polymers, and in particular polypyrrole, are frequently used as biomimetic interfaces facilitating growth and/or differentiation of cells and tissues. Hence, studying forces and local interactions between such polymer interfaces and cells at the nanoscale is of particular interest. Frequently, such force interactions are not directly accessible with high spatial resolution. Consequently, we have developed nanoscopic polypyrrole electrodes, which are integrated in AFM-SECM probes. Bifunctional AFM-SECM probes were modified via ion beam-induced deposition resulting in pyramidal conductive Pt-C composite electrodes. These nanoscopic electrodes then enabled localized polypyrrole deposition, thus resulting in polymer-modified AFM probes with a well

  12. Cyclic hardening in copper described in terms of combined monotonic and cyclic stress-strain curves

    SciTech Connect

    Chandler, H.D. . School of Mechanical Engineering)

    1995-01-01

    Hardening of polycrystalline copper subjected to tension-compression loading cycles in the plastic region is discussed with reference to changes in flow stress determined from equations describing dislocation glide. It is suggested that hardening is as a result of the accumulation of strain on a monotonic stress-strain curve. On initial loading, the behavior is monotonic. On stress reversal, a characteristic cyclic stress-strain curve is followed until the stress reaches a value in reverse loading corresponding to the maximum attained during the preceding half cycle. Thereafter, the monotonic path is followed until strain reversal occurs at completion of the half cycle. Repetition of the process results in cyclic hardening. Steady state cyclic behavior is reached when a stress associated with the monotonic stress-strain curve is reached which is equal to the stress associated with the cyclic stress-strain curve corresponding to the imposed strain amplitude.

  13. Characterization of gold-thiol-8-hydroxyquinoline self-assembled monolayers for selective recognition of aluminum ion using voltammetry and electrochemical impedance spectroscopy.

    PubMed

    Shervedani, Reza Karimi; Rezvaninia, Zeinab; Sabzyan, Hassan; Boeini, Hassan Zali

    2014-05-12

    Gold electrode surface is modified via covalent attachment of a synthesized thiol functionalized with 8-hydroxyquinoline, p-((8-hydroxyquinoline)azo) benzenethiol (SHQ), for the first time. The behavior of the nanostructured electrode surface (Au-SHQ) is characterized by electrochemical techniques including cyclic and differential pulse voltammetry (CV and DPV), and electrochemical impedance spectroscopy (EIS). The modified surface is stable in a wide range of potentials and pHs. A surface pKa of 6.0±0.1 is obtained for Au-SHQ electrode using surface acid/base titration curves constructed by CV and EIS measurements as a function of pH. These results helped to determine the charge state of the surface as a function of pH. The gold modified electrode surface showed good affinity for sensing the Al(III) ion at pH 5.5. The sensing process is based on (i) accumulation and complex formation between Al(III) from the solution phase and 8HQ function on the Au electrode surface (recognition step) and (ii) monitoring the impedance of the Au-SHQ-Al(III) complex against redox reaction rate of parabenzoquinone (PBQ) (signal transduction step). The PBQ is found to be a more suitable probe for this purpose, after testing several others. Thus, the sensor was tested for quantitative determination of Al(III) from the solution phase. At the optimized conditions, a linear response, from 1.0×10(-11) to 1.2×10(-5) M Al(III) in semi-logarithmic scale, with a detection limit of 8.32×10(-12) M and mean relative standard deviation of 3.2% for n=3 at 1.0×10(-7) M Al(III) is obtained. Possible interferences from coexisting cations and anions are also studied. The results show that many ions do not interfere significantly with the sensor response for Al(III). Validity of the method and applicability of the sensor are successfully tested by determination of Al(III) in human blood serum samples. PMID:24767148

  14. Single Nanotube Voltammetry: Current Fluctuations Are Due to Physical Motion of the Nanotube

    PubMed Central

    2016-01-01

    Nanoimpacts of single palladium-coated carbon nanotubes on a gold substrate are studied to elucidate the origins of the fluctuation in the current–time response of the hydrogen oxidation reaction mediated at its surface. The chronoamperometric and cyclic voltammetric responses from a single nanotube immobilized on the gold surface were compared to analogous data on a carbon substrate to determine the possible influence of substrate material on the nanotube–electrode electrical contact. No significant distinction between the gold and carbon was found, indicating in light of the considerable differences in the substrate materials’ intrinsic electronic structures that it is the nanomotion of a nanotube at the electrode surface which is likely responsible for the observed current modulation. This nanomotion creates a varying contact resistance, to which the noise in the current–time signal of the mediated reaction is attributed. In addition, stochastic ex-situ adsorption of single nanotubes onto the gold electrode followed by careful drying of the electrode surface was found to drastically reduce the current fluctuation, again implying that a contact resistance arising from physical motion of the nanotube at the electrode is responsible for the modulation of current. PMID:27066159

  15. Comparison of voltammetry and inductively coupled plasma-mass spectrometry for the determination of heavy metals in PM 10 airborne particulate matter

    NASA Astrophysics Data System (ADS)

    Buzica, Daniela; Gerboles, Michel; Borowiak, Annette; Trincherini, Pier; Passarella, Rosanna; Pedroni, Valerio

    The potential of the voltammetry method was examined for the determination of heavy metals in ambient air particulate matter (PM 10) on quartz filter. Cd, Pb, Cu, Zn, As were determined by anodic stripping voltammetry while adsorptive stripping voltammetry was used for the analysis of Ni. The method detection limit of these metals were 9.3, 0.1, 0.8, 0.3, 0.4, 0.1 ng m -3 for Zn, Cd, Pb, Cu, Ni and As, respectively. In addition, the analysis of a Certified Reference Material NIST 1648, yielded recoveries between 92% and 103%. Consequently, both the detection limit and recovery of the voltammetric method satisfy the requirements of the European Standard for the analyses of heavy metals in PM 10 (EN 14902). A comparison of the inductively coupled plasma-mass spectrometry (ICP-MS) and voltammetry method on the NIST 1648 and PM 10 filters showed the differences between them remained well within the level of uncertainty on the NIST 1648 requested by European Directives for heavy metals (25% for Pb and 40% for As, Cd and Ni, respectively). In addition to its compliance with legislations, the voltammetry method benefits from low investment cost and the potential of complete automation. As such, one may expect voltammetry to provide a reliable alternative to the European laboratories in charge of ambient air monitoring at the time when the European Directives require to measure heavy metals in PM 10 on a regularly basis.

  16. Atom probe, AFM, and STM studies on vacuum-fired stainless steels.

    PubMed

    Stupnik, A; Frank, P; Leisch, M

    2009-04-01

    The surface morphology of grades 304L and 316LN stainless steels, after low-temperature bake-out process and vacuum annealing, has been studied by atomic force microscopy (AFM) and scanning tunnelling microscopy (STM). The local elemental composition on the surface before and after thermal treatment has been investigated by atom probe (AP) depth profiling measurements. After vacuum annealing, AFM and STM show significant changes in the surface structure and topology. Recrystallization and surface reconstruction is less pronounced on the 316LN stainless steel. AP depth profiling analyses result in noticeable nickel enrichment on the surface of grade 304L samples. Since hydrogen recombination is almost controlled by surface structure and composition, a strong influence on the outgassing behaviour by the particular surface microstructure can be deduced. PMID:19167824

  17. Pattern formation and control in polymeric systems: From Minkowski measures to in situ AFM imaging

    NASA Astrophysics Data System (ADS)

    Jacobs, Karin

    2014-03-01

    Thin liquid polymer films are not only of great technical importance, they also exhibit a variety of dynamical instabilities. Some of them may be desired, some rather not. To analyze and finally control pattern formation, modern thin film theories are as vital as techniques to characterize the morphologies and structures in and on the films. Examples for the latter are atomic force microscopy (AFM) as well as scattering techniques. The talk will introduce into the practical applications of Minkowski measures to characterize patterns and explain what thin film properties (e.g. capillary number, solid/liquid boundary condition, glass transition temperature, chain mobility) can further be extracted including new technical possibilities by AFM and scattering techniques.

  18. Carbon nanotube/carbon nanotube composite AFM probes prepared using ion flux molding

    NASA Astrophysics Data System (ADS)

    Chesmore, Grace; Roque, Carrollyn; Barber, Richard

    The performance of carbon nanotube-carbon nanotube composite (CNT/CNT composite) atomic force microscopy (AFM) probes is compared to that of conventional Si probes in AFM tapping mode. The ion flux molding (IFM) process, aiming an ion beam at the CNT probe, aligns the tip to a desired angle. The result is a relatively rigid tip that is oriented to offset the cantilever angle. Scans using these probes reveal an improvement in image accuracy over conventional tips, while allowing higher aspect ratio imaging of 3D surface features. Furthermore, the lifetimes of CNT-CNT composite tips are observed to be longer than both conventional tips and those claimed for other CNT technologies. Novel applications include the imaging of embiid silk. Supported by the Clare Boothe Luce Research Scholars Award and Carbon Design Innovations.

  19. Cell mechanics as a marker for diseases: Biomedical applications of AFM

    NASA Astrophysics Data System (ADS)

    Rianna, Carmela; Radmacher, Manfred

    2016-08-01

    Many diseases are related to changes in cell mechanics. Atomic Force Microscopy (AFM) is one of the most suitable techniques allowing the investigation of both topography and mechanical properties of adherent cells with high spatial resolution under physiological conditions. Over the years the use of this technique in medical and clinical applications has largely increased, resulting in the notion of cell mechanics as a biomarker to discriminate between different physiological and pathological states of cells. Cell mechanics has proven to be a biophysical fingerprint able discerning between cell phenotypes, unraveling processes in aging or diseases, or even detecting and diagnosing cellular pathologies. We will review in this report some of the works on cell mechanics investigated by AFM with clinical and medical relevance in order to clarify the state of research in this field and to highlight the role of cell mechanics in the study of pathologies, focusing on cancer, blood and cardiovascular diseases.

  20. Mapping real-time images of high-speed AFM using multitouch control

    NASA Astrophysics Data System (ADS)

    Carberry, D. M.; Picco, L.; Dunton, P. G.; Miles, M. J.

    2009-10-01

    Conventional AFM is highly restricted by its scan rate, a problem that has been overcome by the development of high-speed AFM systems. As the technology to produce higher scan rates has developed it has pushed forward the design of control software. However, the user interface has not evolved at the same rate, limiting the user to sequential control steps. In this paper we demonstrate the integration of HSAFM with a multitouch interface to produce a highly intuitive and responsive control environment. This enables nanometre resolution to be maintained whilst scanning the sample over tens of microns, and arbitrary paths to be traversed. We illustrate this by scanning around two chromosomes in water, before scanning on top of the chromosome, showing the surface structure.

  1. AFM method to detect differences in adhesion of silica bids to cancer and normal epithelial cells

    NASA Astrophysics Data System (ADS)

    Sokolov, Igor; Iyer, Swaminathan; Gaikwad, Ravi; Woodworth, Craig

    2009-03-01

    To date, the methods of detection of cancer cells have been mostly based on traditional techniques used in biology, such as visual identification of malignant changes, cell growth analysis, specific ligand-receptor labeling, or genetic tests. Despite being well developed, these methods are either insufficiently accurate or require a lengthy complicated analysis. A search for alternative methods for the detection of cancer cells may be a fruitful approach. Here we describe an AFM study that may result in a new method for detection of cancer cells in vitro. Here we use atomic force microscopy (AFM) to study adhesion of single silica beads to malignant and normal cells cultured from human cervix. We found that adhesion depends on the time of contact, and can be statistically different for malignant and normal cells. Using these data, one could develop an optical method of cancer detection based on adhesion of various silica beads.

  2. Mode coupling in a hanging-fiber AFM used as a rheological probe

    NASA Astrophysics Data System (ADS)

    Devailly, C.; Laurent, J.; Steinberger, A.; Bellon, L.; Ciliberto, S.

    2014-06-01

    We analyze the advantages and drawbacks of a method which measures the viscosity of liquids at microscales, using a thin glass fiber fixed on the tip of a cantilever of an ultra-low-noise Atomic Force Microscope (AFM). When the fiber is dipped into a liquid, the dissipation of the cantilever-fiber system, which is linked to the liquid viscosity, can be computed from the power spectral density of the thermal fluctuations of the cantilever deflection. The high sensitivity of the AFM allows us to show the existence and to develop a model of the coupling between the dynamics of the fiber and that of the cantilever. This model, which accurately fits the experimental data, gives also more insights into the dynamics of coupled microdevices in a viscous environment.

  3. Study of relaxation and transport processes by means of AFM based dielectric spectroscopy

    SciTech Connect

    Miccio, Luis A.

    2014-05-15

    Since its birth a few years ago, dielectric spectroscopy studies based on atomic force microscopy (AFM) have gained a growing interest. Not only the frequency and temperature ranges have become broader since then but also the kind of processes that can be studied by means of this approach. In this work we analyze the most adequate experimental setup for the study of several dielectric processes with a spatial resolution of a few nanometers by using force mode AFM based dielectric spectroscopy. Proof of concept experiments were performed on PS/PVAc blends and PMMA homopolymer films, for temperatures ranging from 300 to 400 K. Charge transport processes were also studied by this approach. The obtained results were analyzed in terms of cantilever stray contribution, film thickness and relaxation strength. We found that the method sensitivity is strongly coupled with the film thickness and the relaxation strength, and that it is possible to control it by using an adequate experimental setup.

  4. Temperature Dependence Study of Noncontact Afm Images Using Molecular Dynamics Simulations

    NASA Astrophysics Data System (ADS)

    Nejat Pishkenari, Hossein; Meghdari, Ali

    The effect of temperature on the noncontact atomic force microscopy (NC-AFM) surface imaging is investigated with the aid of molecular dynamics (MD) analysis based on the Sutton-Chen (SC) interatomic potential. Particular attention is devoted to the tip and sample flexibility at different temperatures. When a gold coated probe is brought close to the Au (001) surface at high temperatures, the tip and surface atoms are pulled together and their distance becomes smaller. The tip and sample atoms displacement varies in the different environment temperatures and this leads to the different interaction forces. Along this line, to study the effect of temperature on the resulting images, we have employed the well-known NC-AFM model and carried out realistic non-equilibrium MD 3D simulations of atomic scale imaging at different close approach positions to the surface.

  5. AFM imaging reveals the tetrameric structure of the TRPM8 channel

    SciTech Connect

    Stewart, Andrew P.; Egressy, Kinga; Lim, Annabel; Edwardson, J. Michael

    2010-04-02

    Several members of the transient receptor potential (TRP) channel superfamily have been shown to assemble as tetramers. Here we have determined the subunit stoichiometry of the transient receptor potential M8 (TRPM8) channel using atomic force microscopy (AFM). TRPM8 channels were isolated from transfected cells, and complexes were formed between the channels and antibodies against a V5 epitope tag present on each subunit. The complexes were then subjected to AFM imaging. A frequency distribution of the molecular volumes of antibody decorated channels had a peak at 1305 nm{sup 3}, close to the expected size of a TRPM8 tetramer. The frequency distribution of angles between pairs of bound antibodies had two peaks, at 93{sup o} and 172{sup o}, confirming that the channel assembles as a tetramer. We suggest that this assembly pattern is common to all members of the TRP channel superfamily.

  6. Controlled nanodot fabrication by rippling polycarbonate surface using an AFM diamond tip

    PubMed Central

    2014-01-01

    The single scratching test of polymer polycarbonate (PC) sample surface using an atomic force microscope (AFM) diamond tip for fabricating ripple patterns has been studied with the focus on the evaluation of the effect of the tip scratching angle on the pattern formation. The experimental results indicated that the different oriented ripples can be easily machined by controlling the scratching angles of the AFM. And, the effects of the normal load and the feed on the ripples formation and their periods were also studied. Based on the ripple pattern formation, we firstly proposed a two-step scratching method to fabricate controllable and oriented complex three-dimensional (3D) nanodot arrays. These typical ripple formations can be described via a stick-slip and crack formation process. PMID:25114660

  7. AFM Imaging of Mercaptobenzoic Acid on Au(110): Submolecular Contrast with Metal Tips.

    PubMed

    Hauptmann, Nadine; Robles, Roberto; Abufager, Paula; Lorente, Nicolas; Berndt, Richard

    2016-06-01

    A self-assembled monolayer of mercaptobenzoic acid (MBA) on Au(110) is investigated with scanning tunneling and atomic force microscopy (STM and AFM) and density functional calculations. High-resolution AFM images obtained with metallic tips show clear contrasts between oxygen atoms and phenyl moieties. The contrast above the oxygen atoms is due to attractive covalent interactions, which is different than previously reported high-resolution images, where Pauli repulsion dominated the image contrast. We show that the bonding of MBA to the substrate occurs mainly through dispersion interactions, whereas the thiol-Au bond contributes only a quarter of the adsorption energy. No indication of Au adatoms mediating the thiol-Au interaction was found in contrast to other thiol-bonded systems. However, MBA lifts the Au(110)-(2 × 1) reconstruction. PMID:27183144

  8. Molecular Dynamic Simulations of Interaction of an AFM Probe with the Surface of an SCN Sample

    NASA Technical Reports Server (NTRS)

    Bune, Adris; Kaukler, William; Rose, M. Franklin (Technical Monitor)

    2001-01-01

    Molecular dynamic (MD) simulations is conducted in order to estimate forces of probe-substrate interaction in the Atomic Force Microscope (AFM). First a review of available molecular dynamic techniques is given. Implementation of MD simulation is based on an object-oriented code developed at the University of Delft. Modeling of the sample material - succinonitrile (SCN) - is based on the Lennard-Jones potentials. For the polystyrene probe an atomic interaction potential is used. Due to object-oriented structure of the code modification of an atomic interaction potential is straight forward. Calculation of melting temperature is used for validation of the code and of the interaction potentials. Various fitting parameters of the probe-substrate interaction potentials are considered, as potentials fitted to certain properties and temperature ranges may not be reliable for the others. This research provides theoretical foundation for an interpretation of actual measurements of an interaction forces using AFM.

  9. Conservative and dissipative tip-sample interaction forces probed with dynamic AFM

    NASA Astrophysics Data System (ADS)

    Gotsmann, B.; Seidel, C.; Anczykowski, B.; Fuchs, H.

    1999-10-01

    The conservative and dissipative forces between tip and sample of a dynamic atomic force microscopy (AFM) were investigated using a combination of computer simulations and experimental AFM data obtained by the frequency modulation technique. In this way it became possible to reconstruct complete force versus distance curves and damping coefficient versus distance curves from experimental data without using fit parameters for the interaction force and without using analytical interaction models. A comparison with analytical approaches is given and a way to determine a damping coefficient curve from experimental data is proposed. The results include the determination of the first point of repulsive contact of a vibrating tip when approaching a sample. The capability of quantifying the tip-sample interaction is demonstrated using experimental data obtained with a silicon tip and a mica sample in UHV.

  10. Force-controlled manipulation of single cells: from AFM to FluidFM.

    PubMed

    Guillaume-Gentil, Orane; Potthoff, Eva; Ossola, Dario; Franz, Clemens M; Zambelli, Tomaso; Vorholt, Julia A

    2014-07-01

    The ability to perturb individual cells and to obtain information at the single-cell level is of central importance for addressing numerous biological questions. Atomic force microscopy (AFM) offers great potential for this prospering field. Traditionally used as an imaging tool, more recent developments have extended the variety of cell-manipulation protocols. Fluidic force microscopy (FluidFM) combines AFM with microfluidics via microchanneled cantilevers with nano-sized apertures. The crucial element of the technology is the connection of the hollow cantilevers to a pressure controller, allowing their operation in liquid as force-controlled nanopipettes under optical control. Proof-of-concept studies demonstrated a broad spectrum of single-cell applications including isolation, deposition, adhesion and injection in a range of biological systems. PMID:24856959

  11. BOREAS AFM-5 Level-2 Upper Air Network Standard Pressure Level Data

    NASA Technical Reports Server (NTRS)

    Barr, Alan; Hrynkiw, Charmaine; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The BOREAS AFM-5 team collected and processed data from the numerous radiosonde flights during the project. The goals of the AFM-05 team were to provide large-scale definition of the atmosphere by supplementing the existing AES aerological network, both temporally and spatially. This data set includes basic upper-air parameters interpolated at 0.5 kiloPascal increments of atmospheric pressure from data collected from the network of upper-air stations during the 1993, 1994, and 1996 field campaigns over the entire study region. The data are contained in tabular ASCII files. The data files are available on a CD-ROM (see document number 20010000884) or from the Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC).

  12. Probing of local dissolution of Al-alloys in chloride solutions by AFM and SECM

    NASA Astrophysics Data System (ADS)

    Davoodi, A.; Pan, J.; Leygraf, C.; Norgren, S.

    2006-05-01

    Local dissolution of Al alloys was probed in situ in chloride solutions by using atomic force microscopy (AFM) and scanning electrochemical microscopy (SECM). Preferential dissolution in the boundary region between some intermetallic particles (IMPs) and alloy matrix, and trench formation around large IMPs during free immersion and under electrochemical anodic polarization were observed, which indicate different dissolution behavior associated to different types of IMPs. Moreover, by using an integrated AFM/SECM system with a dual mode cantilever/microelectrode probe, simultaneous probing of electrochemical active sites and topographic changes over the same area was performed with sub-micron resolution. This allowed the ongoing localized corrosion processes related to the IMP to be revealed.

  13. Development of a novel nanoindentation technique by utilizing a dual-probe AFM system

    PubMed Central

    Sahin, Ferat; Yablon, Dalia

    2015-01-01

    Summary A novel instrumentation approach to nanoindentation is described that exhibits improved resolution and depth sensing. The approach is based on a multi-probe scanning probe microscopy (SPM) tool that utilizes tuning-fork based probes for both indentation and depth sensing. Unlike nanoindentation experiments performed with conventional AFM systems using beam-bounce technology, this technique incorporates a second probe system with an ultra-high resolution for depth sensing. The additional second probe measures only the vertical movement of the straight indenter attached to a tuning-fork probe with a high spring constant and it can also be used for AFM scanning to obtain an accurate profiling. Nanoindentation results are demonstrated on silicon, fused silica, and Corning Eagle Glass. The results show that this new approach is viable in terms of accurately characterizing mechanical properties of materials through nanoindentation with high accuracy, and it opens doors to many other exciting applications in the field of nanomechanical characterization. PMID:26665072

  14. AFM characterization of nanobubble formation and slip condition in oxygenated and electrokinetically altered fluids.

    PubMed

    Bhushan, Bharat; Pan, Yunlu; Daniels, Stephanie

    2013-02-15

    Nanobubbles are gas-filled features that spontaneously form at the interface of hydrophobic surfaces and aqueous solutions. In this study, an atomic force microscope (AFM) was used to characterize the morphology of nanobubbles formed on hydrophobic polystyrene (PS) and octadecyltrichlorosilane (OTS) films immersed in DI water, saline, saline with oxygen and an electrokinetically altered saline solution produced with Taylor-Couette-Poiseuille flow under elevated oxygen pressure. AFM force spectroscopy was used to evaluate hydrodynamic and electrostatic forces and boundary slip condition in various fluids. The effect of solution, electric field and surface charge on shape, size and density of nanobubbles as well as slip length was quantified and the results and underlying mechanisms are presented in this paper. PMID:23123096

  15. Aflatoxin M1 Concentration in Various Dairy Products: Evidence for Biologically Reduced Amount of AFM1 in Yoghurt

    PubMed Central

    RAHIMIRAD, Amir; MAALEKINEJAD, Hassan; OSTADI, Araz; YEGANEH, Samal; FAHIMI, Samira

    2014-01-01

    Abstract Background Aflatoxin M1 (AFM1), a carcinogenic substance is found in milk and dairy products. The effect of season and type of dairy products on AFMi level in northern Iran was investigated in this study. Methods Three hundred samples (each season 75 samples) including raw and pasteurized milk, yoghurt, cheese, and cream samples were collected from three distinct milk producing farms. The samples were subjected to chemical and solid phase extractions and were analyzed by using HPLC technique. Recovery percentages, limit of detection and limit of quantification values were determined. Results Seventy percent and 98% were the minimum and maximum recoveries for cheese and raw milk, respectively and 0.021 and 0.063 ppb were the limit of detection and limit of quantification values for AFM1. We found that in autumn and winter the highest level (0.121 ppb) of AFM1 in cheese and cream samples and failed to detect any AFM1 in spring samples. Interestingly, our data showed that the yoghurt samples had the lowest level of AFM1 in all seasons. Conclusion There are significant differences between the AFM1 levels in dairy products in various seasons and also various types of products, suggesting spring and summer yoghurt samples as the safest products from AFM1 level point of view. PMID:25927044

  16. Liquid solution delivery through the pulled nanopipette combined with QTF-AFM system

    NASA Astrophysics Data System (ADS)

    An, Sangmin; Stambaugh, Corey; Kim, Gunn; Lee, Manhee; Kim, Yonghee; Lee, Kunyoung; Jhe, Wonho

    2012-02-01

    Nanopipette is a versatile fluidic tool for biochemical analysis, controlled liquid delivery in bio-nanotechnology. However, most of the researches have been performed in solution based system, thus it is challenge to study nanofluidic properties of the liquid solution delivery through the nanopipette in ambient conditions. In this work, we demonstrated the liquid ejection, dispersion, and subsequent deposition of the nanoparticles via a 30 nm aperture pipette based on the quartz tuning fork -- atomic force microscope (QTF-AFM) combined nanopipette system.

  17. Characterization of the structure of the coating of multilayers using AFM and Interferometric Microscopy

    NASA Astrophysics Data System (ADS)

    Jerez A, Martha I.; O, Laura Lara; Morantes M, Luz D.; Plata G, Arturo; Torres, Yezid; Tsygankov, Petr

    2011-01-01

    Ti / TiN films were deposited on H13 steel and silicon substrates with different deposition voltage, by means of the cathodic arc evaporation (CAE) technique, this process was carried out by nanolayers deposition, requiring a detailed survey on growth films, for the properties characterization such as grain size, thickness and roughness of the film was used the atomic force microscopy (AFM) techniques and Interferometric Microscopy. Obtaining a the films growth when varying the deposition voltage.

  18. Crystallization of Probucol in Nanoparticles Revealed by AFM Analysis in Aqueous Solution.

    PubMed

    Egami, Kiichi; Higashi, Kenjirou; Yamamoto, Keiji; Moribe, Kunikazu

    2015-08-01

    The crystallization behavior of a pharmaceutical drug in nanoparticles was directly evaluated by atomic force microscopy (AFM) force curve measurements in aqueous solution. A ternary spray-dried sample (SPD) was prepared by spray drying the organic solvent containing probucol (PBC), hypromellose (HPMC), and sodium dodecyl sulfate (SDS). The amorphization of PBC in the ternary SPD was confirmed by powder X-ray diffraction (PXRD) and solid-state 13C NMR measurements. A nanosuspension containing quite small particles of 25 nm in size was successfully prepared immediately after dispersion of the ternary SPD into water. Furthermore, solution-state 1H NMR measurements revealed that a portion of HPMC coexisted with PBC as a mixed state in the freshly prepared nanosuspension particles. After storing the nanosuspension at 25 °C, a gradual increase in the size of the nanoparticles was observed, and the particle size changed to 93.9 nm after 7 days. AFM enabled the direct observation of the morphology and agglomeration behavior of the nanoparticles in water. Moreover, AFM force-distance curves were changed from (I) to (IV), depending on the storage period, as follows: (I) complete indentation within an applied force of 1 nN, (II) complete indentation with an applied force of 1-5 nN, (III) partial indentation with an applied force of 5 nN, and (IV) nearly no indentation with an applied force of 5 nN. This stiffness increase of the nanoparticles was attributed to gradual changes in the molecular state of PBC from the amorphous to the crystal state. Solid-state 13C NMR measurements of the freeze-dried samples demonstrated the presence of metastable PBC Form II crystals in the stored nanosuspension, strongly supporting the AFM results. PMID:26106951

  19. Morphological analysis of stainless steel scale like surface morphology using STM and AFM

    SciTech Connect

    Vignal, V.; Olive, J.M.; Desjardins, D.; Roux, J.C.; Genton, V.

    1997-12-19

    A combined atomic force microscopy (AFM) and scanning tunneling microscopy (STM) investigation of stainless steel like surface morphology formed either in electropolishing bath or in HNO{sub 3} medium is reported. A new numerical technique using the Nanoscope III software is proposed. The dimension, slope and orientation of scales can be easily determined. Moreover, grain boundaries structure and probable oxides present in the upper part of the film can be deduced.

  20. Tumor suppressor protein SMAR1 modulates the roughness of cell surface: combined AFM and SEM study

    PubMed Central

    2009-01-01

    Background Imaging tools such as scanning electron microscope (SEM) and atomic force microscope (AFM) can be used to produce high-resolution topographic images of biomedical specimens and hence are well suited for imaging alterations in cell morphology. We have studied the correlation of SMAR1 expression with cell surface smoothness in cell lines as well as in different grades of human breast cancer and mouse tumor sections. Methods We validated knockdown and overexpression of SMAR1 using RT-PCR as well as Western blotting in human embryonic kidney (HEK) 293, human breast cancer (MCF-7) and mouse melanoma (B16F1) cell lines. The samples were then processed for cell surface roughness studies using atomic force microscopy (AFM) and scanning electron microscopy (SEM). The same samples were used for microarray analysis as well. Tumors sections from control and SMAR1 treated mice as well as tissues sections from different grades of human breast cancer on poly L-lysine coated slides were used for AFM and SEM studies. Results Tumor sections from mice injected with melanoma cells showed pronounced surface roughness. In contrast, tumor sections obtained from nude mice that were first injected with melanoma cells followed by repeated injections of SMAR1-P44 peptide, exhibited relatively smoother surface profile. Interestingly, human breast cancer tissue sections that showed reduced SMAR1 expression exhibited increased surface roughness compared to the adjacent normal breast tissue. Our AFM data establishes that treatment of cells with SMAR1-P44 results into increase in cytoskeletal volume that is supported by comparative gene expression data showing an increase in the expression of specific cytoskeletal proteins compared to the control cells. Altogether, these findings indicate that tumor suppressor function of SMAR1 might be exhibited through smoothening of cell surface by regulating expression of cell surface proteins. Conclusion Tumor suppressor protein SMAR1 might be

  1. Time-dependent surface adhesive force and morphology of RBC measured by AFM.

    PubMed

    Wu, Yangzhe; Hu, Yi; Cai, Jiye; Ma, Shuyuan; Wang, Xiaoping; Chen, Yong; Pan, Yunlong

    2009-04-01

    Atomic force microscopy (AFM) is a rapidly developing tool recently introduced into the evaluation of the age of bloodstains, potentially providing legal medical experts useful information for forensic investigation. In this study, the time-dependent, morphological changes of red blood cells (RBC) under three different conditions (including controlled, room-temperature condition, uncontrolled, outdoor-environmental condition, and controlled, low-temperature condition) were observed by AFM, as well as the cellular viscoelasticity via force-vs-distance curve measurements. Firstly, the data indicate that substrate types have different effects on cellular morphology of RBC. RBC presented the typical biconcave shape on mica, whereas either the biconcave shape or flattened shape was evident on glass. The mean volume of RBCs on mica was significantly larger than that of cells on glass. Surprisingly, the adhesive property of RBC membrane surfaces was substrate type-independent (the adhesive forces were statistically similar on glass and mica). With time lapse, the changes in cell volume and adhesive force of RBC under the controlled room-temperature condition were similar to those under the uncontrolled outdoor-environmental condition. Under the controlled low-temperature condition, however, the changes in cell volume occurred mainly due to the collapse of RBCs, and the curves of adhesive force showed the dramatic alternations in viscoelasticity of RBC. Taken together, the AFM detections on the time-dependent, substrate type-dependent, environment (temperature/humidity)-dependent changes in morphology and surface viscoelasticity of RBC imply a potential application of AFM in forensic medicine or investigations, e.g., estimating age of bloodstain or death time. PMID:19019689

  2. Pericellular Brush and Mechanics of Guinea Pig Fibroblast Cells Studied with AFM.

    PubMed

    Dokukin, Maxim; Ablaeva, Yulija; Kalaparthi, Vivekanand; Seluanov, Andrei; Gorbunova, Vera; Sokolov, Igor

    2016-07-12

    The atomic force microscopy (AFM) indentation method combined with the brush model can be used to separate the mechanical response of the cell body from deformation of the pericellular layer surrounding biological cells. Although self-consistency of the brush model to derive the elastic modulus of the cell body has been demonstrated, the model ability to characterize the pericellular layer has not been explicitly verified. Here we demonstrate it by using enzymatic removal of hyaluronic content of the pericellular brush for guinea pig fibroblast cells. The effect of this removal is clearly seen in the AFM force-separation curves associated with the pericellular brush layer. We further extend the brush model for brushes larger than the height of the AFM probe, which seems to be the case for fibroblast cells. In addition, we demonstrate that an extension of the brush model (i.e., double-brush model) is capable of detecting the hierarchical structure of the pericellular brush, which, for example, may consist of the pericellular coat and the membrane corrugation (microridges and microvilli). It allows us to quantitatively segregate the large soft polysaccharide pericellular coat from a relatively rigid and dense membrane corrugation layer. This was verified by comparison of the parameters of the membrane corrugation layer derived from the force curves collected on untreated cells (when this corrugation membrane part is hidden inside the pericellular brush layer) and on treated cells after the enzymatic removal of the pericellular coat part (when the corrugations are exposed to the AFM probe). We conclude that the brush model is capable of not only measuring the mechanics of the cell body but also the parameters of the pericellular brush layer, including quantitative characterization of the pericellular layer structure. PMID:27410750

  3. Recent CD AFM probe developments for sub-45 nm technology nodes

    NASA Astrophysics Data System (ADS)

    Liu, Hao-Chih; Osborne, Jason R.; Dahlen, Gregory A.; Greschner, Johann; Bayer, Thomas; Kalt, Samuel; Fritz, Georg

    2008-03-01

    This paper reports on new developments of advanced CD AFM probes after the prior introduction of "trident probes" in SPIE Advanced Lithography 2007 [1]. Trident probes, having sharpened extensions in the tip apex region, make possible bottom CD measurements within a few nanometers of the feature bottom corner; an area where other CD probes have difficulties due to tip shape limitations. Moreover, new metrology applications of trident probes have been developed for novel devices such as FinFET and vertical read/write hard disk heads. For ever smaller technology nodes, new probes evolved from the design of the trident probe. For example, the number of sharpened tip flares was reduced from three (trident) to two (bi-pod) to prevent possible interference of the third leg in the slow scan direction, as shown in Figure 3. Maintaining tip lateral stiffness as the tip size shrinks to less than 30 nm is vital for successful scanning. Consequently, a significant recent improvement is the change of probe shank cross-sectional geometry in order to maintain tip vertical aspect ratio of 1:5 (and lateral stiffness > 1 N/m). Finally, modifications of probe substrate are proposed and evaluated for current and new CD AFM systems. Hydrophobic, self-assembled monolayer (SAM) coatings were applied on CD probes to reduced tip "pull-away" distance1 during CD AFM scanning. Test results show that the pull away distance can be reduced more than 5 times on average (in some cases, by a factor of 15). Consequently, use of hydrophobic SAM coatings on CD probes mitigates pull-away distance thus allowing narrow trench CD measurements. We discuss limitations of prior CD AFM probes and design considerations of new CD probes. The characterization of first prototypes and evaluation of scan performance are presented in this work.

  4. 40 CFR 721.3440 - Haloalkyl substituted cyclic ethers.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Haloalkyl substituted cyclic ethers... Substances § 721.3440 Haloalkyl substituted cyclic ethers. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances haloalkyl substituted cyclic ethers (PMN P-85-368 and...

  5. 40 CFR 721.3440 - Haloalkyl substituted cyclic ethers.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Haloalkyl substituted cyclic ethers... Substances § 721.3440 Haloalkyl substituted cyclic ethers. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances haloalkyl substituted cyclic ethers (PMN P-85-368 and...

  6. Synthesis of cyclic sulfones by ring-closing metathesis.

    PubMed

    Yao, Qingwei

    2002-02-01

    A general and highly efficient synthesis of cyclic sulfones based on ring-closing metathesis has been developed. The synthetic utility of the resulting cyclic sulfones was demonstrated by their participation in stereoselective Diels-Alder reactions and transformation to cyclic dienes by the Ramberg-Bäcklund reaction. PMID:11820896

  7. Structure and permeability of ion-channels by integrated AFM and waveguide TIRF microscopy.

    PubMed

    Ramachandran, Srinivasan; Arce, Fernando Teran; Patel, Nirav R; Quist, Arjan P; Cohen, Daniel A; Lal, Ratnesh

    2014-01-01

    Membrane ion channels regulate key cellular functions and their activity is dependent on their 3D structure. Atomic force microscopy (AFM) images 3D structure of membrane channels placed on a solid substrate. Solid substrate prevents molecular transport through ion channels thus hindering any direct structure-function relationship analysis. Here we designed a ~70 nm nanopore to suspend a membrane, allowing fluidic access to both sides. We used these nanopores with AFM and total internal reflection fluorescence microscopy (TIRFM) for high resolution imaging and molecular transport measurement. Significantly, membranes over the nanopore were stable for repeated AFM imaging. We studied structure-activity relationship of gap junction hemichannels reconstituted in lipid bilayers. Individual hemichannels in the membrane overlying the nanopore were resolved and transport of hemichannel-permeant LY dye was visualized when the hemichannel was opened by lowering calcium in the medium. This integrated technique will allow direct structure-permeability relationship of many ion channels and receptors. PMID:24651823

  8. Rational fabrication of a gold-coated AFM TERS tip by pulsed electrodeposition.

    PubMed

    Yang, Li-Kun; Huang, Teng-Xiang; Zeng, Zhi-Cong; Li, Mao-Hua; Wang, Xiang; Yang, Fang-Zu; Ren, Bin

    2015-11-21

    Reproducible fabrication of sharp gold- or silver-coated tips has become the bottleneck issue in tip-enhanced Raman spectroscopy, especially for atomic force microscopy (AFM)-based TERS. Herein, we developed a novel method based on pulsed electrodeposition to coat a thin gold layer over atomic force microscopy (AFM) tips to produce plasmonic TERS tips with high reproducibility. We systematically investigated the influence of the deposition potential and step time on the surface roughness and sharpness. This method allows the rational control of the radii of gold-coated TERS tips from a few to hundreds of nanometers, which allows us to systematically study the dependence of the TERS enhancement on the radius of the gold-coated AFM tip. The maximum TERS enhancement was achieved for the tip radius in the range of 60-75 nm in the gap mode. The coated gold layer has a strong adhesion with the silicon tip surface, which is highly stable in water, showing the great potential for application in the aqueous environment. PMID:26482226

  9. A low-cost AFM setup with an interferometer for undergraduates and secondary-school students

    NASA Astrophysics Data System (ADS)

    Bergmann, Antje; Feigl, Daniela; Kuhn, David; Schaupp, Manuel; Quast, Günter; Busch, Kurt; Eichner, Ludwig; Schumacher, Jens

    2013-07-01

    Atomic force microscopy (AFM) is an important tool in nanotechnology. This method makes it possible to observe nanoscopic surfaces beyond the resolution of light microscopy. In order to provide undergraduate and secondary-school students with insights into this world, we have developed a very robust low-cost AFM setup with a Fabry-Perot interferometer as a detecting device. This setup is designed to be operated almost completely manually and its simplicity gives access to a profound understanding of the working principle. Our AFM is operated in a constant height mode, i.e. the topography of the sample surface is represented directly by the deflection of the cantilever. Thus, the measuring procedure can be understood even by secondary-school students; furthermore, it is the method with the lowest cost, totalling not more than 10-15 k Euros. Nevertheless, we are able to examine a large variety of sample topographies such as CD and DVD surfaces, IC structures, blood cells, butterfly wings or moth eyes. Furthermore, force-distance curves can be recorded and the tensile moduli of some materials can be evaluated. We present our setup in detail and describe its working principles. In addition, we show various experiments which have already been performed by students.

  10. Fracture Growth Testing of Titanium 6AL-4V in AF-M315E

    NASA Technical Reports Server (NTRS)

    Sampson, Jeffrey W.; Martinez, Jonathan; McLean, Christopher

    2015-01-01

    The Green Propellant Infusion Mission (GPIM) will demonstrate the performance of AF-M315E monopropellant in orbit. Flight certification requires a safe-life analysis of the titanium alloy fuel tank to ensure inherent flaws will not cause failure during the design life. Material property inputs for this analysis require testing to determine the stress intensity factor for environmentally-assisted cracking (K (sub EAC)) of Ti 6Al-4V in combination with the AF-M315E monopropellant. Testing of single-edge notched specimens SE(B) representing the bulk tank membrane and weld material were performed in accordance with ASTM E1681. Specimens with fatigue pre-cracks were loaded into test fixtures so that the crack tips were exposed to the monopropellant at 50 degrees Centigrade for a duration of 1,000 hours. Specimens that did not fail during exposure were opened to inspect the crack surfaces for evidence of crack growth. The threshold stress intensity value, KEAC, is the highest applied stress intensity that produced neither a failure of the specimen during the exposure nor showed evidence of crack growth. The threshold stress intensity factor of the Ti 6Al-4V forged tank material when exposed to AF-M315E monopropellant was found to be at least 22.0 kilopounds per square inch. The stress intensity factor of the weld material was at least 31.3 kilopounds per square inch.

  11. EEMD based pitch evaluation method for accurate grating measurement by AFM

    NASA Astrophysics Data System (ADS)

    Li, Changsheng; Yang, Shuming; Wang, Chenying; Jiang, Zhuangde

    2016-09-01

    The pitch measurement and AFM calibration precision are significantly influenced by the grating pitch evaluation method. This paper presents the ensemble empirical mode decomposition (EEMD) based pitch evaluation method to relieve the accuracy deterioration caused by high and low frequency components of scanning profile during pitch evaluation. The simulation analysis shows that the application of EEMD can improve the pitch accuracy of the FFT-FT algorithm. The pitch error is small when the iteration number of the FFT-FT algorithms was 8. The AFM measurement of the 500 nm-pitch one-dimensional grating shows that the EEMD based pitch evaluation method could improve the pitch precision, especially the grating line position precision, and greatly expand the applicability of the gravity center algorithm when particles and impression marks were distributed on the sample surface. The measurement indicates that the nonlinearity was stable, and the nonlinearity of x axis and forward scanning was much smaller than their counterpart. Finally, a detailed pitch measurement uncertainty evaluation model suitable for commercial AFMs was demonstrated and a pitch uncertainty in the sub-nanometer range was achieved. The pitch uncertainty was reduced about 10% by EEMD.

  12. Fabrication of nanochannels with ladder nanostructure at the bottom using AFM nanoscratching method.

    PubMed

    Yan, Yongda; Geng, Yanquan; Hu, Zhenjiang; Zhao, Xuesen; Yu, Bowen; Zhang, Qi

    2014-01-01

    This letter presents a novel atomic force microscopy (AFM)-based nanomanufacturing method combining the tip scanning with the high-precision stage movement to fabricate nanochannels with ladder nanostructure at the bottom by continuous scanning with a fixed scan size. Different structures can be obtained according to the matching relation of the tip feeding velocity and the precision stage moving velocity. This relationship was first studied in detail to achieve nanochannels with different ladder nanostructures at the bottom. Machining experiments were then performed to fabricate nanochannels on an aluminum alloy surface to demonstrate the capability of this AFM-based fabrication method presented in this study. Results show that the feed value and the tip orientation in the removing action play important roles in this method which has a significant effect on the machined surfaces. Finally, the capacity of this method to fabricate a large-scale nanochannel was also demonstrated. This method has the potential to advance the existing AFM tip-based nanomanufacturing technique of the formation these complex structures by increasing the removal speed, simplifying the processing procedure and achieving the large-scale nanofabrication. PMID:24940171

  13. AFM volumetric methods for the characterization of proteins and nucleic acids.

    PubMed

    Fuentes-Perez, Maria Eugenia; Dillingham, Mark S; Moreno-Herrero, Fernando

    2013-04-01

    The atomic force microscope overestimates lateral dimensions and underestimates heights of nanometer size objects such as proteins and nucleic acids. This has made researchers cautious of AFM measurements, even though there is no other technique capable of measuring topography with sub-nanometer precision. Nevertheless, several approaches for determining the stoichiometry of protein and protein-DNA complexes have been developed which show that, although the absolute values may be incorrect, the AFM volume is essentially proportional to the mass. This has allowed the determination of the mass of protein complexes with the help of a calibration curve. Here we review the main techniques for AFM volume measurements and detail a methodology that significantly reduces the associated errors. This method uses a fragment of DNA as a fiducial marker by which the volume of a protein is normalized. The use of fiducial markers co-adsorbed together with the protein of interest minimizes the contribution of tip-induced artifacts as they affect both the object of interest and the marker. Finally, we apply this method to the measurement of the length of single-stranded DNA. A linear relationship between length and volume was obtained, opening the door to studies of ssDNA intermediates formed during complex DNA transactions such as replication, recombination and repair. PMID:23454289

  14. A Novel Dog-Bone Oscillating AFM Probe with Thermal Actuation and Piezoresistive Detection †

    PubMed Central

    Xiong, Zhuang; Mairiaux, Estelle; Walter, Benjamin; Faucher, Marc; Buchaillot, Lionel; Legrand, Bernard

    2014-01-01

    In order to effectively increase the resonance frequency and the quality factor of atomic force microscope (AFM) probes, a novel oscillating probe based on a dog-bone shaped MEMS resonator was conceived, designed, fabricated and evaluated. The novel probe with 400 μm in length, 100 μm in width and 5 μm in thickness was enabled to feature MHz resonance frequencies with integrated thermal actuation and piezoresistive detection. Standard silicon micromachining was employed. Both electrical and optical measurements were carried out in air. The resonance frequency and the quality factor of the novel probe were measured to be 5.4 MHz and 4000 respectively, which are much higher than those (about several hundreds of kHz) of commonly used cantilever probes. The probe was mounted onto a commercial AFM set-up through a dedicated probe-holder and circuit board. Topographic images of patterned resist samples were obtained. It is expected that the resonance frequency and the measurement bandwidth of such probes will be further increased by a proper downscaling, thus leading to a significant increase in the scanning speed capability of AFM instruments. PMID:25365463

  15. AFM and pulsed laser ablation methods for Cultural Heritage: application to archeometric analysis of stone artifacts

    NASA Astrophysics Data System (ADS)

    Barberio, M.; Veltri, S.; Stranges, F.; Bonanno, A.; Xu, F.; Antici, P.

    2015-09-01

    In this paper, we introduce the use of the atomic force microscope (AFM) and of the pulsed laser ablation as methods for morphological diagnostic with nanoscale precision of archeological artifacts and corrosive patina removal from stone artifacts. We test our methodology on stone artifacts extracted from the Church of Sotterra (located in Calabria, South Italy). The AFM microscopy was compared with different petrographic, chemical, optical and morphological analysis methods for identifying the textural characteristics, evaluating the state of preservation and formulating some hypotheses about the provenance and composition of the impurity patina located on the artifact surfaces. We demonstrate that with the nanometric precision obtained with AFM microscopy, it is possible to distinguish the different states of preservation, much better than using conventional petrographic methods. The surface's roughness is evaluated from very small artifact's fragments, reducing the coring at micrometric scale with a minimal damage to the artworks. After the diagnosis, we performed restoration tests using the pulsed laser ablation (PLA) method and compared it with the more common micro-sandblasting under dry conditions. We find that the PLA is highly effective for the removal of the surficial patina, with a control of a few hundreds of nanometers in the cleaning of surface, without introducing chemical or morphological damages to the artifacts. Moreover, PLA can be easily implemented in underwater conditions; this has the great advantage that stone and pottery artifacts for marine archeological sites do not need to be removed from the site.

  16. Immunological Identification of Fibrinogen in Dual-Component Protein Films by AFM Imaging

    PubMed Central

    Soman, Pranav; Rice, Zachary; Siedlecki, Christopher A.

    2009-01-01

    The success of long-term blood-contacting implanted devices is largely dependent upon the interaction of the blood components with the device biomaterial surface. The ability to study these interactions has been hindered by a lack of methods to measure single-molecule interactions in complex multi-protein environments similar to the environment found in-vivo. In this paper, we demonstrate the use of atomic force microscopy (AFM) in conjunction with gold nanolabels to detect the protein fibrinogen under aqueous conditions without the topographical clues usually necessary for high resolution visualization. BSA was patterned onto both muscovite mica and plasma-treated polydimethylsiloxane (PDMS) substrates and these test substrates were subsequently backfilled with fibrinogen to yield a featureless protein layer. The fibrinogen in this dual protein layer was detected using high resolution AFM imaging following infusion of anti-fibrinogen conjugated with nanogold particles. This AFM immuno-detection technique will potentially be applicable to complex multi-component protein films adsorbed on clinically-relevant polymers used in medical devices. PMID:18294855

  17. AFM-porosimetry: density and pore volume measurements of particulate materials.

    PubMed

    Sörensen, Malin H; Valle-Delgado, Juan J; Corkery, Robert W; Rutland, Mark W; Alberius, Peter C

    2008-06-01

    We introduced the novel technique of AFM-porosimetry and applied it to measure the total pore volume of porous particles with a spherical geometry. The methodology is based on using an atomic force microscope as a balance to measure masses of individual particles. Several particles within the same batch were measured, and by plotting particle mass versus particle volume, the bulk density of the sample can be extracted from the slope of the linear fit. The pore volume is then calculated from the densities of the bulk and matrix materials, respectively. In contrast to nitrogen sorption and mercury porosimetry, this method is capable of measuring the total pore volume regardless of pore size distribution and pore connectivity. In this study, three porous samples were investigated by AFM-porosimetry: one ordered mesoporous sample and two disordered foam structures. All samples were based on a matrix of amorphous silica templated by a block copolymer, Pluronic F127, swollen to various degrees with poly(propylene glycol). In addition, the density of silica spheres without a template was measured by two independent techniques: AFM and the Archimedes principle. PMID:18503284

  18. Direct comparison of AFM and SEM measurements on the same set of nanoparticles

    NASA Astrophysics Data System (ADS)

    Delvallée, A.; Feltin, N.; Ducourtieux, S.; Trabelsi, M.; Hochepied, J. F.

    2015-08-01

    This article is the first step in the development of a hybrid metrology combining AFM and SEM techniques for measuring the dimensions of a nanoparticle population in 3D space (X,Y,Z). This method exploits the strengths of each technique on the same set of nanoparticles. AFM is used for measuring the nanoparticle height and the measurements along X and Y axes are deduced from SEM images. A sampling method is proposed in order to obtain the best deposition conditions of SiO2 and gold nanoparticles on mica or silicon substrates. Only the isolated nanoparticles are taken into account in the histogram of size distribution. Moreover, a semi-automatic Matlab routine has also been developed to process the AFM and SEM images, measure and count the nanoparticles. This routine allows the user to exclusively select the isolated nanoparticles through a control interface. The measurements have been performed on spherical-like nanoparticles to test the method by comparing the results obtained with both techniques.

  19. Single-cycle-PLL detection for real-time FM-AFM applications.

    PubMed

    Schlecker, Benedikt; Dukic, Maja; Erickson, Blake; Ortmanns, Maurits; Fantner, Georg; Anders, Jens

    2014-04-01

    In this paper we present a novel architecture for phase-locked loop (PLL) based high-speed demodulation of frequency-modulated (FM) atomic force microscopy (AFM) signals. In our approach, we use single-sideband (SSB) frequency upconversion to translate the AFM signal from the position sensitive detector to a fixed intermediate frequency (IF) of 10 MHz. In this way, we fully benefit from the excellent noise performance of PLL-based FM demodulators still avoiding the intrinsic bandwidth limitation of such systems. In addition, the upconversion to a fixed IF renders the PLL demodulator independent of the cantilever's resonance frequency, allowing the system to work with a large range of cantilever frequencies. To investigate if the additional noise introduced by the SSB upconverter degrades the system noise figure we present a model of the AM-to-FM noise conversion in PLLs incorporating a phase-frequency detector. Using this model, we can predict an upper corner frequency for the demodulation bandwidth above which the converted noise from the single-sideband upconverter becomes the dominant noise source and therefore begins to deteriorate the overall system performance. The approach is validated by both electrical and AFM measurements obtained with a PCB-based prototype implementing the proposed demodulator architecture. PMID:24760947

  20. Nano-scale Topographical Studies on the Growth Cones of Nerve Cells using AFM

    NASA Astrophysics Data System (ADS)

    Durkaya, Goksel; Zhong, Lei; Rehder, Vincent; Dietz, Nikolaus

    2009-11-01

    Nerve cells are the fundamental units which are responsible for intercommunication within the nervous system. The neurites, fibrous cable-like extensions for information delivery, of nerve cells are tipped by highly motile sensory structures known as the growth cones which execute important functions; neural construction, decision making and navigation during development and regeneration of the nervous system. The highly dynamic subcomponents of the growth cones are important in neural activity. Atomic Force Microscopy (AFM) is the most powerful microscopy technique which is capable of imaging without conductivity constraint and in liquid media. AFM providing nano-scale topographical information on biological structures is also informative on the physical properties such as: elasticity, adhesion, and softness. This contribution focuses on AFM analysis of the growth cones of the nerve cells removed from the buccal ganglion of Helisoma trivolvis. The results of nano-scale topography and softness analysis on growth cone central domain, filopodia and overlying lamellopodium (veil) are presented. The subcomponents of the growth cones of different nerve cells are compared to each other. The results of the analysis are linked to the mechanical properties and internal molecular density distribution of the growth cones.