Application of Nanocrystalline Graphite‐like Pyrolytic Carbon Film Electrode in the Electroanalytical Determination of Famotidine

Direct electro‐oxidation of famotidine at different graphitic carbon‐based electrode materials was evaluated. These materials included conventional electrodes of edge‐plane pyrolytic graphite, basal‐plane pyrolytic graphite, carbon paste, and glassy carbon as well as nano‐structured carbon‐based materials such as pyrolytic carbon film, carbon nanotube, and nano‐graphene. Raman spectroscopy and scanning electron microscopy were employed to analyze their structural and morphological features. It was found that the pyrolytic carbon film electrode, after a simple and fast anodic activation, shows superior electroanalytical performance. The method was successfully applied for the electroanalytical determination of famotidine in tablet dosage forms and urine samples.     

热解碳包覆的碳纳米管复合二氧化锰薄膜超级电容器

通过化学气相沉积(CVD)的方法,在碳纳米管(CNT)薄膜及其连接处沉积热解碳(PC)来限制CNTs之间的滑移。通过扫描电镜(SEM)观察发现,热解碳(PC)的沉积使得CNT表面更加平整,且表面的孔洞更加均匀。通过应力应变及亲疏水性测试发现,CNT/PC复合薄膜的拉伸强度增加了200%,水与薄膜的静态接触角由123°减小到78°。其后通过电化学沉积的方法,制备得到CNT/PC/MnO2薄膜电极材料,通过电化学测试得知,在1 mA/cm^2的电流下单电极的比电容为326 mF/cm^2,可以稳定循环10000圈,电容的保持率稳定在100%左右。     

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

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.     

Anodic-stripping voltammetry of heavy metals in the presence of organic surfactants

The efficacy of fumed silica for removal of sorption interferences by organic surfactants in the anodic-stripping voltammetry of heavy metals is demonstrated. Appropriate addition of silica to the sample solution rapidly "purifies" it from interfering surfactants during the nitrogen purge step. Up to at least 6 ppm of gelatin, Triton X-100, albumin or Liqui-Nox then does not affect the stripping response of cadmium, lead and zinc at the hanging mercury drop electrode. A relative standard deviation of 5.5% is obtained for 20 successive measurements of 1 x 10(-7)M lead in the presence of 2 ppm Triton X-100. Analogous improvements are observed at the mercury film electrode (in the presence of up to 60 ppm of these surfactants). The use of silica thus possesses the advantages of speed, efficiency, simplicity and low cost compared to other schemes for dealing with surfactant interferences in anodic-stripping voltammetry.     

Direct Oxidation of Ascorbic Acid at an Edge Plane Pyrolytic Graphite Electrode: A Comparison of the Electroanalytical Response with Other Carbon Electrodes

The direct electrochemical oxidation of ascorbic acid at an edge plane pyrolytic graphite electrode (EPPG) is investigated and compared with other common carbon‐based electrodes, specifically glassy carbon, boron doped diamond and basal plane pyrolytic graphite. It is found that the EPPG electrode shows a significantly higher degree of electrochemical reversibility than the other electrode substrates giving rise to an analytically optimized limit of detection and sensitivity of 7.1×10^?5 M and 0.065 A M^?1 respectively.     

Electroanalytical determination of cadmium(II) and lead(II) using an in-situ bismuth film modified edge plane pyrolytic graphite electrode.

A highly sensitive and simple electroanalytical methodology is presented using an in-situ bismuth film modified edge plane pyrolytic graphite electrode (BiF-EPPGE) which is exemplified with the simultaneous determination of cadmium(II) and lead(II). Square-wave anodic stripping voltammetry is utilised with the effects of several experimental variables studied. Simultaneous additions of cadmium(II) and lead(II) were investigated where two linear ranges between 0.1-100 and 0.1-300 microg/L and also detection limits of 0.062 and 0.084 microg/L were obtained, respectively. The method was then successfully applied to the simultaneous determination of cadmium(II) and lead(II) in spiked river water, where recoveries of 100.5 and 98% were obtained, respectively. This electroanalytical protocol using edge plane pyrolytic graphite electrodes is one of the simplest methodologies to date using non-mercury based electrodes and is simpler and cheaper than alternatives such as carbon nanotube electrode arrays, suggesting the use of edge plane pyrolytic graphite electrode for routine sensing.     

Edge Plane Pyrolytic Graphite Electrodes for Halide Detection in Aqueous Solutions

The behavior of chloride, bromide and iodide at edge plane pyrolytic graphite electrodes has been explored in aqueous acid solutions. The voltammetric response in each case has been compared with that of basal plane pyrolytic graphite, glassy carbon and boron‐doped diamond. The electrochemical oxidation of chloride is found to only occur on boron‐doped diamond while the electrochemical reversibility for the oxidation of bromide on edge plane pyrolytic graphite is similar to that seen at glassy carbon whilst being superior to basal plane pyrolytic graphite and boron‐doped diamond. In the case of iodide oxidation, edge plane and basal plane pyrolytic graphite and glassy carbon display similar electrode kinetics but are all superior to boron‐doped diamond. The analytical possibilities were examined using the edge plane pyrolytic graphite electrode for both iodide and bromine where is was found that, based on cyclic voltammetry, detection limits in the order of 10^?6 M are possible.     

A glucose biosensor using methyl viologen redox mediator on carbon film electrodes

A new methyl viologen-mediated amperometric enzyme electrode sensitive to glucose has been developed using carbon film electrode substrates. Carbon film electrodes from resistors fabricated by pyrolytic deposition of carbon were modified by immobilization of glucose oxidase through cross-linking with glutaraldehyde in the presence of bovine serum albumin. The mediator, methyl viologen, was directly immobilised with the enzyme together with Nafion cation-exchange polymer. The electrochemistry of the glucose oxidase/methyl viologen modified electrode was investigated by cyclic voltammetry and by electrochemical impedance spectroscopy. The biosensor response to glucose was evaluated amperometrically; the detection limit was 20 μM, the linear range extended to 1.2 mM and the reproducibility of around 3%. When stored in phosphate buffer at 4 °C and used every day, the sensor showed good stability over more several weeks.     

Electrochemical Characterization of a Pyrolytic Carbon Film Electrode and the Effect of Anodization

A pyrolytic carbon (PC) film electrode was fabricated by the chemical vapor deposition (CVD) method. This report deals with the preparation, characterization and electrochemical behavior of this carbon film. Cyclic voltammetry, linear sweep voltammetry, Raman spectroscopy and scanning electron microscopy were employed to characterize the electrode. Low background current and capacitance were observed and the rate of charge transfer for Fe(CN) redox couple was determined via cyclic voltammetry. Also the effect of the anodic activation on the electrochemical activity was evaluated and characterized with respect to the sequence of voltage applied to the electrode. The excellent electrochemical activity and low background current are the reasons why this electrode is attractive for electroanalysis measurements with lower detection limit.     

Pyrolytic carbon film electrodes

Home-made pyrolytic carbon film electrodes (PCFE) were tested in voltammetric experiments. Different drugs were analyzed by differential pulse voltammetry. In many cases the reproducibility of the signals is as satisfactory as by using glassy carbon electrodes (GCE). The cleaning procedure is very easy to accomplish by wiping off the electrode surface with a paper tissue dipped into methanol. The peak- to residual current rate is much better at the PCFE than at the GCE. Therefore the detection limit is lowered at the former.     

Pyrolytic carbon film electrodes

Home-made pyrolytic carbon film electrodes (PCFE) were tested in voltammetric experiments. Different drugs were analyzed by differential pulse voltammetry. In many cases the reproducibility of the signals is as satisfactory as by using glassy carbon electrodes (GCE). The cleaning procedure is very easy to accomplish by wiping off the electrode surface with a paper tissue dipped into methanol. The peak- to residual current rate is much better at the PCFE than at the GCE. Therefore the detection limit is lowered at the former.     

Attachment of Nanoparticles to Pyrolytic Graphite Electrode and Its Application for the Direct Electrochemistry and Electrocatalytic Behavior of Catalase

Abstract

A highly hydrophilic, nontoxic, and conductive effect of colloidal gold nanoparticles (GNP) and multi-walled carbon nanotubes (MWCNT) on pyrolytic graphite electrode has been demonstrated. The direct electron transfer of catalase (CAT) was achieved based on the immobilization of MWCNT/CAT-GNP on a pyrolytic graphite electrode by a Nafion film. The immobilized catalase displayed a pair of well-defined and nearly reversible redox peaks in 0.1 M phosphate buffer solution (PBS) (pH 6.98). The dependence of E°′on solution pH indicated that the direct electron transfer reaction of catalase was a single-electron-transfer coupled with single-proton-transfer reaction process. The immobilized catalase maintained its biological activity, showing a surface controlled electrode process with an apparent heterogeneous electron transfer rate constant (k _s) of 1.387±0.1 s^?1 and charge-transfer coefficient (α) of 0.49, and displayed electrocatalytic activity in the electrocatalytic reduction of hydrogen peroxide. Therefore, the resulting modified electrode can be used as a biosensor for detecting hydrogen peroxide.     

碳和石墨烯对磷酸锰锂材料性能的影响

在采用溶剂热法制备磷酸锰锂的基础上,以蔗糖和石墨烯为碳源,制备了裂解碳和石墨烯含量不同的磷酸锰锂/碳/石墨烯复合材料,研究了裂解碳和石墨烯对材料性能的影响。采用扫描电镜（SEM）和透射电镜（TEM）对材料的形貌进行了表征。裂解碳包覆可以提高LiMnPO₄纳米片表面的电子导电性,对于材料性能的改善起到主要的作用;石墨烯可以提高纳米片之间的电子和离子导电性,改善材料的电化学性能。电化学测试表明,当裂解碳含量为4%、石墨烯含量为2%时,LiMnPO₄电极具有较好的电化学性能,在0.5C下的放电比容量为139.1 mAh·g^-1,循环100次后,容量保持率为93.6%。与添加单一碳和单一石墨烯的LiMnPO₄电极相比,该电极在0.5C下的放电比容量分别提高了35.0%和48.6%。     

碳和石墨烯对磷酸锰锂材料性能的影响

在采用溶剂热法制备磷酸锰锂的基础上,以蔗糖和石墨烯为碳源,制备了裂解碳和石墨烯含量不同的磷酸锰锂/碳/石墨烯复合材料,研究了裂解碳和石墨烯对材料性能的影响。采用扫描电镜(SEM)和透射电镜(TEM)对材料的形貌进行了表征。裂解碳包覆可以提高LiMnPO_4纳米片表面的电子导电性,对于材料性能的改善起到主要的作用;石墨烯可以提高纳米片之间的电子和离子导电性,改善材料的电化学性能。电化学测试表明,当裂解碳含量为4%、石墨烯含量为2%时,LiMnPO_4电极具有较好的电化学性能,在0.5C下的放电比容量为139.1 m Ah·g-1,循环100次后,容量保持率为93.6%。与添加单一碳和单一石墨烯的LiMnPO_4电极相比,该电极在0.5C下的放电比容量分别提高了35.0%和48.6%。     

Evaluation of differential pulse anodic-stripping voltammetry at a stationary mercury-film electrode with stirred solution

Differential pulse anodic-stripping voltammetry at a stationary mercury-film electrode with the solution stirred during the deposition step has been investigated. The sensitivity achieved by using such a simple set-up is similar to that obtained with a mercury-film rotating disk electrode. The effects of various experimental parameters on the peak current are described. Lead and cadmium were used as test systems, and gave detection limits of around 1 x 10(-10)M with 5-min deposition times.     

Application of anodized edge-plane pyrolytic graphite electrode for analysis of clindamycin in pharmaceutical formulations and human urine samples

Different graphitic carbon-based electrode materials were evaluated for direct electro-oxidation of clindamycin and electroanalytical parameters such as sensitivity, residual background current, and signal-tobackground current ratio were compared to select the best one for the clindamycin electroanalysis. Such electrode materials include glassy carbon, carbon paste, pyrolytic graphite (edge-plane and basal-plane), carbon nanotube, reduced graphene oxide, and carbon black. The edge-plane pyrolytic graphite electrode after a simple and fast electrochemical pretreatment showed superior performance compared with the other carbon electrodes. Raman and Fourier transform infrared spectroscopy were employed to analyze the surface microstructure and chemical bonding of the carbon materials and scanning electron microscopy was used to study their surface morphologic features. The applicability of the electrochemically activated edge-plane pyrolytic graphite electrode for the determination of clindamycin in pharmaceutical formulations and human urine samples was evaluated.     

Effect of surface-active compounds on voltammetric stripping analysis at the mercury film electrode

The effects of various organic compounds on the differential-pulse anodic-stripping voltammetric response at the in-situ plated mercury film electrode are explored. These effects vary from metal to metal and from one organic compound to another. The most pronounced effects are observed in measurements of copper. The main effect of the organic compound is to depress the peak current rather than change the peak shape or potential. The differences between the organic interferences observed at the mercury film electrode and those reported at the hanging mercury drop electrode are explained by the different morphology and geometry of the two electrodes. The implications of these interferences for the reliability and feasibility of stripping measurements in natural waters are discussed. Gelatin, camphor, humic acid, starch, agar, sodium dodecyl sulphate and albumin were used as representative organic compounds, and cadmium, lead, and copper as test metal ions.     

Determination of trace metals by anodic-stripping voltammetry with a new kind of mercury electrode: The long-lasting sessile-drop electrode

A new kind of semi-stationary mercury drop electrode is described, which can be used for the determination of trace metals in natural waters by differential-pulse anodic-stripping voltammetry. Results are reported for the determination of zinc in potassium chloride and in samples of sea-water. The reproducibility of the electrode and of the results obtained with it for zinc at the 10(-8)M level are very satisfactory.     

Cyclic Voltammetric Studies of a Pyrolytic Carbon Film Electrode and the Effect of Laser Irradiation

The effects of laser irradiation with a small N₂ laser on the reactivation of a pyrolytic carbon (PC) film electrode were investigated. Cyclic voltammetry, Raman spectroscopy and scanning electron microscopy (SEM) were used to characterize the electrode. The electrode response decayed during the solution exposure but could be restored to a good performance via this reactivation method. It was found that the effect of laser to promote electron transfer was desorption the physisorbed impurities to exposure more active sites on the surface. Also, the electrochemical results were compared to the results of organic solvent washing and anodization.     

Effect of pyrolytic carbon content on microstructure and tribological properties of C/C-SiC brake composites fabricated by isothermal chemical vapor infiltration

Four types of C/C-SiC composites were prepared by isothermal chemical vapor infiltration (ICVI) of SiC on C/C preforms of different densities. Tribological properties of the composites were evaluated by using MM-1000 testing machine. The results indicated that the friction behaviors of the composites are a strong function of the content of pyrolytic carbon (in matrix). Moreover, friction film was formed on the surface and increased with pyrolytic carbon content. Debris originated of particulate and film-type have been observed after friction testing with ratio and size determined by the content of pyrolytic carbon.