Electrocatalytic determination of captopril using a modified carbon nanotube paste electrode: Application to determination of captopril in pharmaceutical and biological samples

A carbon paste electrode modified with carbon nanotube and benzoylferrocene (BF) was fabricated. The electrochemical study of the modified electrode, as well as its efficiency for electrocatalytic oxidation of captopril (CAP), was described. The electrode was employed to study the electrocatalytic oxidation of CAP, using cyclic voltammetry (CV), chronoamperometry (CHA) and square wave voltammetry (SWV) as diagnostic techniques. It has been found that the oxidation of CAP at the surface of modified electrode occurs at a potential of about 85 mV less positive than that of an unmodified CPE. SWV exhibits a linear dynamic range from 1.0 × 10⁻⁷ to 3.5 × 10⁻⁴ M and a detection limit of 3.0 × 10⁻⁸ M for CAP. Finally the modified electrode was used for determination of CAP in CAP tablet and urine sample.     

The design of polyaniline based sensor for the qualitative estimation of malonaldehyde

The detection of contaminated food in every stage of processing required new technology for fast identification and isolation of toxicity in food. Since effect of food contaminant are severe to human health, the need of pioneer technologies also increasing over last few decades. In the current study, MDA was prepared by hydrolysis of 1,1,3,3-tetramethoxypropane in HCl media and used in the electrochemical studies. The electrochemical sensor was fabricated with modified glassy carbon electrode with polyaniline. These sensors were used for detection of sodium salt of malonaldehyde and observed that a high sensitivity in the concentration range ∼1 × 10⁻¹ M and 1 × 10⁻² M. Tafel plots show the variation of over potential from − 1.73 V to − 3.74 V up to 10⁻⁵ mol/L indicating the lower limit of detection of the system.     

Determination of haloperidol drug in ampoules and in urine samples using a potentiometric modified carbon paste electrode

A modified carbon paste electrode for haloperidol drug based on haloperidol-phosphomolybdate (HP-PM) as an ion-exchanger dissolved in plasticizer DBP and its potentiometric characteristics were discussed. The electrode exhibited a good Nernstian slope of 56.9 ± 0.3 mV/decade with a linear concentration range from 3.2 × 10⁻⁶ to 1.0 × 10⁻² M for the haloperidol ion. The limit of detection (LOD) was 1.5 × 10⁻⁶ M. It had response time of 5–8 seconds (s), useable in pH range of 6.2–8.6 and temperature of 20–60 °C. The electrode shows clear discrimination of haloperidol drug from several inorganic ions, sugars and some common drug excipients. The sensor was applied for determination of haloperidol drug in urine and in pharmaceutical formulations using potentiometric determination, standard addition and the calibration curve methods. The results are satisfactory with excellent percentage recovery comparable or better than those obtained by other routine methods.     

Potential step study of electrooxidation of methanol in 1-butyl-3-methylimidazolium tetrafluoroborate

A potential step method was used to characterize the electrooxidation of methanol on a chemically modified electrode in an ionic liquid solvent. Two major findings were reported from this study. Firstly, the oxidation was dominant 2.2 s after the potential step. Before that, the double layer charging and adsorption were dominant. Therefore, there should be a waiting time of a few seconds if a methanol sensor is developed with a potential step method. Secondly, the oxidation of methanol on the electrode was diffusion controlled. The concentration of methanol affected the diffusion. The diffusion constant D₀ was 8.37 × 10⁻¹⁷ m²/s when the concentration was lower than 0.5 M and was 2.66 × 10⁻¹³ m²/s when the concentration was higher than 1.0 M. This suggests that the methanol concentration should be kept higher than a threshold in an ionic liquid based fuel cell.     

A sensitive nanocomposite-based electrochemical sensor for voltammetric simultaneous determination of isoproterenol,acetaminophen and tryptophan

The electrooxidation of isoproterenol (ISPT), acetaminophen (AC) and tryptophan (Trp) and their mixture has been studied using an 8,9-dihydroxy-7-methyl-12H-benzothiazolo[2,3-b]quinazolin-12-one modified multiwall carbon nanotubes paste electrode (DMBQ-MCNTPE). The novel sensor exhibited potent and persistent electron mediating behavior followed by well separated oxidation peaks towards ISPT, AC and Trp with activation over-potential. The peak currents were linearly dependent on ISPT, AC and Trp concentrations using square wave voltammetry (SWV) method in the range of 0.04–400, 5.0–500, and 10.0–800 μmol L⁻¹, with detection limits of 0.009, 1.0, and 4.0 μmol L⁻¹, respectively. The modified electrode was used for the determination of ISPT, AC and Trp in biological and pharmaceutical samples.     

Silver nanoparticles/polymethacrylic acid (AgNPs/PMA) hybrid nanocomposites-modified electrodes for the electrochemical detection of nitrate ions

AgNPs/PMA hybrid nanocomposite materials with different Ag loadings have been synthesized using a simple chemical route assisted by UV irradiation. The hybrid composites were characterized by means of SEM and TEM, UV–vis spectroscopy and XPS. The as synthesized hybrid samples, composed of small Ag nanoparticles (AgNPs) embedded within the PMA (poly-methacrylic-acid) matrix, have been used to modify the working electrode of disposable screen printed carbon electrodes (SPCEs). It has been observed that hybrid composite with the lowest Ag loading forms dendritic silver structures on the surface of working electrode, whereas at higher loadings massive structures were formed. The electrocatalytic properties of the AgNPs/PMA/SPCEs were investigated toward the reduction of nitrate at neutral pH. Based on these modified electrodes, both voltammetric and amperometric sensors were developed for the electrochemical sensing of nitrate. Voltammetric sensor showed a wide linear range (0–20 mM) and high sensitivity (130 μA mM⁻¹ cm⁻²).     

Rapid and simultaneous determination of tetracycline and cefixime antibiotics by mean of gold nanoparticles-screen printed gold electrode and chemometrics tools

The screen-printed gold electrode (SPGE) modified with the formation of self-assembly monolayer (SAM) of cysteine (Cys) on gold-nanoparticles (Au_nano) was utilized for rapid and simultaneous determination of tetracycline and cefixime antibiotics by square wave voltammetry (SWV). Electrochemical investigation and characterization of the modified electrode was achieved using cyclic voltammetry (CV) and scanning electron microscopy (SEM). A principal component artificial neural network (PCANN) with three layer back-propagation network was utilized for the analysis of the voltammogram data. It is possible to simultaneously determine the tetracycline and cefixime concentrations in the ranges of 10⁻⁵ and 10⁻³ mol L⁻¹, under the optimum conditions. Moreover the SPGE-Au_nano-Cys biosensor together with chemometrics tools was successfully applied to the determination of tetracycline and cefixime in biological fluids, which may provide a promising alternative in routine biosensing applications.     

Application of L-DOPA modified carbon nanotubes as a bifunctional electrocatalyst for simultaneous determination of ascorbic acid,adrenaline, acetaminophen and tyrosine

L-DOPA multi-wall carbon nanotube modified glassy carbon electrode (DOPA-MWCNT-GCE) was used as a bifunctional electrocatalyst for simultaneous quantitative determination of ascorbic acid (AA) and adrenaline (AD). Electrochemical experiments show that the modified electrode plays the role of an excellent bifunctional electrocatalyst for the oxidation of AA and AD in two different potentials. The kinetic parameters such as the electron transfer coefficient, α, and the heterogeneous electron transfer rate constant, k′, for the electrocatalytic oxidation of AA and AD at the DOPA-MWCNT-GCE surface were estimated. Through a different pulse voltammetric (DPV) method, the plot of the electrocatalytic current versus AA and AD concentrations emerged to be constituted of two linear segments with different sensitivities. In addition, detection limits of 1.5 μM for AA and 0.62 μM for AD were obtained. In DPV, the proposed bifunctional electrocatalyst could separate the oxidation peak potentials of AA, AD, acetaminophen (AC) and tyrosine (Tyr) present in a mixture though, at the bare GCE, the peak potentials overlap. Finally, DOPA-MWCNT-GCE was satisfactorily used for the determination of AA, AD, AC and Tyr in pharmaceutical preparations.     

Effect of SiC particles on the friction and wear behavior of Ti3Si(Al)C2-based composites

The non-lubricated, sliding friction and wear behavior of Ti₃Si(Al)C₂ and SiC-reinforced Ti₃Si(Al)C₂ composites against AISI 52100 bearing steel ball were investigated using a ball-on-flat, reciprocating tribometer at room temperature. The contact load was varied from 5 to 20 N. For monolithic Ti₃Si(Al)C₂, high friction coefficients between 0.61 and 0.90 and wear rates between 1.79 × 10⁻³ and 2.68 × 10⁻³ mm³ (N m)⁻¹ were measured. With increasing SiC content in the composites, both the friction coefficients and the wear rates were significantly decreased. The friction coefficients reduced to a value between 0.38 and 0.50, and the wear rates to between 2.64 × 10⁻⁴ and 1.93 × 10⁻⁵ mm³ (N m)⁻¹ when the SiC content ranged from 10 to 30 vol.%. The enhanced wear resistance of Ti₃Si(Al)C₂ is mainly attributed to the facts that the hard SiC particles inhibit the plastic deformation and fracture of the soft matrix, the oxide debris lubricate the counterpair, and the wear mode converts from adhesive wear to abrasive wear during dry sliding.     

Tribological behavior of PEEK components with compositionally graded PEEK/PTFE surfaces

PEEK is a high strength engineering thermoplastic that suffers from a high friction coefficient and a friction induced wear mode. Past studies with 10 μm PEEK and PTFE powders resulted in composite solid lubricant that (at the optimal composition) had a wear rate of k = 2 × 10⁻⁹ mm³/Nm with a friction coefficient of μ = 0.12. A compositional grading of PEEK and PTFE is implemented in this study to create a bulk composite with the functional requirements of component strength, stiffness and wear resistance while providing solid lubrication at the sliding interface. The tribological performances of three functionally graded PEEK components were evaluated on linear reciprocating, rotating pin-on-disk and thrust washer tribometers. Wear rates comparable to samples of the bulk solid lubricant and comparable or improved frictional performance were achieved by compositionally grading the near surface region of PEEK components.     

1-N-alkyl -3-methylimidazolium ionic liquids as neat lubricants and lubricant additives in steel–aluminium contacts

The influence of the alkyl chain length and of the anion on the lubricating ability has been studied for the room-temperature ionic liquids (IL) 1-n-alkyl-3-methylimidazolium X⁻ [X = PF₆; n = 6 (L-P106). X = BF₄; n = 2 (L102), 6 (L106), 8 (L108). X = CF₃SO₃; n = 2 (L-T102). X = (4-CH3C6H4SO3); n = 2 (L-To102)]. Neat IL have been used for AISI 52100 steel-ASTM 2011 aluminium contacts in pin-on-disk tests under variable sliding speed. While all IL give initial friction values lower than 0.15, real-time sharp friction increments related to tribochemical processes have been observed for L102 and L-P106, at room-temperature and at 100 °C. Electronic microscopy (SEM), energy dispersive (EDS) and X-ray photoelectron (XPS) spectroscopies show that wear scar surfaces are oxidized to Al₂O₃ and wear debris contain aluminium and iron (for L102) fluorides. For L-P106, the steel surface is covered with a P-containing tribolayer. A change of anion (L-T102; L-To102) reduces friction and wear, but the lowest values are obtained by increasing the alkyl chain length (L106; L108). When the more reactive L102 and L-P106 are used as 1 wt.% base oil additives at 25 °C, tribocorrosion processes are not observed and a friction reduction (69–75% for 1 wt.% L102) and a change from severe (10⁻³ mm³ m⁻¹) to mild wear (10⁻⁴ to 10⁻⁶ mm³ m⁻¹) is obtained with respect to the neat IL. 1 wt.% IL additives also show good lubricating performance at 100 °C.     

Determination of the thermal conductivity of composted material

The objective of this study was to develop a reliable method for the determination of the thermal conductivity of composted material using the TP08 probe. Study was set out to determine whether the selection of a signal fragment used to establish thermal conductivity (λ), has a significant influence on the results. Also minimum number of measurements was determined for every phase of the composting process. No significant differences were reported between results, but certain changes in the value of λ were noted. In successive stages of the process, thermal conductivity of composted material were: 0.31 ± 0.09, 0.45 ± 0.14, 0.27 ± 0.03 and 0.37 ± 0.17 W m⁻¹ K⁻¹.     

Improved wear resistance in alumina-PTFE nanocomposites with irregular shaped nanoparticles

Past studies with PTFE nanocomposites showed up to 600× improvements in wear resistance over unfilled PTFE with the addition of Al₂O₃ nanoparticles. Irregular shaped nanoparticles are used in this study to increase the mechanical entanglement of PTFE fibrils with the filler. The tribological properties of 1, 2, 5 and 10 wt.% filled samples are evaluated under a normal pressure and sliding speed of 6.3 MPa and 50.8 mm/s, respectively. The wear resistance was found to improve 3000× over unfilled PTFE with the addition of 1 wt.% nanoparticles. The 5 wt.% sample had the lowest steady state wear rate of K = 1.3 × 10⁻⁷ mm³/N m and the lowest steady friction coefficient with μ = 0.21.     

Nano force sensing using symmetric double stage micro resonator

A new approach is proposed to improve a graphical approach with considering intensity coupling loss coefficients in the analytical derivation of the optical transfer functions for a symmetric double stage vertically coupled microring resonator. An optimum transmission coupling condition is determined with considering terms of couplers intensity loss which leads to low insertion loss of 1.2 dB, finesse of 1525, the out of band rejection ratio of 61.8 dB. The resonating system is used as an optical force sensing system to make the benefit of the accuracy of measurements in micro and nano scales. The sensitivity of proposed force sensor in terms of wavelength-shift is 33 nm/nN and the limit of detection is 1.6 × 10⁻² nN. The proposed sensing system has the advantages of self-calibration and the low power consumption due to the low intensity.     

A comparison of tribological properties of evenly distributed and agglomerated diamond nanoparticles in lubricated high-load steel–steel contact

The tribological properties of evenly distributed and agglomerated nanodiamonds on steel contact surfaces were compared in ethylene glycol lubricated tests using a pin-on-disc tribometer with a steel counter ball. The nanodiamond distributions were studied on silicon and steel surfaces using scanning electron microscopy. Friction and wear decreasing effects were observed with both sprayed and agglomerated nanodiamonds. The average friction coefficient with pure ethylene glycol lubricated contacts decreased from 0.16 to 0.12 with agglomerated nanodiamonds when 100 N load was applied. A minimum for both disc wear rate (0.40×10⁻⁶ mm³/Nm) and ball wear rate (0.29×10⁻⁶ mm³/Nm) was observed with agglomerated nanodiamonds. One of the mechanisms of nanodiamond lubrication was observed to be the incorporation of nanodiamond particles in to the tribolayer.     

Uncertainty evaluation of a 10N·m dead weight torque standard machine and comparison with a 1kN·m dead weight torque standard machine

A 10N·m dead weight torque standard machine (10-N·m-DWTSM) has been developed and evaluated since 2006 at the National Metrology Institute of Japan (NMIJ), a part of the National Institute of Advanced Industrial Science and Technology (AIST). Previously, the lengths of a moment arm, made of a low-thermal-expansion alloy (Super Invar), and the sensitivity limit of the fulcrum were evaluated. However, it is known that mechanical parts made of Super Invar vary in size with time. Therefore, the sensitivity limit of the fulcrum should be investigated under real calibration conditions. In this study, the moment arm lengths and the sensitivity limit of the fulcrum were re-evaluated. The moment arm lengths were found to have increased by an average of 6.3 μm in five years. The relative combined standard uncertainty of the moment arm length, w_arm, was re-evaluated in consideration of the uncertainty of the secular length change and was found to be 1.8 × 10⁻⁵. The sensitivity limit of the fulcrum was investigated by using a highly accurate, small-rated-capacity torque measuring device. The relative combined standard uncertainty due to the sensitivity limit of the fulcrum was 2.5 × 10⁻⁵ in the 0.1–10N·m torque range. The uncertainty budget table of the 10-N·m-DWTSM was completed. The relative expanded uncertainty of torque realized by the 10-N·m-DWTSM, W_tsm, was evaluated in the 0.1–10N·m torque range and was found to be 6.6 × 10⁻⁵, with a coverage factor, k, being equal to 2. In addition, the 10-N·m-DWTSM was compared with the existing 1-kN·m-DWTSM at NMIJ by using small-rated-capacity torque measuring devices at 5N·m and 10N·m torque steps. Two loading conditions were adopted in this comparison. The comparison results showed good agreement within the uncertainties in all cases. Thus, the torque realized by the 10-N·m-DWTSM was shown to be equivalent to that achieved by the 1-kN·m-DWTSM.     

Synthesis of multiple degrees-of-freedom spatial-motion compliant parallel mechanisms with desired stiffness and dynamics characteristics

This paper presents a new design method to synthesize multiple degrees-of-freedom (DOF) spatial-motion compliant parallel mechanisms (CPMs). Termed as the beam-based structural optimization approach, a novel curved-and-twisted (C-T) beam configuration is used as the basic design module to optimize the design parameters of the CPMs so as to achieve the targeted stiffness and dynamic characteristics. To derive well-defined fitness (objective) functions for the optimization algorithm, a new analytical approach is introduced to normalize the differences in the units, e.g., N/m or N m/rad, etc., for every component within the stiffness matrix. To evaluate the effectiveness of this design method, it was used to synthesize a 3-DOF spatial-motion (θ_x − θ_y − Z) CPM that delivers an optimized stiffness characteristics with a desired natural frequency of 100 Hz. A working prototype was developed and the experimental investigations show that the synthesized 3-DOF CPM can achieved a large workspace of 8°×8°×5.5 mm, high stiffness ratios, i.e., >200 for non-actuating over actuating stiffness, and a measured natural frequency of 84.4 Hz.     

Mechanical and unlubricated tribological properties of titanium-containing diamond-like carbon coatings

Titanium-containing diamond-like carbon (Ti-DLC) coatings were deposited on steel with a close-field unbalanced magnetron sputtering in a mixed argon/acetylene atmosphere. The morphology and structure of Ti-DLC coatings were investigated by scanning electron microscopy, transmission electron microscopy, atomic force microscopy and Raman spectroscopy. Nanoindentation, nanoscratch and unlubricated wear tests were carried out to evaluate the hardness, adhesive and tribological properties of Ti-DLC coatings. Electron microscopic observations demonstrated the presence of titanium-rich nanoscale regions surrounded by amorphous carbon structures in Ti-DLC coating. The Ti-DLC coatings exhibit friction coefficients of 0.12–0.25 and wear rates of 1.82 × 10^?9 to 4.29 × 10^?8 mm³/Nm, depending on the counterfaces, sliding speed and temperature. The Ti-DLC/alumina tribo-pair shows a lower friction coefficient than the Ti-DLC/steel tribo-pair under the identical wear conditions. Increasing the test temperature from room temperature to 200 °C reduces the coefficient of friction and, however, clearly increases the wear rate of Ti-DLC coatings. Different wear mechanisms, such as surface polishing, delamination and tribo-chemical reactions, were found in the tribo-contact areas, depending on different wear conditions.     

A comparative study on the wear properties of coarse-grained Al6061 alloy and nanostructured Al6061–Al2O3 composites

Wear behavior of nanostructured Al6061 alloy and Al6061–Al₂O₃ nanocomposites produced by milling and hot consolidation were investigated. The samples were characterized by hardness test, pin-on-disk wear test, X-ray diffraction (XRD), and scanning electron microscopy (SEM). Nanocomposites containing 3 vol% Al₂O₃ showed a maximum hardness of 235 HV and optimum wear rate of 4×10⁻³ mg/m. Increasing the amount of Al₂O₃ up to 5 vol% resulted in decrease in hardness values (∼112 HV) and a sharp rise in wear rate (∼18×10⁻³ mg/m).     

Structural optimization for flexure-based parallel mechanisms – Towards achieving optimal dynamic and stiffness properties

Flexure-based parallel mechanisms (FPMs) are a type of compliant mechanisms that consist of a rigid end-effector that is articulated by several parallel, flexible limbs (a.k.a. sub-chains). Existing design methods can enhance the FPMs’ dynamic and stiffness properties by conducting a size optimization on their sub-chains. A similar optimization process, however, was not performed for their sub-chains’ topology, and this may severely limit the benefits of a size optimization. Thus, this paper proposes to use a structural optimization approach to synthesize and optimize the topology, shape and size of the FPMs’ sub-chains. The benefits of this approach are demonstrated via the design and development of a planar X − Y − θ_z FPM. A prototype of this FPM was evaluated experimentally to have a large workspace of 1.2 mm × 1.2 mm × 6°, a fundamental natural frequency of 102 Hz, and stiffness ratios that are greater than 120. The achieved properties show significant improvement over existing 3-degrees-of-freedom compliant mechanisms that can deflect more than 0.5 mm and 0.5°. These compliant mechanisms typically have stiffness ratios that are less than 60 and a fundamental natural frequency that is less than 45 Hz.