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In this paper, methods of sample preparation for potentiometric measurement of phenylalanine are presented. Basing on the spectrophotometric measurements of phenylalanine, the concentrations of reagents of the enzymatic reaction (10 mM L-Phe, 0,4 mM NAD+, 2U L-PheDH) were determined. Then, the absorption spectrum of the reaction product, NADH, was monitored (maximum peak at 340 nm). The results obtained by the spectrophotometric method were compared with the results obtained by the colourimetry, using pH indicators. The above-mentioned two methods will be used as references for potentiometric measurements of phenylalanine concentration.
Hydrophobic magnetic nanoparticles (NPs) consisting of undecanoate-capped magnetite (Fe3O4, average diameter ca. 5 nm) are used to control quantized electron transfer to surface-confined redox units and metal NPs. A two-phase system consisting of an aqueous electrolyte solution and a toluene phase that includes the suspended undecanoatecapped magnetic NPs is used to control the interfacial properties of the electrode surface. The attracted magnetic NPs form a hydrophobic layer on the electrode surface resulting in the change of the mechanisms of the surface-confined electrochemical processes. A quinone-monolayer modified Au electrode demonstrates an aqueous-type of the electrochemical process (2e-+2H+ redox mechanism) for the quinone units in the absence of the hydrophobic magnetic NPs, while the attraction of the magnetic NPs to the surface results in the stepwise single-electron transfer mechanism characteristic of a dry nonaqueous medium. Also, the attraction of the hydrophobic magnetic NPs to the Au electrode surface modified with Au NPs (ca. 1.4 nm) yields a microenvironment with a low dielectric constant that results in the single-electron quantum charging of the Au NPs.
Micromachined thermal heater platforms offer low electrical power consumption and high modulation speed, i.e. properties which are advantageous for realizing nondispersive infrared (NDIR) gas- and liquid monitoring systems. In this paper, we report on investigations on silicon-on-insulator (SOI) based infrared (IR) emitter devices heated by employing different kinds of metallic and semiconductor heater materials. Our results clearly reveal the superior high-temperature performance of semiconductor over metallic heater materials. Long-term stable emitter operation in the vicinity of 1300 K could be attained using heavily antimony-doped tin dioxide (SnO2:Sb) heater elements.
Various planar technologies are employed for developing solid-state sensors having low cost, small size and high reproducibility; thin- and thick-film technologies are most suitable for such productions. Screen-printing is especially suitable due to its simplicity, low-cost, high reproducibility and efficiency in large-scale production. This technology enables the deposition of a thick layer and allows precise pattern control. Moreover, this is a highly economic technology, saving large amounts of the used inks. In the course of repetitions of the film-deposition procedure there is no waste of material due to additivity of this thick-film technology. Finally, the thick films can be easily and quickly deposited on inexpensive substrates. In this contribution, thick-film ion-selective electrodes based on ionophores as well as crystalline ion-selective materials dedicated for potentiometric measurements are demonstrated. Analytical parameters of these sensors are comparable with those reported for conventional potentiometric electrodes. All mentioned thick-film strip electrodes have been totally fabricated in only one, fully automated thickfilm technology, without any additional manual, chemical or electrochemical steps. In all cases simple, inexpensive, commercially available materials, i.e. flexible, plastic substrates and easily cured polymer-based pastes were used.
Multi-interface level sensors and new development in monitoring and control of oil separators
(2006)
In the oil industry, huge saving may be made if suitable multi-interface level measurement systems are employed for effectively monitoring crude oil separators and efficient control of their operation. A number of techniques, e.g. externally mounted displacers, differential pressure transmitters and capacitance rod devices, have been developed to measure the separation process with gas, oil, water and other components. Because of the unavailability of suitable multi-interface level measurement systems, oil separators are currently operated by the trial-and-error approach. In this paper some conventional techniques, which have been used for level measurement in industry, and new development are discussed.
In this paper, methods of surface modification of different supports, i.e. glass and polymeric beads for enzyme immobilisation are described. The developed method of enzyme immobilisation is based on Schiff’s base formation between the amino groups on the enzyme surface and the aldehyde groups on the chemically modified surface of the supports. The surface of silicon modified by APTS and GOPS with immobilised enzyme was characterised by atomic force microscopy (AFM), time-of-flight secondary ion mass spectroscopy (ToF-SIMS) and infrared spectroscopy (FTIR). The supports with immobilised enzyme (urease) were also tested in combination with microreactors fabricated in silicon and Perspex, operating in a flow-through system. For microreactors filled with urease immobilised on glass beads (Sigma) and on polymeric beads (PAN), a very high and stable signal (pH change) was obtained. The developed method of urease immobilisation can be stated to be very effective.
A new and simple method for nanostructuring using conventional photolithography and layer expansion or pattern-size reduction technique is presented, which can further be applied for the fabrication of different nanostructures and nano-devices. The method is based on the conversion of a photolithographically patterned metal layer to a metal-oxide mask with improved pattern-size resolution using thermal oxidation. With this technique, the pattern size can be scaled down to several nanometer dimensions. The proposed method is experimentally demonstrated by preparing nanostructures with different configurations and layouts, like circles, rectangles, trapezoids, “fluidic-channel”-, “cantilever”- and meander-type structures.
GaAs-based Gunn diodes with graded AlGaAs hot electron injector heterostructures have been developed under the special needs in automotive applications. The fabrication of the Gunn diode chips was based on total substrate removal and processing of integrated Au heat sinks. Especially, the thermal and RF behavior of the diodes have been analyzed by DC, impedance and S-parameter measurements. The electrical investigations have revealed the functionality of the hot electron injector. An optimized layer structure could fulfill the requirements in adaptive cruise control (ACC) systems at 77 GHz with typical output power between 50 and 90 mW.
A concept for a sensitive micro total analysis system for high throughput fluorescence imaging
(2006)
This paper discusses possible methods for on-chip fluorescent imaging for integrated bio-sensors. The integration of optical and electro-optical accessories, according to suggested methods, can improve the performance of fluorescence imaging. It can boost the signal to background ratio by a few orders of magnitudes in comparison to conventional discrete setups. The methods that are present in this paper are oriented towards building reproducible arrays for high-throughput micro total analysis systems (µTAS). The first method relates to side illumination of the fluorescent material placed into microcompartments of the lab-on-chip. Its significance is in high utilization of excitation energy for low concentration of fluorescent material. The utilization of a transparent µLED chip, for the second method, allows the placement of the excitation light sources on the same optical axis with emission detector, such that the excitation and emission rays are directed controversly. The third method presents a spatial filtering of the excitation background.
An array of 50 MHz quartz microbalances (QMBs) coated with a dendronized polymer was used to detect small amounts of volatile organic compounds (VOCs) in the gas phase. The results were compared to those obtained with the commonly used 10 MHz QMBs. The 50 MHz QMBs proved to be a powerful tool for the detection of VOCs in the gas phase; therefore, they represent a promising alternative to the much more delicate surface acoustic wave devices (SAWs).
Quartz crystal nanobalance (QCN) sensors are considered as powerful masssensitive sensors to determine materials in the sub-nanogram level. In this study, a single piezoelectric quartz crystal nanobalance modified with polystyrene was employed to detect benzene, toluene, ethylbenzene and xylene (BTEX compounds). The frequency shift of the QCN sensor was found to be linear against the BTEX compound concentrations in the range about 1-45 mg l-1. The correlation coefficients for benzene, toluene, ethylbenzene, and xylene were 0.991, 0.9977, 0.9946 and 0.9971, respectively. The principal component analysis was also utilized to process the frequency response data of the single piezoelectric crystal at different times, considering to the different adsorption-desorption dynamics of BTEX compounds. Using principal component analysis, it was found that over 90% of the data variance could still be explained by use of two principal components (PC1 and PC2). Subsequently, the successful identification of benzene and toluene was possible through the principal component analysis of the transient responses of the polystyrene modified QCN sensor. The results showed that the polystyrene-modified QCN had favorable identification and quantification performances for the BTEX compounds.
We report on the synthesis and CO gas-sensing properties of mesoporous tin(IV) oxides (SnO2). For the synthesis cetyltrimethylammonium bromide (CTABr) was used as a structure-directing agent; the resulting SnO2 powders were applied as films to commercially available sensor substrates by drop coating. Nitrogen physisorption shows specific surface areas up to 160 m2·g-1 and mean pore diameters of about 4 nm, as verified by TEM. The film conductance was measured in dependence on the CO concentration in humid synthetic air at a constant temperature of 300 °C. The sensors show a high sensitivity at low CO concentrations and turn out to be largely insensitive towards changes in the relative humidity. We compare the materials with commercially available SnO2-based sensors.
An H2O2 sensor for the application in industrial sterilisation processes has been developed. Therefore, automated sterilisation equipment at laboratory scale has been constructed using parts from industrial sterilisation facilities. In addition, a software tool has been developed for the control of the sterilisation equipment at laboratory scale. First measurements with the developed sensor set-up as part of the sterilisation equipment have been performed and the sensor has been physically characterised by optical microscopy and SEM.
The workflow of a high throughput screening setup for the rapid identification of new and improved sensor materials is presented. The polyol method was applied to prepare nanoparticular metal oxides as base materials, which were functionalised by surface doping. Using multi-electrode substrates and high throughput impedance spectroscopy (HT-IS) a wide range of materials could be screened in a short time. Applying HT-IS in search of new selective gas sensing materials a NO2-tolerant NO sensing material with reduced sensitivities towards other test gases was identified based on iridium doped zinc oxide. Analogous behaviour was observed for iridium doped indium oxide.
A solid-state amperometric hydrogen sensor based on a protonated Nafion membrane and catalytic active electrode operating at room temperature was fabricated and tested. Ionic conducting polymer-metal electrode interfaces were prepared chemically by using the impregnation-reduction method. The polymer membrane was impregnated with tetra-ammine platinum chloride hydrate and the metal ions were subsequently reduced by using either sodium tetrahydroborate or potassium tetrahydroborate. The hydrogen sensing characteristics with air as reference gas is reported. The sensors were capable of detecting hydrogen concentrations from 10 ppm to 10% in nitrogen. The response time was in the range of 10-30 s and a stable linear current output was observed. The thin Pt films were characterized by XRD, Infrared Spectroscopy, Optical Microscopy, Atomic Force Microscopy, Scanning Electron Microscopy and EDAX.
A multi-sensor system is a chemical sensor system which quantitatively and qualitatively records gases with a combination of cross-sensitive gas sensor arrays and pattern recognition software. This paper addresses the issue of data analysis for identification of gases in a gas sensor array. We introduce a software tool for gas sensor array configuration and simulation. It concerns thereby about a modular software package for the acquisition of data of different sensors. A signal evaluation algorithm referred to as matrix method was used specifically for the software tool. This matrix method computes the gas concentrations from the signals of a sensor array. The software tool was used for the simulation of an array of five sensors to determine gas concentration of CH4, NH3, H2, CO and C2H5OH. The results of the present simulated sensor array indicate that the software tool is capable of the following: (a) identify a gas independently of its concentration; (b) estimate the concentration of the gas, even if the system was not previously exposed to this concentration; (c) tell when a gas concentration exceeds a certain value. A gas sensor data base was build for the configuration of the software. With the data base one can create, generate and manage scenarios and source files for the simulation. With the gas sensor data base and the simulation software an on-line Web-based version was developed, with which the user can configure and simulate sensor arrays on-line.
Study of swift heavy ion modified conduction polymer composites for application as gas sensor
(2006)
A polyaniline-based conducting composite was prepared by oxidative polymerisation of aniline in a polyvinylchloride (PVC) matrix. The coherent free standing thin films of the composite were prepared by a solution casting method. The polyvinyl chloride-polyaniline composites exposed to 120 MeV ions of silicon with total ion fluence ranging from 1011 to 1013 ions/cm2, were observed to be more sensitive towards ammonia gas than the unirradiated composite. The response time of the irradiated composites was observed to be comparably shorter. We report for the first time the application of swift heavy ion modified insulating polymer conducting polymer (IPCP) composites for sensing of ammonia gas.
Functional testing and characterisation of ISFETs on wafer level by means of a micro-droplet cell
(2006)
A wafer-level functionality testing and characterisation system for ISFETs (ionsensitive field-effect transistor) is realised by means of integration of a specifically designed capillary electrochemical micro-droplet cell into a commercial wafer prober-station. The developed system allows the identification and selection of “good” ISFETs at the earliest stage and to avoid expensive bonding, encapsulation and packaging processes for nonfunctioning ISFETs and thus, to decrease costs, which are wasted for bad dies. The developed system is also feasible for wafer-level characterisation of ISFETs in terms of sensitivity, hysteresis and response time. Additionally, the system might be also utilised for wafer-level testing of further electrochemical sensors.
Close interrelations between sound and image are not a mere phenomenon of today’s multimedia technology. The idea of the synthesis of different media lies at the core of the concept of the Gesamtkunstwerk in the second half of the 19th century and it can also be traced back to the synaesthesia debate at the beginning of the 20th century [...].
This paper presents the direct route to Design by Analysis (DBA) of the new European pressure vessel standard in the language of limit and shakedown analysis (LISA). This approach leads to an optimization problem. Its solution with Finite Element Analysis is demonstrated for some examples from the DBA-Manual. One observation from the examples is, that the optimisation approach gives reliable and close lower bound solutions leading to simple and optimised design decision.
Safety and reliability of structures may be assessed indirectly by stress distributions. Limit and shakedown theorems are simplified but exact methods of plasticity that provide safety factors directly in the loading space. These theorems may be used for a direct definition of the limit state function for failure by plastic collapse or by inadaptation. In a FEM formulation the limit state function is obtained from a nonlinear optimization problem. This direct approach reduces considerably the necessary knowledge of uncertain technological input data, the computing time, and the numerical error. Moreover, the direct way leads to highly effective and precise reliability analyses. The theorems are implemented into a general purpose FEM program in a way capable of large-scale analysis.
Structural design analyses are conducted with the aim of verifying the exclusion of ratcheting. To this end it is important to make a clear distinction between the shakedown range and the ratcheting range. In cyclic plasticity more sophisticated hardening models have been suggested in order to model the strain evolution observed in ratcheting experiments. The hardening models used in shakedown analysis are comparatively simple. It is shown that shakedown analysis can make quite stable predictions of admissible load ranges despite the simplicity of the underlying hardening models. A linear and a nonlinear kinematic hardening model of two-surface plasticity are compared in material shakedown analysis. Both give identical or similar shakedown ranges. Structural shakedown analyses show that the loading may have a more pronounced effect than the hardening model.
Large industrial facilities and power plants often require a huge number fo information and control cables between the differnet structures. These I&C-cables can be routed in reinforced concrete cable ducts or in isolated buried cable runs. KTA 2206 is the German lightning protection standard for nuclear power plants. During the last several years considerable effort has been made to revise this standard. Despite the well established principles and design guidelines for the construction of the lightning protection system, this standard puts special emphasis on the coupling of transient overvoltages to I&C-cables.
Lightning protection design of a renewable energy hybrid-system without power mains connection
(2001)
In the year 2000 a direct lightning strike to the hybridsystem without power mains connection VATALI on the Greek island Crete results in the destruction and damage of some mechanical and electrical components. The hybrid-system VATALI was not lightning protected at that time. The hardware damage costs are approx. 60,000 €. The exposed site of the hybrid-system on top of a mountain was and still is the reason for a high risk of lightning strikes. Also in the future further lightning strikes have to be taken into consideration. In the paper a fundamental lightning protection design concept for renewable energy hybrid-systems without power mains connection and protection measures against direct strikes and overvoltages are shown in detail. The design concept was realized exemplarily for the hybrid-system VATALI. The hardware costs for the protection measures were about 15,000 €. About 50% of the costs are due to protection measures against direct strikes, 50% are due to overvoltage protection. Future extensions, new installations, or modifications have to be included into the lightning protection design concept of the hybrid-system.
In IEC 61312-2 equations for the assessment of the magnetic fields inside structures due to a direct lightning strike are given. These equations are based on computer simulations for shields consisting of a single-layer steel grid of a given mesh width. Real constructions, however, contain at least two layers of reinforcement steel grids. The objective of this study was to experimentally determine the additional shielding effectiveness of a second reinforcement layer compared to a single-layer grid. To this end, simulated structures were set up in the high current laboratory. The structures consisted of cubic cages of 2 m side length with one or with two reinforcement grids, respectively. The structures were exposed to direct lightning currents representing the variety of anticipated lightning current waveforms. The magnetic fields and their derivatives at several positions inside the structure as well as the voltage between “floor” and “roof” in the center were determined for different current injection points. From these data the improvement of the shielding caused by a second reinforcement layer is derived.
In the paper a lightning protection design concept for renewable energy hybrid-systems without power mains connection is described. Based on a risk analysis protection measures against direct strikes and overvoltages are shown in an overview. The design concept is realized exemplarily for the hybrid-system VATALI on the Greek island Crete. VATALI, not lightning protected at that time, was a victim of a lightning strike in the year 2000 causing destructions and damages of some mechanical and electrical components with costs of approx. 60.000 €. The hardware costs for the protection measures were about 15.000 €: about 50% of the costs are due to protection measures against direct strikes, 50% are due to overvoltage protection.
The paper deals with the development of the probabilistic approach to the assessment of risk due to lightning. Sources of damage, types of damage and types of loss are defined and, accordingly, the procedure for risk analysis and the way of assessment of different risk components is proposed. The way to evaluate the influence of different protection measures (lightning protection system; shielding of structure, cables and equipment; routing of internal wiring; surge protective device) in reducing such probabilities is considered. The paper has been prepared within the framework of the activity of IEC TC81-WG9/CLC TC81-WG4 directed to prepare the draft IEC 62305-2 Risk Management, in cooperation with the Secretary of IEC/CLC TC81.
For the application of the concept of Lightning Protection Zones (LPZ), the knowledge of the magnetic fields and induced voltages inside a structure is necessary. Laboratory experiments have been conducted at a downscaled model of a building (scale factor 1:6) to determine these electromagnetic quantities in case of a direct strike to the structure. The model (3 m x 2 m x 2 m) represented a small industrial building using the reinforcement of the concrete as electromagnetic shield. The magnetic fields and magnetic field derivatives were measured at several location inside the scaled model. Further, the voltages induced on three typical cable routes inside the model was determined. The influence of the lightning current waveshape, point-of-strike, bonding of the cable routes, and bridging of an expansion joint in the middle of the building on these quantities was studied.
In the paper the results obtained from experiments at a modelled reinforced building in case of a direct lightning strike are compared with calculations. The comparison includes peak values of the magnetic field Hmax, its derivative (dH/dt)max and of induced voltages umax in typical cable routings. The experiments are performed at a 1:6 scaled building and the results are extrapolated using the similarity relations theory. The calculations are based on the approximate formulae given in IEC 62305-4 and have to be supplemented by a rough estimation of the additional shielding effect of a second reinforcement layer. The comparison shows, that the measured peak values of the magnetic field and its derivative are mostly lower than the calculated. The induced voltages are in good agreement. Hence, calculations of the induced voltages based on IEC 62305-4 are a good method for lightning protection studies of buildings, where the reinforcement is used as a grid-like electromagnetic shield.
IEC Technical Committee 81 is currently creating the new IEC 62305 series of standards on Lightning Protection. Working Group 9 is responsible for Part 2 of this series, which deals with the assessment and management of risk its CDV (Committee Draft for Voting) stage and has been circulated to National Committees for comment. The paper details the development of the Simplified IEC Risk Assessment Calculator software tool as described in Informative Annex J of IEC62305-2 Ed.1/CDV 2. This tool is intended as a simplified implementation of the more rigorous treatment of risk management found in the written document. It is designed to be relatively intuitive for users who wish to obtain an initial assessment of risk sensitivity, but should not be considered a substitute to a full understanding of the methods provided in the standard when dealing with more complicated structures or those where greater risks to personal or system operation are involved.