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12 The competitive business environment of manufacturing industries requires efficient strategies to increase yield and quality, while decreasing waste, down-time, and energy used. Among these strategies, analyzers are becoming vital to automated process monitoring and control. This conference includes the primary steps required to bring an advanced sensor, analyzer or instrument from inception to implemented process control. Here we present a lighthearted view of the pitfalls encountered in bringing an analytical instrument from the laboratory to the production plant. Two worst case scenarios are given. The `lessons learned' from these experiences are discussed in terms of a step-by-step path to implementing process instrumentation.
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12 Many spectroscopic monitoring techniques employ chemometric algorithms like principal component regression for calibration and evaluation of optical spectra. Systems based on this method, however, suffer from unknown spectral features appearing after calibration, which may result in major errors. The detection of non-calibrated absorption lines is important for treating errors in chemical processes. For these two reasons, the detection and classification of non-calibrated absorption features is of great importance in on-line spectroscopy. A novel approach is proposed here. A wavelet representation of principal components and measured spectra is shown to be appropriate for detection of non-calibrated spectral features. The algorithm can also be applied in combination with partial least-squares.
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12 Infrared absorption method in analyzing gas components is a traditional spectrum analyzing method of gas. Nevertheless, the distribution of the absorption spectrum of a certain kind of gas intercrosses with another's, which means that the absorption peaks of two kinds of gases are near very close. So, when those kinds of gases aforementioned are mixed together, the spectrum analysis will have the cross sensitivity. In this paper, the genetic neural network algorithm is adopted to recognize the patterns of the mixed gases with three components in the simulation recognition. The genetic algorithm decreases the cross sensitivity of the gas sensor. Especially the staged-sectional method is used to increase the recognition accuracy of various over-limit value.
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12 We have assembled and used several different phase-modulated optical polarimeters to measure transient retardance and molecular orientation angle in complex fluids and materials. The main difference in the instrumentation of the polarimeters lies in their modulation technique. Three different phase modulation techniques were used. These included techniques incorporating photoelastic, electro- optic and liquid crystal elements as the modulation source. The precise measurement of a material's retardance and average molecular orientation angle depends on an accurate calibration within the modulation range. In this paper, we address some of the problems associated with phase-modulated polarimeter calibration and techniques used to overcome them.
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12 Argonne National Laboratory has been creating a special- purpose software-engineering tool to support research and development of spectrum-output-type [chemical] sensors. The modular software system is called SAGE, the Sensor Algorithm Generation Environment and includes general- purpose signal conditioning algorithms (GP/SAGE) as well as intelligent classifiers, pattern recognizers, response accelerators, and sensitivity analyzers. GP/SAGE is an implementation of an approach for delivering a level of encapsulated intelligence to a wide range of sensors and instruments. It capitalizes on the generic classification and analysis needed to process most profile-type data. The GP/SAGe native data format is a generalized 1D vector, signature, or spectrum. GP/SAGE modules form a computer- aided software engineering `workbench' where users can experiment with various conditioning, filtering, and pattern recognition stages, then automatically generate final algorithm source code for data acquisition and analysis systems.
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On-Line Instrumentation: Biotech and Pharmaceutical
12 Modern bioprocess control requires fast data acquisition and in-time evaluation of bioprocess variables. On-line fluorescence spectroscopy for data acquisition and the use of chemometric methods accomplish these requirements. The presented investigations were performed with fluorescence spectrometers with wide ranges of excitation and emission wavelength. By detection of several biogenic fluorophors (amino acids, coenzymes and vitamins) a large amount of information about the state of the bioprocess are obtained. For the evaluation of the process variables partial least squares regression is used. This technique was applied to several bioprocesses: the production of ergotamine by Claviceps purpurea, the production of t-PA (tissue plasminogen activator) by animal cells and brewing processes. The main point of monitoring the brewing processes was to determine the process variables cell count and extract concentration.
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12 The objective of this paper is to describe a method for detecting x-ray in real time with high spatial resolution. The method uses a 1-meter glass fiber, a 2 mm plastic scintillator, and a collecting device such as photomultiplier tube to respond to the radiation field. This device can be automated for use in any industries, which uses radiation for their processes. The resolution can only be limited by the size of the detector. This plastic scintillator probe has a homogeneous sensitivity and it water equivalent. The scintillator minimizes dose perturbation in water, and it has a emission peak around 432 nm. The reproducibility of the system has been tested, and the percent variation has been less than 3%. The results compared with GafChromic film showed this device is reliable, and it could be used in real time measurements.
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12 In the paper, a new method of flaw evaluation in time for an organized production is presented. A statistical correlation between the number of flows, the degree of gravity, the optimum production volume, the operators qualification level and their testing charge was established. The demerit method is a statistics one based on according a number of points to the defect types as function of their gravity degree. The `demerit' (term derived from French `sans merite') represents a mediation coefficient of the defects frequency pondered according to the assigned points. The `demerit' represents a synthetic complex and complete indicator, related to the defect number as well as to their gravity level.
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On-Line Instrumentation: Chemical and Petrochemical
12 The Gas-Oil Ratio (GOR) of crude oil has a tremendous impact on the processes used for oil production from subsurface formations. Determination of GOR thus becomes of central importance to oil operating companies. Here, it is shown that near-infrared (NIR) spectral measurements on single- phase crude oils (with dissolved gas) can be used to obtain a reliable estimate of the GOR. Furthermore, the NIR measurement is shown to be compatible with process flow streams at elevated temperatures and pressures.
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12 The present work reports measurements on a General Electric Dry Low NOx premixed combustor (mod. DLN for gas turbine LM 1600, 2500 and 6000) by using broadband Coherent Anti-Stokes Raman Spectroscopy in the planar BOXCARS configuration. Experimental spectra have been compared with theoretical nitrogen spectra at atmospheric pressure through a neural network analysis. In order to obtain instantaneous temperature measurements the simulated spectra have been calculated in a wide range of temperatures (300 - 2500 degree(s)K), thus permitting a fast comparison with the experimental spectra obtained from the flame. The data obtained in this work are now used to test numerical simulations of kinetic and chemical models employed in the code FLUENT.
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12 Non-dispersive analyzers have been used for measurement of gases for many years and were recently introduced as on-line meters for continuous stack emission measurements in industrial plants. SO2 and NO2 are among the most important gases in the emissions of the petrochemical industry. The development of a UV-visible meter for these gases is presented. It consists of three optical channels sensing different spectral regions: 300 nm for SO2, 380 nm for NO2 and 320 nm used as a common reference. Each channel has an interference filter of 10 nm bandwidth centered at each channel's wavelength. Each filter is followed by a photodiode and its electronics which are housed in a single compartment with no moving parts. An incandescent lamp with high output in the UV region was selected and mounted on the opposite side of the stack by appropriate flanges. The equipment was designed to measure in the range between 0 and 500 ppmv with a resolution of about 2 ppmv. Performance parameters like signal stability, dark current, detection limit and calibration curves are shown.
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12 The superior engineering properties of fiber reinforced polymer matrix composites, primarily the high strength-to- weight ratio, make them suitable to applications ranging from sporting goods to aircraft components (e.g. helicopter blades). Unfortunately, consistent fabrication of components with desired mechanical properties has proven difficult, and has led to high production costs. This is largely due to the inability to monitor and control polymer cure, loosely defined as the process of polymer chain extension and cross- linking. Even with stringent process control, slight variations in the pre-polymer formulations (e.g. prepreg) can influence reaction rates, reaction mechanisms, and ultimately, product properties. In an effort to optimize the performance of thermoset composite, we have integrated fiber optic probes between the plies of laminates and monitored cure by Raman spectroscopy, with the eventual goal of process control. Here we present real-time measurements of two high performance aerospace companies cured within an industrial autoclave.
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12 An optical fiber probe designed for use with molecularly imprinted polymers (MIP) is detailed and evaluated with respect to fluorescence sensitivity enhancements. MIPs are polymeric materials that are selective towards a molecule included in the mixture during the formation of the polymer. MIPs allow the selective analysis of a single analyte contained in a complex mixture through the interactions of the analyte with analyte-specific cavities formed within the polymer matrix. The optical design involves a dual optical fiber probe coupled to a transparent capillary for enhanced fluorescence excitation and emission collection. The inner capillary surface is coated with the MIP to select the analyte of choice while the capillary serves to enhance the fluorescence signal obtained. The selectivity and sensitivity of the MIP probe toward anthracene in water is discussed.
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12 An advanced multiple gas analyzer based on in-situ Fourier transform infrared spectroscopy has been used to successfully measure the exhaust plume composition and temperature of an operating gas turbine engine at a jet engine test stand. The sensor, which was optically coupled to the test cell using novel broadband hollow glass waveguides, performed well in this harsh environment (high acoustical noise and vibration, considerable temperature swings in the ambient with engine operation), providing quantitative gas phase information. Measurements were made through the diameter of the engine's one meter exhaust plume, about 0.7 meters downstream of the engine exit plane. The sensor performed near simultaneous infrared transmission and infrared emission measurements through the centerline of the plume. Automated analysis of the emission and transmission spectra provided the temperature and concentration information needed for engine tuning and control that will ensure optimal engine operation and reduced emissions. As a demonstration of the utility and accuracy of the technique, carbon monoxide, nitric oxide, water, and carbon dioxide were quantified in spite of significant variations in the exhaust gas temperature. At some conditions, unburned fuel, particulates (soot/fuel droplets), methane, ethylene and aldehydes were identified, but not yet quantified.
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12 According to the principle of the multibubble cavitation oxidation and chemiluminescence of the luminol in aqueous alkaline solution, this paper introduces an ultrasound- induced fluorescence: sonofluorescence (SF) and designs its experimental set-up. Using the set-up, the authors detect the SF emission of the aqueous luminol-NaOH solution, take the pictures of the SF of the cavitating aqueous luminol- NaOH and -NaHCO3 solutions and observe the impacts of Cu2+ on the SF spectra of the aqueous solutions of luminol-NaOH, -Ca(OH)2 and -Na2CO3. Finally, the authors discuss the experimental SF and its potential applications.
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12 To address the inherent issues with extractive sampling, Air Liquide and PSI are collaborating on the development of an in-situ multi-functional near-IR tunable diode laser system. The system is specifically targeted for application in harsh combustion environments with flue gas temperatures > 1600 degree(s)C and high particle densities. The multiplexing capability of the diode laser system allows near simultaneous detection of CO, O2, and H2O. These are essential species in characterizing the combustion state of the process, i.e., fuel-rich or fuel-lean, and the flue gas temperature. Sensor development and testing are conducted on a 700 kW oxy-fuel pilot furnace to evaluate the performance under simulated industrial conditions. Here we present pilot test results for dynamic stoichiometry changes, effect of particle entrainment, and air infiltration monitoring.
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12 In recent years a big effort has been made by gas turbine manufacturers in order to design industrial combustion apparata with high efficiency. Laser based diagnostic methods have become now a powerful tool for monitoring the performance of these devices. A portable high sensitive diode laser gas analyzer has been used to detect the unburned methane in the exhaust of a 213 kW combustor (General Electric DLE). The main features of the methane analyzer are a tunable diode laser operating at room temperature emitting radiation at 1.65 micrometers and a Chernin optical multipass cell. The gas analyzer is controlled by a computer program, which can supply real time concentration measurements. The latter characteristic coupled to its limited dimensions allow for in situ implementation of the spectroscopic tool.
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12 An optical near-IR process sensor for electric arc furnace pollution control and energy efficiency has been proposed. A near-infrared laser has performed simultaneous in-situ measurements of CO (1577.97 nm), H2O (1577.8 nm and 1578.1 nm) and temperature in the exhaust gas region above a laboratory burner fueled with methane and propane. The applicable range of conditions tested is representative of those found in a commercial electric arc furnace and includes temperatures from 1250 - 1750 K, CO concentrations from 0 to 10% and H2O concentrations from 3 to 27%. Two- tone frequency modulation was used to increase the detection sensitivity. An analysis of the method's accuracy has been conducted using 209 calibration and 105 unique test burner setpoints. Based on the standard deviation of differences between optical predictions and independently measured values, the minimum accuracy of the technique has been estimated as 36 K for temperature, 0.47% for CO and 3.4% for H2O. This accuracy is sufficient for electric arc furnace control. The sensor's ability to non-intrusively measure CO and temperature in real time will allow for improved process control in this application.
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On-Line Instrumentation: Chemical and Petrochemical
12 Mercury emissions from industrial stacks pose a hazardous threat to human being. Conventional methods of atomic absorption and plasma emission spectroscopy have their limitations. In order to develop a sensitive real-time measurement approach for industrial applications, an ultraviolet interferometer system capable of Fourier transform spectrochemical measurements has been preliminary studied in our laboratory. Though interferometry approach is mostly used in infrared, the interferometer we developed has showed its great potential for application in atomic emission detection in ultraviolet. We have set up the interferometer in Michelson configuration. Light source of our choice is low pressure mercury pen lamp which provides strong atomic mercury emissions at 253.7 nm. Fringe patterns at 253.7 nm and 546.1 nm were pictured by a charge-coupled- device camera. Moving fringes was generated by linear displacement of the movable mirror of the Michelson interferometer. The interferograms at both ultraviolet and visible regions of atomic mercury emission spectrum were recorded. Based on the translation function of movable mirror, wavelength information is retrieved from the interferogram. The error of experimental resolved wavelength is within 2%.
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