Direct determination of calcium in milk by atomic absorption spectrometry using flow-injection analysis

A flow-injection system with sample and reagent addition by the synchronous merging zones approach for calcium determination in milk by flame AAS is proposed. Main parameters were optimized using a factorial design with central point. The optimum conditions were 2.5% (m/v) for La concentration, 8 mL min-1 for the carrier flow-rate, 20 cm for coiled reactor and 250 ìL for sample volume. Different sample preparation procedures were evaluated such as dilution in water or acid and microwave-assisted decomposition using concentrated or diluted acids. The optimized flow system was applied to determine Ca in eleven commercial milk samples and two standard reference materials diluted in water. Similar calcium levels were encountered comparing the results obtained by the proposed method (dilution in water) with those obtained using microwave-oven digestion. Results obtained in two standard reference materials were in agreement at 95% confidence level with those certified. Recoveries of spiked samples were in the 93% - 116% range. Relative standard deviation (n = 12) was < 5.4% and the sample throughput was 150 measurements per hour, corresponding to a consumption of 250 µL of sample and 6.25 mg La per determination.

Harmonical oscillator and electro-mechanical analogy: an interdiscinary experiment to high precision mass variation measurements

In general, the traditional Physics courses needs examples of the aplications of the Physics concepts in other areas such as Chemistry and Biology. This lacks tend to demotivate Chemistry and Biology students regarding to deal with Physical concepts developed in classroom. In this work, the analogy among mechanic and electric oscillators is investigated to be applied in Chemistry and Biology areas, showing to be valuable due to its aplication in techniques that aims to measure mass variation with high precision. This measure could be made in a direct or indirect way. These techniques are known as electrogravimetric techniques and they are important in biosensor aplications. Thus, this paper explores the electromechanic analogy in an interdisciplinary way involving areas like Physics, Chemistry and Biology. Based on this analogy, it is proposed an experiment that can be applied in different ways, i.e. by an basic approach or more deeper, depending on the students specific formation, in other words, Physics, Chemistry or Biology.

Online Ultrasound Measurements of Membrane Compaction

There are several filtration applications in the pulp and paper industry where the capacity and cost-effectiveness of processes are of importance. Ultrafiltration is used to clean process water. Ultrafiltration is a membrane process that separates a certain component or compound from a liquid stream. The pressure difference across the membrane sieves macromolecules smaller than 0.001-0.02 μm through the membrane. When optimizing the filtration process capacity, online information about the conditions of the membrane is needed. Fouling and compaction of the membrane both affect the capacity of the filtration process. In fouling a “cake” layer starts to build on the surface of the membrane. This layer blocks the molecules from sieving through the membrane thereby decreasing the yield of the process. In compaction of the membrane the structure is flattened out because of the high pressure applied. The higher pressure increases the capacity but may damage the structure of the membrane permanently. Information about the compaction is needed to effectively operate the filters. The objective of this study was to develop an accurate system for online monitoring of the condition of the membrane using ultrasound reflectometry. Measurements of ultrafiltration membrane compaction were made successfully utilizing ultrasound. The results were confirmed by permeate flux decline, measurements of compaction with a micrometer, mechanical compaction using a hydraulic piston and a scanning electron microscope (SEM). The scientific contribution of this thesis is to introduce a secondary ultrasound transducer to determine the speed of sound in the fluid used. The speed of sound is highly dependent on the temperature and pressure used in the filters. When the exact speed of sound is obtained by the reference transducer, the effect of temperature and pressure is eliminated. This speed is then used to calculate the distances with a higher accuracy. As the accuracy or the resolution of the ultrasound measurement is increased, the method can be applied to a higher amount of applications especially for processes where fouling layers are thinner because of smaller macromolecules. With the help of the transducer, membrane compaction of 13 μm was measured in the pressure of 5 bars. The results were verified with the permeate flux decline, which indicated that compaction had taken place. The measurements of compaction with a micrometer showed compaction of 23–26 μm. The results are in the same range and confirm the compaction. Mechanical compaction measurements were made using a hydraulic piston, and the result was the same 13 μm as obtained by applying the ultrasound time domain reflectometry (UTDR). A scanning electron microscope (SEM) was used to study the structure of the samples before and after the compaction.

Compton scattering tomography for agricultural measurements

This paper presents a new approach in tomographic instrumentation for agriculture based on Compton scattering, which allows for the simultaneous measurements of density and moisture of soil samples. Compton tomography is a technique that can be used to obtain a spatial map of electronic density of samples. Quantitative results can be obtained by using a reconstruction algorithm that takes into account the absorption of incident and scattered radiation. Results show a coefficient of linear correlation better than 0.81, when comparison is made between soil density measurements based on this method and direct transmission tomography. For soil water contents, a coefficient of linear correlation better than 0.79 was found when compared with measurements obtained by time domain reflectrometry (TDR). In addition, a set of Compton scatter images are presented to illustrate the efficacy of this imaging technique, which makes possible improved spatial variability analysis of pre-established planes.

Frequency-Domain and Wide-Pulse Time-Domain Measurements of Lanthanide Luminescence and Lanthanide-Based Resonance Energy Transfer

Resonance energy transfer (RET) is a non-radiative transfer of the excitation energy from the initially excited luminescent donor to an acceptor. The requirements for the resonance energy transfer are: i) the spectral overlap between the donor emission spectrum and the acceptor absorption spectrum, ii) the close proximity of the donor and the acceptor, and iii) the suitable relative orientations of the donor emission and the acceptor absorption transition dipoles. As a result of the RET process the donor luminescence intensity and the donor lifetime are decreased. If the acceptor is luminescent, a sensitized acceptor emission appears. The rate of RET depends strongly on the donor–acceptor distance (r) and is inversely proportional to r6. The distance dependence of RET is utilized in binding assays. The proximity requirement and the selective detection of the RET-modified emission signal allow homogeneous separation free assays. The term lanthanide-based RET is used when luminescent lanthanide compounds are used as donors. The long luminescence lifetimes, the large Stokes’ shifts and the intense, sharply-spiked emission spectra of the lanthanide donors offer advantages over the conventional organic donor molecules. Both the organic lanthanide chelates and the inorganic up-converting phosphor (UCP) particles have been used as donor labels in the RET based binding assays. In the present work lanthanide luminescence and lanthanide-based resonance energy transfer phenomena were studied. Luminescence lifetime measurements had an essential role in the research. Modular frequency-domain and time-domain luminometers were assembled and used successfully in the lifetime measurements. The frequency-domain luminometer operated in the low frequency domain ( 100 kHz) and utilized a novel dual-phase lock-in detection of the luminescence. One of the studied phenomena was the recently discovered non-overlapping fluorescence resonance energy transfer (nFRET). The studied properties were the distance and temperature dependences of nFRET. The distance dependence was found to deviate from the Förster theory and a clear temperature dependence was observed whereas conventional RET was completely independent of the temperature. Based on the experimental results two thermally activated mechanisms were proposed for the nFRET process. The work with the UCP particles involved the measurement of the luminescence properties of the UCP particles synthesized in our laboratory. The goal of the UCP particle research is to develop UCP donor labels for binding assays. In the present work the effect of the dopant concentrations and the core–shell structure on the total up-conversion luminescence intensity, the red–green emission ratio, and the luminescence lifetime was studied. Also the non-radiative nature of the energy transfer from the UCP particle donors to organic acceptors was demonstrated for the first time in aqueous environment and with a controlled donor–acceptor distance.

Positron measurements in Mg-doped GaN and development of digital Doppler broadening spectroscopy

In this work parameters of Mg-doped GaN samples were studied using positron annihilation spectroscopy and analyzed. It is shown that gallium vacancies exist in an unintentionally doped sample. Next, the sample with higher concentration of Mg and low growth temperature contains vacancy clusters. In case of low concentration of Mg the growth temperature does not affect the formation of defects. Analog electronics can be replaced by a modern digital device. While promising a high quantity of benefits, the performance of these digitizers requires thorough adjustment. A 14-bit two channel digitizer has been tested in order to achieve better performance than the one of a traditional analog setup, and the adjustment process is described. It has been shown that the digital device is unable to achieve better energy resolution, but it is quite close to the corresponding attribute of the available analog system, which had been used for measurements in Mg-doped GaN.

Quantum Tomography with Phase Space Measurements

This thesis addresses the use of covariant phase space observables in quantum tomography. Necessary and sufficient conditions for the informational completeness of covariant phase space observables are proved, and some state reconstruction formulae are derived. Different measurement schemes for measuring phase space observables are considered. Special emphasis is given to the quantum optical eight-port homodyne detection scheme and, in particular, on the effect of non-unit detector efficiencies on the measured observable. It is shown that the informational completeness of the observable does not depend on the efficiencies. As a related problem, the possibility of reconstructing the position and momentum distributions from the marginal statistics of a phase space observable is considered. It is shown that informational completeness for the phase space observable is neither necessary nor sufficient for this procedure. Two methods for determining the distributions from the marginal statistics are presented. Finally, two alternative methods for determining the state are considered. Some of their shortcomings when compared to the phase space method are discussed.

Tunable lumped-element bandpass filters for Cognitive Radio application

In this thesis the design of bandpass filters tunable at 400 MHz – 800 MHz was under research. Microwave filters are vital components which provide frequency selectivity in wide variety of electronic systems operating at high frequencies. Due to the occurrence of multi-frequency bands communication and diverse applications of wireless devices, requirement of tunable filters exists. The one of potential implementation of frequency-agile filters is frontends and spectrum sensors in Cognitive Radio (CR). The principle of CR is to detect and operate at a particular available spectrum without interfering with the primary user’s signals. This new method allows improving the efficiency of utilizing allocated spectrum such as TV band (400 MHz – 800 MHz). The focus of this work is development of sufficiently compact, low cost tunable filters with quite narrow bandwidth using currently available lumped-element components and PCB board technology. Filter design, different topologies and methods of tuning of bandpass filters are considered in this work. As a result, three types of topologies of bandpass filter were simulated and realised. They use digitally tunable capacitors (DTCs) for adjusting central frequency at TV "white space" spectrum. Measurements revealed that schematics presented in this work have proper output response and filters are successfully tuned by DTCs.

Mathematical modeling of level of anaesthesia from EEG measurements

Problem of modeling of anaesthesia depth level is studied in this Master Thesis. It applies analysis of EEG signals with nonlinear dynamics theory and further classification of obtained values. The main stages of this study are the following: data preprocessing; calculation of optimal embedding parameters for phase space reconstruction; obtaining reconstructed phase portraits of each EEG signal; formation of the feature set to characterise obtained phase portraits; classification of four different anaesthesia levels basing on previously estimated features. Classification was performed with: Linear and quadratic Discriminant Analysis, k Nearest Neighbours method and online clustering. In addition, this work provides overview of existing approaches to anaesthesia depth monitoring, description of basic concepts of nonlinear dynamics theory used in this Master Thesis and comparative analysis of several different classification methods.

A high frequency electronic transducer for multiphase flow measurements

This paper describes an electronic transducer for multiphase flow measurement. Its high sensitivity, good signal to noise ratio and accuracy are achieved through an electrical impedance sensor with a special guard technique. The transducer consists of a wide bandwidth and high slew rate differentiator where the lead inductance and stray capacitance effects are compensated. The sensor edge effect is eliminated by using a guard electrode based on the virtual ground potential of the operational amplifier. A theoretical modeling and a calibration method are also presented. The results obtained seem to confirm the validity of the proposed technique.

Drop Size Measurements in a Laboratory Scale Venturi Scrubber

Venturi scrubbers are high efficiency gas cleaners in which suspended particles are removed from gas streams by droplets formed by liquid atomisation, usually in the venturi throat. The size of the droplets formed is of fundamental importance to the performance of the equipment, both in terms of pressure drop and collection efficiency. In this study, drop sizes in a cylindrical laboratory scale venturi scrubber were measured using a laser diffraction technique. Gas velocity and liquid to gas ratios varied from 50 to 90 m/s and 0.5 to 2.0 l/m3, respectively. Water was inserted as perpendicular jets at the beginning of the throat. Measurements were performed at three positions: two located along the throat, and the last one at the end of the diffuser. The data presented here are a typical example of pneumatic atomisation and can be relevant to other industrial applications such as combustion and engine technology. Finally, results are compared to available correlations and the validity of these equations is discussed.

Characterization of capacitive sensors for measurements of the moisture in irrigated soils

The irrigation is a technique developed to supply the hydric needs of the plants. The use of the water should be optimized so that the culture just has enough for its growth, avoiding waste. The objective of this work was to characterize the behavior of capacitive sensors of humidity to monitor the moisture in the soils. In first instance, it was appraised sensors with dielectric built of synthetic pomes stone (Rd = 0,4 and Rd = 0,8) and of soil samples (Rd = 0,8 and Rd = 1,0), being the Rd parameter a geometric factor that relates the distance between the capacitor plates with radius of the plates. For the calibration, the sensors were installed in PVC recipient of cylindrical shape, filled with soil. The set (sensor and soil) was humidified by capillary effect and submitted by a natural drying very slowly. The parameter readings were taken daily, which allowed obtain the curves relating the humidity percentage, expressed in terms of dry weight, with the output voltage fort the sensor. The experiments were performed in sand soil and in dark red latossolo. The obtained results allowed to infer that the behavior of the sensor has a specific feature for each type of soil, being, therefore, necessary to develop a own calibration curve for the sensor, when used in soil with specific characteristic.

Machine vision methods for process measurements in pulping

The papermaking industry has been continuously developing intelligent solutions to characterize the raw materials it uses, to control the manufacturing process in a robust way, and to guarantee the desired quality of the end product. Based on the much improved imaging techniques and image-based analysis methods, it has become possible to look inside the manufacturing pipeline and propose more effective alternatives to human expertise. This study is focused on the development of image analyses methods for the pulping process of papermaking. Pulping starts with wood disintegration and forming the fiber suspension that is subsequently bleached, mixed with additives and chemicals, and finally dried and shipped to the papermaking mills. At each stage of the process it is important to analyze the properties of the raw material to guarantee the product quality. In order to evaluate properties of fibers, the main component of the pulp suspension, a framework for fiber characterization based on microscopic images is proposed in this thesis as the first contribution. The framework allows computation of fiber length and curl index correlating well with the ground truth values. The bubble detection method, the second contribution, was developed in order to estimate the gas volume at the delignification stage of the pulping process based on high-resolution in-line imaging. The gas volume was estimated accurately and the solution enabled just-in-time process termination whereas the accurate estimation of bubble size categories still remained challenging. As the third contribution of the study, optical flow computation was studied and the methods were successfully applied to pulp flow velocity estimation based on double-exposed images. Finally, a framework for classifying dirt particles in dried pulp sheets, including the semisynthetic ground truth generation, feature selection, and performance comparison of the state-of-the-art classification techniques, was proposed as the fourth contribution. The framework was successfully tested on the semisynthetic and real-world pulp sheet images. These four contributions assist in developing an integrated factory-level vision-based process control.