Fiber Bragg grating sensor interrogation system using a CCD side detection method with Superimposed blazed gratings

We present, for the first time to our knowledge, experimental evidence showing that superimposed blazed fiber Bragg gratings may be fabricated and used to extend the dynamic range of a grating-based spectrometer. Blazed gratings of 4° and 8° were superimposed in germanosilicate fiber by ultraviolet inscription and used in conjunction with a coated charged-coupled device array to interrogate a wavelength-division-multiplexing sensor array. We show that the system can be used to monitor strain and temperature sensors simultaneously with an employable bandwidth which is extendable to 70 nm.

The design of fault tolerant software for loosely coupled distributed systems

Requirements for systems to continue to operate satisfactorily in the presence of faults has led to the development of techniques for the construction of fault tolerant software. This thesis addresses the problem of error detection and recovery in distributed systems which consist of a set of communicating sequential processes. A method is presented for the `a priori' design of conversations for this class of distributed system. Petri nets are used to represent the state and to solve state reachability problems for concurrent systems. The dynamic behaviour of the system can be characterised by a state-change table derived from the state reachability tree. Systematic conversation generation is possible by defining a closed boundary on any branch of the state-change table. By relating the state-change table to process attributes it ensures all necessary processes are included in the conversation. The method also ensures properly nested conversations. An implementation of the conversation scheme using the concurrent language occam is proposed. The structure of the conversation is defined using the special features of occam. The proposed implementation gives a structure which is independent of the application and is independent of the number of processes involved. Finally, the integrity of inter-process communications is investigated. The basic communication primitives used in message passing systems are seen to have deficiencies when applied to systems with safety implications. Using a Petri net model a boundary for a time-out mechanism is proposed which will increase the integrity of a system which involves inter-process communications.

A novel detection method for determining a surgeon's fatigue and hand tremor

The thesis presents new methodology and algorithms that can be used to analyse and measure the hand tremor and fatigue of surgeons while performing surgery. This will assist them in deriving useful information about their fatigue levels, and make them aware of the changes in their tool point accuracies. This thesis proposes that muscular changes of surgeons, which occur through a day of operating, can be monitored using Electromyography (EMG) signals. The multi-channel EMG signals are measured at different muscles in the upper arm of surgeons. The dependence of EMG signals has been examined to test the hypothesis that EMG signals are coupled with and dependent on each other. The results demonstrated that EMG signals collected from different channels while mimicking an operating posture are independent. Consequently, single channel fatigue analysis has been performed. In measuring hand tremor, a new method for determining the maximum tremor amplitude using Principal Component Analysis (PCA) and a new technique to detrend acceleration signals using Empirical Mode Decomposition algorithm were introduced. This tremor determination method is more representative for surgeons and it is suggested as an alternative fatigue measure. This was combined with the complexity analysis method, and applied to surgically captured data to determine if operating has an effect on a surgeon’s fatigue and tremor levels. It was found that surgical tremor and fatigue are developed throughout a day of operating and that this could be determined based solely on their initial values. Finally, several Nonlinear AutoRegressive with eXogenous inputs (NARX) neural networks were evaluated. The results suggest that it is possible to monitor surgeon tremor variations during surgery from their EMG fatigue measurements.

Two-dimensional optical power distribution of side-out-coupled radiation from tilted FBGs in multimode fibre

Two-dimensional optical power distribution of the out-coupled radiation from UV-inscribed tilted fibre Bragg gratings (TFBGs) in multimode fibre (MMF) has been side-detected with high spatial/spectral resolution, showing a near-identical radiation mode profile to that measured from the fibre-end detection method. A comparative investigation of the radiation characteristics of TFBGs fabricated in singlemode fibre (SMF) and MMF clearly indicates that the radiation out-coupling is stronger and spatially more confined in MMF. The unique spatial-to-spectral encoding property of the coupling mechanism offers potential application in low-cost WDM devices.

Fiber Bragg grating sensor interrogation system using a CCD side detection method with superimposed blazed gratings

We present, for the first time to our knowledge, experimental evidence showing that superimposed blazed fiber Bragg gratings may be fabricated and used to extend the dynamic range of a grating-based spectrometer. Blazed gratings of 4° and 8° were superimposed in germanosilicate fiber by ultraviolet inscription and used in conjunction with a coated charged-coupled device array to interrogate a wavelength-division-multiplexing sensor array. We show that the system can be used to monitor strain and temperature sensors simultaneously with an employable bandwidth which is extendedable to 70 nm.

Two-dimensional optical power distribution of side-out-coupled radiation from tilted FBGs in multimode fibre

Two-dimensional optical power distribution of the out-coupled radiation from UV-inscribed tilted fibre Bragg gratings (TFBGs) in multimode fibre (MMF) has been side-detected with high spatial/spectral resolution, showing a near-identical radiation mode profile to that measured from the fibre-end detection method. A comparative investigation of the radiation characteristics of TFBGs fabricated in singlemode fibre (SMF) and MMF clearly indicates that the radiation out-coupling is stronger and spatially more confined in MMF. The unique spatial-to-spectral encoding property of the coupling mechanism offers potential application in low-cost WDM devices.

Two-dimensional optical power distribution of side-out-coupled radiation from tilted FBGs in multimode fibre

Two-dimensional optical power distribution of the out-coupled radiation from UV-inscribed tilted fibre Bragg gratings (TFBG) in multimode fibre (MMF) has been side-detected with high spatial spectral resolution, showing a near-identical radiation mode profile to that measured from the fibre-end detection method. A comparative investigation of the radiation characteristics of TFBGs fabricated in singlemode fibre (SMF) and MMF clearly indicates that the radiation out-coupling is stronger and spatially more confined in MMF. The unique spatial-to-spectral encoding property of the coupling mechanism offers potential application in low-cost WDM devices.

State detection of bond wires in IGBT modules using eddy current pulsed thermography

Insulated gate bipolar transistor (IGBT) modules are important safety critical components in electrical power systems. Bond wire lift-off, a plastic deformation between wire bond and adjacent layers of a device caused by repeated power/thermal cycles, is the most common failure mechanism in IGBT modules. For the early detection and characterization of such failures, it is important to constantly detect or monitor the health state of IGBT modules, and the state of bond wires in particular. This paper introduces eddy current pulsed thermography (ECPT), a nondestructive evaluation technique, for the state detection and characterization of bond wire lift-off in IGBT modules. After the introduction of the experimental ECPT system, numerical simulation work is reported. The presented simulations are based on the 3-D electromagnetic-thermal coupling finite-element method and analyze transient temperature distribution within the bond wires. This paper illustrates the thermal patterns of bond wires using inductive heating with different wire statuses (lifted-off or well bonded) under two excitation conditions: nonuniform and uniform magnetic field excitations. Experimental results show that uniform excitation of healthy bonding wires, using a Helmholtz coil, provides the same eddy currents on each, while different eddy currents are seen on faulty wires. Both experimental and numerical results show that ECPT can be used for the detection and characterization of bond wires in power semiconductors through the analysis of the transient heating patterns of the wires. The main impact of this paper is that it is the first time electromagnetic induction thermography, so-called ECPT, has been employed on power/electronic devices. Because of its capability of contactless inspection of multiple wires in a single pass, and as such it opens a wide field of investigation in power/electronic devices for failure detection, performance characterization, and health monitoring.

Optimisation of chromatographic separation of oxidised phospholipids and detection with targeted approaches provides greater coverage of the oxidised lipidome

Phospholipid oxidation by adventitious damage generates a wide variety of products with potentially novel biological activities that can modulate inflammatory processes associated with various diseases. To understand the biological importance of oxidised phospholipids (OxPL) and their potential role as disease biomarkers requires precise information about the abundance of these compounds in cells and tissues. There are many chemiluminescence and spectrophotometric assays available for detecting oxidised phospholipids, but they all have some limitations. Mass spectrometry coupled with liquid chromatography is a powerful and sensitive approach that can provide detailed information about the oxidative lipidome, but challenges still remain. The aim of this work is to develop improved methods for detection of OxPLs by optimisation of chromatographic separation through testing several reverse phase columns and solvent systems, and using targeted mass spectrometry approaches. Initial experiments were carried out using oxidation products generated in vitro to optimise the chromatography separation parameters and mass spectrometry parameters. We have evaluated the chromatographic separation of oxidised phosphatidylcholines (OxPCs) and oxidised phosphatidylethanolamines (OXPEs) using C8, C18 and C30 reverse phase, polystyrene – divinylbenzene based monolithic and mixed – mode hydrophilic interaction (HILIC) columns, interfaced with mass spectrometry. Our results suggest that the monolithic column was best able to separate short chain OxPCs and OxPEs from long chain oxidised and native PCs and PEs. However, variation in charge of polar head groups and extreme diversity of oxidised species make analysis of several classes of OxPLs within one analytical run impractical. We evaluated and optimised the chromatographic separation of OxPLs by serially coupling two columns: HILIC and monolith column that provided us the larger coverage of OxPL species in a single analytical run.

Elemental analysis of glass and ink by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and laser induced breakdown spectroscopy (LIBS)

The necessity of elemental analysis techniques to solve forensic problems continues to expand as the samples collected from crime scenes grow in complexity. Laser ablation ICP-MS (LA-ICP-MS) has been shown to provide a high degree of discrimination between samples that originate from different sources. In the first part of this research, two laser ablation ICP-MS systems were compared, one using a nanosecond laser and another a femtosecond laser source for the forensic analysis of glass. The results showed that femtosecond LA-ICP-MS did not provide significant improvements in terms of accuracy, precision and discrimination, however femtosecond LA-ICP-MS did provide lower detection limits. In addition, it was determined that even for femtosecond LA-ICP-MS an internal standard should be utilized to obtain accurate analytical results for glass analyses. In the second part, a method using laser induced breakdown spectroscopy (LIBS) for the forensic analysis of glass was shown to provide excellent discrimination for a glass set consisting of 41 automotive fragments. The discrimination power was compared to two of the leading elemental analysis techniques, μXRF and LA-ICP-MS, and the results were similar; all methods generated >99% discrimination and the pairs found indistinguishable were similar. An extensive data analysis approach for LIBS glass analyses was developed to minimize Type I and II errors en route to a recommendation of 10 ratios to be used for glass comparisons. Finally, a LA-ICP-MS method for the qualitative analysis and discrimination of gel ink sources was developed and tested for a set of ink samples. In the first discrimination study, qualitative analysis was used to obtain 95.6% discrimination for a blind study consisting of 45 black gel ink samples provided by the United States Secret Service. A 0.4% false exclusion (Type I) error rate and a 3.9% false inclusion (Type II) error rate was obtained for this discrimination study. In the second discrimination study, 99% discrimination power was achieved for a black gel ink pen set consisting of 24 self collected samples. The two pairs found to be indistinguishable came from the same source of origin (the same manufacturer and type of pen purchased in different locations). It was also found that gel ink from the same pen, regardless of the age, was indistinguishable as were gel ink pens (four pens) originating from the same pack.

Elemental analysis of biological matrices by laser ablation high resolution inductively coupled plasma mass spectrometry (LA-HR-ICP-MS) and high resolution inductively coupled plasma mass spectrometry (HR -ICP -MS)

The need for elemental analysis of biological matrices such as bone, teeth, and plant matter for sourcing purposes has emerged within the forensic and geochemical laboratories. Trace elemental analyses for the comparison of materials such as glass by inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS has been shown to offer a high degree of discrimination between different manufacturing sources. Unit resolution ICP-MS instruments may suffer from some polyatomic interferences including 40Ar16O+, 40Ar 16O1H+, and 40Ca 16O+ that affect iron measurement at trace levels. Iron is an important element in the analysis of glass and also of interest for the analysis of several biological matrices. A comparison of the analytical performance of two different ICP-MS systems for iron analysis in glass for determining the method detection limits (MDLs), accuracy, and precision of the measurement is presented. Acid digestion and laser ablation methods are also compared. Iron polyatomic interferences were reduced or resolved by using dynamic reaction cell and high resolution ICP-MS. MDLs as low as 0.03 μg g-1 and 0.14 μg g-1 for laser ablation and solution based analyses respectively were achieved. The use of helium as a carrier gas demonstrated improvement in the detection limits of both iron isotopes (56Fe and 57Fe) in medium resolution for the HR-ICP-MS and with a dynamic reaction cell (DRC) coupled to a quadrupole ICP-MS system. ^ The development and application of robust analytical methods for the quantification of trace elements in biological matrices has lead to a better understanding of the potential utility of these measurements in forensic chemical analyses. Standard reference materials (SRMs) were used in the development of an analytical method using HR-ICP-MS and LA-HR-ICP-MS that was subsequently applied on the analysis of real samples. Bone, teeth and ashed marijuana samples were analyzed with the developed method. ^ Elemental analysis of bone samples from 12 different individuals provided discrimination between individuals, when femur and humerus bones were considered separately. Discrimination of 14 teeth samples based on elemental composition was achieved with the exception of one case where samples from the same individual were not associated with each other. The discrimination of 49 different ashed plant (cannabis) samples was achieved using the developed method. ^

Elemental analysis and forensic comparison of soils by laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

The elemental analysis of soil is useful in forensic and environmental sciences. Methods were developed and optimized for two laser-based multi-element analysis techniques: laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and laser-induced breakdown spectroscopy (LIBS). This work represents the first use of a 266 nm laser for forensic soil analysis by LIBS. Sample preparation methods were developed and optimized for a variety of sample types, including pellets for large bulk soil specimens (470 mg) and sediment-laden filters (47 mg), and tape-mounting for small transfer evidence specimens (10 mg). Analytical performance for sediment filter pellets and tape-mounted soils was similar to that achieved with bulk pellets. An inter-laboratory comparison exercise was designed to evaluate the performance of the LA-ICP-MS and LIBS methods, as well as for micro X-ray fluorescence (μXRF), across multiple laboratories. Limits of detection (LODs) were 0.01-23 ppm for LA-ICP-MS, 0.25-574 ppm for LIBS, 16-4400 ppm for μXRF, and well below the levels normally seen in soils. Good intra-laboratory precision (≤ 6 % relative standard deviation (RSD) for LA-ICP-MS; ≤ 8 % for μXRF; ≤ 17 % for LIBS) and inter-laboratory precision (≤ 19 % for LA-ICP-MS; ≤ 25 % for μXRF) were achieved for most elements, which is encouraging for a first inter-laboratory exercise. While LIBS generally has higher LODs and RSDs than LA-ICP-MS, both were capable of generating good quality multi-element data sufficient for discrimination purposes. Multivariate methods using principal components analysis (PCA) and linear discriminant analysis (LDA) were developed for discriminations of soils from different sources. Specimens from different sites that were indistinguishable by color alone were discriminated by elemental analysis. Correct classification rates of 94.5 % or better were achieved in a simulated forensic discrimination of three similar sites for both LIBS and LA-ICP-MS. Results for tape-mounted specimens were nearly identical to those achieved with pellets. Methods were tested on soils from USA, Canada and Tanzania. Within-site heterogeneity was site-specific. Elemental differences were greatest for specimens separated by large distances, even within the same lithology. Elemental profiles can be used to discriminate soils from different locations and narrow down locations even when mineralogy is similar.

Development of advanced capillary electrophoresis techniques with UV and mass spectrometry detection for forensic, pharmaceutical and environmental applications

Capillary electrophoresis (CE) is a modern analytical technique, which is electrokinetic separation generated by high voltage and taken place inside the small capillaries. In this dissertation, several advanced capillary electrophoresis methods are presented using different approaches of CE and UV and mass spectrometry are utilized as the detection methods. ^ Capillary electrochromatography (CEC), as one of the CE modes, is a recent developed technique which is a hybrid of capillary electrophoresis and high performance liquid chromatography (HPLC). Capillary electrochromatography exhibits advantages of both techniques. In Chapter 2, monolithic capillary column are fabricated using in situ photoinitiation polymerization method. The column was then applied for the separation of six antidepressant compounds. ^ Meanwhile, a simple chiral separation method is developed and presented in Chapter 3. Beta cycodextrin was utilized to achieve the goal of chiral separation. Not only twelve cathinone analytes were separated, but also isomers of several analytes were enantiomerically separated. To better understand the molecular information on the analytes, the TOF-MS system was coupled with the CE. A sheath liquid and a partial filling technique (PFT) were employed to reduce the contamination of MS ionization source. Accurate molecular information was obtained. ^ It is necessary to propose, develop, and optimize new techniques that are suitable for trace-level analysis of samples in forensic, pharmaceutical, and environmental applications. Capillary electrophoresis (CE) was selected for this task, as it requires lower amounts of samples, it simplifies sample preparation, and it has the flexibility to perform separations of neutral and charged molecules as well as enantiomers. ^ Overall, the study demonstrates the versatility of capillary electrophoresis methods in forensic, pharmaceutical, and environmental applications.^

Monitoring of down-hole parameters for early kick detection

The sudden hydrocarbon influx from the formation into the wellbore poses a serious risk to the safety of the well. This sudden influx is termed a kick, which, if not controlled, may lead to a blowout. Therefore, early detection of the kick is crucial to minimize the possibility of a blowout occurrence. There is a high probability of delay in kick detection, apart from other issues when using a kick detection system that is exclusively based on surface monitoring. Down-hole monitoring techniques have a potential to detect a kick at its early stage. Down-hole monitoring could be particularly beneficial when the influx occurs as a result of a lost circulation scenario. In a lost circulation scenario, when the down-hole pressure becomes lower than the formation pore pressure, the formation fluid may starts to enter the wellbore. The lost volume of the drilling fluid is compensated by the formation fluid flowing into the well bore, making it difficult to identify the kick based on pit (mud tank) volume observations at the surface. This experimental study investigates the occurrence of a kick based on relative changes in the mass flow rate, pressure, density, and the conductivity of the fluid in the down-hole. Moreover, the parameters that are most sensitive to formation fluid are identified and a methodology to detect a kick without false alarms is reported. Pressure transmitter, the Coriolis flow and density meter, and the conductivity sensor are employed to observe the deteriorating well conditions in the down-hole. These observations are used to assess the occurrence of a kick and associated blowout risk. Monitoring of multiple down-hole parameters has a potential to improve the accuracy of interpretation related to kick occurrence, reduces the number of false alarms, and provides a broad picture of down-hole conditions. The down-hole monitoring techniques have a potential to reduce the kick detection period. A down-hole assembly of the laboratory scale drilling rig model and kick injection setup were designed, measuring instruments were acquired, a frame was fabricated, and the experimental set-up was assembled and tested. This set-up has the necessary features to evaluate kick events while implementing down-hole monitoring techniques. Various kick events are simulated on the drilling rig model. During the first set of experiments compressed air (which represents the formation fluid) is injected with constant pressure margin. In the second set of experiments the compressed air is injected with another pressure margin. The experiments are repeated with another pump (flow) rate as well. This thesis consists of three main parts. The first part gives the general introduction, motivation, outline of the thesis, and a brief description of influx: its causes, various leading and lagging indicators, and description of the several kick detection systems that are in practice in the industry. The second part describes the design and construction of the laboratory scale down-hole assembly of the drilling rig and kick injection setup, which is used to implement the proposed methodology for early kick detection. The third part discusses the experimental work, describes the methodology for early kick detection, and presents experimental results that show how different influx events affect the mass flow rate, pressure, conductivity, and density of the fluid in the down-hole, and the discussion of the results. The last chapter contains summary of the study and future research.

Synthesis & retention mechanisms of novel mixed mode stationary phase for detection of specific polar low molecular weight biological samples

The thesis primarily reports the synthesis, characterization and application of novel mixed mode stationary phases for Hydrophilic Interaction Liquid Chromatography (HILIC). HILIC is a rapidly emerging chromatographic mode that is finding great applicability in the analysis of polar organic molecules. In addition, there is a chapter on the analysis of Bisphenol A and related species using capillary electrophoresis (CE) coupled with boron-doped diamond electrodes for electrochemical detection. The synthesis and characterization of the novel mixed mode stationary phases prepared in this work is an important contribution to the field as the materials prepared exhibited better performance than similar materials obtained commercially. In addition a more thorough characterization of the materials (e.g.,thermogravimetric analysis, various NMR modes, elemental analysis, etc.) and resulting columns (e.g., H) than is typically encountered. The application of these new materials to the analysis of sugars using evaporative light scattering is also novel. In CE studies, electrochemical detection is sufficiently rare that the work is also novel.