Search results for: photocopying procedure.

Authors: Mourtou Efstratia, Abdel-Badeeh M. Salem, Pavlidis George

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Hierarchical high-level PNs (HHPNs) with time versions are a useful tool to model systems in a variety of application domains, ranging from logistics to complex workflows. This paper addresses an application domain which is receiving more and more attention: procedure that arranges the final inpatient charge in payment-s office and their management. We shall prove that Petri net based analysis is able to improve the delays during the procedure, in order that inpatient charges could be more reliable and on time.

Keywords: eHealth, Petri-Nets, Hospital Services, InpatientCharges, Workflow Modeling.

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Authors: M. Guillard, M. Philippe, F. Laurent, J. Martinerie, J. P. Lachaux, G. Florence

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One approach to assess neural networks underlying the cognitive processes is to study Electroencephalography (EEG). It is relevant to detect various mental states and characterize the physiological changes that help to discriminate two situations. That is why an EEG (amplitude, synchrony) classification procedure is described, validated. The two situations are "eyes closed" and "eyes opened" in order to study the "alpha blocking response" phenomenon in the occipital area. The good classification rate between the two situations is 92.1 % (SD = 3.5%) The spatial distribution of a part of amplitude features that helps to discriminate the two situations are located in the occipital regions that permit to validate the localization method. Moreover amplitude features in frontal areas, "short distant" synchrony in frontal areas and "long distant" synchrony between frontal and occipital area also help to discriminate between the two situations. This procedure will be used for mental fatigue detection.

Keywords: Classification, EEG Synchrony, alpha, resting situation.

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Authors: Nassima Cheikh, Abdelmadjid Cheikh, Said Hamou

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The objective of this work which is based on the approach of simultaneous engineering is to contribute to the development of a CIM tool for the synthesis of functional design dimensions expressed by average values and tolerance intervals. In this paper, the dispersions method known as the Δl method which proved reliable in the simulation of manufacturing dimensions is used to develop a methodology for the automation of the simulation. This methodology is constructed around three procedures. The first procedure executes the verification of the functional requirements by automatically extracting the functional dimension chains in the mechanical sub-assembly. Then a second procedure performs an optimization of the dispersions on the basis of unknown variables. The third procedure uses the optimized values of the dispersions to compute the optimized average values and tolerances of the functional dimensions in the chains. A statistical and cost based approach is integrated in the methodology in order to take account of the capabilities of the manufacturing processes and to distribute optimal values among the individual components of the chains.

Keywords: functional tolerances, manufacturing dispersions, simulation, CIM.

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Authors: M. Graus, K. Westhoff, X. Xu

Abstract:

The climate change causes a change in all aspects of society. While the expansion of renewable energies proceeds, industry could not be convinced based on general studies about the potential of demand side management to reinforce smart grid considerations in their operational business. In this article, a procedure model for a case-specific data-driven decision support for industrial energy management based on a holistic data analytics approach is presented. The model is executed on the example of the strategic decision problem, to integrate the aspect of renewable energies into industrial energy management. This question is induced due to considerations of changing the electricity contract model from a standard rate to volatile energy prices corresponding to the energy spot market which is increasingly more affected by renewable energies. The procedure model corresponds to a data analytics process consisting on a data model, analysis, simulation and optimization step. This procedure will help to quantify the potentials of sustainable production concepts based on the data from a factory. The model is validated with data from a printer in analogy to a simple production machine. The overall goal is to establish smart grid principles for industry via the transformation from knowledge-driven to data-driven decisions within manufacturing companies.

Keywords: Data analytics, green production, industrial energy management, optimization, renewable energies, simulation.

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Authors: Abdelouahab Moussaoui, Nabila Ferahta, Victor Chen

Abstract:

The development of aid's systems for the medical diagnosis is not easy thing because of presence of inhomogeneities in the MRI, the variability of the data from a sequence to the other as well as of other different source distortions that accentuate this difficulty. A new automatic, contextual, adaptive and robust segmentation procedure by MRI brain tissue classification is described in this article. A first phase consists in estimating the density of probability of the data by the Parzen-Rozenblatt method. The classification procedure is completely automatic and doesn't make any assumptions nor on the clusters number nor on the prototypes of these clusters since these last are detected in an automatic manner by an operator of mathematical morphology called skeleton by influence zones detection (SKIZ). The problem of initialization of the prototypes as well as their number is transformed in an optimization problem; in more the procedure is adaptive since it takes in consideration the contextual information presents in every voxel by an adaptive and robust non parametric model by the Markov fields (MF). The number of bad classifications is reduced by the use of the criteria of MPM minimization (Maximum Posterior Marginal).

Keywords: Clustering, Automatic Classification, SKIZ, MarkovFields, Image segmentation, Maximum Posterior Marginal (MPM).

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Authors: Elena Carcano, Mirzi Betasolo

Abstract:

This study aims to provide sub-hourly streamflow predictions and associated rating curves for small catchments of intermittent and torrential flow regime characterized by flash floods occurring especially during April and November. The methodology entails two lumped conceptual hydrological models which work in series. The total model is based upon eleven parameters and shows good flexibility in handling different input sets. Runoff Coefficient has contributed to improving the model’s performances and has been treated as an additional parameter; while Sensitivity Analysis has highlighted how slight changes in the model’s input can lead to changes in model’s output. The adopted procedure is steady and useful to give very practical engineering information at the expense of a parsimonious request both in input data and in the number of adopted parameters. According to the obtained results, the authors encourage the test of this combined procedure on different hydrological scenarios in order to provide information for poorly monitored catchments and not updated sites.

Keywords: Streamflow rating curve, chronological data, streamflow sequences, conceptual models.

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Authors: Tatyana Aleksandrovna Barbasova, Lev Sergeevich Kazarinov, Olga Valerevna Kolesnikova, Aleksandra Aleksandrovna Filimonova

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We regard forecasting of energy consumption by private production areas of a large industrial facility as well as by the facility itself. As for production areas, the forecast is made based on empirical dependencies of the specific energy consumption and the production output. As for the facility itself, implementation of the task to minimize the energy consumption forecasting error is based on adjustment of the facility’s actual energy consumption values evaluated with the metering device and the total design energy consumption of separate production areas of the facility. The suggested procedure of optimal energy consumption was tested based on the actual data of core product output and energy consumption by a group of workshops and power plants of the large iron and steel facility. Test results show that implementation of this procedure gives the mean accuracy of energy consumption forecasting for winter 2014 of 0.11% for the group of workshops and 0.137% for the power plants.

Keywords: Energy consumption, energy consumption forecasting error, energy efficiency, forecasting accuracy, forecasting.

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Authors: S. Raissi

Abstract:

Response surface methodology (RSM) is a very efficient tool to provide a good practical insight into developing new process and optimizing them. This methodology could help engineers to raise a mathematical model to represent the behavior of system as a convincing function of process parameters. Through this paper the sequential nature of the RSM surveyed for process engineers and its relationship to design of experiments (DOE), regression analysis and robust design reviewed. The proposed four-step procedure in two different phases could help system analyst to resolve the parameter design problem involving responses. In order to check accuracy of the designed model, residual analysis and prediction error sum of squares (PRESS) described. It is believed that the proposed procedure in this study can resolve a complex parameter design problem with one or more responses. It can be applied to those areas where there are large data sets and a number of responses are to be optimized simultaneously. In addition, the proposed procedure is relatively simple and can be implemented easily by using ready-made standard statistical packages.

Keywords: Response Surface Methodology (RSM), Design of Experiments (DOE), Process modeling, Process setting, Process optimization.

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Authors: Yen-Cheng Chen, Fu-Chen Yang

Abstract:

IETF defines mobility support in IPv6, i.e. MIPv6, to allow nodes to remain reachable while moving around in the IPv6 internet. When a node moves and visits a foreign network, it is still reachable through the indirect packet forwarding from its home network. This triangular routing feature provides node mobility but increases the communication latency between nodes. This deficiency can be overcome by using a Binding Update (BU) scheme, which let nodes keep up-to-date IP addresses and communicate with each other through direct IP routing. To further protect the security of BU, a Return Routability (RR) procedure was developed. However, it has been found that RR procedure is vulnerable to many attacks. In this paper, we will propose a lightweight RR procedure based on geometric computing. In consideration of the inherent limitation of computing resources in mobile node, the proposed scheme is developed to minimize the cost of computations and to eliminate the overhead of state maintenance during binding updates. Compared with other CGA-based BU schemes, our scheme is more efficient and doesn-t need nonce tables in nodes.

Keywords: Mobile IPv6, Binding update, Geometric computing.

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Authors: A. Rifa’i, Y. Takeshita, M. Komatsu

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After Yogyakarta earthquake in 2006, the main problem that occurred in the first yard of Prambanan Temple is ponding area that occurred after rainfall. Soil characterization needs to be determined by conducting several processes, especially permeability coefficient (k) in both saturated and unsaturated conditions to solve this problem. More accurate and efficient field testing procedure is required to obtain permeability data that present the field condition. One of the field permeability test equipment is Constant Discharge procedure to determine the permeability coefficient. Necessary adjustments of the Constant Discharge procedure are needed to be determined especially the value of geometric factor (F) to improve the corresponding value of permeability coefficient. The value of k will be correlated with the value of volumetric water content (θ) of an unsaturated condition until saturated condition. The principle procedure of Constant Discharge model provides a constant flow in permeameter tube that flows into the ground until the water level in the tube becomes constant. Constant water level in the tube is highly dependent on the tube dimension. Every tube dimension has a shape factor called the geometric factor that affects the result of the test. Geometric factor value is defined as the characteristic of shape and radius of the tube. This research has modified the geometric factor parameters by using empty material tube method so that the geometric factor will change. Saturation level is monitored by using soil moisture sensor. The field test results were compared with the results of laboratory tests to validate the results of the test. Field and laboratory test results of empty tube material method have an average difference of 3.33 x 10^-4 cm/sec. The test results showed that modified geometric factor provides more accurate data. The improved methods of constant discharge procedure provide more relevant results.

Keywords: Constant discharge, geometric factor, permeability coefficient, unsaturated soils.

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Authors: Sukrit Ghorai

Abstract:

Proof of controlling crack width is a basic condition for securing suitable performance in serviceability limit state. The cracking in concrete can occur at any time from the casting of time to the years after the concrete has been set in place. Most codes struggle with offering procedure for crack width calculation. There is lack in availability of design charts for designers to compute crack width with ease. The focus of the study is to utilize design charts and parametric equations in calculating crack width with minimum error. The paper contains a simplified procedure to calculate crack width for reinforced concrete (RC) sections subjected to bending with axial tensile force following the guidelines of Euro code [DS EN-1992-1-1 & DS EN-1992-1-2]. Numerical examples demonstrate the application of the suggested procedure. Comparison with parallel analytical tools supports the validity of result and show the percentage deviation of crack width in both the procedures. The technique is simple, user friendly and ready to evolve for a greater spectrum of section sizes and materials.

Keywords: Concrete structures, crack width calculation, serviceability limit state, structural design, bridge engineering.

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Authors: Fatimah Almah Saaid, Darfiana Nur, Robert King

Abstract:

This paper presents a procedure for estimating VAR using Sequential Discounting VAR (SDVAR) algorithm for online model learning to detect fraudulent acts using the telecommunications call detailed records (CDR). The volatility of the VAR is observed allowing for non-linearity, outliers and change points based on the works of [1]. This paper extends their procedure from univariate to multivariate time series. A simulation and a case study for detecting telecommunications fraud using CDR illustrate the use of the algorithm in the bivariate setting.

Keywords: Telecommunications Fraud, SDVAR Algorithm, Multivariate time series, Vector Autoregressive, Change points.

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Authors: Jinfeng Wang, Yang Liu, Hong Li

Abstract:

In this article, we propose a new approximate procedure based on He’s variational iteration method for solving nonlinear hyperbolic equations. We introduce two transformations q = ut and σ = ux and formulate a first-order system of equations. We can obtain the approximation solution for the scalar unknown u, time derivative q = ut and space derivative σ = ux, simultaneously. Finally, some examples are provided to illustrate the effectiveness of our method.

Keywords: Hyperbolic wave equation, Nonlinear, He’s variational iteration method, Transformations

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Authors: Javad Marzbanrad, Mostafa Pahlavani

Abstract:

This study has investigated a vehicle Lumped Parameter Model (LPM) in frontal crash. There are several ways for determining spring and damper characteristics and type of problem shall be considered as system identification. This study use Genetic Algorithm (GA) procedure, being an effective procedure in case of optimization issues, for optimizing errors, between target data (experimental data) and calculated results (being obtained by analytical solving). In this study analyzed model in 5-DOF then compared our results with 5-DOF serial model. Finally, the response of model due to external excitement is investigated.

Keywords: Vehicle, Lumped-Parameter Model, GeneticAlgorithm, Optimization

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Authors: Fereidoon Nowshiravan Rahatabad, Mohammad Hassan Moradi, Vahid Reza Nafisi

Abstract:

Nothing that an effective cure for infertility happens when we can find a unique solution, a great deal of study has been done in this field and this is a hot research subject for to days study. So we could analyze the men-s seaman and find out about fertility and infertility and from this find a true cure for this, since this will be a non invasive and low risk procedure, it will be greatly welcomed. In this research, the procedure has been based on few Algorithms enhancement and segmentation of images which has been done on the images taken from microscope in different fertility institution and have obtained a suitable result from the computer images which in turn help us to distinguish these sperms from fluids and its surroundings.

Keywords: Computer-Assisted Sperm Analysis (CASA), Spermidentification, Segmentation.

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Authors: P. Puustinen, A. Kanto

Abstract:

This paper proposes a new procedure for analyzing means-end chain data in marketing research. Most commonly the collected data is summarized in the Hierarchical Value Map (HVM) illustrating the main attribute-consequence-value linkages. This paper argues that traditionally constructed HVM may give an erroneous impression of the results of a means-end study. To justify the arguments, an alternative procedure to (1) determine the dominant attribute-consequence-value linkages and (2) construct HVM in a precise manner is presented. The current approach makes a contribution to means-end analysis, allowing marketers to address a set of marketing problems, such as advertising strategy.

Keywords: Means-end chain analysis, Laddering, Hierarchical Value Map.

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Authors: Madhukar Nagare, Pankaj Dutta

Abstract:

Inventory decisional environment of short life-cycle products is full of uncertainties arising from randomness and fuzziness of input parameters like customer demand requiring modeling under hybrid uncertainty. Prior inventory models incorporating fuzzy demand have unfortunately ignored stochastic variation of demand. This paper determines an unambiguous optimal order quantity from a set of n fuzzy observations in a newsvendor inventory setting in presence of fuzzy random variable demand capturing both fuzzy perception and randomness of customer demand. The stress of this paper is in providing solution procedure that attains optimality in two steps with demand information availability in linguistic phrases leading to fuzziness along with stochastic variation. The first step of solution procedure identifies and prefers one best fuzzy opinion out of all expert opinions and the second step determines optimal order quantity from the selected event that maximizes profit. The model and solution procedure is illustrated with a numerical example.

Keywords: Fuzzy expected value, Fuzzy random demand, Hybrid uncertainty, Optimal order quantity, Single-period inventory

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Authors: J. Arneric, E. Jurun, L. Kordic

Abstract:

This paper deals with econometric analysis of real retail trade turnover. It is a part of an extensive scientific research about modern trends in Croatian national economy. At the end of the period of transition economy, Croatia confronts with challenges and problems of high consumption society. In such environment as crucial economic variables: real retail trade turnover, average monthly real wages and household loans are chosen for consequence analysis. For the purpose of complete procedure of multiple econometric analysis data base adjustment has been provided. Namely, it has been necessary to deflate original national statistics data of retail trade turnover using consumer price indices, as well as provide process of seasonally adjustment of its contemporary behavior. In model establishment it has been necessary to involve the overcoming procedure for the autocorrelation and colinearity problems. Moreover, for case of time-series shift a specific appropriate econometric instrument has been applied. It would be emphasize that the whole methodology procedure is based on the real Croatian national economy time-series.

Keywords: Consumption society, multiple econometric model, real retail trade turnover, second order autocorrelation.

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Authors: Saad M. Al-Garni, Adel A. Abdennour

Abstract:

Vehicle detection is the critical step for highway monitoring. In this paper we propose background subtraction and edge detection technique for vehicle detection. This technique uses the advantages of both approaches. The practical applications approved the effectiveness of this method. This method consists of two procedures: First, automatic background extraction procedure, in which the background is extracted automatically from the successive frames; Second vehicles detection procedure, which depend on edge detection and background subtraction. Experimental results show the effective application of this algorithm. Vehicles detection rate was higher than 91%.

Keywords: Image processing, Automatic background extraction, Moving vehicle detection.

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Authors: Mhand Hifi, Hedi Mhalla, Mustapha Michaphy

Abstract:

In this paper, we study the multi-scenario knapsack problem, a variant of the well-known NP-Hard single knapsack problem. We investigate the use of an adaptive algorithm for solving heuristically the problem. The used method combines two complementary phases: a size reduction phase and a dynamic 2- opt procedure one. First, the reduction phase applies a polynomial reduction strategy; that is used for reducing the size problem. Second, the adaptive search procedure is applied in order to attain a feasible solution Finally, the performances of two versions of the proposed algorithm are evaluated on a set of randomly generated instances.

Keywords: combinatorial optimization, max-min optimization, knapsack, heuristics, problem reduction

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Authors: Tebogo P. Phetla, Edison Muzenda

Abstract:

This study was carried out to develop a flotation procedure for an oxide copper ore from a Region in Central Africa for producing an 18% copper concentrate for downstream processing at maximum recovery from a 4% copper feed grade. The copper recoveries achieved from the test work were less than 50% despite changes in reagent conditions (multistage sulphidisation, use of RCA emulsion and mixture, use of AM 2, etc). The poor recoveries were attributed to the mineralogy of the ore from which copper silicates accounted for approximately 70% (mass) of the copper minerals in the ore. These can be complex and difficult to float using conventional flotation methods. Best results were obtained using basic sulphidisation procedures, a high flotation temperature and extended flotation residence time.

Keywords: Froth flotation, Sulphidisation, Copper oxide ore, Mineralogy, Recovery

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Authors: H. Zare Aliabadi

Abstract:

The equilibrium chemical reactions taken place in a converter reactor of the Khorasan Petrochemical Ammonia plant was studied using the minimization of Gibbs free energy method. In the minimization of the Gibbs free energy function the Davidon– Fletcher–Powell (DFP) optimization procedure using the penalty terms in the well-defined objective function was used. It should be noted that in the DFP procedure along with the corresponding penalty terms the Hessian matrices for the composition of constituents in the Converter reactor can be excluded. This, in fact, can be considered as the main advantage of the DFP optimization procedure. Also the effect of temperature and pressure on the equilibrium composition of the constituents was investigated. The results obtained in this work were compared with the data collected from the converter reactor of the Khorasan Petrochemical Ammonia plant. It was concluded that the results obtained from the method used in this work are in good agreement with the industrial data. Notably, the algorithm developed in this work, in spite of its simplicity, takes the advantage of short computation and convergence time.

Keywords: Gibbs free energy, converter reactors, Chemical equilibrium

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Authors: Alexander Goncharenko, Andrey Denisov, Sergey Alyamkin, Evgeny Terentev

Abstract:

The neural network quantization is highly desired procedure to perform before running neural networks on mobile devices. Quantization without fine-tuning leads to accuracy drop of the model, whereas commonly used training with quantization is done on the full set of the labeled data and therefore is both time- and resource-consuming. Real life applications require simplification and acceleration of quantization procedure that will maintain accuracy of full-precision neural network, especially for modern mobile neural network architectures like Mobilenet-v1, MobileNet-v2 and MNAS. Here we present a method to significantly optimize training with quantization procedure by introducing the trained scale factors for discretization thresholds that are separate for each filter. Using the proposed technique, we quantize the modern mobile architectures of neural networks with the set of train data of only ∼ 10% of the total ImageNet 2012 sample. Such reduction of train dataset size and small number of trainable parameters allow to fine-tune the network for several hours while maintaining the high accuracy of quantized model (accuracy drop was less than 0.5%). Ready-for-use models and code are available in the GitHub repository.

Keywords: Distillation, machine learning, neural networks, quantization.

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Authors: J. Cheeneebash, S. Jugee

Abstract:

In this paper, the Tabu search algorithm is used to solve a transportation problem which consists of determining the shortest routes with the appropriate vehicle capacity to facilitate the travel of the students attending the University of Mauritius. The aim of this work is to minimize the total cost of the distance travelled by the vehicles in serving all the customers. An initial solution is obtained by the TOUR algorithm which basically constructs a giant tour containing all the customers and partitions it in an optimal way so as to produce a set of feasible routes. The Tabu search algorithm then makes use of a search procedure, a swapping procedure and the intensification and diversification mechanism to find the best set of feasible routes.

Keywords: Tabu Search, Vehicle Routing, Transport.

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Authors: S. A. Faizi, S. Yoshitomi

Abstract:

The optimal design procedure of buckling restrained braces (BRBs) in reinforced concrete (RC) building structures can provide the distribution of horizontal stiffness of BRBs at each story, which minimizes story drift response of the structure under the constraint of specified total stiffness of BRBs. In this paper, a simple rule is proposed to convert continuous horizontal stiffness of BRBs into sectional sizes of BRB which are available from standardized section list assuming realistic structural design stage.

Keywords: Buckling restrained brace, building engineering, optimal damper placement, structural engineering.

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Authors: Qasim Kriri, Harsh B. Desai

Abstract:

Water supply and sanitation in Saudi Arabia is portrayed by difficulties and accomplishments. One of the fundamental difficulties is water shortage. With a specific end goal to beat water shortage, significant ventures have been attempted in sea water desalination, water circulation, sewerage, and wastewater treatment. The motivation behind Statistical Process Control (SPC) is to decide whether the execution of a procedure is keeping up an acceptable quality level [AQL]. SPC is an analytical decision-making method. A fundamental apparatus in the SPC is the Control Charts, which follow the inconstancy in the estimations of the item quality attributes. By utilizing the suitable outline, administration can decide whether changes should be made with a specific end goal to keep the procedure in charge. The two most important quality factors in the distilled water which were taken into consideration were pH (Potential of Hydrogen) and TDS (Total Dissolved Solids). There were three stages at which the quality checks were done. The stages were as follows: (1) Water at the source, (2) water after chemical treatment & (3) water which is sent for packing. The upper specification limit, central limit and lower specification limit are taken as per Saudi water standards. The procedure capacity to accomplish the particulars set for the quality attributes of Berain water Factory chose to be focused by the proposed SPC system.

Keywords: Acceptable quality level, statistical quality control, control charts, process charts.

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Authors: Carlos L. Antunes, Tony R. Almeida, Nélia Raposeiro, Belarmino Gonçalves, Paulo Almeida, André Antunes

Abstract:

In the last two decades radiofrequency ablation (RFA) has been considered a promising medical procedure for the treatment of primary and secondary malignancies. However, the needle-based electrodes so far developed for this kind of treatment are not suitable for the thermal ablation of tumors located in hollow organs like esophagus, colon or bile duct. In this work a tubular electrode solution is presented. Numerical and experimental analyses were performed to characterize the volume of the lesion induced. Results show that this kind of electrode is a feasible solution and numerical simulation might provide a tool for planning RFA procedure with some accuracy.

Keywords: 3D modeling, cancer, medical therapy, radiofrequency ablation.

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Authors: P I Jagad, B P Puranik, A W Date

Abstract:

Flow through micro and mini channels requires relatively high driving pressure due to the large fluid pressure drop through these channels. Consequently the forces acting on the walls of the channel due to the fluid pressure are also large. Due to these forces there are displacement fields set up in the solid substrate containing the channels. If the movement of the substrate is constrained at some points, then stress fields are established in the substrate. On the other hand, if the deformation of the channel shape is sufficiently large then its effect on the fluid flow is important to be calculated. Such coupled fluid-solid systems form a class of problems known as fluidstructure interactions. In the present work a co-located finite volume discretization procedure on unstructured meshes is described for solving fluid-structure interaction type of problems. A linear elastic solid is assumed for which the effect of the channel deformation on the flow is neglected. Thus the governing equations for the fluid and the solid are decoupled and are solved separately. The procedure is validated by solving two benchmark problems, one from fluid mechanics and another from solid mechanics. A fluid-structure interaction problem of flow through a U-shaped channel embedded in a plate is solved.

Keywords: Finite volume method, flow induced stresses, fluidstructureinteraction, unstructured meshes.

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Authors: Jingming Wu, Ruikang Hu, Junqi Yue, Zhaoguang Yang, Lifeng Zhang

Abstract:

Fecal sterol has been proposed as a chemical indicator of human fecal pollution even when fecal coliform populations have diminished due to water chlorination or toxic effects of industrial effluents. This paper describes an improved derivatization procedure for simultaneous determination of four fecal sterols including coprostanol, epicholestanol, cholesterol and cholestanol using gas chromatography-mass spectrometry (GC-MS), via optimization study on silylation procedures using N-O-bis (trimethylsilyl)-trifluoroacetamide (BSTFA), and N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and tert-butyldimethylsilyl (TBS) derivatives, respectively. Two derivatization processes of injection-port derivatization and water bath derivatization (60 oC, 1h) were inspected and compared. Furthermore, the methylation procedure at 25 oC for 2h with trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also studied. It was found that most of TMS derivatives demonstrated the highest sensitivities, followed by methylated derivatives. For BSTFA or MTBSTFA derivatization processes, the simple injection-port derivatization process could achieve the same efficiency as that in the tedious water bath derivatization procedure.

Keywords: Fecal Sterols, Methylation, Silylation, BSTFA, MTBSTFA, TMSD, GC-MS.

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Authors: Jingming Wu, Ruikang Hu, Junqi Yue, Zhaoguang Yang, Lifeng Zhang

Abstract:

Fecal sterol has been proposed as a chemical indicator of human fecal pollution even when fecal coliform populations have diminished due to water chlorination or toxic effects of industrial effluents. This paper describes an improved derivatization procedure for simultaneous determination of four fecal sterols including coprostanol, epicholestanol, cholesterol and cholestanol using gas chromatography-mass spectrometry (GC-MS), via optimization study on silylation procedures using N-O-bis (trimethylsilyl)-trifluoroacetamide (BSTFA), and N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and tert-butyldimethylsilyl (TBS) derivatives, respectively. Two derivatization processes of injection-port derivatization and water bath derivatization (60 oC, 1h) were inspected and compared. Furthermore, the methylation procedure at 25 oC for 2h with trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also studied. It was found that most of TMS derivatives demonstrated the highest sensitivities, followed by methylated derivatives. For BSTFA or MTBSTFA derivatization processes, the simple injection-port derivatization process could achieve the same efficiency as that in the tedious water bath derivatization procedure.

Keywords: Fecal Sterols, Methylation, Silylation, BSTFA, MTBSTFA, TMSD, GC-MS.

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