999 resultados para titrimetric determination


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A method for determination of lactose in food samples by Osteryoung square wave voltammetry (OSWV) was developed. It was based on the nucleophilic addition reaction between lactose and aqua ammonia. The carbonyl group of lactose can be changed into imido group, and this increases the electrochemical activity in reduction and the sensitivity. The optimal condition for the nucleophilic addition reaction was investigated and it was found that in NH4Cl–NH3 buffer of pH 10.1, the linear range between the peak current and the concentration of lactose was 0.6–8.4 mg L−1, and the detection limits was 0.44 mg L−1. The proposed method was applied to the determination of lactose in food samples and satisfactory results were obtained.

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A simple and sensitive spectrophotometric method for the simultaneous determination of acesulfame-K, sodium cyclamate and saccharin sodium sweeteners in foodstuff samples has been researched and developed. This analytical method relies on the different kinetic rates of the analytes in their oxidative reaction with KMnO4 to produce the green manganate product in an alkaline solution. As the kinetic rates of acesulfame-K, sodium cyclamate and saccharin sodium were similar and their kinetic data seriously overlapped, chemometrics methods, such as partial least squares (PLS), principal component regression (PCR) and classical least squares (CLS), were applied to resolve the kinetic data. The results showed that the PLS prediction model performed somewhat better. The proposed method was then applied for the determination of the three sweeteners in foodstuff samples, and the results compared well with those obtained by the reference HPLC method.

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A fast and accurate procedure has been researched and developed for the simultaneous determination of maltol and ethyl maltol, based on their reaction with iron(III) in the presence of o-phenanthroline in sulfuric acid medium. This reaction was the basis for an indirect kinetic spectrophotometric method, which followed the development of the pink ferroin product (λmax = 524 nm). The kinetic data were collected in the 370–900 nm range over 0–30 s. The optimized method indicates that individual analytes followed Beer’s law in the concentration range of 4.0–76.0 mg L−1 for both maltol and ethyl maltol. The LOD values of 1.6 mg L−1 for maltol and 1.4 mg L−1 for ethyl maltol agree well with those obtained by the alternative high performance liquid chromatography with ultraviolet detection (HPLC-UV). Three chemometrics methods, principal component regression (PCR), partial least squares (PLS) and principal component analysis–radial basis function–artificial neural networks (PC–RBF–ANN), were used to resolve the measured data with small kinetic differences between the two analytes as reflected by the development of the pink ferroin product. All three performed satisfactorily in the case of the synthetic verification samples, and in their application for the prediction of the analytes in several food products. The figures of merit for the analytes based on the multivariate models agreed well with those from the alternative HPLC-UV method involving the same samples.

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A kinetic spectrophotometric method with aid of chemometrics is proposed for the simultaneous determination of norfloxacin and rifampicin in mixtures. The proposed method was applied for the simultaneous determination of these two compounds in pharmaceutical formulation and human urine samples, and the results obtained are similar to those obtained by high performance liquid chromatography.

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A spectrophotometric method for the simultaneous determination of the important pharmaceuticals, pefloxacin and its structurally similar metabolite, norfloxacin, is described for the first time. The analysis is based on the monitoring of a kinetic spectrophotometric reaction of the two analytes with potassium permanganate as the oxidant. The measurement of the reaction process followed the absorbance decrease of potassium permanganate at 526 nm, and the accompanying increase of the product, potassium manganate, at 608 nm. It was essential to use multivariate calibrations to overcome severe spectral overlaps and similarities in reaction kinetics. Calibration curves for the individual analytes showed linear relationships over the concentration ranges of 1.0–11.5 mg L−1 at 526 and 608 nm for pefloxacin, and 0.15–1.8 mg L−1 at 526 and 608 nm for norfloxacin. Various multivariate calibration models were applied, at the two analytical wavelengths, for the simultaneous prediction of the two analytes including classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), radial basis function-artificial neural network (RBF-ANN) and principal component-radial basis function-artificial neural network (PC-RBF-ANN). PLS and PC-RBF-ANN calibrations with the data collected at 526 nm, were the preferred methods—%RPET not, vert, similar 5, and LODs for pefloxacin and norfloxacin of 0.36 and 0.06 mg L−1, respectively. Then, the proposed method was applied successfully for the simultaneous determination of pefloxacin and norfloxacin present in pharmaceutical and human plasma samples. The results compared well with those from the alternative analysis by HPLC.

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Transportation disadvantage has been recognised to be the key source of social exclusion. Therefore an appropriate process is required to investigate and seek to resolve this problem. Currently, determination of Transportation Disadvantage is postulate based on income, poverty and mobility level. Transportation disadvantage may best regard be based on accessibility perspectives as they represent inability of the individual to access desired activities. This paper attempts to justify a process in determining transportation disadvantage by incorporating accessibility and social transporation conflict as the essence of a framework. The framework embeds space time organisation within the dimension of accessibility to identify a rigorous definition of transportation disadvantage. In developing the framework, the definition, dimension, component and measure of accessibility were scrutinised. The findings suggest the definition and dimension are the significant approach of research to evaluate travel experience of the disadvantaged. Concurrently, location accessibility measures will be incorprated to strenghten the determination of accessibility level. Literature review in social exclusion and mobility-related exclusion identified the dimension and source of transportation disadvantage. It was revealed that the appropriate approach to justify trasnportation disadvantaged is to incorporate space-time organisation within the studied components. The suggested framework is an inter-related process consisting of component of accessibility; individual, networking (transport system) and activities (destination). The integration and correlation among the components shall determine the level of transportation disadvantage. Prior findings are used to retrieve the spatial distribution of transportation disadvantaged and appropriate policies are developed to resolve the problems.

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A deconvolution method that combines nanoindentation and finite element analysis was developed to determine elastic modulus of thin coating layer in a coating-substrate bilayer system. In this method, the nanoindentation experiments were conducted to obtain the modulus of both the bilayer system and the substrate. The finite element analysis was then applied to deconvolve the elastic modulus of the coating. The results demonstrated that the elastic modulus obtained using the developed method was in good agreement with that reported in literature.

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Integrity of Real Time Kinematic (RTK) positioning solutions relates to the confidential level that can be placed in the information provided by the RTK system. It includes the ability of the RTK system to provide timely valid warnings to users when the system must not be used for the intended operation. For instance, in the controlled traffic farming (CTF) system that controls traffic separates wheel beds and root beds, RTK positioning error causes overlap and increases the amount of soil compaction. The RTK system’s integrity capacity can inform users when the actual positional errors of the RTK solutions have exceeded Horizontal Protection Levels (HPL) within a certain Time-To-Alert (TTA) at a given Integrity Risk (IR). The later is defined as the probability that the system claims its normal operational status while actually being in an abnormal status, e.g., the ambiguities being incorrectly fixed and positional errors having exceeded the HPL. The paper studies the required positioning performance (RPP) of GPS positioning system for PA applications such as a CTF system, according to literature review and survey conducted among a number of farming companies. The HPL and IR are derived from these RPP parameters. A RTK-specific rover autonomous integrity monitoring (RAIM) algorithm is developed to determine the system integrity according to real time outputs, such as residual square sum (RSS), HDOP values. A two-station baseline data set is analyzed to demonstrate the concept of RTK integrity and assess the RTK solution continuity, missed detection probability and false alarm probability.

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A Split System Approach (SSA) based methodology is presented to assist in making optimal Preventive Maintenance decisions for serial production lines. The methodology treats a production line as a complex series system with multiple PM actions over multiple intervals. Both risk related cost and maintenance related cost are factored into the methodology as either deterministic or random variables. This SSA based methodology enables Asset Management (AM) decisions to be optimized considering a variety of factors including failure probability, failure cost, maintenance cost, PM performance, and the type of PM strategy. The application of this new methodology and an evaluation of the effects of these factors on PM decisions are demonstrated using an example. The results of this work show that the performance of a PM strategy can be measured by its Total Expected Cost Index (TECI). The optimal PM interval is dependent on TECI, PM performance and types of PM strategies. These factors are interrelated. Generally it was found that a trade-off between reliability and the number of PM actions needs to be made so that one can minimize Total Expected Cost (TEC) for asset maintenance.

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Promoted ignition testing [1–3] is used to determine the relative flammability of metal rods in oxygen-enriched atmospheres. In these tests, a promoter is used to ignite each metal rod to start the sample burning. Experiments were performed to better understand the promoted ignition test by obtaining insight into the effect a burning promoter has on the preheating of a test sample. Test samples of several metallic materials were prepared and coupled to fast-responding thermocouples along their length. Various ignition promoters were used to ignite the test samples. The thermocouple measurements and test video were synchronized to determine temperature increase with respect to time and length along each test sample. A recommended length of test sample that must be consumed to be considered a flammable material was determined based on the preheated zone measured from these tests. This length was determined to be 30 mm (1.18 in.). Validation of this length and its rationale are presented.

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This is a book review of Indigenous Peoples: Self-Determination Knowledge Indigeneity. Edited by Henry Minde in collaboration with Harald Gaski, Svein Jentoft and Georges Midre. Published by Eburon Academic Publishers in Delft, the Netherlands. Paperback, 382 pages, no index. AUD. $79.99. ISBN 978-90-5972-204-0.

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In a recent decision by Mr Justice Laddie, a patent was held anticipated by, inter alia, prior use of a device which fell within the claims of the patent in suit, even though its circuitry was enclosed in resin. The anticipating invention had been "made available to the public" within the terms of section 2 (2) of the Patents Act 1977 because its essential integers would have been revealed by an interesting character, the "skilled forensic engineer".