943 resultados para Pechini method and chromium


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A novel and environment friendly analytical method is reported for total chromium determination and chromium speciation in water samples, whereby tungsten coil atomic emission spectrometry (WCAES) is combined with in situ ionic liquid formation dispersive liquid–liquid microextraction (in situ IL-DLLME). A two stage multivariate optimization approach has been developed employing a Plackett–Burman design for screening and selection of the significant factor involved in the in situ IL-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were complexant concentration: 0.5% (or 0.1%); complexant type: DDTC; IL anion: View the MathML sourcePF6−; [Hmim][Cl] IL amount: 60 mg; ionic strength: 0% NaCl; pH: 5 (or 2); centrifugation time: 10 min; and centrifugation speed: 1000 rpm. Under the optimized experimental conditions the method was evaluated and proper linearity was obtained with a correlation coefficient of 0.991 (5 calibration standards). Limits of detection and quantification for both chromium species were 3 and 10 µg L−1, respectively. This is a 233-fold improvement when compared with chromium determination by WCAES without using preconcentration. The repeatability of the proposed method was evaluated at two different spiking levels (10 and 50 µg L−1) obtaining coefficients of variation of 11.4% and 3.6% (n=3), respectively. A certified reference material (SRM-1643e NIST) was analyzed in order to determine the accuracy of the method for total chromium determination and 112.3% and 2.5 µg L−1 were the recovery (trueness) and standard deviation values, respectively. Tap, bottled mineral and natural mineral water samples were analyzed at 60 µg L−1 spiking level of total Cr content at two Cr(VI)/Cr(III) ratios, and relative recovery values ranged between 88% and 112% showing that the matrix has a negligible effect. To our knowledge, this is the first time that combines in situ IL-DLLME and WCAES.

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In this paper, we present a technique for equilibria characterization of activated carbon having slit-shaped pores. This method was first developed by Do (Do, D. D. A new method for the characterisation of micro-mesoporous materials. Presented at the International Symposium on New Trends in Colloid and Interface Science, September 24-26, 1998 Chiba, Japan) and applied by his group and other groups for characterization of pore size distribution (PSD) as well as adsorption equilibria determination of a wide range of hydrocarbons. It is refined in this paper and compared with the grand canonical Monte Carlo (GCMG) simulation and density functional theory (DFT). The refined theory results in a good agreement between the pore filling pressure versus pore width and those obtained by GCMG and DFT. Furthermore, our local isotherms are qualitatively in good agreement with those obtained by the GCMC simulations. The main advantage of this method is that it is about 4 orders of magnitude faster than the GCMC simulations, making it suitable for optimization studies and design purposes. Finally, we apply our method and the GCMG in the derivation of the PSD of a commercial activated carbon. It was found that the PSD derived from our method is comparable to that derived from the GCMG simulations.

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The purpose of this study was to systematically investigate the effect of lipid chain length and number of lipid chains present on lipopeptides on their ability to be incorporated within liposomes. The peptide KAVYNFATM was synthesized and conjugated to lipoamino acids having acyl chain lengths of C-8, C-12 and C-16. The C-12 construct was also prepared in the monomeric, dimeric and trimeric form. Liposomes were prepared by two techniques: hydration of dried lipid films (Bangham method) and hydration of freeze-dried monophase systems. Encapsulation of lipopeptide within liposomes prepared by hydration of dried lipid films was incomplete in all cases ranging from an entrapment efficiency of 70% for monomeric lipoamino acids at a 5% (w/w) loading to less than 20% for di- and trimeric forms at loadings of 20% (w/w). The incomplete entrapment of lipopeptides within liposomes appeared to be a result of the different solubilities of the lipopeptide and the phospholipids in the solvent used for the preparation of the lipid film. In contrast, encapsulation of lipopeptide within liposomes prepared by hydration of freeze-dried monophase systems was high, even up to a loading of 20% (w/w) and was much less affected by the acyl chain length and number than when liposomes were prepared by hydration of dried lipid films. Freeze drying of monophase systems is better at maintaining a molecular dispersion of the lipopeptide within the solid phospholipid matrix compared to preparation of lipid film by evaporation, particularly if the solubility of the lipopeptide in solvents is markedly different from that of the polar lipids used for liposome preparation. Consequently, upon hydration, the lipopeptide is more efficiently intercalated within the phospholipid bilayers. (C) 2005 Elsevier B.V. All rights reserved.

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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.

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The deposition efficiencies of a number of electroless nickel and cobalt plating solutions were studied and in the case of nickel compared with a commercial plating solution Nifoss 80. At the optimum plating conditions (92ºC and pH 4.5) Nifoss 80 produced nickel layers most efficiently, the alkaline cobalt solution operated most efficiently at 90ºC and pH 9. The methods of producing compostte layers containing 2-3 µm carbide particles and chromium powder is described. Nickel and cobalt layers containing approximately 27% carbide particles, or 40% (Ni) and 30% (Co) chromium particles by volume were obtained. This value is independent of the particle concentration in the plating solution within the range (20~200 g/l). Hardness of the nickel. as deposited was 515 Hv, this was increased to a maximum of 1155 Hv by heat treatment at 200ºC for 5 hours in vacuum. Incorporation. of .chromium carbide particles resulted in a maximum hardness of 1225 Hv after heating at 500ºC for 5 hours in vacuum and chromium particles resulted in a maximum hardness of 16S0 Hv after heat treatment at 400ºC for 2 hours in vacuum. Similarly the hardness of cobalt as deposited was 600 Hv, this was increased to a maximum of 1300 Hv after heat treatment at 400ºC for 1 hour. Incorporation of chromium carbide particles resulted jn a maximum hardness of 1405 Hv after heating at 400ºC for 5 hours in vacuum and chromium particles resulted in a maximum hardness of 1440 Hv after. heat treating for 2 hours at 400ºC in vacuum. The structure of the deposits was studied by optical and scanning electron microscopy. The wear rate and coefficient of friction was determined by a pin and disc method. Wear rate and coefficient of friction decreased with increase in hardness. The wear resistance of the materials was also determined using a simulated forging test. Dies made of standard die steel were coated and the wear rates of the layers as deposited and after heat treatment were compared with those of uncoated tools. The wear resistance generally increased with hardness, it was 50-75% more than the uncoated die steel. Acetic acid salt spray test and outdoor exposure for six months was used to study the corrosion behaviour of the deposits and potentiodynamic curves plotted to find their corrosion potential. Nickel deposit exhibited less staining than carbide composite deposits and nickel-chromium deposits had the most noble corrosion potential.

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The microstructure and thermoelectric properties of Yb-doped Ca0.9-x Yb x La0.1 MnO3 (0 ≤ x ≤ 0.05) ceramics prepared by using the Pechini method derived powders have been investigated. X-ray diffraction analysis has shown that all samples exhibit single phase with orthorhombic perovskite structure. All ceramic samples possess high relative densities, ranging from 97.04% to 98.65%. The Seebeck coefficient is negative, indicating n-type conduction in all samples. The substitution of Yb for Ca leads to a marked decrease in the electrical resistivity, along with a moderate decrease in the absolute value of the Seebeck coefficient. The highest power factor is obtained for the sample with x = 0.05. The electrical conduction in these compounds is due to electrons hopping between Mn3+ and Mn4+, which is enhanced by increasing Yb content.

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This article presents the principal results of the Ph.D. thesis Investigation and classification of doubly resolvable designs by Stela Zhelezova (Institute of Mathematics and Informatics, BAS), successfully defended at the Specialized Academic Council for Informatics and Mathematical Modeling on 22 February 2010.

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There is an increasing demand for DNA analysis because of the sensitivity of the method and the ability to uniquely identify and distinguish individuals with a high degree of certainty. But this demand has led to huge backlogs in evidence lockers since the current DNA extraction protocols require long processing time. The DNA analysis procedure becomes more complicated when analyzing sexual assault casework samples where the evidence contains more than one contributor. Additional processing to separate different cell types in order to simplify the final data interpretation further contributes to the existing cumbersome protocols. The goal of the present project is to develop a rapid and efficient extraction method that permits selective digestion of mixtures. ^ Selective recovery of male DNA was achieved with as little as 15 minutes lysis time upon exposure to high pressure under alkaline conditions. Pressure cycling technology (PCT) is carried out in a barocycler that has a small footprint and is semi-automated. Typically less than 10% male DNA is recovered using the standard extraction protocol for rape kits, almost seven times more male DNA was recovered from swabs using this novel method. Various parameters including instrument setting and buffer composition were optimized to achieve selective recovery of sperm DNA. Some developmental validation studies were also done to determine the efficiency of this method in processing samples exposed to various conditions that can affect the quality of the extraction and the final DNA profile. ^ Easy to use interface, minimal manual interference and the ability to achieve high yields with simple reagents in a relatively short time make this an ideal method for potential application in analyzing sexual assault samples.^

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Purpose: Computed Tomography (CT) is one of the standard diagnostic imaging modalities for the evaluation of a patient’s medical condition. In comparison to other imaging modalities such as Magnetic Resonance Imaging (MRI), CT is a fast acquisition imaging device with higher spatial resolution and higher contrast-to-noise ratio (CNR) for bony structures. CT images are presented through a gray scale of independent values in Hounsfield units (HU). High HU-valued materials represent higher density. High density materials, such as metal, tend to erroneously increase the HU values around it due to reconstruction software limitations. This problem of increased HU values due to metal presence is referred to as metal artefacts. Hip prostheses, dental fillings, aneurysm clips, and spinal clips are a few examples of metal objects that are of clinical relevance. These implants create artefacts such as beam hardening and photon starvation that distort CT images and degrade image quality. This is of great significance because the distortions may cause improper evaluation of images and inaccurate dose calculation in the treatment planning system. Different algorithms are being developed to reduce these artefacts for better image quality for both diagnostic and therapeutic purposes. However, very limited information is available about the effect of artefact correction on dose calculation accuracy. This research study evaluates the dosimetric effect of metal artefact reduction algorithms on severe artefacts on CT images. This study uses Gemstone Spectral Imaging (GSI)-based MAR algorithm, projection-based Metal Artefact Reduction (MAR) algorithm, and the Dual-Energy method.

Materials and Methods: The Gemstone Spectral Imaging (GSI)-based and SMART Metal Artefact Reduction (MAR) algorithms are metal artefact reduction protocols embedded in two different CT scanner models by General Electric (GE), and the Dual-Energy Imaging Method was developed at Duke University. All three approaches were applied in this research for dosimetric evaluation on CT images with severe metal artefacts. The first part of the research used a water phantom with four iodine syringes. Two sets of plans, multi-arc plans and single-arc plans, using the Volumetric Modulated Arc therapy (VMAT) technique were designed to avoid or minimize influences from high-density objects. The second part of the research used projection-based MAR Algorithm and the Dual-Energy Method. Calculated Doses (Mean, Minimum, and Maximum Doses) to the planning treatment volume (PTV) were compared and homogeneity index (HI) calculated.

Results: (1) Without the GSI-based MAR application, a percent error between mean dose and the absolute dose ranging from 3.4-5.7% per fraction was observed. In contrast, the error was decreased to a range of 0.09-2.3% per fraction with the GSI-based MAR algorithm. There was a percent difference ranging from 1.7-4.2% per fraction between with and without using the GSI-based MAR algorithm. (2) A range of 0.1-3.2% difference was observed for the maximum dose values, 1.5-10.4% for minimum dose difference, and 1.4-1.7% difference on the mean doses. Homogeneity indexes (HI) ranging from 0.068-0.065 for dual-energy method and 0.063-0.141 with projection-based MAR algorithm were also calculated.

Conclusion: (1) Percent error without using the GSI-based MAR algorithm may deviate as high as 5.7%. This error invalidates the goal of Radiation Therapy to provide a more precise treatment. Thus, GSI-based MAR algorithm was desirable due to its better dose calculation accuracy. (2) Based on direct numerical observation, there was no apparent deviation between the mean doses of different techniques but deviation was evident on the maximum and minimum doses. The HI for the dual-energy method almost achieved the desirable null values. In conclusion, the Dual-Energy method gave better dose calculation accuracy to the planning treatment volume (PTV) for images with metal artefacts than with or without GE MAR Algorithm.

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There is an increasing demand for DNA analysis because of the sensitivity of the method and the ability to uniquely identify and distinguish individuals with a high degree of certainty. But this demand has led to huge backlogs in evidence lockers since the current DNA extraction protocols require long processing time. The DNA analysis procedure becomes more complicated when analyzing sexual assault casework samples where the evidence contains more than one contributor. Additional processing to separate different cell types in order to simplify the final data interpretation further contributes to the existing cumbersome protocols. The goal of the present project is to develop a rapid and efficient extraction method that permits selective digestion of mixtures. Selective recovery of male DNA was achieved with as little as 15 minutes lysis time upon exposure to high pressure under alkaline conditions. Pressure cycling technology (PCT) is carried out in a barocycler that has a small footprint and is semi-automated. Typically less than 10% male DNA is recovered using the standard extraction protocol for rape kits, almost seven times more male DNA was recovered from swabs using this novel method. Various parameters including instrument setting and buffer composition were optimized to achieve selective recovery of sperm DNA. Some developmental validation studies were also done to determine the efficiency of this method in processing samples exposed to various conditions that can affect the quality of the extraction and the final DNA profile. Easy to use interface, minimal manual interference and the ability to achieve high yields with simple reagents in a relatively short time make this an ideal method for potential application in analyzing sexual assault samples.

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Aflatoxins are one kind of fungal toxins produced by species of toxigenic Aspergillus (A. flavus and A. parasiticus) and in other words they are secondary metabolites which are considered as one of the threatening factors of food consumer's health. In this research 96 samples of cold-water cultural fish feed, rainbow trout, during the seasons of spring and summer of 2007 (every fifteenth of the month) were randomized (by simple and stratified random) to determine: 1. The prevalence rate of aflatoxigenic species of Aspergillus in stored feed of cold-water cultural fish in West Azarbayjan cultural fish farms in both seasons (spring and summer); 2. The residues of total aflatoxin in stored feed of fish in cultural fish farms of West Azarbayjan in both seasons by ELISA method; and 3. The residues of that toxin in feed produced in aquatic feed factories in Tehran and West Azarbyjan provinces with the same method. In order to study prevalence rate of toxigenic species of Aspergillus, pour-plate culture method by general medium such as Malt Extract Agar (M.E.A.) and Sabouraud-Dextrose Agar (S.D.A.) and by standard No.997 of Iranian Standard Institute were used. The produced colonies were examined microscopically. To determine the aflatoxins residues, ELISA method using Agra-Quant kit of Romer Lab company, were applied. The results of this survey indicated that only 8.3% of the samples were infected by A. flavus. A. parasiticus was not observed. There were no significant differences between the prevalence rate of AFT and seasons/months, either (P<0.05). Evaluating mean of aflatoxin rate showed that the rates of this variable are lower than the tolerance levels designated by the joint FAO/WHO expert committee (The mean of AFT in all data was lower than 11 ppb). Furthermore, mean of total AFT residues rates of stored feed of various cultural center of West Azarbayjan and Tehran factories were comparable in spring and summer, and no significant differences were observed (P<0.05). But there were significant differences between the total aflatoxin rates in the feed of West Azarbayjan factory and spring and summer (P<0.05), and AFT residues in spring (8.6 ppb) were higher than summer (6.1 ppb). Prevalence rates of AFT in Tehran feed factories (9.2 ppb) are higher than W. Azarbayjan (7.4 ppb). In other words, location was considered as a decisive factor in total AFT rates of samples. Moreover, the results indicated that there was significant difference between total aflatoxin rates of feed and cultural centers (P<0.05). The mean of AFT rates in embankment dam cultural fish farms (6.75 ppb) and multi-functions cultural fish farms (6.25 ppb) was higher than individual cultural pond (4.67 ppb). In conclusion, the finally results of this survey indicated that the lower rates of Aspergillus is not effective on the presence of total aflatoxin rates in trout feed. Due to low levels of aflatoxin rates (lower than 20 ppb), the produced feed of cold-cultural fishes, Rainbow Trout, in Tehran and West Azarbayjan provinces, in spring and summer of 2007, were safe and healthy both for fish and their consumers.

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Aquaculture has been expanded rapidly to become a major commercial and food-producing sector worldwide in recent decade. In parallel, viral diseases rapidly spread among farms causing enormous economic losses. The accurate detection of pathogens at early stages of infection is a key point for disease control in aquaculture. Spring Viraemia of Carp Virus (SVCV) is a very severe pathogen of carp fishes in different parts of the world and is categorized as a reportable listed disease in the annual published list of World Organization for animal Health (OIE). The objective of this study was to develop and evaluate RT- PCR test for detecting SVC virus and also the sensitivity and specificity of this test. A semi nested RT- PCR was designed using combination of three primers: two external (SVCF , SVCR) and one internal (SVCS) primers which based on conserved region of G gen. The specificity of designed primers (only external ones) by examination on Viral Hemorrhagic Septicemia Virus (VHSV) and Infectious Hematopoietic Necrosis Virus (IHNV) was confirmed. For optimizing of the PCR test, primer concentration, primer annealing temperature, cycle number and Mgcl2 concentration were surveyed. Also for validity test, prevention of false negative and Assurance of its accuracy, a competitive internal control (mimic) designed and its suitable concentration was defined. Evaluation of the sensitivity of designed test were conducted first by comparing the different commercially available RNA isolation guidelines, two guidelines: isotiocyanate phenol–chloroform based protocols (RNX–Plus Iran, Iq2000 kit Taiwan ) and two column based protocols (Cinna pure RNA Iran , high pure viral RNA kit, Roche Germany ). The results indicated that the column based protocols (Roche method and Cinna pure), yield 36.77 ng/μl and 16/47 ng/μl RNA concentration respectively, which were significantly higher than other protocols(P<0.05). Then for evaluation of extracted RNA sensitivity, Serial dilution of SVCV strain 56.70 grown in EPC (1.9×105 TCID50/ml) was examined To compare sensitivity. Extracted RNA from serial dilution with stone's primers and commercial IQ-2000 kit were examined simultaneously. The result indicated that designed semi- nested RT- PCR was able to recognize SVC virus to 10-4 dilution and stone's primer recognize to 10-3 dilution whereas Iq-2000 commercial kit did not recognized in any dilution. In high virus titer in designed test two DNA band (462 bp and 266 bp) produced, and by decreasing virus titer 462 bp was omitted. In low virus titer or lack of virus, just DNA band (mimic) 729 bp can propagate. After designing and optimizing PCR test, a total of 400 suspected cultured Cyprinus carpio with high mortality from 4 aquaculture zone of Khuzestan province were collected and tested for SVCV during 2012- 2013 using developed PCR method and IQ- 2000. The results indicated that SVC virus was not observed in samples using both methods.

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In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

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The cerium oxide has a high potential for use in removing pollutants after combustion, removal of organic matter in waste water and the fuel-cell technology. The nickel oxide is an attractive material due to its excellent chemical stability and their optical properties, electrical and magnetic. In this work, CeO2-NiO- systems on molars reasons 1:1(I), 1:2(II) e 1:3(III) metal-citric acid were synthesized using the Pechini method. We used techniques of TG / DTG and ATD to monitor the degradation process of organic matter to the formation of the oxide. By thermogravimetric analysis and applying the dynamic method proposed by Coats-Redfern, it was possible to study the reactions of thermal decomposition in order to propose the possible mechanism by which the reaction takes place, as well as the determination of kinetic parameters as activation energy, Ea, pre-exponential factor and parameters of activation. It was observed that both variables exert a significant influence on the formation of complex polymeric precursor. The model that best fitted the experimental data in the dynamic mode was R3, which consists of nuclear growth, which formed the nuclei grow to a continuous reaction interface, it proposes a spherical symmetry (order 2 / 3). The values of enthalpy of activation of the system showed that the reaction in the state of transition is exothermic. The variables of composition, together with the variable temperature of calcination were studied by different techniques such as XRD, IV and SEM. Also a study was conducted microstructure by the Rietveld method, the calculation routine was developed to run the package program FullProf Suite, and analyzed by pseudo-Voigt function. It was found that the molar ratio of variable metal-citric acid in the system CeO2-NiO (I), (II), (III) has strong influence on the microstructural properties, size of crystallites and microstrain network, and can be used to control these properties

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Designers need to develop good observational skills in order to conduct user studies that reveal the subtleties of human interactions and adequately inform design activity. In this paper we describe a game format that we have used in concert with wiki-web technology, to engage our IT and Information Environments students in developing much sharper observational skills. The Video Card Game is a method of video analysis that is suited to design practitioners as well as to researchers. It uses the familiar format of a card game similar to "Happy Families,, to help students develop themes of interactions from watching video clips. Students then post their interaction themes on wiki-web pages, which allows the teaching team and other students to edit and comment on them. We found that the tangible (cards), game, role playing and sharing aspects of this method led to a much larger amount of interaction and discussion between student groups and between students and the teaching team, than we have achieved using our traditional teaching methods, while taking no more time on the part of the teaching staff. The quality of the resulting interaction themes indicates that this method fosters development of observational skills.In the paper we describe the motivations, method and results in full. We also describe the research context in which we collected the videotape data, and how this method relates to state of the art research methods in interaction design for ubiquitous computing technology.