Analysis Study of Stevioside and Rebaudioside A from Stevia rebaudiana Bertoni by Normal Phase SPE and RP-HPLC

NASA Astrophysics Data System (ADS)

Martono, Y.; Rohman, A.; Riyanto, S.; Martono, S.

2018-04-01

Solid Phase Extraction (SPE) method using silica as sorbent for stevioside and rebaudiosida A analysis in Stevia rebaudiana Bertoni leaf have not been performed. The aim of this study is to develop SPE method using silica as sorbent for Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) analysis of stevioside and rebaudiosida A in S. rebaudiana leaf. The results of this study indicate that the optimal conditions for normal phase SPE (silica) are conditioned with 3.0 mL of hexane. The sample loading volume is 0.1 mL. Cartridge is eluted with 1.0 mL acetonitrile: water (80: 20, v/v) to separate both analytes. The cartridge is washed with chloroform and water of 0.3 mL respectively. The developed SPE sample preparation method meets the accuracy and precision test and can be used for the analysis of stevioside and rebaudioside A by RP-HPLC.

Tau-independent Phase Analysis: A Novel Method for Accurately Determining Phase Shifts.

PubMed

Tackenberg, Michael C; Jones, Jeff R; Page, Terry L; Hughey, Jacob J

2018-06-01

Estimations of period and phase are essential in circadian biology. While many techniques exist for estimating period, comparatively few methods are available for estimating phase. Current approaches to analyzing phase often vary between studies and are sensitive to coincident changes in period and the stage of the circadian cycle at which the stimulus occurs. Here we propose a new technique, tau-independent phase analysis (TIPA), for quantifying phase shifts in multiple types of circadian time-course data. Through comprehensive simulations, we show that TIPA is both more accurate and more precise than the standard actogram approach. TIPA is computationally simple and therefore will enable accurate and reproducible quantification of phase shifts across multiple subfields of chronobiology.

More About the Phase-Synchronized Enhancement Method

NASA Technical Reports Server (NTRS)

Jong, Jen-Yi

2004-01-01

A report presents further details regarding the subject matter of "Phase-Synchronized Enhancement Method for Engine Diagnostics" (MFS-26435), NASA Tech Briefs, Vol. 22, No. 1 (January 1998), page 54. To recapitulate: The phase-synchronized enhancement method (PSEM) involves the digital resampling of a quasi-periodic signal in synchronism with the instantaneous phase of one of its spectral components. This resampling transforms the quasi-periodic signal into a periodic one more amenable to analysis. It is particularly useful for diagnosis of a rotating machine through analysis of vibration spectra that include components at the fundamental and harmonics of a slightly fluctuating rotation frequency. The report discusses the machinery-signal-analysis problem, outlines the PSEM algorithms, presents the mathematical basis of the PSEM, and presents examples of application of the PSEM in some computational simulations.

Phase unwrapping using region-based markov random field model.

PubMed

Dong, Ying; Ji, Jim

2010-01-01

Phase unwrapping is a classical problem in Magnetic Resonance Imaging (MRI), Interferometric Synthetic Aperture Radar and Sonar (InSAR/InSAS), fringe pattern analysis, and spectroscopy. Although many methods have been proposed to address this problem, robust and effective phase unwrapping remains a challenge. This paper presents a novel phase unwrapping method using a region-based Markov Random Field (MRF) model. Specifically, the phase image is segmented into regions within which the phase is not wrapped. Then, the phase image is unwrapped between different regions using an improved Highest Confidence First (HCF) algorithm to optimize the MRF model. The proposed method has desirable theoretical properties as well as an efficient implementation. Simulations and experimental results on MRI images show that the proposed method provides similar or improved phase unwrapping than Phase Unwrapping MAx-flow/min-cut (PUMA) method and ZpM method.

Comparative Analysis of Methods of Evaluating the Lower Ionosphere Parameters by Tweek Atmospherics

NASA Astrophysics Data System (ADS)

Krivonos, A. P.; Shvets, A. V.

2016-12-01

Purpose: A comparative analysis of the phase and frequency methods for determining the Earth-ionosphere effective waveguide heights for the basic and higher types of normal waves (modes) and distance to the source of radiation - lightning - has been made by analyzing pulse signals in the ELF-VLF range - tweek-atmospherics (tweeks). Design/methodology/approach: To test the methods in computer simulations, the tweeks waveforms were synthesized for the Earth-ionosphere waveguide model with the exponential conductivity profile of the lower ionosphere. The calculations were made for a 20-40 dB signal/noise ratio. Findings: The error of the frequency method of determining the effective height of the waveguide for different waveguide modes was less than 0.5 %. The error of the phase method for determining the effective height of the waveguide was less than 0.8 %. Errors in determining the distance to the lightning was less than 1 % for the phase method, and less than 5 % for the frequency method for the source ranges 1000-3000 km. Conclusions: The analysis results have showed the accuracy of the frequency and phase methods being practically the same within distances of 1000-3000 km. For distances less than 1000 km, the phase method shows a more accurate evaluation of the range, so the combination of the two methods can be used to improve estimating the tweek’s propagation path parameters.

Analysis of imazaquin in soybeans by solid-phase extraction and high-performance liquid chromatography.

PubMed

Guo, C; Hu, J-Y; Chen, X-Y; Li, J-Z

2008-02-01

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.

Inferring Functional Neural Connectivity with Phase Synchronization Analysis: A Review of Methodology

PubMed Central

Sun, Junfeng; Li, Zhijun; Tong, Shanbao

2012-01-01

Functional neural connectivity is drawing increasing attention in neuroscience research. To infer functional connectivity from observed neural signals, various methods have been proposed. Among them, phase synchronization analysis is an important and effective one which examines the relationship of instantaneous phase between neural signals but neglecting the influence of their amplitudes. In this paper, we review the advances in methodologies of phase synchronization analysis. In particular, we discuss the definitions of instantaneous phase, the indexes of phase synchronization and their significance test, the issues that may affect the detection of phase synchronization and the extensions of phase synchronization analysis. In practice, phase synchronization analysis may be affected by observational noise, insufficient samples of the signals, volume conduction, and reference in recording neural signals. We make comments and suggestions on these issues so as to better apply phase synchronization analysis to inferring functional connectivity from neural signals. PMID:22577470

Respiratory-phase domain analysis of heart rate variability can accurately estimate cardiac vagal activity during a mental arithmetic task.

PubMed

Kotani, Kiyoshi; Takamasu, Kiyoshi; Tachibana, Makoto

2007-01-01

The objectives of this paper were to present a method to extract the amplitude of RSA in the respiratory-phase domain, to compare that with subjective or objective indices of the MWL (mental workload), and to compare that with a conventional frequency analysis in terms of its accuracy during a mental arithmetic task. HRV (heart rate variability), ILV (instantaneous lung volume), and motion of the throat were measured under a mental arithmetic experiment and subjective and objective indices were also obtained. The amplitude of RSA was extracted in the respiratory-phase domain, and its correlation with the load level was compared with the results of the frequency domain analysis, which is the standard analysis of the HRV. The subjective and objective indices decreased as the load level increased, showing that the experimental protocol was appropriate. Then, the amplitude of RSA in the respiratory-phase domain also decreased with the increase in the load level. The results of the correlation analysis showed that the respiratory-phase domain analysis has higher negative correlations, -0.84 and -0.82, with the load level as determined by simple correlation and rank correlation, respectively, than does frequency analysis, for which the correlations were found to be -0.54 and -0.63, respectively. In addition, it was demonstrated that the proposed method could be applied to the short-term extraction of RSA amplitude. We proposed a simple and effective method to extract the amplitude of the respiratory sinus arrhythmia (RSA) in the respiratory-phase domain and the results show that this method can estimate cardiac vagal activity more accurately than frequency analysis.

Phase walk analysis of leptokurtic time series.

PubMed

Schreiber, Korbinian; Modest, Heike I; Räth, Christoph

2018-06-01

The Fourier phase information play a key role for the quantified description of nonlinear data. We present a novel tool for time series analysis that identifies nonlinearities by sensitively detecting correlations among the Fourier phases. The method, being called phase walk analysis, is based on well established measures from random walk analysis, which are now applied to the unwrapped Fourier phases of time series. We provide an analytical description of its functionality and demonstrate its capabilities on systematically controlled leptokurtic noise. Hereby, we investigate the properties of leptokurtic time series and their influence on the Fourier phases of time series. The phase walk analysis is applied to measured and simulated intermittent time series, whose probability density distribution is approximated by power laws. We use the day-to-day returns of the Dow-Jones industrial average, a synthetic time series with tailored nonlinearities mimicing the power law behavior of the Dow-Jones and the acceleration of the wind at an Atlantic offshore site. Testing for nonlinearities by means of surrogates shows that the new method yields strong significances for nonlinear behavior. Due to the drastically decreased computing time as compared to embedding space methods, the number of surrogate realizations can be increased by orders of magnitude. Thereby, the probability distribution of the test statistics can very accurately be derived and parameterized, which allows for much more precise tests on nonlinearities.

Gamma model and its analysis for phase measuring profilometry.

PubMed

Liu, Kai; Wang, Yongchang; Lau, Daniel L; Hao, Qi; Hassebrook, Laurence G

2010-03-01

Phase measuring profilometry is a method of structured light illumination whose three-dimensional reconstructions are susceptible to error from nonunitary gamma in the associated optical devices. While the effects of this distortion diminish with an increasing number of employed phase-shifted patterns, gamma distortion may be unavoidable in real-time systems where the number of projected patterns is limited by the presence of target motion. A mathematical model is developed for predicting the effects of nonunitary gamma on phase measuring profilometry, while also introducing an accurate gamma calibration method and two strategies for minimizing gamma's effect on phase determination. These phase correction strategies include phase corrections with and without gamma calibration. With the reduction in noise, for three-step phase measuring profilometry, analysis of the root mean squared error of the corrected phase will show a 60x reduction in phase error when the proposed gamma calibration is performed versus 33x reduction without calibration.

An approach for automated fault diagnosis based on a fuzzy decision tree and boundary analysis of a reconstructed phase space.

PubMed

Aydin, Ilhan; Karakose, Mehmet; Akin, Erhan

2014-03-01

Although reconstructed phase space is one of the most powerful methods for analyzing a time series, it can fail in fault diagnosis of an induction motor when the appropriate pre-processing is not performed. Therefore, boundary analysis based a new feature extraction method in phase space is proposed for diagnosis of induction motor faults. The proposed approach requires the measurement of one phase current signal to construct the phase space representation. Each phase space is converted into an image, and the boundary of each image is extracted by a boundary detection algorithm. A fuzzy decision tree has been designed to detect broken rotor bars and broken connector faults. The results indicate that the proposed approach has a higher recognition rate than other methods on the same dataset. © 2013 ISA Published by ISA All rights reserved.

Measurement of edge residual stresses in glass by the phase-shifting method

NASA Astrophysics Data System (ADS)

Ajovalasit, A.; Petrucci, G.; Scafidi, M.

2011-05-01

Control and measurement of residual stress in glass is of great importance in the industrial field. Since glass is a birefringent material, the residual stress analysis is based mainly on the photoelastic method. This paper considers two methods of automated analysis of membrane residual stress in glass sheets, based on the phase-shifting concept in monochromatic light. In particular these methods are the automated versions of goniometric compensation methods of Tardy and Sénarmont. The proposed methods can effectively replace manual methods of compensation (goniometric compensation of Tardy and Sénarmont, Babinet and Babinet-Soleil compensators) provided by current standards on the analysis of residual stresses in glasses.

Solving phase appearance/disappearance two-phase flow problems with high resolution staggered grid and fully implicit schemes by the Jacobian-free Newton–Krylov Method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zou, Ling; Zhao, Haihua; Zhang, Hongbin

2016-04-01

The phase appearance/disappearance issue presents serious numerical challenges in two-phase flow simulations. Many existing reactor safety analysis codes use different kinds of treatments for the phase appearance/disappearance problem. However, to our best knowledge, there are no fully satisfactory solutions. Additionally, the majority of the existing reactor system analysis codes were developed using low-order numerical schemes in both space and time. In many situations, it is desirable to use high-resolution spatial discretization and fully implicit time integration schemes to reduce numerical errors. In this work, we adapted a high-resolution spatial discretization scheme on staggered grid mesh and fully implicit time integrationmore » methods (such as BDF1 and BDF2) to solve the two-phase flow problems. The discretized nonlinear system was solved by the Jacobian-free Newton Krylov (JFNK) method, which does not require the derivation and implementation of analytical Jacobian matrix. These methods were tested with a few two-phase flow problems with phase appearance/disappearance phenomena considered, such as a linear advection problem, an oscillating manometer problem, and a sedimentation problem. The JFNK method demonstrated extremely robust and stable behaviors in solving the two-phase flow problems with phase appearance/disappearance. No special treatments such as water level tracking or void fraction limiting were used. High-resolution spatial discretization and second- order fully implicit method also demonstrated their capabilities in significantly reducing numerical errors.« less

Deformation analysis of MEMS structures by modified digital moiré methods

NASA Astrophysics Data System (ADS)

Liu, Zhanwei; Lou, Xinhao; Gao, Jianxin

2010-11-01

Quantitative deformation analysis of micro-fabricated electromechanical systems is of importance for the design and functional control of microsystems. In this paper, two modified digital moiré processing methods, Gaussian blurring algorithm combined with digital phase shifting and geometrical phase analysis (GPA) technique based on digital moiré method, are developed to quantitatively analyse the deformation behaviour of micro-electro-mechanical system (MEMS) structures. Measuring principles and experimental procedures of the two methods are described in detail. A digital moiré fringe pattern is generated by superimposing a specimen grating etched directly on a microstructure surface with a digital reference grating (DRG). Most of the grating noise is removed from the digital moiré fringes, which enables the phase distribution of the moiré fringes to be obtained directly. Strain measurement result of a MEMS structure demonstrates the feasibility of the two methods.

Using the phase-space imager to analyze partially coherent imaging systems: bright-field, phase contrast, differential interference contrast, differential phase contrast, and spiral phase contrast

NASA Astrophysics Data System (ADS)

Mehta, Shalin B.; Sheppard, Colin J. R.

2010-05-01

Various methods that use large illumination aperture (i.e. partially coherent illumination) have been developed for making transparent (i.e. phase) specimens visible. These methods were developed to provide qualitative contrast rather than quantitative measurement-coherent illumination has been relied upon for quantitative phase analysis. Partially coherent illumination has some important advantages over coherent illumination and can be used for measurement of the specimen's phase distribution. However, quantitative analysis and image computation in partially coherent systems have not been explored fully due to the lack of a general, physically insightful and computationally efficient model of image formation. We have developed a phase-space model that satisfies these requirements. In this paper, we employ this model (called the phase-space imager) to elucidate five different partially coherent systems mentioned in the title. We compute images of an optical fiber under these systems and verify some of them with experimental images. These results and simulated images of a general phase profile are used to compare the contrast and the resolution of the imaging systems. We show that, for quantitative phase imaging of a thin specimen with matched illumination, differential phase contrast offers linear transfer of specimen information to the image. We also show that the edge enhancement properties of spiral phase contrast are compromised significantly as the coherence of illumination is reduced. The results demonstrate that the phase-space imager model provides a useful framework for analysis, calibration, and design of partially coherent imaging methods.

Optimization of solar cells for air mass zero operation and study of solar cells at high temperatures, phase 4

NASA Technical Reports Server (NTRS)

Hovel, H. J.; Woodall, J. M.

1980-01-01

The Pd contact to GaAs was studied using backscattering, Auger analysis, and sheet resistance measurements. Several metallurgical phases were present at low temperatures, but PdGa was the dominant phase in samples annealed at 500 C. Ti/Pd/Ag contacts appeared to have the lowest contact resistance. Etchback epitaxy (EBE) was compared to saturated melt epitaxy (SME) method of growing liquid phase epitaxial layers. The SME method resulted in a lower density of Ga microdroplets in the grown layer, although the best solar cells were made by the EBE method. Photoluminescence was developed as a tool for contactless analysis of GaAs cells. Efficiencies of over 8 percent were measured at 250 C.

Estimation of phase derivatives using discrete chirp-Fourier-transform-based method.

PubMed

Gorthi, Sai Siva; Rastogi, Pramod

2009-08-15

Estimation of phase derivatives is an important task in many interferometric measurements in optical metrology. This Letter introduces a method based on discrete chirp-Fourier transform for accurate and direct estimation of phase derivatives, even in the presence of noise. The method is introduced in the context of the analysis of reconstructed interference fields in digital holographic interferometry. We present simulation and experimental results demonstrating the utility of the proposed method.

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review.

PubMed

Rahman, Md Musfiqur; Abd El-Aty, A M; Kim, Sung-Woo; Shin, Sung Chul; Shin, Ho-Chul; Shim, Jae-Han

2017-01-01

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An effective method to accurately calculate the phase space factors for β - β - decay

DOE Office of Scientific and Technical Information (OSTI.GOV)

Neacsu, Andrei; Horoi, Mihai

2016-01-01

Accurate calculations of the electron phase space factors are necessary for reliable predictions of double-beta decay rates and for the analysis of the associated electron angular and energy distributions. Here, we present an effective method to calculate these phase space factors that takes into account the distorted Coulomb field of the daughter nucleus, yet it allows one to easily calculate the phase space factors with good accuracy relative to the most exact methods available in the recent literature.

Advanced electron microscopy methods for the analysis of MgB2 superconductor

NASA Astrophysics Data System (ADS)

Birajdar, B.; Peranio, N.; Eibl, O.

2008-02-01

Advanced electron microscopy methods used for the analysis of superconducting MgB2 wires and tapes are described. The wires and tapes were prepared by the powder in tube method using different processing technologies and thoroughly characterised for their superconducting properties within the HIPERMAG project. Microstructure analysis on μm to nm length scales is necessary to understand the superconducting properties of MgB2. For the MgB2 phase analysis on μm scale an analytical SEM, and for the analysis on nm scale a energy-filtered STEM is used. Both the microscopes were equipped with EDX detector and field emission gun. Electron microscopy and spectroscopy of MgB2 is challenging because of the boron analysis, carbon and oxygen contamination, and the presence of large number of secondary phases. Advanced electron microscopy involves, combined SEM, EPMA and TEM analysis with artefact free sample preparation, elemental mapping and chemical quantification of point spectra. Details of the acquisition conditions and achieved accuracy are presented. Ex-situ wires show oxygen-free MgB2 colonies (a colony is a dense arrangement of several MgB2 grains) embedded in a porous and oxygen-rich matrix, introducing structural granularity. In comparison, in-situ wires are generally more dense, but show inhibited MgB2 phase formation with significantly higher fraction of B-rich secondary phases. SiC additives in the in-situ wires forms Mg2Si secondary phases. The advanced electron microscopy has been used to extract the microstructure parameters like colony size, B-rich secondary phase fraction, O mole fraction and MgB2 grain size, and establish a microstructure-critical current density model [1]. In summary, conventional secondary electron imaging in SEM and diffraction contrast imaging in the TEM are by far not sufficient and advanced electron microscopy methods are essential for the analysis of superconducting MgB2 wires and tapes.

3D geometric phase analysis and its application in 3D microscopic morphology measurement

NASA Astrophysics Data System (ADS)

Zhu, Ronghua; Shi, Wenxiong; Cao, Quankun; Liu, Zhanwei; Guo, Baoqiao; Xie, Huimin

2018-04-01

Although three-dimensional (3D) morphology measurement has been widely applied on the macro-scale, there is still a lack of 3D measurement technology on the microscopic scale. In this paper, a microscopic 3D measurement technique based on the 3D-geometric phase analysis (GPA) method is proposed. In this method, with machine vision and phase matching, the traditional GPA method is extended to three dimensions. Using this method, 3D deformation measurement on the micro-scale can be realized using a light microscope. Simulation experiments were conducted in this study, and the results demonstrate that the proposed method has a good anti-noise ability. In addition, the 3D morphology of the necking zone in a tensile specimen was measured, and the results demonstrate that this method is feasible.

The statistical analysis of circadian phase and amplitude in constant-routine core-temperature data

NASA Technical Reports Server (NTRS)

Brown, E. N.; Czeisler, C. A.

1992-01-01

Accurate estimation of the phases and amplitude of the endogenous circadian pacemaker from constant-routine core-temperature series is crucial for making inferences about the properties of the human biological clock from data collected under this protocol. This paper presents a set of statistical methods based on a harmonic-regression-plus-correlated-noise model for estimating the phases and the amplitude of the endogenous circadian pacemaker from constant-routine core-temperature data. The methods include a Bayesian Monte Carlo procedure for computing the uncertainty in these circadian functions. We illustrate the techniques with a detailed study of a single subject's core-temperature series and describe their relationship to other statistical methods for circadian data analysis. In our laboratory, these methods have been successfully used to analyze more than 300 constant routines and provide a highly reliable means of extracting phase and amplitude information from core-temperature data.

Classification of LC columns based on the QSRR method and selectivity toward moclobemide and its metabolites.

PubMed

Plenis, Alina; Olędzka, Ilona; Bączek, Tomasz

2013-05-05

This paper focuses on a comparative study of the column classification system based on the quantitative structure-retention relationships (QSRR method) and column performance in real biomedical analysis. The assay was carried out for the LC separation of moclobemide and its metabolites in human plasma, using a set of 24 stationary phases. The QSRR models established for the studied stationary phases were compared with the column test performance results under two chemometric techniques - the principal component analysis (PCA) and the hierarchical clustering analysis (HCA). The study confirmed that the stationary phase classes found closely related by the QSRR approach yielded comparable separation for moclobemide and its metabolites. Therefore, the QSRR method could be considered supportive in the selection of a suitable column for the biomedical analysis offering the selection of similar or dissimilar columns with a relatively higher certainty. Copyright © 2013 Elsevier B.V. All rights reserved.

Realist explanatory theory building method for social epidemiology: a protocol for a mixed method multilevel study of neighbourhood context and postnatal depression.

PubMed

Eastwood, John G; Jalaludin, Bin B; Kemp, Lynn A

2014-01-01

A recent criticism of social epidemiological studies, and multi-level studies in particular has been a paucity of theory. We will present here the protocol for a study that aims to build a theory of the social epidemiology of maternal depression. We use a critical realist approach which is trans-disciplinary, encompassing both quantitative and qualitative traditions, and that assumes both ontological and hierarchical stratification of reality. We describe a critical realist Explanatory Theory Building Method comprising of an: 1) emergent phase, 2) construction phase, and 3) confirmatory phase. A concurrent triangulated mixed method multilevel cross-sectional study design is described. The Emergent Phase uses: interviews, focus groups, exploratory data analysis, exploratory factor analysis, regression, and multilevel Bayesian spatial data analysis to detect and describe phenomena. Abductive and retroductive reasoning will be applied to: categorical principal component analysis, exploratory factor analysis, regression, coding of concepts and categories, constant comparative analysis, drawing of conceptual networks, and situational analysis to generate theoretical concepts. The Theory Construction Phase will include: 1) defining stratified levels; 2) analytic resolution; 3) abductive reasoning; 4) comparative analysis (triangulation); 5) retroduction; 6) postulate and proposition development; 7) comparison and assessment of theories; and 8) conceptual frameworks and model development. The strength of the critical realist methodology described is the extent to which this paradigm is able to support the epistemological, ontological, axiological, methodological and rhetorical positions of both quantitative and qualitative research in the field of social epidemiology. The extensive multilevel Bayesian studies, intensive qualitative studies, latent variable theory, abductive triangulation, and Inference to Best Explanation provide a strong foundation for Theory Construction. The study will contribute to defining the role that realism and mixed methods can play in explaining the social determinants and developmental origins of health and disease.

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

NASA Astrophysics Data System (ADS)

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-12-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34-80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics.

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

PubMed Central

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-01-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34–80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics. PMID:28000704

Investigation to realize a computationally efficient implementation of the high-order instantaneous-moments-based fringe analysis method

NASA Astrophysics Data System (ADS)

Gorthi, Sai Siva; Rajshekhar, Gannavarpu; Rastogi, Pramod

2010-06-01

Recently, a high-order instantaneous moments (HIM)-operator-based method was proposed for accurate phase estimation in digital holographic interferometry. The method relies on piece-wise polynomial approximation of phase and subsequent evaluation of the polynomial coefficients from the HIM operator using single-tone frequency estimation. The work presents a comparative analysis of the performance of different single-tone frequency estimation techniques, like Fourier transform followed by optimization, estimation of signal parameters by rotational invariance technique (ESPRIT), multiple signal classification (MUSIC), and iterative frequency estimation by interpolation on Fourier coefficients (IFEIF) in HIM-operator-based methods for phase estimation. Simulation and experimental results demonstrate the potential of the IFEIF technique with respect to computational efficiency and estimation accuracy.

Measurement of Stress Distribution Around a Circular Hole in a Plate Under Bending Moment Using Phase-shifting Method with Reflective Polariscope Arrangement

NASA Astrophysics Data System (ADS)

Baek, Tae Hyun

Photoelasticity is one of the most widely used whole-field optical methods for stress analysis. The technique of birefringent coatings, also called the method of photoelastic coatings, extends the classical procedures of model photoelasticity to the measurement of surface strains in opaque models made of any structural material. Photoelastic phase-shifting method can be used for the determination of the phase values of isochromatics and isoclinics. In this paper, photoelastic phase-shifting technique and conventional Babinet-Soleil compensation method were utilized to analyze a specimen with a triangular hole and a circular hole under bending. Photoelastic phase-shifting technique is whole-field measurement. On the other hand, conventional compensation method is point measurement. Three groups of results were obtained by phase-shifting method with reflective polariscope arrangement, conventional compensation method and FEM simulation, respectively. The results from the first two methods agree with each other relatively well considering experiment error. The advantage of photoelastic phase-shifting method is that it is possible to measure the stress distribution accurately close to the edge of holes.

Investigation of Portevin-Le Chatelier band with temporal phase analysis of speckle interferometry

NASA Astrophysics Data System (ADS)

Jiang, Zhenyu; Zhang, Qingchuan; Wu, Xiaoping

2003-04-01

A new method combining temporal phase analysis with dynamic digital speckle pattern interferometry is proposed to study Portevin-Le Chatelier effect quantitatively. The principle bases on that the phase difference of interference speckle patterns is a time-dependent function related to the object deformation. The interference speckle patterns of specimen are recorded with high sampling rate while PLC effect occurs, and the 2D displacement map of PLC band and its width are obtained by analyzing the displacement of specimen with proposed method.

Classification of Phase Transitions by Microcanonical Inflection-Point Analysis

NASA Astrophysics Data System (ADS)

Qi, Kai; Bachmann, Michael

2018-05-01

By means of the principle of minimal sensitivity we generalize the microcanonical inflection-point analysis method by probing derivatives of the microcanonical entropy for signals of transitions in complex systems. A strategy of systematically identifying and locating independent and dependent phase transitions of any order is proposed. The power of the generalized method is demonstrated in applications to the ferromagnetic Ising model and a coarse-grained model for polymer adsorption onto a substrate. The results shed new light on the intrinsic phase structure of systems with cooperative behavior.

Thin-layer chromatography with stationary phase gradient as a method for separation of water-soluble vitamins.

PubMed

Cimpoiu, Claudia; Hosu, Anamaria; Puscas, Anitta

2012-02-03

The group of hydrophilic vitamins play an important role in human health, and their lack or excess produces specific diseases. Therefore, the analysis of these compounds is indispensable for monitoring their content in pharmaceuticals and food in order to prevent some human diseases. TLC was successfully applied in the analysis of hydrophilic vitamins, but the most difficult problem in the simultaneous analysis of all these compounds is to find an optimum stationary phase-mobile phase system due to different chemical characteristics of analytes. Unfortunately structural analogues are difficult to separate in one chromatographic run, and this is the case in hydrophilic vitamins investigations. TLC gives the possibility to perform two-dimensional separations by using stationary phase gradient achieving the highest resolution by combining two systems with different selectivity. The goal of this work was to develop a method of analysis enabling separation of hydrophilic vitamins using TLC with adsorbent gradient. The developed method was used for identifying the water-soluble vitamins in alcoholic extracts of Hippophae rhamnoides and of Ribes nigrum. Copyright © 2011 Elsevier B.V. All rights reserved.

Quality assessment of Herba Leonuri based on the analysis of multiple components using normal- and reversed-phase chromatographic methods.

PubMed

Dong, Shuya; He, Jiao; Hou, Huiping; Shuai, Yaping; Wang, Qi; Yang, Wenling; Sun, Zheng; Li, Qing; Bi, Kaishun; Liu, Ran

2017-12-01

A novel, improved, and comprehensive method for quality evaluation and discrimination of Herba Leonuri has been developed and validated based on normal- and reversed-phase chromatographic methods. To identify Herba Leonuri, normal- and reversed-phase high-performance thin-layer chromatography fingerprints were obtained by comparing the colors and R f values of the bands, and reversed-phase high-performance liquid chromatography fingerprints were obtained by using an Agilent Poroshell 120 SB-C18 within 28 min. By similarity analysis and hierarchical clustering analysis, we show that there are similar chromatographic patterns in Herba Leonuri samples, but significant differences in counterfeits and variants. To quantify the bio-active components of Herba Leonuri, reversed-phase high-performance liquid chromatography was performed to analyze syringate, leonurine, quercetin-3-O-robiniaglycoside, hyperoside, rutin, isoquercitrin, wogonin, and genkwanin simultaneously by single standard to determine multi-components method with rutin as internal standard. Meanwhile, normal-phase high-performance liquid chromatography was performed by using an Agilent ZORBAX HILIC Plus within 6 min to determine trigonelline and stachydrine using trigonelline as internal standard. Innovatively, among these compounds, bio-active components of quercetin-3-O-robiniaglycoside and trigonelline were first determined in Herba Leonuri. In general, the method integrating multi-chromatographic analyses offered an efficient way for the standardization and identification of Herba Leonuri. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quality by Design approach in the development of hydrophilic interaction liquid chromatographic method for the analysis of iohexol and its impurities.

PubMed

Jovanović, Marko; Rakić, Tijana; Tumpa, Anja; Jančić Stojanović, Biljana

2015-06-10

This study presents the development of hydrophilic interaction liquid chromatographic method for the analysis of iohexol, its endo-isomer and three impurities following Quality by Design (QbD) approach. The main objective of the method was to identify the conditions where adequate separation quality in minimal analysis duration could be achieved within a robust region that guarantees the stability of method performance. The relationship between critical process parameters (acetonitrile content in the mobile phase, pH of the water phase and ammonium acetate concentration in the water phase) and critical quality attributes is created applying design of experiments methodology. The defined mathematical models and Monte Carlo simulation are used to evaluate the risk of uncertainty in models prediction and incertitude in adjusting the process parameters and to identify the design space. The borders of the design space are experimentally verified and confirmed that the quality of the method is preserved in this region. Moreover, Plackett-Burman design is applied for experimental robustness testing and method is fully validated to verify the adequacy of selected optimal conditions: the analytical column ZIC HILIC (100 mm × 4.6 mm, 5 μm particle size); mobile phase consisted of acetonitrile-water phase (72 mM ammonium acetate, pH adjusted to 6.5 with glacial acetic acid) (86.7:13.3) v/v; column temperature 25 °C, mobile phase flow rate 1 mL min(-1), wavelength of detection 254 nm. Copyright © 2015 Elsevier B.V. All rights reserved.

Separation of aromatic carboxylic acids using quaternary ammonium salts on reversed-phase HPLC. 2. Application for the analysis of Loy Yang coal oxidation products

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kawamura, K.; Okuwaki, A.; Verheyen, T.V.

In order to develop separation processes and analytical methods for aromatic carboxylic acids for the coal oxidation products, the separation behavior of aromatic carboxylic acids on a reversed-phase HPLC using eluent containing quaternary ammonium salt was optimized using the solvent gradient method. This method was applied for the analysis of Loy Yang coal oxidation products. It was confirmed that the analytical data using this method were consistent with those determined using gas chromatography.

SPACE PROPULSION SYSTEM PHASED-MISSION PROBABILITY ANALYSIS USING CONVENTIONAL PRA METHODS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Curtis Smith; James Knudsen

As part of a series of papers on the topic of advance probabilistic methods, a benchmark phased-mission problem has been suggested. This problem consists of modeling a space mission using an ion propulsion system, where the mission consists of seven mission phases. The mission requires that the propulsion operate for several phases, where the configuration changes as a function of phase. The ion propulsion system itself consists of five thruster assemblies and a single propellant supply, where each thruster assembly has one propulsion power unit and two ion engines. In this paper, we evaluate the probability of mission failure usingmore » the conventional methodology of event tree/fault tree analysis. The event tree and fault trees are developed and analyzed using Systems Analysis Programs for Hands-on Integrated Reliability Evaluations (SAPHIRE). While the benchmark problem is nominally a "dynamic" problem, in our analysis the mission phases are modeled in a single event tree to show the progression from one phase to the next. The propulsion system is modeled in fault trees to account for the operation; or in this case, the failure of the system. Specifically, the propulsion system is decomposed into each of the five thruster assemblies and fed into the appropriate N-out-of-M gate to evaluate mission failure. A separate fault tree for the propulsion system is developed to account for the different success criteria of each mission phase. Common-cause failure modeling is treated using traditional (i.e., parametrically) methods. As part of this paper, we discuss the overall results in addition to the positive and negative aspects of modeling dynamic situations with non-dynamic modeling techniques. One insight from the use of this conventional method for analyzing the benchmark problem is that it requires significant manual manipulation to the fault trees and how they are linked into the event tree. The conventional method also requires editing the resultant cut sets to obtain the correct results. While conventional methods may be used to evaluate a dynamic system like that in the benchmark, the level of effort required may preclude its use on real-world problems.« less

Apparatus and method for optimal phase balancing using dynamic programming with spatial consideration

DOEpatents

Robertazzi, Thomas G.; Skiena, Steven; Wang, Kai

2017-08-08

Provided are an apparatus and method for load-balancing of a three-phase electric power distribution system having a multi-phase feeder, including obtaining topology information of the feeder identifying supply points for customer loads and feeder sections between the supply points, obtaining customer information that includes peak customer load at each of the points between each of the feeder sections, performing a phase balancing analysis, and recommending phase assignment at the customer load supply points.

Spectrum of the Laplace-Beltrami operator and the phase structure of causal dynamical triangulations

NASA Astrophysics Data System (ADS)

Clemente, Giuseppe; D'Elia, Massimo

2018-06-01

We propose a new method to characterize the different phases observed in the nonperturbative numerical approach to quantum gravity known as causal dynamical triangulations. The method is based on the analysis of the eigenvalues and the eigenvectors of the Laplace-Beltrami operator computed on the triangulations: it generalizes previous works based on the analysis of diffusive processes and proves capable of providing more detailed information on the geometric properties of the triangulations. In particular, we apply the method to the analysis of spatial slices, showing that the different phases can be characterized by a new order parameter related to the presence or absence of a gap in the spectrum of the Laplace-Beltrami operator, and deriving an effective dimensionality of the slices at the different scales. We also propose quantities derived from the spectrum that could be used to monitor the running to the continuum limit around a suitable critical point in the phase diagram, if any is found.

Analytical methodologies for broad metabolite coverage of exhaled breath condensate.

PubMed

Aksenov, Alexander A; Zamuruyev, Konstantin O; Pasamontes, Alberto; Brown, Joshua F; Schivo, Michael; Foutouhi, Soraya; Weimer, Bart C; Kenyon, Nicholas J; Davis, Cristina E

2017-09-01

Breath analysis has been gaining popularity as a non-invasive technique that is amenable to a broad range of medical uses. One of the persistent problems hampering the wide application of the breath analysis method is measurement variability of metabolite abundances stemming from differences in both sampling and analysis methodologies used in various studies. Mass spectrometry has been a method of choice for comprehensive metabolomic analysis. For the first time in the present study, we juxtapose the most commonly employed mass spectrometry-based analysis methodologies and directly compare the resultant coverages of detected compounds in exhaled breath condensate in order to guide methodology choices for exhaled breath condensate analysis studies. Four methods were explored to broaden the range of measured compounds across both the volatile and non-volatile domain. Liquid phase sampling with polyacrylate Solid-Phase MicroExtraction fiber, liquid phase extraction with a polydimethylsiloxane patch, and headspace sampling using Carboxen/Polydimethylsiloxane Solid-Phase MicroExtraction (SPME) followed by gas chromatography mass spectrometry were tested for the analysis of volatile fraction. Hydrophilic interaction liquid chromatography and reversed-phase chromatography high performance liquid chromatography mass spectrometry were used for analysis of non-volatile fraction. We found that liquid phase breath condensate extraction was notably superior compared to headspace extraction and differences in employed sorbents manifested altered metabolite coverages. The most pronounced effect was substantially enhanced metabolite capture for larger, higher-boiling compounds using polyacrylate SPME liquid phase sampling. The analysis of the non-volatile fraction of breath condensate by hydrophilic and reverse phase high performance liquid chromatography mass spectrometry indicated orthogonal metabolite coverage by these chromatography modes. We found that the metabolite coverage could be enhanced significantly with the use of organic solvent as a device rinse after breath sampling to collect the non-aqueous fraction as opposed to neat breath condensate sample. Here, we show the detected ranges of compounds in each case and provide a practical guide for methodology selection for optimal detection of specific compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantitative comparison of tympanic membrane displacements using two optical methods to recover the optical phase

NASA Astrophysics Data System (ADS)

Santiago-Lona, Cynthia V.; Hernández-Montes, María del Socorro; Mendoza-Santoyo, Fernando; Esquivel-Tejeda, Jesús

2018-02-01

The study and quantification of the tympanic membrane (TM) displacements add important information to advance the knowledge about the hearing process. A comparative statistical analysis between two commonly used demodulation methods employed to recover the optical phase in digital holographic interferometry, namely the fast Fourier transform and phase-shifting interferometry, is presented as applied to study thin tissues such as the TM. The resulting experimental TM surface displacement data are used to contrast both methods through the analysis of variance and F tests. Data are gathered when the TMs are excited with continuous sound stimuli at levels 86, 89 and 93 dB SPL for the frequencies of 800, 1300 and 2500 Hz under the same experimental conditions. The statistical analysis shows repeatability in z-direction displacements with a standard deviation of 0.086, 0.098 and 0.080 μm using the Fourier method, and 0.080, 0.104 and 0.055 μm with the phase-shifting method at a 95% confidence level for all frequencies. The precision and accuracy are evaluated by means of the coefficient of variation; the results with the Fourier method are 0.06143, 0.06125, 0.06154 and 0.06154, 0.06118, 0.06111 with phase-shifting. The relative error between both methods is 7.143, 6.250 and 30.769%. On comparing the measured displacements, the results indicate that there is no statistically significant difference between both methods for frequencies at 800 and 1300 Hz; however, errors and other statistics increase at 2500 Hz.

Topological analysis of nuclear pasta phases

NASA Astrophysics Data System (ADS)

Kycia, Radosław A.; Kubis, Sebastian; Wójcik, Włodzimierz

2017-08-01

In this article the analysis of the result of numerical simulations of pasta phases using algebraic topology methods is presented. These considerations suggest that some phases can be further split into subphases and therefore should be more refined in numerical simulations. The results presented in this article can also be used to relate the Euler characteristic from numerical simulations to the geometry of the phases. The Betti numbers are used as they provide finer characterization of the phases. It is also shown that different boundary conditions give different outcomes.

Detecting phase separation of freeze-dried binary amorphous systems using pair-wise distribution function and multivariate data analysis.

PubMed

Chieng, Norman; Trnka, Hjalte; Boetker, Johan; Pikal, Michael; Rantanen, Jukka; Grohganz, Holger

2013-09-15

The purpose of this study is to investigate the use of multivariate data analysis for powder X-ray diffraction-pair-wise distribution function (PXRD-PDF) data to detect phase separation in freeze-dried binary amorphous systems. Polymer-polymer and polymer-sugar binary systems at various ratios were freeze-dried. All samples were analyzed by PXRD, transformed to PDF and analyzed by principal component analysis (PCA). These results were validated by differential scanning calorimetry (DSC) through characterization of glass transition of the maximally freeze-concentrate solute (Tg'). Analysis of PXRD-PDF data using PCA provides a more clear 'miscible' or 'phase separated' interpretation through the distribution pattern of samples on a score plot presentation compared to residual plot method. In a phase separated system, samples were found to be evenly distributed around the theoretical PDF profile. For systems that were miscible, a clear deviation of samples away from the theoretical PDF profile was observed. Moreover, PCA analysis allows simultaneous analysis of replicate samples. Comparatively, the phase behavior analysis from PXRD-PDF-PCA method was in agreement with the DSC results. Overall, the combined PXRD-PDF-PCA approach improves the clarity of the PXRD-PDF results and can be used as an alternative explorative data analytical tool in detecting phase separation in freeze-dried binary amorphous systems. Copyright © 2013 Elsevier B.V. All rights reserved.

Tomographic phase analysis to detect the site of accessory conduction pathway in Wolff-Parkinson-White syndrome

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nakajima, K.; Bunko, H.; Tada, A.

1984-01-01

Phase analysis has been applied to Wolff-Parkinson-White syndrome (WPW) to detect the site of accessory conduction pathway (ACP); however, there was a limitation to estimate the precise location of ACP by planar phase analysis. In this study, the authors applied phase analysis to gated blood pool tomography. Twelve patients with WPW who underwent epicardial mapping and surgical division of ACP were studied by both of gated emission computed tomography (GECT) and routine gated blood pool study (GBPS). The GBPS was performed with Tc-99m red blood cells in multiple projections; modified left anterior oblique, right anterior oblique and/or left lateral views.more » In GECT, short axial, horizontal and vertical long axial blood pool images were reconstructed. Phase analysis was performed using fundamental frequency of the Fourier transform in both GECT and GBPS images, and abnormal initial contractions on both the planar and tomographic phase analysis were compared with the location of surgically confirmed ACPs. In planar phase analysis, abnormal initial phase was identified in 7 out of 12 (58%) patients, while in tomographic phase analysis, the localization of ACP was predicted in 11 out of 12 (92%) patients. Tomographic phase analysis is superior to planar phase images in 8 out of 12 patients to estimate the location of ACP. Phase analysis by GECT can avoid overlap of blood pool in cardiac chambers and has advantage to identify the propagation of phase three-dimensionally. Tomographic phase analysis is a good adjunctive method for patients with WPW to estimate the site of ACP.« less

Discussion and a new method of optical cryptosystem based on interference

NASA Astrophysics Data System (ADS)

Lu, Dajiang; He, Wenqi; Liao, Meihua; Peng, Xiang

2017-02-01

A discussion and an objective security analysis of the well-known optical image encryption based on interference are presented in this paper. A new method is also proposed to eliminate the security risk of the original cryptosystem. For a possible practical application, we expand this new method into a hierarchical authentication scheme. In this authentication system, with a pre-generated and fixed random phase lock, different target images indicating different authentication levels are analytically encoded into corresponding phase-only masks (phase keys) and amplitude-only masks (amplitude keys). For the authentication process, a legal user can obtain a specified target image at the output plane if his/her phase key, and amplitude key, which should be settled close against the fixed internal phase lock, are respectively illuminated by two coherent beams. By comparing the target image with all the standard certification images in the database, the system can thus verify the user's legality even his/her identity level. Moreover, in despite of the internal phase lock of this system being fixed, the crosstalk between different pairs of keys held by different users is low. Theoretical analysis and numerical simulation are both provided to demonstrate the validity of this method.

Rapid Quantitative Analysis of Naringenin in the Fruit Bodies of Inonotus vaninii by Two-phase Acid Hydrolysis Followed by Reversed Phase-high Performance Liquid Chromatography-ultra Violet.

PubMed

Guohua, Xia; Pan, Ruirong; Bao, Rui; Ge, Yanru; Zhou, Cunshan; Shen, Yuping

2017-01-01

Sanghuang is one of mystical traditional Chinese medicines recorded earliest 2000 years ago, that included various fungi of Inonotus genus and was well-known for antitumor effect in modern medicine. Inonotus vaninii is grown in natural forest of Northeastern China merely and used as Sanghuang commercially, but it has no quality control specification until now. This study was to establish a rapid method of two-phase acid hydrolysis followed by reversed phase-high performance liquid chromatography-ultra violet (RP-HPLC-UV) to quantify naringenin in the fruit body of I. vaninii . Sample solution was prepared by pretreatment of raw material in two-phase acid hydrolysis and the hydrolysis technology was optimized. After reconstitution, analysis was performed using RP-HPLC-UV. The method validation was investigated and the naringenin content of sample and comparison were determined. The naringenin was obtained by two-phase acid hydrolysis method, namely, 10.0 g of raw material was hydrolyzed in 200 mL of 1% sulfuric acid aqueous solution (v/v) and 400 mL of chloroform in oil bath at 110°C for 2 h. Good linearity ( r = 0.9992) was achieved between concentration of analyte and peak area. The relative standard deviation (RSD) of precision was 2.47% and the RSD of naringenin contents for repeatability was 3.13%. The accuracy was supported with recoveries at 96.37%, 97.30%, and 99.31%. The sample solution prepared using the proposed method contained higher content of naringenin than conventional method and was stable for 8 h. Due to the high efficiency of sample preparation and high reliability of the HPLC method, it is feasible to use this method for routine analysis of naringenin in the fungus. A convenient two-phase acid hydrolysis was employed to produce naringenin from raw material, and then an efficient and reliable reversed phase-high performance liquid chromatography-ultra violet method was established to monitor naringenin in the fruit bodies of Inonotus vaninii . The newly established method could be used to control the quality of the herb. Abbreviations used: RP-HPLC-UV: Reversed Phase-High Performance Liquid Chromatography-Ultra Violet, RSD: Relative Standard Deviation, EtOAc: Ethyl acetate, ACN: Acetonitrile, MeOH: Methanol, RH: Relative Humility.

Simultaneous estimation of multiple phases in digital holographic interferometry using state space analysis

NASA Astrophysics Data System (ADS)

Kulkarni, Rishikesh; Rastogi, Pramod

2018-05-01

A new approach is proposed for the multiple phase estimation from a multicomponent exponential phase signal recorded in multi-beam digital holographic interferometry. It is capable of providing multidimensional measurements in a simultaneous manner from a single recording of the exponential phase signal encoding multiple phases. Each phase within a small window around each pixel is appproximated with a first order polynomial function of spatial coordinates. The problem of accurate estimation of polynomial coefficients, and in turn the unwrapped phases, is formulated as a state space analysis wherein the coefficients and signal amplitudes are set as the elements of a state vector. The state estimation is performed using the extended Kalman filter. An amplitude discrimination criterion is utilized in order to unambiguously estimate the coefficients associated with the individual signal components. The performance of proposed method is stable over a wide range of the ratio of signal amplitudes. The pixelwise phase estimation approach of the proposed method allows it to handle the fringe patterns that may contain invalid regions.

Integrative health care - Toward a common understanding: A mixed method study.

PubMed

Leach, Matthew J; Wiese, Marlene; Thakkar, Manisha; Agnew, Tamara

2018-02-01

To generate a multidisciplinary stakeholder-informed definition of integrative health care (IHC). A mixed-method study design was used, employing the use of focus groups/semi-structured interviews (phase-1) and document analysis (phases 2 and 3). Phase-1 recruited a purposive sample of Australian health consumers/health providers. Phase-2 interrogated websites of international IHC organisations for definitions of IHC. Phase-3 systematically searched bibliographic databases for articles defining IHC. Data were analysed using thematic analysis. Data were drawn from 54 health consumers/providers (phase-1), 23 IHC organisation webpages (phase-2) and 23 eligible articles (phase-3). Seven themes emerged from the data. Consensus was reached on a single, 65-word definition of IHC. An unambiguous definition of IHC is critical to establishing a clearer identity for IHC, as well as providing greater clarity for consumers, health providers and policy makers. In recognising the need for a clearer description, we propose a scientifically-grounded, multi-disciplinary stakeholder-informed definition of IHC. Copyright © 2017 Elsevier Ltd. All rights reserved.

New approaches to the analysis of complex samples using fluorescence lifetime techniques and organized media

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hertz, P.R.

Fluorescence spectroscopy is a highly sensitive and selective tool for the analysis of complex systems. In order to investigate the efficacy of several steady state and dynamic techniques for the analysis of complex systems, this work focuses on two types of complex, multicomponent samples: petrolatums and coal liquids. It is shown in these studies dynamic, fluorescence lifetime-based measurements provide enhanced discrimination between complex petrolatum samples. Additionally, improved quantitative analysis of multicomponent systems is demonstrated via incorporation of organized media in coal liquid samples. This research provides the first systematic studies of (1) multifrequency phase-resolved fluorescence spectroscopy for dynamic fluorescence spectralmore » fingerprinting of complex samples, and (2) the incorporation of bile salt micellar media to improve accuracy and sensitivity for characterization of complex systems. In the petroleum studies, phase-resolved fluorescence spectroscopy is used to combine spectral and lifetime information through the measurement of phase-resolved fluorescence intensity. The intensity is collected as a function of excitation and emission wavelengths, angular modulation frequency, and detector phase angle. This multidimensional information enhances the ability to distinguish between complex samples with similar spectral characteristics. Examination of the eigenvalues and eigenvectors from factor analysis of phase-resolved and steady state excitation-emission matrices, using chemometric methods of data analysis, confirms that phase-resolved fluorescence techniques offer improved discrimination between complex samples as compared with conventional steady state methods.« less

Accurate, efficient, and (iso)geometrically flexible collocation methods for phase-field models

NASA Astrophysics Data System (ADS)

Gomez, Hector; Reali, Alessandro; Sangalli, Giancarlo

2014-04-01

We propose new collocation methods for phase-field models. Our algorithms are based on isogeometric analysis, a new technology that makes use of functions from computational geometry, such as, for example, Non-Uniform Rational B-Splines (NURBS). NURBS exhibit excellent approximability and controllable global smoothness, and can represent exactly most geometries encapsulated in Computer Aided Design (CAD) models. These attributes permitted us to derive accurate, efficient, and geometrically flexible collocation methods for phase-field models. The performance of our method is demonstrated by several numerical examples of phase separation modeled by the Cahn-Hilliard equation. We feel that our method successfully combines the geometrical flexibility of finite elements with the accuracy and simplicity of pseudo-spectral collocation methods, and is a viable alternative to classical collocation methods.

Multi-Scale Morphological Analysis of Conductance Signals in Vertical Upward Gas-Liquid Two-Phase Flow

NASA Astrophysics Data System (ADS)

Lian, Enyang; Ren, Yingyu; Han, Yunfeng; Liu, Weixin; Jin, Ningde; Zhao, Junying

2016-11-01

The multi-scale analysis is an important method for detecting nonlinear systems. In this study, we carry out experiments and measure the fluctuation signals from a rotating electric field conductance sensor with eight electrodes. We first use a recurrence plot to recognise flow patterns in vertical upward gas-liquid two-phase pipe flow from measured signals. Then we apply a multi-scale morphological analysis based on the first-order difference scatter plot to investigate the signals captured from the vertical upward gas-liquid two-phase flow loop test. We find that the invariant scaling exponent extracted from the multi-scale first-order difference scatter plot with the bisector of the second-fourth quadrant as the reference line is sensitive to the inhomogeneous distribution characteristics of the flow structure, and the variation trend of the exponent is helpful to understand the process of breakup and coalescence of the gas phase. In addition, we explore the dynamic mechanism influencing the inhomogeneous distribution of the gas phase in terms of adaptive optimal kernel time-frequency representation. The research indicates that the system energy is a factor influencing the distribution of the gas phase and the multi-scale morphological analysis based on the first-order difference scatter plot is an effective method for indicating the inhomogeneous distribution of the gas phase in gas-liquid two-phase flow.

Quasi-closed phase forward-backward linear prediction analysis of speech for accurate formant detection and estimation.

PubMed

Gowda, Dhananjaya; Airaksinen, Manu; Alku, Paavo

2017-09-01

Recently, a quasi-closed phase (QCP) analysis of speech signals for accurate glottal inverse filtering was proposed. However, the QCP analysis which belongs to the family of temporally weighted linear prediction (WLP) methods uses the conventional forward type of sample prediction. This may not be the best choice especially in computing WLP models with a hard-limiting weighting function. A sample selective minimization of the prediction error in WLP reduces the effective number of samples available within a given window frame. To counter this problem, a modified quasi-closed phase forward-backward (QCP-FB) analysis is proposed, wherein each sample is predicted based on its past as well as future samples thereby utilizing the available number of samples more effectively. Formant detection and estimation experiments on synthetic vowels generated using a physical modeling approach as well as natural speech utterances show that the proposed QCP-FB method yields statistically significant improvements over the conventional linear prediction and QCP methods.

Sexual Satisfaction Concept Analysis in Iranian Married Women: A Hybrid Model Study

PubMed Central

Yekta, Zohre Parsa; Raisi, Firoozeh; Ebadi, Abbas; Shahvari, Zahra

2015-01-01

Background: Sexual satisfaction is considered to be a sexual right and an important component of sexual health. The purpose of this qualitative study was to clarify the meaning and the nature of sexual satisfaction in Iranian married women, and to provide a cultural-based definition of it. Method: Sexual satisfaction was examined in three phases by the Hybrid Model of concept analysis: (1) the theoretical phase; (2) the fieldwork phase and (3) the analytical phase. Hybrid concept analysis method was chosen because its inclusion of married women’s perspectives enriches the limits of sexual health search literature. Result: The critical attributes of sexual satisfaction were investigated. They included ‘two-dimensional structure’, ‘an affective response’, ‘a means to achieve marital satisfaction’, ‘unique’, ‘a concept based on expectations’ and ‘a concept on shadow of values’. Conclusion: The concept analysis of sexual satisfaction showed some of the attributes and antecedents for this concept that, have not been mentioned in the literature. PMID:26153166

Method of analysis of polymerizable monomeric species in a complex mixture

DOEpatents

Hermes, Robert E

2014-03-18

Method of selective quantitation of a polymerizable monomeric species in a well spacer fluid, said method comprising the steps of adding at least one solvent having a refractive index of less than about 1.33 to a sample of the complex mixture to produce a solvent phase, and measuring the refractive index of the solvent phase.

Development and Multi-laboratory Verification of U.S. EPA Method 540 for the Analysis of Drinking Water Contaminants by Solid Phase Extraction-LC/MS/MS

EPA Science Inventory

A drinking water method for 12 chemicals, predominately pesticides, is presented that addresses the occurrence monitoring needs of the U.S. Environmental Protection Agency (EPA) for a future Unregulated Contaminant Monitoring Regulation (UCMR). The method employs solid phase ext...

A METHOD FOR AUTOMATED ANALYSIS OF 10 ML WATER SAMPLES CONTAINING ACIDIC, BASIC, AND NEUTRAL SEMIVOLATILE COMPOUNDS LISTED IN USEPA METHOD 8270 BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GAS CHROMATOGRAPHY/MASS SPECTROMETRY

EPA Science Inventory

Data is presented showing the progress made towards the development of a new automated system combining solid phase extraction (SPE) with gas chromatography/mass spectrometry for the single run analysis of water samples containing a broad range of acid, base and neutral compounds...

Phase unwrapping method for three-dimensional stress analysis by scattered-light photoelasticity with unpolarized light. 2. Experiment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kihara, Toshiki

2007-09-01

A phase unwrapping method that employs scattered-light photoelasticity with unpolarized light was proposed for automated three-dimensional stress analysis [Appl. Opt. 45, 8848 (2006)]. I now demonstrate the validity of this method by performing nondestructive measurements at three different wavelengths of the secondary principal stress direction {psi}j and the total relative phase retardation {rho}jtot in the plane that contains the rotated principal stress directions in a spherical frozen stress model and compare the results obtained with mechanically sliced models. The parameters {psi}j and {rho}jtot were measured nondestructively over the entire field of view for the first time, to the best ofmore » my knowledge.« less

Phase and vortex correlations in superconducting Josephson-junction arrays at irrational magnetic frustration.

PubMed

Granato, Enzo

2008-07-11

Phase coherence and vortex order in a Josephson-junction array at irrational frustration are studied by extensive Monte Carlo simulations using the parallel-tempering method. A scaling analysis of the correlation length of phase variables in the full equilibrated system shows that the critical temperature vanishes with a power-law divergent correlation length and critical exponent nuph, in agreement with recent results from resistivity scaling analysis. A similar scaling analysis for vortex variables reveals a different critical exponent nuv, suggesting that there are two distinct correlation lengths associated with a decoupled zero-temperature phase transition.

DEVELOPMENT OF METHOD 535 FOR THE DETERMINATION OF CHLOROACETANILIDE AND OTHER ACETAMIDE HERBICIDE DEGRADATES IN DRINKING WATER BY SOLID PHASE EXTRACTION AND LIQUID CHROMATOGRAPHY/TANDEM MASS SPECTROMETRY

EPA Science Inventory

EPA Method 535 has been developed in order to provide a method for the analysis of "Alachlor ESA and other acetanilide degradation products" which are listed on U.S. EPA's 1998 Drinking Water Contaminant Candidate List. Method 535 uses solid phase extraction with a nonporous gr...

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jenkins, T.F.; Thorne, P.G.; Myers, K.F.

Salting-out solvent extraction (SOE) was compared with cartridge and membrane solid-phase extraction (SPE) for preconcentration of nitroaromatics, nitramines, and aminonitroaromatics prior to determination by reversed-phase high-performance liquid chromatography. The solid phases used were manufacturer-cleaned materials, Porapak RDX for the cartridge method and Empore SDB-RPS for the membrane method. Thirty-three groundwater samples from the Naval Surface Warfare Center, Crane, Indiana, were analyzed using the direct analysis protocol specified in SW846 Method 8330, and the results were compared with analyses conducted after preconcentration using SOE with acetonitrile, cartridge-based SPE, and membrane-based SPE. For high-concentration samples, analytical results from the three preconcentration techniquesmore » were compared with results from the direct analysis protocol; good recovery of all target analytes was achieved by all three pre-concentration methods. For low-concentration samples, results from the two SPE methods were correlated with results from the SOE method; very similar data was obtained by the SOE and SPE methods, even at concentrations well below 1 microgram/L.« less

High-performance liquid chromatography separation and intact mass analysis of detergent-solubilized integral membrane proteins

PubMed Central

Berridge, Georgina; Chalk, Rod; D’Avanzo, Nazzareno; Dong, Liang; Doyle, Declan; Kim, Jung-In; Xia, Xiaobing; Burgess-Brown, Nicola; deRiso, Antonio; Carpenter, Elisabeth Paula; Gileadi, Opher

2011-01-01

We have developed a method for intact mass analysis of detergent-solubilized and purified integral membrane proteins using liquid chromatography–mass spectrometry (LC–MS) with methanol as the organic mobile phase. Membrane proteins and detergents are separated chromatographically during the isocratic stage of the gradient profile from a 150-mm C3 reversed-phase column. The mass accuracy is comparable to standard methods employed for soluble proteins; the sensitivity is 10-fold lower, requiring 0.2–5 μg of protein. The method is also compatible with our standard LC–MS method used for intact mass analysis of soluble proteins and may therefore be applied on a multiuser instrument or in a high-throughput environment. PMID:21093405

Detection and analysis of a transient energy burst with beamforming of multiple teleseismic phases

NASA Astrophysics Data System (ADS)

Retailleau, Lise; Landès, Matthieu; Gualtieri, Lucia; Shapiro, Nikolai M.; Campillo, Michel; Roux, Philippe; Guilbert, Jocelyn

2018-01-01

Seismological detection methods are traditionally based on picking techniques. These methods cannot be used to analyse emergent signals where the arrivals cannot be picked. Here, we detect and locate seismic events by applying a beamforming method that combines multiple body-wave phases to USArray data. This method explores the consistency and characteristic behaviour of teleseismic body waves that are recorded by a large-scale, still dense, seismic network. We perform time-slowness analysis of the signals and correlate this with the time-slowness equivalent of the different body-wave phases predicted by a global traveltime calculator, to determine the occurrence of an event with no a priori information about it. We apply this method continuously to one year of data to analyse the different events that generate signals reaching the USArray network. In particular, we analyse in detail a low-frequency secondary microseismic event that occurred on 2010 February 1. This event, that lasted 1 d, has a narrow frequency band around 0.1 Hz, and it occurred at a distance of 150° to the USArray network, South of Australia. We show that the most energetic phase observed is the PKPab phase. Direct amplitude analysis of regional seismograms confirms the occurrence of this event. We compare the seismic observations with models of the spectral density of the pressure field generated by the interferences between oceanic waves. We attribute the observed signals to a storm-generated microseismic event that occurred along the South East Indian Ridge.

Quantum phase space with a basis of Wannier functions

NASA Astrophysics Data System (ADS)

Fang, Yuan; Wu, Fan; Wu, Biao

2018-02-01

A quantum phase space with Wannier basis is constructed: (i) classical phase space is divided into Planck cells; (ii) a complete set of Wannier functions are constructed with the combination of Kohn’s method and Löwdin method such that each Wannier function is localized at a Planck cell. With these Wannier functions one can map a wave function unitarily onto phase space. Various examples are used to illustrate our method and compare it to Wigner function. The advantage of our method is that it can smooth out the oscillations in wave functions without losing any information and is potentially a better tool in studying quantum-classical correspondence. In addition, we point out that our method can be used for time-frequency analysis of signals.

Solid-phase reductive amination for glycomic analysis.

PubMed

Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

2017-04-15

Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

ANALYSIS OF SELECTED PYRETHROID PESTICIDES USING REVERSE PHASE HIGH PRESSURE LIQUID CHROMATOGRAPHY/UV

EPA Science Inventory

This research was conducted in cooperation with EPA Region 4 in Athens, GA to develop a method to analyze selected pyrethroid pesticides using Reverse Phase-High Pressure Liquid Chromatography (HPLC). This HPLC method will aid researchers in separating and identifying these py...

SOLID PHASE MICROEXTRACTION FOR TRACE LEVEL ANALYSIS OF DISINFECTION BY-PRODUCTS

EPA Science Inventory

This presentation focuses on the development of a solid-phase microextraction (SPME)-gas chromatography (GC)/ion trap mass spectrometry (MS) method for the analysis of semivolatile disinfection by-products (DBPs) in drinking water in the low ug/L range. These DBPs were selected ...

Spectrophotometric and HPLC Methods for Simultaneous Estimation of Amlodipine Besilate, Losartan Potassium and Hydrochlorothiazide in Tablets

PubMed Central

Wankhede, S. B.; Raka, K. C.; Wadkar, S. B.; Chitlange, S. S.

2010-01-01

Two UV-spectrophotometric and one reverse phase high performance liquid chromatography methods have been developed for the simultaneous estimation of amlodipine besilate, losartan potassium and hydrochlorothiazide in tablet dosage form. The first UV spectrophotometric method was a determination using the simultaneous equation method at 236.5, 254 and 271 nm over the concentration range 5-25, 10-50 and 5-25 μg/ml for amlodipine besilate, losartan potassium and hydrochlorothiazide, respectively. The second UV method was a determination using the area under curve method at 231.5-241.5, 249-259 and 266-276 nm over the concentration range of 5-25, 5-25 and 10-50 μg/ml for amlodipine besilate, hydrochlorothiazide and losartan potassium, respectively. In reverse phase high performance liquid chromatography analysis is carried out using 0.025 M phosphate buffer (pH 3.7):acetonitrile (57:43 v/v) as the mobile phase and Kromasil C18 (4.6 mm i.d×250 mm) column as stationery phase with detection wavelength of 232 nm linearity was obtained in the concentration range of 2-14, 20-140 and 5-40 μg/ml for amlodipine besilate, losartan potassium and hydrochlorothiazide, respectively. Both UV-spectrophotometric and reverse phase high performance liquid chromatography methods were statistically validated and can be used for analysis of combined dose tablet formulation containing amlodipine besilate, losartan potassium and hydrochlorothiazide. PMID:20582208

A novel transmitter IQ imbalance and phase noise suppression method utilizing pilots in PDM CO-OFDM system

NASA Astrophysics Data System (ADS)

Zhang, Haoyuan; Ma, Xiurong; Li, Pengru

2018-04-01

In this paper, we develop a novel pilot structure to suppress transmitter in-phase and quadrature (Tx IQ) imbalance, phase noise and channel distortion for polarization division multiplexed (PDM) coherent optical orthogonal frequency division multiplexing (CO-OFDM) systems. Compared with the conventional approach, our method not only significantly improves the system tolerance of IQ imbalance as well as phase noise, but also provides higher transmission speed. Numerical simulations of PDM CO-OFDM system is used to validate the theoretical analysis under the simulation conditions: the amplitude mismatch 3 dB, the phase mismatch 15°, the transmission bit rate 100 Gb/s and 560 km standard signal-mode fiber transmission. Moreover, the proposed method is 63% less complex than the compared method.

Theoretical analysis of a method for extracting the phase of a phase-amplitude modulated signal generated by a direct-modulated optical injection-locked semiconductor laser

NASA Astrophysics Data System (ADS)

Lee, Hwan; Cho, Jun-Hyung; Sung, Hyuk-Kee

2017-05-01

The phase modulation (PM) and amplitude modulation (AM) of optical signals can be achieved using a direct-modulated (DM) optical injection-locked (OIL) semiconductor laser. We propose and theoretically analyze a simple method to extract the phase component of a PM signal produced by a DM-OIL semiconductor laser. The pure AM component of the combined PM-AM signal can be isolated by square-law detection in a photodetector and can then be used to compensate for the PM-AM signal based on an optical homodyne method. Using the AM compensation technique, we successfully developed a simple and cost-effective phase extraction method applicable to the PM-AM optical signal of a DM-OIL semiconductor laser.

Coformer screening using thermal analysis based on binary phase diagrams.

PubMed

Yamashita, Hiroyuki; Hirakura, Yutaka; Yuda, Masamichi; Terada, Katsuhide

2014-08-01

The advent of cocrystals has demonstrated a growing need for efficient and comprehensive coformer screening in search of better development forms, including salt forms. Here, we investigated a coformer screening system for salts and cocrystals based on binary phase diagrams using thermal analysis and examined the effectiveness of the method. Indomethacin and tenoxicam were used as models of active pharmaceutical ingredients (APIs). Physical mixtures of an API and 42 kinds of coformers were analyzed using Differential Scanning Calorimetry (DSC) and X-ray DSC. We also conducted coformer screening using a conventional slurry method and compared these results with those from the thermal analysis method and previous studies. Compared with the slurry method, the thermal analysis method was a high-performance screening system, particularly for APIs with low solubility and/or propensity to form solvates. However, this method faced hurdles for screening coformers combined with an API in the presence of kinetic hindrance for salt or cocrystal formation during heating or if there is degradation near the metastable eutectic temperature. The thermal analysis and slurry methods are considered complementary to each other for coformer screening. Feasibility of the thermal analysis method in drug discovery practice is ensured given its small scale and high throughput.

Fine tuning breath-hold-based cerebrovascular reactivity analysis models.

PubMed

van Niftrik, Christiaan Hendrik Bas; Piccirelli, Marco; Bozinov, Oliver; Pangalu, Athina; Valavanis, Antonios; Regli, Luca; Fierstra, Jorn

2016-02-01

We elaborate on existing analysis methods for breath-hold (BH)-derived cerebrovascular reactivity (CVR) measurements and describe novel insights and models toward more exact CVR interpretation. Five blood-oxygen-level-dependent (BOLD) fMRI datasets of neurovascular patients with unilateral hemispheric hemodynamic impairment were used to test various BH CVR analysis methods. Temporal lag (phase), percent BOLD signal change (CVR), and explained variance (coherence) maps were calculated using three different sine models and two novel "Optimal Signal" model-free methods based on the unaffected hemisphere and the sagittal sinus fMRI signal time series, respectively. All models showed significant differences in CVR and coherence between the affected-hemodynamic impaired-and unaffected hemisphere. Voxel-wise phase determination significantly increases CVR (0.60 ± 0.18 vs. 0.82 ± 0.27; P < 0.05). Incorporating different durations of breath hold and resting period in one sine model (two-task) did increase coherence in the unaffected hemisphere, as well as eliminating negative phase commonly obtained by one-task frequency models. The novel model-free "optimal signal" methods both explained the BOLD MR data similar to the two task sine model. Our CVR analysis demonstrates an improved CVR and coherence after implementation of voxel-wise phase and frequency adjustment. The novel "optimal signal" methods provide a robust and feasible alternative to the sine models, as both are model-free and independent of compliance. Here, the sagittal sinus model may be advantageous, as it is independent of hemispheric CVR impairment.

Application of Analytical Quality by Design concept for bilastine and its degradation impurities determination by hydrophilic interaction liquid chromatographic method.

PubMed

Terzić, Jelena; Popović, Igor; Stajić, Ana; Tumpa, Anja; Jančić-Stojanović, Biljana

2016-06-05

This paper deals with the development of hydrophilic interaction liquid chromatographic (HILIC) method for the analysis of bilastine and its degradation impurities following Analytical Quality by Design approach. It is the first time that the method for bilastine and its impurities is proposed. The main objective was to identify the conditions where an adequate separation in minimal analysis duration could be achieved within a robust region. Critical process parameters which have the most influence on method performance were defined as acetonitrile content in the mobile phase, pH of the aqueous phase and ammonium acetate concentration in the aqueous phase. Box-Behnken design was applied for establishing a relationship between critical process parameters and critical quality attributes. The defined mathematical models and Monte Carlo simulations were used to identify the design space. Fractional factorial design was applied for experimental robustness testing and the method is validated to verify the adequacy of selected optimal conditions: the analytical column Luna(®) HILIC (100mm×4.6mm, 5μm particle size); mobile phase consisted of acetonitrile-aqueous phase (50mM ammonium acetate, pH adjusted to 5.3 with glacial acetic acid) (90.5:9.5, v/v); column temperature 30°C, mobile phase flow rate 1mLmin(-1), wavelength of detection 275nm. Copyright © 2016 Elsevier B.V. All rights reserved.

Generalized Fourier analyses of the advection-diffusion equation - Part I: one-dimensional domains

NASA Astrophysics Data System (ADS)

Christon, Mark A.; Martinez, Mario J.; Voth, Thomas E.

2004-07-01

This paper presents a detailed multi-methods comparison of the spatial errors associated with finite difference, finite element and finite volume semi-discretizations of the scalar advection-diffusion equation. The errors are reported in terms of non-dimensional phase and group speed, discrete diffusivity, artificial diffusivity, and grid-induced anisotropy. It is demonstrated that Fourier analysis provides an automatic process for separating the discrete advective operator into its symmetric and skew-symmetric components and characterizing the spectral behaviour of each operator. For each of the numerical methods considered, asymptotic truncation error and resolution estimates are presented for the limiting cases of pure advection and pure diffusion. It is demonstrated that streamline upwind Petrov-Galerkin and its control-volume finite element analogue, the streamline upwind control-volume method, produce both an artificial diffusivity and a concomitant phase speed adjustment in addition to the usual semi-discrete artifacts observed in the phase speed, group speed and diffusivity. The Galerkin finite element method and its streamline upwind derivatives are shown to exhibit super-convergent behaviour in terms of phase and group speed when a consistent mass matrix is used in the formulation. In contrast, the CVFEM method and its streamline upwind derivatives yield strictly second-order behaviour. In Part II of this paper, we consider two-dimensional semi-discretizations of the advection-diffusion equation and also assess the affects of grid-induced anisotropy observed in the non-dimensional phase speed, and the discrete and artificial diffusivities. Although this work can only be considered a first step in a comprehensive multi-methods analysis and comparison, it serves to identify some of the relative strengths and weaknesses of multiple numerical methods in a common analysis framework. Published in 2004 by John Wiley & Sons, Ltd.

Cloud Service Provider Methods for Managing Insider Threats: Analysis Phase 1

DTIC Science & Technology

2013-11-01

of Standards and Technology (NIST) Special Publication 800-145 (NIST SP 800-145) defines three types of cloud services : Software as a Service ( SaaS ...among these three models. NIST SP 800-145 describes the three service models as follows: SaaS —The capability provided to the consumer is to use the...Cloud Service Provider Methods for Managing Insider Threats: Analysis Phase I Greg Porter November 2013 TECHNICAL NOTE CMU/SEI-2013-TN-020

Determination of total phthalate in cosmetics using a simple three-phase sample preparation method.

PubMed

Liu, Laping; Wang, Zhengmeng; Zhao, Sihan; Duan, Jiahui; Tao, Hu; Wang, Wenji; Liu, Shuhui

2018-02-01

A simple sample preparation method requiring minimal organic solvents is proposed for the determination of the total phthalate content in cosmetics by high-performance liquid chromatography-tandem mass spectrometry. The hydrolysis of phthalates and purification of interfering substances were performed in a three-phase system that included an upper n-hexane phase, a middle ethanol phase, and a lower aqueous alkali solution. This three-phase system utilized an incremental purification strategy. The apolar ingredients were extracted with n-hexane, the polar pigments accumulated in the ethanol phase, and the hydrolysis product, phthalic acid, remained in the hydrolysate. Under the optimized conditions, the correlation coefficients (r) for the calibration curves were 0.998-0.999 in the range 0.60-12 mol L -1 . The limit of detection was 5.1 μmol kg -1 , and the limit of quantification was 9.2 μmol kg -1 . The recoveries varied from 84 to 97% with RSDs equal to or lower than 11%. The intra-day and inter-day repeatability values, expressed as the relative standard deviation, were less than 8.7 and 9.8, respectively. No obvious matrix effect existed in the different cosmetics matrices. The validated method was applied for the analysis of 57 commercial cosmetic samples. Graphical abstract Analysis of phthalates in cosmetics using a three-phase preparation method.

Phase II cancer clinical trials for biomarker-guided treatments.

PubMed

Jung, Sin-Ho

2018-01-01

The design and analysis of cancer clinical trials with biomarker depend on various factors, such as the phase of trials, the type of biomarker, whether the used biomarker is validated or not, and the study objectives. In this article, we demonstrate the design and analysis of two Phase II cancer clinical trials, one with a predictive biomarker and the other with an imaging prognostic biomarker. Statistical testing methods and their sample size calculation methods are presented for each trial. We assume that the primary endpoint of these trials is a time to event variable, but this concept can be used for any type of endpoint.

(PRESENT AT NCCU) ANALYSIS OF SELECTED PYRETHROID PESTICIDES USING REVERSE PHASE HIGH LIQUID CHROMATOGRAPHY

EPA Science Inventory

This research was conducted in cooperation with EPA Region 4 in Athens, GA to develop a method to analyze selected pyrethroid pesticides using Reverse Phase-High Pressure Liquid Chromatography (HPLC). This HPLC method will aid researchers in separating and identifying these pyre...

Development of a Solid Phase Extraction Method for Agricultural Pesticides in Large-Volume Water Samples

EPA Science Inventory

An analytical method using solid phase extraction (SPE) and analysis by gas chromatography/mass spectrometry (GC/MS) was developed for the trace determination of a variety of agricultural pesticides and selected transformation products in large-volume high-elevation lake water sa...

Headspace analysis of polar organic compounds in biological matrixes using solid phase microextraction (SPME)

USDA-ARS?s Scientific Manuscript database

Analysis of biological fluids and waste material is difficult and tedious given the sample matrix. A rapid automated method for the determination of volatile fatty acids and phenolic and indole compounds was developed using a multipurpose sampler (MPS) with solid phase microextraction (SPME) and GC-...

Analysis of ecologically relevant pharmaceuticals in wastewater and surface water using selective solid phase extraction and UPLC/MS/MS

EPA Science Inventory

A rapid and sensitive method has been developed for the analysis of 48 human prescription active pharmaceutical ingredients (APIs) and 6 metabolites of interest, utilizing selective solid-phase extraction (SPE) and ultra performance liquid chromatography in combination with tripl...

Novel Methods for Analysing Bacterial Tracks Reveal Persistence in Rhodobacter sphaeroides

PubMed Central

Rosser, Gabriel; Fletcher, Alexander G.; Wilkinson, David A.; de Beyer, Jennifer A.; Yates, Christian A.; Armitage, Judith P.; Maini, Philip K.; Baker, Ruth E.

2013-01-01

Tracking bacteria using video microscopy is a powerful experimental approach to probe their motile behaviour. The trajectories obtained contain much information relating to the complex patterns of bacterial motility. However, methods for the quantitative analysis of such data are limited. Most swimming bacteria move in approximately straight lines, interspersed with random reorientation phases. It is therefore necessary to segment observed tracks into swimming and reorientation phases to extract useful statistics. We present novel robust analysis tools to discern these two phases in tracks. Our methods comprise a simple and effective protocol for removing spurious tracks from tracking datasets, followed by analysis based on a two-state hidden Markov model, taking advantage of the availability of mutant strains that exhibit swimming-only or reorientating-only motion to generate an empirical prior distribution. Using simulated tracks with varying levels of added noise, we validate our methods and compare them with an existing heuristic method. To our knowledge this is the first example of a systematic assessment of analysis methods in this field. The new methods are substantially more robust to noise and introduce less systematic bias than the heuristic method. We apply our methods to tracks obtained from the bacterial species Rhodobacter sphaeroides and Escherichia coli. Our results demonstrate that R. sphaeroides exhibits persistence over the course of a tumbling event, which is a novel result with important implications in the study of this and similar species. PMID:24204227

Automated nystagmus analysis. [on-line computer technique for eye data processing

NASA Technical Reports Server (NTRS)

Oman, C. M.; Allum, J. H. J.; Tole, J. R.; Young, L. R.

1973-01-01

Several methods have recently been used for on-line analysis of nystagmus: A digital computer program has been developed to accept sampled records of eye position, detect fast phase components, and output cumulative slow phase position, continuous slow phase velocity, instantaneous fast phase frequency, and other parameters. The slow phase velocity is obtained by differentiation of the calculated cumulative position rather than the original eye movement record. Also, a prototype analog device has been devised which calculates the velocity of the slow phase component during caloric testing. Examples of clinical and research eye movement records analyzed with these devices are shown.

Optimization of the solvent-based dissolution method to sample volatile organic compound vapors for compound-specific isotope analysis.

PubMed

Bouchard, Daniel; Wanner, Philipp; Luo, Hong; McLoughlin, Patrick W; Henderson, James K; Pirkle, Robert J; Hunkeler, Daniel

2017-10-20

The methodology of the solvent-based dissolution method used to sample gas phase volatile organic compounds (VOC) for compound-specific isotope analysis (CSIA) was optimized to lower the method detection limits for TCE and benzene. The sampling methodology previously evaluated by [1] consists in pulling the air through a solvent to dissolve and accumulate the gaseous VOC. After the sampling process, the solvent can then be treated similarly as groundwater samples to perform routine CSIA by diluting an aliquot of the solvent into water to reach the required concentration of the targeted contaminant. Among solvents tested, tetraethylene glycol dimethyl ether (TGDE) showed the best aptitude for the method. TGDE has a great affinity with TCE and benzene, hence efficiently dissolving the compounds during their transition through the solvent. The method detection limit for TCE (5±1μg/m 3 ) and benzene (1.7±0.5μg/m 3 ) is lower when using TGDE compared to methanol, which was previously used (385μg/m 3 for TCE and 130μg/m 3 for benzene) [2]. The method detection limit refers to the minimal gas phase concentration in ambient air required to load sufficient VOC mass into TGDE to perform δ 13 C analysis. Due to a different analytical procedure, the method detection limit associated with δ 37 Cl analysis was found to be 156±6μg/m 3 for TCE. Furthermore, the experimental results validated the relationship between the gas phase TCE and the progressive accumulation of dissolved TCE in the solvent during the sampling process. Accordingly, based on the air-solvent partitioning coefficient, the sampling methodology (e.g. sampling rate, sampling duration, amount of solvent) and the final TCE concentration in the solvent, the concentration of TCE in the gas phase prevailing during the sampling event can be determined. Moreover, the possibility to analyse for TCE concentration in the solvent after sampling (or other targeted VOCs) allows the field deployment of the sampling method without the need to determine the initial gas phase TCE concentration. The simplified field deployment approach of the solvent-based dissolution method combined with the conventional analytical procedure used for groundwater samples substantially facilitates the application of CSIA to gas phase studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Algorithms for image recovery calculation in extended single-shot phase-shifting digital holography

NASA Astrophysics Data System (ADS)

Hasegawa, Shin-ya; Hirata, Ryo

2018-04-01

The single-shot phase-shifting method of image recovery using an inclined reference wave has the advantages of reducing the effects of vibration, being capable of operating in real time, and affording low-cost sensing. In this method, relatively low reference angles compared with that in the conventional method using phase shift between three or four pixels has been required. We propose an extended single-shot phase-shifting technique which uses the multiple-step phase-shifting algorithm and the corresponding multiple pixels which are the same as that of the period of an interference fringe. We have verified the theory underlying this recovery method by means of Fourier spectral analysis and its effectiveness by evaluating the visibility of the image using a high-resolution pattern. Finally, we have demonstrated high-contrast image recovery experimentally using a resolution chart. This method can be used in a variety of applications such as color holographic interferometry.

Phase derivative method for reconstruction of slightly off-axis digital holograms.

PubMed

Guo, Cheng-Shan; Wang, Ben-Yi; Sha, Bei; Lu, Yu-Jie; Xu, Ming-Yuan

2014-12-15

A phase derivative (PD) method is proposed for reconstruction of off-axis holograms. In this method, a phase distribution of the tested object wave constrained within 0 to pi radian is firstly worked out by a simple analytical formula; then it is corrected to its right range from -pi to pi according to the sign characteristics of its first-order derivative. A theoretical analysis indicates that this PD method is particularly suitable for reconstruction of slightly off-axis holograms because it only requires the spatial frequency of the reference beam larger than spatial frequency of the tested object wave in principle. In addition, because the PD method belongs to a pure local method with no need of any integral operation or phase shifting algorithm in process of the phase retrieval, it could have some advantages in reducing computer load and memory requirements to the image processing system. Some experimental results are given to demonstrate the feasibility of the method.

Determining Individual Phase Properties in a Multi-phase Q&P Steel using Multi-scale Indentation Tests

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cheng, Guang; Choi, Kyoo Sil; Hu, Xiaohua

2016-01-15

A new inverse method was developed to predict the stress-strain behaviors of constituent phases in a multi-phase steel using the load-depth curves measured in nanoindentation tests combined with microhardness measurements. A power law hardening response was assumed for each phase, and an empirical relationship between hardness and yield strength was assumed. Adjustment was made to eliminate the indentation size effect and indenter bluntness effect. With the newly developed inverse method and statistical analysis of the hardness histogram for each phase, the average stress-strain curves of individual phases in a quench and partitioning (Q&P) steel, including austenite, tempered martensite and untemperedmore » martensite, were calculated and the results were compared with the phase properties obtained by in-situ high energy X-ray diffraction (HEXRD) test. It is demonstrated that multi-scale instrumented indentation tests together with the new inverse method are capable of determining the individual phase flow properties in multi-phase alloys.« less

Reconstructed phase spaces of intrinsic mode functions. Application to postural stability analysis.

PubMed

Snoussi, Hichem; Amoud, Hassan; Doussot, Michel; Hewson, David; Duchêne, Jacques

2006-01-01

In this contribution, we propose an efficient nonlinear analysis method characterizing postural steadiness. The analyzed signal is the displacement of the centre of pressure (COP) collected from a force plate used for measuring postural sway. The proposed method consists of analyzing the nonlinear dynamics of the intrinsic mode functions (IMF) of the COP signal. The nonlinear properties are assessed through the reconstructed phase spaces of the different IMFs. This study shows some specific geometries of the attractors of some intrinsic modes. Moreover, the volume spanned by the geometric attractors in the reconstructed phase space represents an efficient indicator of the postural stability of the subject. Experiments results corroborate the effectiveness of the method to blindly discriminate young subjects, elderly subjects and subjects presenting a risk of falling.

Analytical model and error analysis of arbitrary phasing technique for bunch length measurement

NASA Astrophysics Data System (ADS)

Chen, Qushan; Qin, Bin; Chen, Wei; Fan, Kuanjun; Pei, Yuanji

2018-05-01

An analytical model of an RF phasing method using arbitrary phase scanning for bunch length measurement is reported. We set up a statistical model instead of a linear chirp approximation to analyze the energy modulation process. It is found that, assuming a short bunch (σφ / 2 π → 0) and small relative energy spread (σγ /γr → 0), the energy spread (Y =σγ 2) at the exit of the traveling wave linac has a parabolic relationship with the cosine value of the injection phase (X = cosφr|z=0), i.e., Y = AX2 + BX + C. Analogous to quadrupole strength scanning for emittance measurement, this phase scanning method can be used to obtain the bunch length by measuring the energy spread at different injection phases. The injection phases can be randomly chosen, which is significantly different from the commonly used zero-phasing method. Further, the systematic error of the reported method, such as the influence of the space charge effect, is analyzed. This technique will be especially useful at low energies when the beam quality is dramatically degraded and is hard to measure using the zero-phasing method.

A method searching for optimum fractional order and its application in self-phase modulation induced nonlinear phase noise estimation in coherent optical fiber transmission systems

NASA Astrophysics Data System (ADS)

Huang, Chuan; Guo, Peng; Yang, Aiying; Qiao, Yaojun

2018-07-01

In single channel systems, the nonlinear phase noise only comes from the channel itself through self-phase modulation (SPM). In this paper, a fast-nonlinear effect estimation method is proposed based on fractional Fourier transformation (FrFT). The nonlinear phase noise caused by Self-phase modulation effect is accurately estimated for single model 10Gbaud OOK and RZ-QPSK signals with the fiber length range of 0-200 km and the launch power range of 1-10 mW. The pulse windowing is adopted to search the optimum fractional order for the OOK and RZ-QPSK signals. Since the nonlinear phase shift caused by the SPM effect is very small, the accurate optimum fractional order of the signal cannot be found based on the traditional method. In this paper, a new method magnifying the phase shift is proposed to get the accurate optimum order and thus the nonlinear phase shift is calculated. The simulation results agree with the theoretical analysis and the method is applicable to signals whose pulse type has the similar characteristics with Gaussian pulse.

Analysis on optical heterodyne frequency error of full-field heterodyne interferometer

NASA Astrophysics Data System (ADS)

Li, Yang; Zhang, Wenxi; Wu, Zhou; Lv, Xiaoyu; Kong, Xinxin; Guo, Xiaoli

2017-06-01

The full-field heterodyne interferometric measurement technology is beginning better applied by employing low frequency heterodyne acousto-optical modulators instead of complex electro-mechanical scanning devices. The optical element surface could be directly acquired by synchronously detecting the received signal phases of each pixel, because standard matrix detector as CCD and CMOS cameras could be used in heterodyne interferometer. Instead of the traditional four-step phase shifting phase calculating, Fourier spectral analysis method is used for phase extracting which brings lower sensitivity to sources of uncertainty and higher measurement accuracy. In this paper, two types of full-field heterodyne interferometer are described whose advantages and disadvantages are also specified. Heterodyne interferometer has to combine two different frequency beams to produce interference, which brings a variety of optical heterodyne frequency errors. Frequency mixing error and beat frequency error are two different kinds of inescapable heterodyne frequency errors. In this paper, the effects of frequency mixing error to surface measurement are derived. The relationship between the phase extraction accuracy and the errors are calculated. :: The tolerance of the extinction ratio of polarization splitting prism and the signal-to-noise ratio of stray light is given. The error of phase extraction by Fourier analysis that caused by beat frequency shifting is derived and calculated. We also propose an improved phase extraction method based on spectrum correction. An amplitude ratio spectrum correction algorithm with using Hanning window is used to correct the heterodyne signal phase extraction. The simulation results show that this method can effectively suppress the degradation of phase extracting caused by beat frequency error and reduce the measurement uncertainty of full-field heterodyne interferometer.

Optimization of SEM-EDS to determine the C–A–S–H composition in matured cement paste samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rossen, J.E., E-mail: john.rossen@alumni.epfl.ch

Microanalysis of characteristic X-rays in the SEM is a powerful method to assess the chemical composition of phases in cement pastes, in particular the calcium silicate hydrate containing aluminium (C–A–S–H). Nevertheless, many variables may influence the results obtained, due mainly to the intimate mixing of C–A–S–H with other hydrate phases and the susceptibility of this phase to damage by the electron beam. In this study the effect of various acquisition parameters was examined, along with methods to determine an “average” C–A–S–H composition. The results acquired in the SEM were compared with the analysis of the same samples in the TEM,more » where phases can be analyzed without intermixing. A simple method was used to obtain compositions from SEM based analysis that are very close to those which can be obtained in the TEM. - Highlights: •The intermixing of phases is the limiting factor in the analysis of C–A–S–H composition by SEM-EDS •Guidelines to limit beam damage and properly analyze C–A–S–H composition by SEM-EDS are given •SEM-EDS and TEM-EDS give similar results when proper data treatment is made.« less

Methods for consistent forewarning of critical events across multiple data channels

DOEpatents

Hively, Lee M.

2006-11-21

This invention teaches further method improvements to forewarn of critical events via phase-space dissimilarity analysis of data from biomedical equipment, mechanical devices, and other physical processes. One improvement involves conversion of time-serial data into equiprobable symbols. A second improvement is a method to maximize the channel-consistent total-true rate of forewarning from a plurality of data channels over multiple data sets from the same patient or process. This total-true rate requires resolution of the forewarning indications into true positives, true negatives, false positives and false negatives. A third improvement is the use of various objective functions, as derived from the phase-space dissimilarity measures, to give the best forewarning indication. A fourth improvement uses various search strategies over the phase-space analysis parameters to maximize said objective functions. A fifth improvement shows the usefulness of the method for various biomedical and machine applications.

Direct magnetic field estimation based on echo planar raw data.

PubMed

Testud, Frederik; Splitthoff, Daniel Nicolas; Speck, Oliver; Hennig, Jürgen; Zaitsev, Maxim

2010-07-01

Gradient recalled echo echo planar imaging is widely used in functional magnetic resonance imaging. The fast data acquisition is, however, very sensitive to field inhomogeneities which manifest themselves as artifacts in the images. Typically used correction methods have the common deficit that the data for the correction are acquired only once at the beginning of the experiment, assuming the field inhomogeneity distribution B(0) does not change over the course of the experiment. In this paper, methods to extract the magnetic field distribution from the acquired k-space data or from the reconstructed phase image of a gradient echo planar sequence are compared and extended. A common derivation for the presented approaches provides a solid theoretical basis, enables a fair comparison and demonstrates the equivalence of the k-space and the image phase based approaches. The image phase analysis is extended here to calculate the local gradient in the readout direction and improvements are introduced to the echo shift analysis, referred to here as "k-space filtering analysis." The described methods are compared to experimentally acquired B(0) maps in phantoms and in vivo. The k-space filtering analysis presented in this work demonstrated to be the most sensitive method to detect field inhomogeneities.

Comprehensive automation of the solid phase extraction gas chromatographic mass spectrometric analysis (SPE-GC/MS) of opioids, cocaine, and metabolites from serum and other matrices.

PubMed

Lerch, Oliver; Temme, Oliver; Daldrup, Thomas

2014-07-01

The analysis of opioids, cocaine, and metabolites from blood serum is a routine task in forensic laboratories. Commonly, the employed methods include many manual or partly automated steps like protein precipitation, dilution, solid phase extraction, evaporation, and derivatization preceding a gas chromatography (GC)/mass spectrometry (MS) or liquid chromatography (LC)/MS analysis. In this study, a comprehensively automated method was developed from a validated, partly automated routine method. This was possible by replicating method parameters on the automated system. Only marginal optimization of parameters was necessary. The automation relying on an x-y-z robot after manual protein precipitation includes the solid phase extraction, evaporation of the eluate, derivatization (silylation with N-methyl-N-trimethylsilyltrifluoroacetamide, MSTFA), and injection into a GC/MS. A quantitative analysis of almost 170 authentic serum samples and more than 50 authentic samples of other matrices like urine, different tissues, and heart blood on cocaine, benzoylecgonine, methadone, morphine, codeine, 6-monoacetylmorphine, dihydrocodeine, and 7-aminoflunitrazepam was conducted with both methods proving that the analytical results are equivalent even near the limits of quantification (low ng/ml range). To our best knowledge, this application is the first one reported in the literature employing this sample preparation system.

PFOA and PFOS: Analytics

EPA Science Inventory

EPA Method 537 was developed for the analysis of perfluoroalkyl acids (PFAAs) in drinking water to address the occurrence monitoring needs under EPA’s Unregulated Contaminant Monitoring Regulation (UCMR). The method employs solid-phase extraction with analysis by liquid chr...

A method for the quantitative determination of crystalline phases by X-ray

NASA Technical Reports Server (NTRS)

Petzenhauser, I.; Jaeger, P.

1988-01-01

A mineral analysis method is described for rapid quantitative determination of crystalline substances in those cases in which the sample is present in pure form or in a mixture of known composition. With this method there is no need for prior chemical analysis.

Simultaneous separation and analysis of water- and fat-soluble vitamins on multi-modal reversed-phase weak anion exchange material by HPLC-UV.

PubMed

Dabre, Romain; Azad, Nazanin; Schwämmle, Achim; Lämmerhofer, Michael; Lindner, Wolfgang

2011-04-01

Several methods for the separation of vitamins on HPLC columns were already validated in the last 20 years. However, most of the techniques focus on separating either fat- or water-soluble vitamins and only few methods are intended to separate lipophilic and hydrophilic vitamins simultaneously. A mixed-mode reversed-phase weak anion exchange (RP-WAX) stationary phase was developed in our laboratory in order to address such mixture of analytes with different chemical characteristics, which are difficult to separate on standard columns. The high versatility in usage of the RP-WAX chromatographic material allowed a baseline separation of ten vitamins within a single run, seven water-soluble and three fat-soluble, using three different chromatographic modes: some positively charged vitamins are eluted in ion exclusion and ion repulsion modes whereas the negatively charged molecules are eluted in the ion exchange mechanism. The non-charged molecules are eluted in a classical reversed-phase mode, regarding their polarities. The method was validated for the vitamin analysis in tablets, evaluating selectivity, robustness, linearity, accuracy, and precision. The validated method was finally employed for the analysis of the vitamin content of some commercially available supplement tablets. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry.

PubMed

Ponce-Robles, Laura; Rivas, Gracia; Esteban, Belen; Oller, Isabel; Malato, Sixto; Agüera, Ana

2017-10-01

An analytical method was developed and validated for the determination of ten pesticides in sewage sludge coming from an agro-food industry. The method was based on the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction for solid sewage sludge and SPE extraction for sludge aqueous phase, followed by liquid chromatography (LC) coupled to hybrid quadrupole/linear ion trap mass spectrometry (QqLIT-MS). The QuEChERS method was reported 14 years ago and nowadays is mainly applied to the analysis of pesticides in food. More recent applications have been reported in other matrices as sewage sludge, but the complexity of the matrix makes necessary the optimization of the cleanup step to improve the efficiency of the analysis. With this aim, several dispersive solid-phase extraction cleanup sorbents were tested, choosing C18 + PSA as a d-SPE sorbent. The proposed method was satisfactorily validated for most compounds investigated, showing recoveries higher than 80% in most cases, with the only exception of prochloraz (71%) at low concentration level. Limits of quantification were lower than 40 ng l -1 in the aqueous phase and below 40 ng g -1 in the solid phase for the majority of the analytes. The method was applied to solid sludge and the sludge aqueous phase coming from an agro-food industry which processes fruits and vegetables. Graphical abstract Application of LC/MS/MS advanced analytical techniques for determination of pesticides contained in sewage sludge.

The Study of Phase-shift Super-Frequency Induction Heating Power Supply

NASA Astrophysics Data System (ADS)

Qi, Hairun; Peng, Yonglong; Li, Yabin

This paper combines pulse-width phase-shift power modulation with fixed-angle phase-locked-control to adjust the inverter's output power, this method not only meets the work conditions of voltage inverter, but also realizes the large-scale of power modulation, and the main circuit is simple, the switching devices realize soft switching. This paper analyzes the relationship between the output power and phase-shift angle, the control strategy is simulated by Matlab/Simulink, and the results show that the method is feasible and meets the theoretical analysis

Two-step Raman spectroscopy method for tumor diagnosis

NASA Astrophysics Data System (ADS)

Zakharov, V. P.; Bratchenko, I. A.; Kozlov, S. V.; Moryatov, A. A.; Myakinin, O. O.; Artemyev, D. N.

2014-05-01

Two-step Raman spectroscopy phase method was proposed for differential diagnosis of malignant tumor in skin and lung tissue. It includes detection of malignant tumor in healthy tissue on first step with identification of concrete cancer type on the second step. Proposed phase method analyze spectral intensity alteration in 1300-1340 and 1640-1680 cm-1 Raman bands in relation to the intensity of the 1450 cm-1 band on first step, and relative differences between RS intensities for tumor area and healthy skin closely adjacent to the lesion on the second step. It was tested more than 40 ex vivo samples of lung tissue and more than 50 in vivo skin tumors. Linear Discriminant Analysis, Quadratic Discriminant Analysis and Support Vector Machine were used for tumors type classification on phase planes. It is shown that two-step phase method allows to reach 88.9% sensitivity and 87.8% specificity for malignant melanoma diagnosis (skin cancer); 100% sensitivity and 81.5% specificity for adenocarcinoma diagnosis (lung cancer); 90.9% sensitivity and 77.8% specificity for squamous cell carcinoma diagnosis (lung cancer).

Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

PubMed

Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

2016-08-01

Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A chemometric strategy for optimization of solid-phase microextraction: determination of bisphenol A and 4-nonylphenol with HPLC.

PubMed

Liu, Xiaoyan; Zhang, Xiaoyun; Zhang, Haixia; Liu, Mancang

2008-08-01

A sensitive method for the analysis of bisphenol A and 4-nonylphenol is developed by means of the optimization of solid-phase microextraction using Uniform Experimental Design methodology followed by high-performance liquid chromatographic analysis with fluorescence detection. The optimal extraction conditions are determined based on the relationship between parameters and the peak area. The curve calibration plots are linear (r2>or=0.9980) over the concentration range of 1.25-125 ng/mL for bisphenol A and 2.59-202.96 ng/mL for 4-nonylphenol, respectively. The detection limits, based on a signal-to-noise ratio of 3, are 0.097 ng/mL for bisphenol A and 0.27 ng/mL for 4-nonylphenol, respectively. The validity of the proposed method is demonstrated by the analysis of the investigated analytes in real water samples and sensitivity of the optimized method is verified by comparing results with those obtained by previous methods using the same commercial solid-phase microextraction fiber.

Solid cation exchange phase to remove interfering anthocyanins in the analysis of other bioactive phenols in red wine.

PubMed

da Silva, Letícia Flores; Guerra, Celito Crivellaro; Klein, Diandra; Bergold, Ana Maria

2017-07-15

Bioactive phenols (BPs) are often targets in red wine analysis. However, other compounds interfere in the liquid chromatography methods used for this analysis. Here, purification procedures were tested to eliminate anthocyanin interference during the determination of 19 red-wine BPs. Liquid chromatography, coupled to a diode array detector (HPLC-DAD) and a mass spectrometer (UPLC-MS), was used to compare the direct injection of the samples with solid-phase extractions: reversed-phase (C18) and strong cation-exchange (SCX). The HPLC-DAD method revealed that, out of 13BPs, only six are selectively analyzed with or without C18 treatment, whereas SCX enabled the detection of all BPs. The recovery with SCX was above 86.6% for eight BPs. Moreover, UPLC-MS demonstrated the potential of SCX sample preparation for the determination of 19BPs. The developed procedure may be extended to the analysis of other red wine molecules or to other analytical methods where anthocyanins may interfere. Copyright © 2017 Elsevier Ltd. All rights reserved.

A New Unified Analysis of Estimate Errors by Model-Matching Phase-Estimation Methods for Sensorless Drive of Permanent-Magnet Synchronous Motors and New Trajectory-Oriented Vector Control, Part I

NASA Astrophysics Data System (ADS)

Shinnaka, Shinji; Sano, Kousuke

This paper presents a new unified analysis of estimate errors by model-matching phase-estimation methods such as rotor-flux state-observers, back EMF state-observers, and back EMF disturbance-observers, for sensorless drive of permanent-magnet synchronous motors. Analytical solutions about estimate errors, whose validity is confirmed by numerical experiments, are rich in universality and applicability. As an example of universality and applicability, a new trajectory-oriented vector control method is proposed, which can realize directly quasi-optimal strategy minimizing total losses with no additional computational loads by simply orienting one of vector-control coordinates to the associated quasi-optimal trajectory. The coordinate orientation rule, which is analytically derived, is surprisingly simple. Consequently the trajectory-oriented vector control method can be applied to a number of conventional vector control systems using one of the model-matching phase-estimation methods.

Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

PubMed

Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

2016-04-01

In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Convergence of Heat, Groundwater & Fracture Permeability. Innovative Play Fairway Modelling Applied to the Tularosa Basin Phase 1 Project Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bennett, Carlon R.; Nash, Gregory D.; Sorkhabi, Rasoul

This report summarizes the activities and key findings of the project team occurring during Phase 1 (August 2014-October 2015) of the Tularosa Basin Geothermal Play Fairway Analysis Project. The Tularosa Basin Play Fairway Analysis (PFA) project tested two distinct geothermal exploration methodologies covering the entire basin within South Central New Mexico and Far West Texas. Throughout the initial phase of the project, the underexplored basin proved to be a challenging, yet ideal test bed to evaluate effectiveness of the team’s data collection techniques as well as the effectiveness of our innovative PFA. Phase 1 of the effort employed a low-cost,more » pragmatic approach using two methods to identify potential geothermal plays within the study area and then compared and contrasted the results of each method to rank and evaluate potential plays. Both methods appear to be very effective and highly transferable to other areas.« less

Quantitative x-ray phase-contrast imaging using a single grating of comparable pitch to sample feature size.

PubMed

Morgan, Kaye S; Paganin, David M; Siu, Karen K W

2011-01-01

The ability to quantitatively retrieve transverse phase maps during imaging by using coherent x rays often requires a precise grating or analyzer-crystal-based setup. Imaging of live animals presents further challenges when these methods require multiple exposures for image reconstruction. We present a simple method of single-exposure, single-grating quantitative phase contrast for a regime in which the grating period is much greater than the effective pixel size. A grating is used to create a high-visibility reference pattern incident on the sample, which is distorted according to the complex refractive index and thickness of the sample. The resolution, along a line parallel to the grating, is not restricted by the grating spacing, and the detector resolution becomes the primary determinant of the spatial resolution. We present a method of analysis that maps the displacement of interrogation windows in order to retrieve a quantitative phase map. Application of this analysis to the imaging of known phantoms shows excellent correspondence.

Tacholess order-tracking approach for wind turbine gearbox fault detection

NASA Astrophysics Data System (ADS)

Wang, Yi; Xie, Yong; Xu, Guanghua; Zhang, Sicong; Hou, Chenggang

2017-09-01

Monitoring of wind turbines under variable-speed operating conditions has become an important issue in recent years. The gearbox of a wind turbine is the most important transmission unit; it generally exhibits complex vibration signatures due to random variations in operating conditions. Spectral analysis is one of the main approaches in vibration signal processing. However, spectral analysis is based on a stationary assumption and thus inapplicable to the fault diagnosis of wind turbines under variable-speed operating conditions. This constraint limits the application of spectral analysis to wind turbine diagnosis in industrial applications. Although order-tracking methods have been proposed for wind turbine fault detection in recent years, current methods are only applicable to cases in which the instantaneous shaft phase is available. For wind turbines with limited structural spaces, collecting phase signals with tachometers or encoders is difficult. In this study, a tacholess order-tracking method for wind turbines is proposed to overcome the limitations of traditional techniques. The proposed method extracts the instantaneous phase from the vibration signal, resamples the signal at equiangular increments, and calculates the order spectrum for wind turbine fault identification. The effectiveness of the proposed method is experimentally validated with the vibration signals of wind turbines.

Ionic liquids as stationary phases for fatty acid analysis by gas chromatography.

PubMed

Fanali, C; Micalizzi, G; Dugo, P; Mondello, L

2017-12-04

The present paper provides an overview of the application of ionic liquid (IL) columns for GC analysis of fatty acid methyl esters (FAMEs). Although their separation can be carried out utilizing GC columns containing polar stationary phases, some ILs have been employed as stationary phases, either commercial or laboratory made, in GC analysis. Monodimensional and bidimensional GC methods have been optimized in order to achieve the best separation especially considering the geometric and positional isomers of unsaturated fatty acids. Several methods for the analysis of trans-fatty acids have also been reported. The use of GC-GC, using either the same IL columns or different columns in the first and second dimensions, allowed the separation of a large number of FAMEs. The application of the IL columns for GC analysis of FAMEs in different types of real samples is described, e.g., oil of different nature (fish, flaxseed, and olive), margarine and butter, biodiesel, milk, bacteria etc.

Porous Graphitic Carbon Liquid Chromatography-Mass Spectrometry Analysis of Drought Stress-Responsive Raffinose Family Oligosaccharides in Plant Tissues.

PubMed

Jorge, Tiago F; Florêncio, Maria H; António, Carla

2017-01-01

Drought is a major limiting factor in agriculture and responsible for dramatic crop yield losses worldwide. The adjustment of the metabolic status via accumulation of drought stress-responsive osmolytes is one of the many strategies that some plants have developed to cope with water deficit conditions. Osmolytes are highly polar compounds, analysis of whcih is difficult with typical reversed-phase chromatography. Porous graphitic carbon (PGC) has shown to be a suitable alternative to reversed-phase stationary phases for the analysis of highly polar compounds typically found in the plant metabolome. In this chapter, we describe the development and validation of a PGC-based liquid chromatography tandem mass spectrometry (LC-MS n ) method suitable for the target analysis of water-soluble carbohydrates, such as raffinose family oligosaccharides (RFOs). We present detailed information regarding PGC column equilibration, LC-MS n system operation, data analysis, and important notes to be considered during the steps of method development and validation.

Compiled visualization with IPI method for analysing of liquid liquid mixing process

NASA Astrophysics Data System (ADS)

Jasikova, Darina; Kotek, Michal; Kysela, Bohus; Sulc, Radek; Kopecky, Vaclav

2018-06-01

The article deals with the research of mixing process using visualization techniques and IPI method. Characteristics of the size distribution and the evolution of two liquid-liquid phase's disintegration were studied. A methodology has been proposed for visualization and image analysis of data acquired during the initial phase of the mixing process. IPI method was used for subsequent detailed study of the disintegrated droplets. The article describes advantages of usage of appropriate method, presents the limits of each method, and compares them.

Formation of Al15Mn3Si2 Phase During Solidification of a Novel Al-12%Si-4%Cu-1.2%Mn Heat-Resistant Alloy and Its Thermal Stability

NASA Astrophysics Data System (ADS)

Suo, Xiaojing; Liao, Hengcheng; Hu, Yiyun; Dixit, Uday S.; Petrov, Pavel

2018-02-01

The formation of Al15Mn3Si2 phase in Al-12Si-4Cu-1.2Mn (wt.%) alloy during solidification was investigated by adopting CALPHAD method and microstructural observation by optical microscopy, SEM-EDS, TEM-EDS/SAD and XRD analysis; SEM fixed-point observation method was applied to evaluate its thermal stability. As-cast microstructural observation consistently demonstrates the solidification sequence of the studied alloy predicted by phase diagram calculation. Based on the phase diagram calculation, SEM-EDS, TEM-EDS/SAD and XRD analysis, as well as evidences on Al-Si-Mn-Fe compounds from the literature, the primary and eutectic Mn-rich phases with different morphologies in the studied alloy are identified to be Al15Mn3Si2 that has a body-centered cubic (BCC) structure with a lattice constant of a = 1.352 nm. SEM fixed-point observation and XRD analysis indicate that Al15Mn3Si2 phase has more excellent thermal stability at high temperature than that of CuAl2 phase and can serve as the major strengthening phase in heat-resistant aluminum alloy that has to face a high-temperature working environment. Results of tension test show that addition of Mn can improve the strength of Al-Si-Cu alloy, especially at elevated temperature.

Investigation on phase transitions of 1-decylammonium hydrochloride as the potential thermal energy storage material

NASA Astrophysics Data System (ADS)

Dan, Wen-Yan; Di, You-Ying; He, Dong-Hua; Liu, Yu-Pu

2011-02-01

1-Decylammonium hydrochloride was synthesized by the method of liquid phase synthesis. Chemical analysis, elemental analysis, and X-ray single crystal diffraction techniques were applied to characterize its composition and structure. Low-temperature heat capacities of the compounds were measured with a precision automated adiabatic calorimeter over the temperature range from 78 to 380 K. Three solid-solid phase transitions have been observed at the peak temperatures of 307.52 ± 0.13, 325.02 ± 0.19, and 327.26 ± 0.07 K. The molar enthalpies and entropies of three phase transitions were determined based on the analysis of heat capacity curves. Experimental molar heat capacities were fitted to two polynomial equations of the heat capacities as a function of temperature by least square method. Smoothed heat capacities and thermodynamic functions of the compound relative to the standard reference temperature 298.15 K were calculated and tabulated at intervals of 5 K based on the fitted polynomials.

Retrieval of complex χ(2) parts for quantitative analysis of sum-frequency generation intensity spectra

PubMed Central

Hofmann, Matthias J.; Koelsch, Patrick

2015-01-01

Vibrational sum-frequency generation (SFG) spectroscopy has become an established technique for in situ surface analysis. While spectral recording procedures and hardware have been optimized, unique data analysis routines have yet to be established. The SFG intensity is related to probing geometries and properties of the system under investigation such as the absolute square of the second-order susceptibility χ(2)2. A conventional SFG intensity measurement does not grant access to the complex parts of χ(2) unless further assumptions have been made. It is therefore difficult, sometimes impossible, to establish a unique fitting solution for SFG intensity spectra. Recently, interferometric phase-sensitive SFG or heterodyne detection methods have been introduced to measure real and imaginary parts of χ(2) experimentally. Here, we demonstrate that iterative phase-matching between complex spectra retrieved from maximum entropy method analysis and fitting of intensity SFG spectra (iMEMfit) leads to a unique solution for the complex parts of χ(2) and enables quantitative analysis of SFG intensity spectra. A comparison between complex parts retrieved by iMEMfit applied to intensity spectra and phase sensitive experimental data shows excellent agreement between the two methods. PMID:26450297

Application of Ultrasound Phase-Shift Analysis to Authenticate Wooden Panel Paintings

PubMed Central

Bravo, José M.; Sánchez-Pérez, Juan V.; Ferri, Marcelino; Redondo, Javier; Picó, Rubén

2014-01-01

Artworks are a valuable part of the World's cultural and historical heritage. Conservation and authentication of authorship are important aspects to consider in the protection of cultural patrimony. In this paper we present a novel application of a well-known method based on the phase-shift analysis of an ultrasonic signal, providing an integrated encoding system that enables authentication of the authorship of wooden panel paintings. The method has been evaluated in comparison with optical analysis and shows promising results. The proposed method provides an integrated fingerprint of the artwork, and could be used to enrich the cataloging and protection of artworks. Other advantages that make particularly attractive the proposed technique are its robustness and the use of low-cost sensors. PMID:24803191

Spectroscopic Doppler analysis for visible-light optical coherence tomography

NASA Astrophysics Data System (ADS)

Shu, Xiao; Liu, Wenzhong; Duan, Lian; Zhang, Hao F.

2017-12-01

Retinal oxygen metabolic rate can be effectively measured by visible-light optical coherence tomography (vis-OCT), which simultaneously quantifies oxygen saturation and blood flow rate in retinal vessels through spectroscopic analysis and Doppler measurement, respectively. Doppler OCT relates phase variation between sequential A-lines to the axial flow velocity of the scattering medium. The detectable phase shift is between -π and π due to its periodicity, which limits the maximum measurable unambiguous velocity without phase unwrapping. Using shorter wavelengths, vis-OCT is more vulnerable to phase ambiguity since flow induced phase variation is linearly related to the center wavenumber of the probing light. We eliminated the need for phase unwrapping using spectroscopic Doppler analysis. We split the whole vis-OCT spectrum into a series of narrow subbands and reconstructed vis-OCT images to extract corresponding Doppler phase shifts in all the subbands. Then, we quantified flow velocity by analyzing subband-dependent phase shift using linear regression. In the phantom experiment, we showed that spectroscopic Doppler analysis extended the measurable absolute phase shift range without conducting phase unwrapping. We also tested this method to quantify retinal blood flow in rodents in vivo.

Benzene-induced myelotoxicity: application of flow cytofluorometry for the evaluation of early proliferative change in bone marrow.

PubMed Central

Irons, R D

1981-01-01

A detailed description of flow cytofluorometric DNA cell cycle analysis is presented. A number of studies by the author and other investigators are reviewed in which a method is developed for the analysis of cell cycle phase in bone marrow of experimental animals. Bone marrow cell cycle analysis is a sensitive indicator of changes in bone marrow proliferative activity occurring early in chemically-induced myelotoxicity. Cell cycle analysis, used together with other hematologic methods, has revealed benzene-induced toxicity in proliferating bone marrow cells to be cycle specific, appearing to affect a population in late S phase which then accumulate in G2/M. PMID:7016521

On the peculiarities of LDA method in two-phase flows with high concentrations of particles

NASA Astrophysics Data System (ADS)

Poplavski, S. V.; Boiko, V. M.; Nesterov, A. U.

2016-10-01

Popular applications of laser Doppler anemometry (LDA) in gas dynamics are reviewed. It is shown that the most popular method cannot be used in supersonic flows and two-phase flows with high concentrations of particles. A new approach to implementation of the known LDA method based on direct spectral analysis, which offers better prospects for such problems, is presented. It is demonstrated that the method is suitable for gas-liquid jets. Owing to the progress in laser engineering, digital recording of spectra, and computer processing of data, the method is implemented at a higher technical level and provides new prospects of diagnostics of high-velocity dense two-phase flows.

Film thickness measurement based on nonlinear phase analysis using a Linnik microscopic white-light spectral interferometer.

PubMed

Guo, Tong; Chen, Zhuo; Li, Minghui; Wu, Juhong; Fu, Xing; Hu, Xiaotang

2018-04-20

Based on white-light spectral interferometry and the Linnik microscopic interference configuration, the nonlinear phase components of the spectral interferometric signal were analyzed for film thickness measurement. The spectral interferometric signal was obtained using a Linnik microscopic white-light spectral interferometer, which includes the nonlinear phase components associated with the effective thickness, the nonlinear phase error caused by the double-objective lens, and the nonlinear phase of the thin film itself. To determine the influence of the effective thickness, a wavelength-correction method was proposed that converts the effective thickness into a constant value; the nonlinear phase caused by the effective thickness can then be determined and subtracted from the total nonlinear phase. A method for the extraction of the nonlinear phase error caused by the double-objective lens was also proposed. Accurate thickness measurement of a thin film can be achieved by fitting the nonlinear phase of the thin film after removal of the nonlinear phase caused by the effective thickness and by the nonlinear phase error caused by the double-objective lens. The experimental results demonstrated that both the wavelength-correction method and the extraction method for the nonlinear phase error caused by the double-objective lens improve the accuracy of film thickness measurements.

Multi-layer solid-phase extraction and evaporation-enrichment methods for polar organic chemicals from aqueous matrices.

PubMed

Köke, Niklas; Zahn, Daniel; Knepper, Thomas P; Frömel, Tobias

2018-03-01

Analysis of polar organic chemicals in the aquatic environment is exacerbated by the lack of suitable and widely applicable enrichment methods. In this work, we assessed the suitability of a novel combination of well-known solid-phase extraction (SPE) materials in one cartridge as well as an evaporation method and for the enrichment of 26 polar model substances (predominantly log D < 0) covering a broad range of physico-chemical properties in three different aqueous matrices. The multi-layer solid-phase extraction (mlSPE) and evaporation method were investigated for the recovery and matrix effects of the model substances and analyzed with hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). In total, 65% of the model substances were amenable (> 10% recovery) to the mlSPE method with a mean recovery of 76% while 73% of the model substances were enriched with the evaporation method achieving a mean recovery of 78%. Target and non-target screening comparison of both methods with a frequently used reversed-phase SPE method utilizing "hydrophilic and lipophilic balanced" (HLB) material was performed. Target analysis showed that the mlSPE and evaporation method have pronounced advantages over the HLB method since the HLB material retained only 30% of the model substances. Non-target screening of a ground water sample with the investigated enrichment methods showed that the median retention time of all detected features on a HILIC system decreased in the order mlSPE (3641 features, median t R 9.7 min), evaporation (1391, 9.3 min), HLB (4414, 7.2 min), indicating a higher potential of the described methods to enrich polar analytes from water compared with HLB-SPE. Graphical abstract Schematic of the method evaluation (recovery and matrix effects) and method comparison (target and non-target analysis) of the two investigated enrichment methods for very polar chemicals in aqueousmatrices.

Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods

NASA Technical Reports Server (NTRS)

Dragoi, D.; Kanik, I.; Bar-Cohen, Y.; Sherrit, S.; Tsapin, A.; Kulleck, J.

2004-01-01

In this work we describe an analytical method for determining the presence of organic compounds in rocks, limestone, and other composite materials. Our preliminary laboratory experiments on different rocks/limestone show that the organic component in mineralogical matrices is a minor phase on order of hundreds of ppm and can be better detected using high precision liquid chromatography (HPLC). The matrix, which is the major phase, plays an important role in embedding and protecting the organic molecules from the harsh Martian environment. Some rocks bear significant amounts of amino acids therefore, it is possible to identify these phases using powder x-ray diffraction (XRD) by crystallizing the organic. The method of detection/analysis of organics, in particular amino acids, that have been associated with life will be shown in the next section.

Analysis of group-velocity dispersion of high-frequency Rayleigh waves for near-surface applications

USGS Publications Warehouse

Luo, Y.; Xia, J.; Xu, Y.; Zeng, C.

2011-01-01

The Multichannel Analysis of Surface Waves (MASW) method is an efficient tool to obtain the vertical shear (S)-wave velocity profile using the dispersive characteristic of Rayleigh waves. Most MASW researchers mainly apply Rayleigh-wave phase-velocity dispersion for S-wave velocity estimation with a few exceptions applying Rayleigh-wave group-velocity dispersion. Herein, we first compare sensitivities of fundamental surface-wave phase velocities with group velocities with three four-layer models including a low-velocity layer or a high-velocity layer. Then synthetic data are simulated by a finite difference method. Images of group-velocity dispersive energy of the synthetic data are generated using the Multiple Filter Analysis (MFA) method. Finally we invert a high-frequency surface-wave group-velocity dispersion curve of a real-world example. Results demonstrate that (1) the sensitivities of group velocities are higher than those of phase velocities and usable frequency ranges are wider than that of phase velocities, which is very helpful in improving inversion stability because for a stable inversion system, small changes in phase velocities do not result in a large fluctuation in inverted S-wave velocities; (2) group-velocity dispersive energy can be measured using single-trace data if Rayleigh-wave fundamental-mode energy is dominant, which suggests that the number of shots required in data acquisition can be dramatically reduced and the horizontal resolution can be greatly improved using analysis of group-velocity dispersion; and (3) the suspension logging results of the real-world example demonstrate that inversion of group velocities generated by the MFA method can successfully estimate near-surface S-wave velocities. ?? 2011 Elsevier B.V.

Sealed-tube synthesis and phase diagram of Li{sub x}TiS{sub 2} (0 ≤ x ≤1)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Ziping; National Laboratory for Superconductivity, Institute of Physics, Chinese Academy of Science, Beijing 100190; Dong, Cheng, E-mail: chengdon@aphy.iphy.ac.cn

2015-01-15

Graphical abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S aslithium source. A schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed based on the DTA and XRD data. - Abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S as lithium source. The Li{sub x}TiS{sub 2} samples were characterized by powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and differential thermal analysis. Themore » variations of the lattice parameters with lithium content x in Li{sub x}TiS{sub 2} were determined by X-ray powder diffraction analysis for both 1T and 3R phases. The phase transition between low-temperature 1T phase and high-temperature 3R phase was confirmed by the powder X-ray diffraction analysis. Based on the differential thermal analysis and X-ray diffraction results, a schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed, providing a guideline to synthesize Li{sub x}TiS{sub 2} in 1T structure or 3R structure.« less

Radioisotope measurements of the liquid-gas flow in the horizontal pipeline using phase method

NASA Astrophysics Data System (ADS)

Hanus, Robert; Zych, Marcin; Jaszczur, Marek; Petryka, Leszek; Świsulski, Dariusz

2018-06-01

The paper presents application of the gamma-absorption method to a two-phase liquid-gas flow investigation in a horizontal pipeline. The water-air mixture was examined by a set of two Am-241 radioactive sources and two NaI(Tl) scintillation probes. For analysis of the electrical signals obtained from detectors the cross-spectral density function (CSDF) was applied. Results of the gas phase average velocity measurements for CSDF were compared with results obtained by application of the classical cross-correlation function (CCF). It was found that the combined uncertainties of the gas-phase velocity in the presented experiments did not exceed 1.6% for CSDF method and 5.5% for CCF.

Off-line real-time FTIR analysis of a process step in imipenem production

NASA Astrophysics Data System (ADS)

Boaz, Jhansi R.; Thomas, Scott M.; Meyerhoffer, Steven M.; Staskiewicz, Steven J.; Lynch, Joseph E.; Egan, Richard S.; Ellison, Dean K.

1992-08-01

We have developed an FT-IR method, using a Spectra-Tech Monit-IR 400 systems, to monitor off-line the completion of a reaction in real-time. The reaction is moisture-sensitive and analysis by more conventional methods (normal-phase HPLC) is difficult to reproduce. The FT-IR method is based on the shift of a diazo band when a conjugated beta-diketone is transformed into a silyl enol ether during the reaction. The reaction mixture is examined directly by IR and does not require sample workup. Data acquisition time is less than one minute. The method has been validated for specificity, precision and accuracy. The results obtained by the FT-IR method for known mixtures and in-process samples compare favorably with those from a normal-phase HPLC method.

Unsteady RANS/DES analysis of flow around helicopter rotor blades at forword flight conditions

NASA Astrophysics Data System (ADS)

Zhang, Zhenyu; Qian, Yaoru

2018-05-01

In this paper, the complex flows around forward-flying helicopter blades are numerically investigated. Both the Reynolds-averaged Navier-Stokes (RANS) and the Detached Eddy Simulation (DES) methods are used for the analysis of characteristics like local dynamic flow separation, effects of radial sweeping and reversed flow. The flow was solved by a highly efficient finite volume solver with multi-block structured grids. Focusing upon the complexity of the advance ratio effects, above properties are fully recognized. The current results showed significant agreements between both RANS and DES methods at phases with attached flow phases. Detailed information of separating flow near the withdrawal phases are given by DES results. The flow analysis of these blades under reversed flow reveals a significant interaction between the reversed flow and the span-wise sweeping.

The local properties of ocean surface waves by the phase-time method

NASA Technical Reports Server (NTRS)

Huang, Norden E.; Long, Steven R.; Tung, Chi-Chao; Donelan, Mark A.; Yuan, Yeli; Lai, Ronald J.

1992-01-01

A new approach using phase information to view and study the properties of frequency modulation, wave group structures, and wave breaking is presented. The method is applied to ocean wave time series data and a new type of wave group (containing the large 'rogue' waves) is identified. The method also has the capability of broad applications in the analysis of time series data in general.

ANALYSIS OF SWINE LAGOONS AND GROUND WATER FOR ENVIRONMENTAL ESTROGENS

EPA Science Inventory

A method was developed for analysis of low levels of natural (estradiol, estrone, estriol) and synthetic (ethynylestradiol) estrogens in ground water and swine waste lagoon effluent. The method includes solid phase extraction of the estrogens, preparation of pentafluorobenzyl der...

ANALYSIS OF ALDEHYDES AND KETONES IN THE GAS PHASE

EPA Science Inventory

The development and testing of a 2,4-dinitrophenylhydrazine-acetonitrile (DNPH-ACN) method for the analysis of aldehydes and ketones in ambient air are described. A discussion of interferences, preparation of calibration standards, analytical testing, fluorescence methods and car...

Auto Correlation Analysis of Coda Waves from Local Earthquakes for Detecting Temporal Changes in Shallow Subsurface Structures: the 2011 Tohoku-Oki, Japan Earthquake

NASA Astrophysics Data System (ADS)

Nakahara, Hisashi

2015-02-01

For monitoring temporal changes in subsurface structures I propose to use auto correlation functions of coda waves from local earthquakes recorded at surface receivers, which probably contain more body waves than surface waves. Use of coda waves requires earthquakes resulting in decreased time resolution for monitoring. Nonetheless, it may be possible to monitor subsurface structures in sufficient time resolutions in regions with high seismicity. In studying the 2011 Tohoku-Oki, Japan earthquake (Mw 9.0), for which velocity changes have been previously reported, I try to validate the method. KiK-net stations in northern Honshu are used in this analysis. For each moderate earthquake normalized auto correlation functions of surface records are stacked with respect to time windows in the S-wave coda. Aligning the stacked, normalized auto correlation functions with time, I search for changes in phases arrival times. The phases at lag times of <1 s are studied because changes at shallow depths are focused. Temporal variations in the arrival times are measured at the stations based on the stretching method. Clear phase delays are found to be associated with the mainshock and to gradually recover with time. The amounts of the phase delays are 10 % on average with the maximum of about 50 % at some stations. The deconvolution analysis using surface and subsurface records at the same stations is conducted for validation. The results show the phase delays from the deconvolution analysis are slightly smaller than those from the auto correlation analysis, which implies that the phases on the auto correlations are caused by larger velocity changes at shallower depths. The auto correlation analysis seems to have an accuracy of about several percent, which is much larger than methods using earthquake doublets and borehole array data. So this analysis might be applicable in detecting larger changes. In spite of these disadvantages, this analysis is still attractive because it can be applied to many records on the surface in regions where no boreholes are available.

Elucidation of reaction mechanism involved in the formation of LaNiO3 from XRD and TG analysis

NASA Astrophysics Data System (ADS)

Dharmadhikari, Dipti V.; Athawale, Anjali A.

2013-06-01

The present work is focused on the synthesis and elucidation of reaction mechanism involved in the formation of LaNiO3 with the help of X-ray diffraction (XRD) and thermogravimetric (TG) analysis. LaNiO3 was synthesized by hydrothermal method by heating at 160°C under autogenous pressure for 6h. Pure phase product was obtained after calcining the hydrothermally activated product for 6h at 700°C. The various phases of the product obtained after hydrothermal treatment and calcination followed by the formation of pure phase nanocrystalline lanthanum nickel oxide could be determined from XRD analysis of the samples. The reaction mechanism and phase formation temperature has been interpreted by thermogravimetric analysis of the hydrothermally synthesized product and XRD analysis.

Freeze-thaw method improves the detection of volatile compounds in insects using Headspace Solid-Phase Microextraction (HS-SPME)

USDA-ARS?s Scientific Manuscript database

Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS) is commonly used in analyzing insect volatiles. In order to improve the detection of volatiles in insects, a freeze-thaw method was applied to insect samples before the HS-SPME-GC-MS analysis. ...

Exploring and Testing the Predictors of New Faculty Success: A Mixed Methods Study

ERIC Educational Resources Information Center

Stupnisky, R. H.; Weaver-Hightower, M. B.; Kartoshkina, Y.

2015-01-01

The purpose of this mixed methods study was to investigate and test the factors contributing to new faculty members' success. In the first phase, qualitative analysis of focus groups revealed four prominent themes affecting new faculty members: expectations, collegiality, balance, and location. In the second phase, new faculty members completed an…

Micro versus macro solid phase extraction for monitoring water contaminants: a preliminary study using trihalomethanes.

PubMed

Alexandrou, Lydon D; Spencer, Michelle J S; Morrison, Paul D; Meehan, Barry J; Jones, Oliver A H

2015-04-15

Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental science. However, traditional methods need electrically powered pumps, can use large volumes of solvent (if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and provides comparable concentration factors to established methods. It is also an enclosed system so volatile components are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required. However, the technology is new and has not been much used for environmental analysis. In this study we compare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile trihalomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane). The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with similar recovery rates for the target compounds. This method shows potential for further development in a range of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

A total variation diminishing finite difference algorithm for sonic boom propagation models

NASA Technical Reports Server (NTRS)

Sparrow, Victor W.

1993-01-01

It is difficult to accurately model the rise phases of sonic boom waveforms with traditional finite difference algorithms because of finite difference phase dispersion. This paper introduces the concept of a total variation diminishing (TVD) finite difference method as a tool for accurately modeling the rise phases of sonic booms. A standard second order finite difference algorithm and its TVD modified counterpart are both applied to the one-way propagation of a square pulse. The TVD method clearly outperforms the non-TVD method, showing great potential as a new computational tool in the analysis of sonic boom propagation.

Frequency-phase analysis of resting-state functional MRI

PubMed Central

Goelman, Gadi; Dan, Rotem; Růžička, Filip; Bezdicek, Ondrej; Růžička, Evžen; Roth, Jan; Vymazal, Josef; Jech, Robert

2017-01-01

We describe an analysis method that characterizes the correlation between coupled time-series functions by their frequencies and phases. It provides a unified framework for simultaneous assessment of frequency and latency of a coupled time-series. The analysis is demonstrated on resting-state functional MRI data of 34 healthy subjects. Interactions between fMRI time-series are represented by cross-correlation (with time-lag) functions. A general linear model is used on the cross-correlation functions to obtain the frequencies and phase-differences of the original time-series. We define symmetric, antisymmetric and asymmetric cross-correlation functions that correspond respectively to in-phase, 90° out-of-phase and any phase difference between a pair of time-series, where the last two were never introduced before. Seed maps of the motor system were calculated to demonstrate the strength and capabilities of the analysis. Unique types of functional connections, their dominant frequencies and phase-differences have been identified. The relation between phase-differences and time-delays is shown. The phase-differences are speculated to inform transfer-time and/or to reflect a difference in the hemodynamic response between regions that are modulated by neurotransmitters concentration. The analysis can be used with any coupled functions in many disciplines including electrophysiology, EEG or MEG in neuroscience. PMID:28272522

High Frequency Resolution TOA Analysis for ELF/VLFWave Generation Experiments at HAARP

NASA Astrophysics Data System (ADS)

Ruddle, J. D.; Moore, R. C.

2014-12-01

Modulated HF heating of the ionosphere in the presence of natural ionospheric current sources has been used as a method to generate electromagnetic ELF/VLF waves since the 1970's. In the ~1-5 kHz band, the amplitude and phase of the received ELF/VLF signal depends on the amplitude and phase of the conductivity modulation generated throughout the HF-heated ionospheric body, as well as on the signal propagation parameters (i.e., the attenuation and phase constants) between each of the current sources and the receiver. Recent signal processing advances have produced an accurate ELF/VLF time-of-arrival (TOA) analysis technique that differentiates line-of-sight and ionospherically-reflected signal components, determining the amplitude and phase of each component observed at the receiver. This TOA method requires a wide bandwidth (> 2.5 kHz) and therefore is relatively insensitive to the frequency-dependent nature of ELF/VLF wave propagation. In this paper, we present an improved ELF/VLF TOA method that is capable of providing high frequency resolution. The new analysis technique is applied to experimental observations of ELF/VLF signals generated by modulated heating at HAARP. We present measurements of the amplitude and phase of the received ELF/VLF signal as a function of frequency and compare the results with the predictions of an HF heating model.

Reliable two-dimensional phase unwrapping method using region growing and local linear estimation.

PubMed

Zhou, Kun; Zaitsev, Maxim; Bao, Shanglian

2009-10-01

In MRI, phase maps can provide useful information about parameters such as field inhomogeneity, velocity of blood flow, and the chemical shift between water and fat. As phase is defined in the (-pi,pi] range, however, phase wraps often occur, which complicates image analysis and interpretation. This work presents a two-dimensional phase unwrapping algorithm that uses quality-guided region growing and local linear estimation. The quality map employs the variance of the second-order partial derivatives of the phase as the quality criterion. Phase information from unwrapped neighboring pixels is used to predict the correct phase of the current pixel using a linear regression method. The algorithm was tested on both simulated and real data, and is shown to successfully unwrap phase images that are corrupted by noise and have rapidly changing phase. (c) 2009 Wiley-Liss, Inc.

Simultaneous assessment of phase chemistry, phase abundance and bulk chemistry with statistical electron probe micro-analyses: Application to cement clinkers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wilson, William; Krakowiak, Konrad J.; Ulm, Franz-Josef, E-mail: ulm@mit.edu

2014-01-15

According to recent developments in cement clinker engineering, the optimization of chemical substitutions in the main clinker phases offers a promising approach to improve both reactivity and grindability of clinkers. Thus, monitoring the chemistry of the phases may become part of the quality control at the cement plants, along with the usual measurements of the abundance of the mineralogical phases (quantitative X-ray diffraction) and the bulk chemistry (X-ray fluorescence). This paper presents a new method to assess these three complementary quantities with a single experiment. The method is based on electron microprobe spot analyses, performed over a grid located onmore » a representative surface of the sample and interpreted with advanced statistical tools. This paper describes the method and the experimental program performed on industrial clinkers to establish the accuracy in comparison to conventional methods. -- Highlights: •A new method of clinker characterization •Combination of electron probe technique with cluster analysis •Simultaneous assessment of phase abundance, composition and bulk chemistry •Experimental validation performed on industrial clinkers.« less

Generalization of the Poincare sphere to process 2D displacement signals

NASA Astrophysics Data System (ADS)

Sciammarella, Cesar A.; Lamberti, Luciano

2017-06-01

Traditionally the multiple phase method has been considered as an essential tool for phase information recovery. The in-quadrature phase method that theoretically is an alternative pathway to achieve the same goal failed in actual applications. The authors in a previous paper dealing with 1D signals have shown that properly implemented the in-quadrature method yields phase values with the same accuracy than the multiple phase method. The present paper extends the methodology developed in 1D to 2D. This extension is not a straight forward process and requires the introduction of a number of additional concepts and developments. The concept of monogenic function provides the necessary tools required for the extension process. The monogenic function has a graphic representation through the Poincare sphere familiar in the field of Photoelasticity and through the developments introduced in this paper connected to the analysis of displacement fringe patterns. The paper is illustrated with examples of application that show that multiple phases method and the in-quadrature are two aspects of the same basic theoretical model.

Lindemann histograms as a new method to analyse nano-patterns and phases

NASA Astrophysics Data System (ADS)

Makey, Ghaith; Ilday, Serim; Tokel, Onur; Ibrahim, Muhamet; Yavuz, Ozgun; Pavlov, Ihor; Gulseren, Oguz; Ilday, Omer

The detection, observation, and analysis of material phases and atomistic patterns are of great importance for understanding systems exhibiting both equilibrium and far-from-equilibrium dynamics. As such, there is intense research on phase transitions and pattern dynamics in soft matter, statistical and nonlinear physics, and polymer physics. In order to identify phases and nano-patterns, the pair correlation function is commonly used. However, this approach is limited in terms of recognizing competing patterns in dynamic systems, and lacks visualisation capabilities. In order to solve these limitations, we introduce Lindemann histogram quantification as an alternative method to analyse solid, liquid, and gas phases, along with hexagonal, square, and amorphous nano-pattern symmetries. We show that the proposed approach based on Lindemann parameter calculated per particle maps local number densities to material phase or particles pattern. We apply the Lindemann histogram method on dynamical colloidal self-assembly experimental data and identify competing patterns.

Analysis of phase error effects in multishot diffusion-prepared turbo spin echo imaging

PubMed Central

Cervantes, Barbara; Kooijman, Hendrik; Karampinos, Dimitrios C.

2017-01-01

Background To characterize the effect of phase errors on the magnitude and the phase of the diffusion-weighted (DW) signal acquired with diffusion-prepared turbo spin echo (dprep-TSE) sequences. Methods Motion and eddy currents were identified as the main sources of phase errors. An analytical expression for the effect of phase errors on the acquired signal was derived and verified using Bloch simulations, phantom, and in vivo experiments. Results Simulations and experiments showed that phase errors during the diffusion preparation cause both magnitude and phase modulation on the acquired data. When motion-induced phase error (MiPe) is accounted for (e.g., with motion-compensated diffusion encoding), the signal magnitude modulation due to the leftover eddy-current-induced phase error cannot be eliminated by the conventional phase cycling and sum-of-squares (SOS) method. By employing magnitude stabilizers, the phase-error-induced magnitude modulation, regardless of its cause, was removed but the phase modulation remained. The in vivo comparison between pulsed gradient and flow-compensated diffusion preparations showed that MiPe needed to be addressed in multi-shot dprep-TSE acquisitions employing magnitude stabilizers. Conclusions A comprehensive analysis of phase errors in dprep-TSE sequences showed that magnitude stabilizers are mandatory in removing the phase error induced magnitude modulation. Additionally, when multi-shot dprep-TSE is employed the inconsistent signal phase modulation across shots has to be resolved before shot-combination is performed. PMID:28516049

Phase-recovery improvement using analytic wavelet transform analysis of a noisy interferogram cepstrum.

PubMed

Etchepareborda, Pablo; Vadnjal, Ana Laura; Federico, Alejandro; Kaufmann, Guillermo H

2012-09-15

We evaluate the extension of the exact nonlinear reconstruction technique developed for digital holography to the phase-recovery problems presented by other optical interferometric methods, which use carrier modulation. It is shown that the introduction of an analytic wavelet analysis in the ridge of the cepstrum transformation corresponding to the analyzed interferogram can be closely related to the well-known wavelet analysis of the interferometric intensity. Subsequently, the phase-recovery process is improved. The advantages and limitations of this framework are analyzed and discussed using numerical simulations in singular scalar light fields and in temporal speckle pattern interferometry.

ANALYSIS OF SWINE LAGOONS AND GROUND WATER FOR ENVIRONMENTAL ESTROGENS

EPA Science Inventory

A method was developed for analysis of low levels of natural (estradiol, estrone, estriol) and synthetic (ethinyl estradiol) estrogens in ground water and swine waste lagoon effluent. The method includes solid phase extraction of the estrogens, preparation of pentafluorobenzyl de...

Simple method for the extraction and reversed-phase high-performance liquid chromatographic analysis of carotenoid pigments from red yeasts (Basidiomycota, Fungi).

PubMed

Weber, Roland W S; Anke, Heidrun; Davoli, Paolo

2007-03-23

A simple method for the extraction of carotenoid pigments from frozen wet cells of red yeasts (Basidiomycota) and their analysis by reversed-phase HPLC using a C(18) column and a water/acetone solvent system is described. Typical red yeast carotenoids belonging to an oxidative series from the monocyclic gamma-carotene to 2-hydroxytorularhodin and from the bicyclic beta-carotene to astaxanthin were separated. Pigment identity was confirmed by LC-atmospheric pressure chemical ionisation (APCI) mass spectrometry using similar chromatographic conditions.

Realist theory construction for a mixed method multilevel study of neighbourhood context and postnatal depression.

PubMed

Eastwood, John G; Kemp, Lynn A; Jalaludin, Bin B

2016-01-01

We have recently described a protocol for a study that aims to build a theory of neighbourhood context and postnatal depression. That protocol proposed a critical realist Explanatory Theory Building Method comprising of an: (1) emergent phase, (2) construction phase, and (3) confirmatory phase. A concurrent triangulated mixed method multilevel cross-sectional study design was described. The protocol also described in detail the Theory Construction Phase which will be presented here. The Theory Construction Phase will include: (1) defining stratified levels; (2) analytic resolution; (3) abductive reasoning; (4) comparative analysis (triangulation); (5) retroduction; (6) postulate and proposition development; (7) comparison and assessment of theories; and (8) conceptual frameworks and model development. The stratified levels of analysis in this study were predominantly social and psychological. The abductive analysis used the theoretical frames of: Stress Process; Social Isolation; Social Exclusion; Social Services; Social Capital, Acculturation Theory and Global-economic level mechanisms. Realist propositions are presented for each analysis of triangulated data. Inference to best explanation is used to assess and compare theories. A conceptual framework of maternal depression, stress and context is presented that includes examples of mechanisms at psychological, social, cultural and global-economic levels. Stress was identified as a necessary mechanism that has the tendency to cause several outcomes including depression, anxiety, and health harming behaviours. The conceptual framework subsequently included conditional mechanisms identified through the retroduction including the stressors of isolation and expectations and buffers of social support and trust. The meta-theory of critical realism is used here to generate and construct social epidemiological theory using stratified ontology and both abductive and retroductive analysis. The findings will be applied to the development of a middle range theory and subsequent programme theory for local perinatal child and family interventions.

Investigation into the propagation of Omega very low frequency signals and techniques for improvement of navigation accuracy including differential and composite omega

NASA Technical Reports Server (NTRS)

1973-01-01

An analysis of Very Low Frequency propagation in the atmosphere in the 10-14 kHz range leads to a discussion of some of the more significant causes of phase perturbation. The method of generating sky-wave corrections to predict the Omega phase is discussed. Composite Omega is considered as a means of lane identification and of reducing Omega navigation error. A simple technique for generating trapezoidal model (T-model) phase prediction is presented and compared with the Navy predictions and actual phase measurements. The T-model prediction analysis illustrates the ability to account for the major phase shift created by the diurnal effects on the lower ionosphere. An analysis of the Navy sky-wave correction table is used to provide information about spatial and temporal correlation of phase correction relative to the differential mode of operation.

DC/DC Converter Stability Testing Study

NASA Technical Reports Server (NTRS)

Wang, Bright L.

2008-01-01

This report presents study results on hybrid DC/DC converter stability testing methods. An input impedance measurement method and a gain/phase margin measurement method were evaluated to be effective to determine front-end oscillation and feedback loop oscillation. In particular, certain channel power levels of converter input noises have been found to have high degree correlation with the gain/phase margins. It becomes a potential new method to evaluate stability levels of all type of DC/DC converters by utilizing the spectral analysis on converter input noises.

Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

PubMed

Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

2016-04-01

Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

Evaluation of comprehensive multidimensional separations using reversed-phase, reversed-phase liquid chromatography/mass spectrometry for shotgun proteomics.

PubMed

Nakamura, Tatsuji; Kuromitsu, Junro; Oda, Yoshiya

2008-03-01

Two-dimensional liquid-chromatographic (LC) separation followed by mass spectrometric (MS) analysis was examined for the identification of peptides in complex mixtures as an alternative to widely used two-dimensional gel electrophoresis followed by MS analysis for use in proteomics. The present method involves the off-line coupling of a narrow-bore, polymer-based, reversed-phase column using an acetonitrile gradient in an alkaline mobile phase in the first dimension with octadecylsilanized silica (ODS)-based nano-LC/MS in the second dimension. After the first separation, successive fractions were acidified and dried off-line, then loaded on the second dimension column. Both columns separate peptides according to hydrophobicity under different pH conditions, but more peptides were identified than with the conventional technique for shotgun proteomics, that is, the combination of a strong cation exchange column with an ODS column, and the system was robust because no salts were included in the mobile phases. The suitability of the method for proteomics measurements was evaluated.

Measurement of cellular copper levels in Bacillus megaterium during exponential growth and sporulation.

PubMed

Krueger, W B; Kolodziej, B J

1976-01-01

Both atomic absorption spectrophotometry (AAS) and neutron activation analysis have been utilized to determine cellular Cu levels in Bacillus megaterium ATCC 19213. Both methods were selected for their sensitivity to detection of nanogram quantities of Cu. Data from both methods demonstrated identical patterms of Cu uptake during exponenetial growth and sporulation. Late exponential phase cells contained less Cu than postexponential t2 cells while t5 cells contained amounts equivalent to exponential cells. The t11 phase-bright forespore containing cells had a higher Cu content than those of earlier time periods, and the free spores had the highest Cu content. Analysis of the culture medium by AAS corroborated these data by showing concomitant Cu uptake during exponential growth and into t2 postexponential phase of sporulation. From t2 to t4, Cu egressed from the cells followed by a secondary uptake during the maturation of phase-dark forespores into phase-bright forespores (t6--t9).

Solid-phase extraction with the metal-organic framework MIL-101(Cr) combined with direct analysis in real time mass spectrometry for the fast analysis of triazine herbicides.

PubMed

Li, Xianjiang; Xing, Jiawei; Chang, Cuilan; Wang, Xin; Bai, Yu; Yan, Xiuping; Liu, Huwei

2014-06-01

MIL-101(Cr) is an excellent metal-organic framework with high surface area and nanoscale cavities, making it promising in solid-phase extraction. Herein, we used MIL-101(Cr) as a solid-phase extraction packing material combined with fast detection of direct analysis in real time mass spectrometry (DART-MS) for the analysis of triazine herbicides. After systematic optimization of the operation parameters, including the gas temperature of DART, the moving speed of the 1D platform, solvent for desorption, amount of MIL-101(Cr) extraction time, eluent volume and salt concentration, this method can realize the simultaneous detection of five kinds of triazine herbicides. The limits of detection were 0.1∼0.2 ng/mL and the linear ranges covered more than two orders of magnitude with the quantitation limits of 0.5∼1 ng/mL. Moreover, the developed method has been applied for the analysis of lake water samples and the recoveries for spiked analytes were in the range of 85∼110%. These results showed that solid-phase extraction with metal-organic frameworks is an efficient sample preparation approach for DART-MS analysis and could find more applications in environmental analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biofilm thickness measurement using an ultrasound method in a liquid phase.

PubMed

Maurício, R; Dias, C J; Jubilado, N; Santana, F

2013-10-01

In this report, the development of an online, noninvasive, measurement method of the biofilm thickness in a liquid phase is presented. The method is based in the analysis of the ultrasound wave pulse-echo behavior in a liquid phase reproducing the real reactor conditions. It does not imply the removal of the biomass from the support or any kind of intervention in the support (pipes) to detect and perform the measurements (non-invasiveness). The developed method allows for its sensor to be easily and quickly mounted and unmounted in any location along a pipe or reactor wall. Finally, this method is an important innovation because it allows the thickness measurement of a biofilm, in liquid phase conditions that can be used in monitoring programs, to help in scheduling cleaning actions to remove the unwanted biofilm, in several application areas, namely in potable water supply pipes.

Automatic detection and analysis of cell motility in phase-contrast time-lapse images using a combination of maximally stable extremal regions and Kalman filter approaches.

PubMed

Kaakinen, M; Huttunen, S; Paavolainen, L; Marjomäki, V; Heikkilä, J; Eklund, L

2014-01-01

Phase-contrast illumination is simple and most commonly used microscopic method to observe nonstained living cells. Automatic cell segmentation and motion analysis provide tools to analyze single cell motility in large cell populations. However, the challenge is to find a sophisticated method that is sufficiently accurate to generate reliable results, robust to function under the wide range of illumination conditions encountered in phase-contrast microscopy, and also computationally light for efficient analysis of large number of cells and image frames. To develop better automatic tools for analysis of low magnification phase-contrast images in time-lapse cell migration movies, we investigated the performance of cell segmentation method that is based on the intrinsic properties of maximally stable extremal regions (MSER). MSER was found to be reliable and effective in a wide range of experimental conditions. When compared to the commonly used segmentation approaches, MSER required negligible preoptimization steps thus dramatically reducing the computation time. To analyze cell migration characteristics in time-lapse movies, the MSER-based automatic cell detection was accompanied by a Kalman filter multiobject tracker that efficiently tracked individual cells even in confluent cell populations. This allowed quantitative cell motion analysis resulting in accurate measurements of the migration magnitude and direction of individual cells, as well as characteristics of collective migration of cell groups. Our results demonstrate that MSER accompanied by temporal data association is a powerful tool for accurate and reliable analysis of the dynamic behaviour of cells in phase-contrast image sequences. These techniques tolerate varying and nonoptimal imaging conditions and due to their relatively light computational requirements they should help to resolve problems in computationally demanding and often time-consuming large-scale dynamical analysis of cultured cells. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

ANALYSIS OF A GAS-PHASE PARTITIONING TRACER TEST CONDUCTED IN AN UNSATURATED FRACTURED-CLAY FORMATION

EPA Science Inventory

The gas-phase partitioning tracer method was used to estimate non-aqueous phase liquid (NAPL), water, and air saturations in the vadose zone at a chlorinated-solvent contaminated field site in Tucson, AZ. The tracer test was conducted in a fractured-clay system that is the confin...

Financial time series analysis based on effective phase transfer entropy

NASA Astrophysics Data System (ADS)

Yang, Pengbo; Shang, Pengjian; Lin, Aijing

2017-02-01

Transfer entropy is a powerful technique which is able to quantify the impact of one dynamic system on another system. In this paper, we propose the effective phase transfer entropy method based on the transfer entropy method. We use simulated data to test the performance of this method, and the experimental results confirm that the proposed approach is capable of detecting the information transfer between the systems. We also explore the relationship between effective phase transfer entropy and some variables, such as data size, coupling strength and noise. The effective phase transfer entropy is positively correlated with the data size and the coupling strength. Even in the presence of a large amount of noise, it can detect the information transfer between systems, and it is very robust to noise. Moreover, this measure is indeed able to accurately estimate the information flow between systems compared with phase transfer entropy. In order to reflect the application of this method in practice, we apply this method to financial time series and gain new insight into the interactions between systems. It is demonstrated that the effective phase transfer entropy can be used to detect some economic fluctuations in the financial market. To summarize, the effective phase transfer entropy method is a very efficient tool to estimate the information flow between systems.

Multi-decadal evolution characteristics of global surface temperature anomaly data shown by observation and CMIP5 models

NASA Astrophysics Data System (ADS)

Zhu, X.

2017-12-01

Based on methods of statistical analysis, the time series of global surface air temperature(SAT) anomalies from 1860-2014 has been defined by three types of phase changes that occur through the division of temperature changes into different stages. The characteristics of the three types of phase changes simulated by CMIP5 models were evaluated. The conclusion is as follows: the SAT from 1860-2014 can be divided into six stages according to trend differences, and this subdivision is proved to be statistically significant. Based on trend analysis and the distribution of slopes between any two points (two points' slope) in every stage, the six stages can be summarized as three phase changes of warming, cooling, and hiatus. Between 1860 and 2014, the world experienced three heating phases (1860-1878, 1909-1942,1975-2004), one cooling phase (1878-1909), and two hiatus phases (1942-1975, 2004-2014).Using the definition method, whether the next year belongs to the previous phase can be estimated. Furthermore, the temperature in 2015 was used as an example to validate the feasibility of this method. The simulations of the heating period by CMIP5 models are well; however the characteristics shown by SAT during the cooling and hiatus period cannot be represented by CMIP5 models. As such, the projections of future heating phases using the CMIP5 models are credible, but for cooling and hiatus events they are unreliable.

Reverse phase HPLC method for detection and quantification of lupin seed γ-conglutin.

PubMed

Mane, Sharmilee; Bringans, Scott; Johnson, Stuart; Pareek, Vishnu; Utikar, Ranjeet

2017-09-15

A simple, selective and accurate reverse phase HPLC method was developed for detection and quantitation of γ-conglutin from lupin seed extract. A linear gradient of water and acetonitrile containing trifluoroacetic acid (TFA) on a reverse phase column (Agilent Zorbax 300SB C-18), with a flow rate of 0.8ml/min was able to produce a sharp and symmetric peak of γ-conglutin with a retention time at 29.16min. The identity of γ-conglutin in the peak was confirmed by mass spectrometry (MS/MS identification) and sodium dodecyl sulphate polyacrylamide gel electrophoresis (SDS-PAGE) analysis. The data obtained from MS/MS analysis was matched against the specified database to obtain the exact match for the protein of interest. The proposed method was validated in terms of specificity, linearity, sensitivity, precision, recovery and accuracy. The analytical parameters revealed that the validated method was capable of selectively performing a good chromatographic separation of γ-conglutin from the lupin seed extract with no interference of the matrix. The detection and quantitation limit of γ-conglutin were found to be 2.68μg/ml and 8.12μg/ml respectively. The accuracy (precision and recovery) analysis of the method was conducted under repeatable conditions on different days. Intra-day and inter-day precision values less than 0.5% and recovery greater than 97% indicated high precision and accuracy of the method for analysis of γ-conglutin. The method validation findings were reproducible and can be successfully applied for routine analysis of γ-conglutin from lupin seed extract. Copyright © 2017 Elsevier B.V. All rights reserved.

Sensitivity analysis and optimization method for the fabrication of one-dimensional beam-splitting phase gratings

PubMed Central

Pacheco, Shaun; Brand, Jonathan F.; Zaverton, Melissa; Milster, Tom; Liang, Rongguang

2015-01-01

A method to design one-dimensional beam-spitting phase gratings with low sensitivity to fabrication errors is described. The method optimizes the phase function of a grating by minimizing the integrated variance of the energy of each output beam over a range of fabrication errors. Numerical results for three 1x9 beam splitting phase gratings are given. Two optimized gratings with low sensitivity to fabrication errors were compared with a grating designed for optimal efficiency. These three gratings were fabricated using gray-scale photolithography. The standard deviation of the 9 outgoing beam energies in the optimized gratings were 2.3 and 3.4 times lower than the optimal efficiency grating. PMID:25969268

Advantages of using tetrahydrofuran-water as mobile phases in the quantitation of cyclosporin A in monkey and rat plasma by liquid chromatography-tandem mass spectrometry.

PubMed

Li, Austin C; Li, Yinghe; Guirguis, Micheal S; Caldwell, Robert G; Shou, Wilson Z

2007-01-04

A new analytical method is described here for the quantitation of anti-inflammatory drug cyclosporin A (CyA) in monkey and rat plasma. The method used tetrahydrofuran (THF)-water mobile phases to elute the analyte and internal standard, cyclosporin C (CyC). The gradient mobile phase program successfully eluted CyA into a sharp peak and therefore improved resolution between the analyte and possible interfering materials compared with previously reported analytical approaches, where CyA was eluted as a broad peak due to the rapid conversion between different conformers. The sharp peak resulted from this method facilitated the quantitative calculation as multiple smoothing and large number of bunching factors were not necessary. The chromatography in the new method was performed at 30 degrees C instead of 65-70 degrees C as reported previously. Other advantages of the method included simple and fast sample extraction-protein precipitation, direct injection of the extraction supernatant to column for analysis, and elimination of evaporation and reconstitution steps, which were needed in solid phase extraction or liquid-liquid extraction reported before. This method is amenable to high-throughput analysis with a total chromatographic run time of 3 min. This approach has been verified as sensitive, linear (0.977-4000 ng/mL), accurate and precise for the quantitation of CyA in monkey and rat plasma. However, compared with the usage of conventional mobile phases, the only drawback of this approach was the reduced detection response from the mass spectrometer that was possibly caused by poor desolvation in the ionization source. This is the first report to demonstrate the advantages of using THF-water mobile phases to elute CyA in liquid chromatography.

Frequency domain phase-shifted confocal microscopy (FDPCM) with array detection

NASA Astrophysics Data System (ADS)

Ge, Baoliang; Huang, Yujia; Fang, Yue; Kuang, Cuifang; Xiu, Peng; Liu, Xu

2017-09-01

We proposed a novel method to reconstruct images taken by array detected confocal microscopy without prior knowledge about its detector distribution. The proposed frequency domain phase-shifted confocal microscopy (FDPCM) shifts the image from each detection channel to its corresponding place by substituting the phase information in Fourier domain. Theoretical analysis shows that our method could approach the resolution nearly twofold of wide-field microscopy. Simulation and experiment results are also shown to verify the applicability and effectiveness of our method. Compared to Airyscan, our method holds the advantage of simplicity and convenience to be applied to array detectors with different structure, which makes FDPCM have great potential in the application of biomedical observation in the future.

X-Ray Phase Imaging for Breast Cancer Detection

DTIC Science & Technology

2012-09-01

the Gerchberg-Saxton algorithm in the Fresnel diffraction regime, and is much more robust against image noise than the TIE-based method. For details...developed efficient coding with the software modules for the image registration, flat-filed correction , and phase retrievals. In addition, we...X, Liu H. 2010. Performance analysis of the attenuation-partition based iterative phase retrieval algorithm for in-line phase-contrast imaging

Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sciancalepore, Corrado, E-mail: corrado.sciancalepore@unimore.it; Bondioli, Federica; INSTM Consortium, Via G. Giusti 9, 51121 Firenze

2015-02-15

An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals wasmore » followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe{sub 3}O{sub 4} nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis.« less

An innovative approach to the analysis of 3-[4-(2-methylpropyl)phenyl]propanoic acid as an impurity of ibuprofen on a carbon-coated zirconia stationary phase.

PubMed

Kalafut, P; Kucera, R; Klimes, J; Sochor, J

2009-07-12

3-[4-(2-Methylpropyl)phenyl]propanoic acid has been introduced as impurity F to the European Pharmacopoeia in its Supplement 4.2. In contrast to other impurities, which are evaluated by HPLC, the content of impurity F is determined by gas chromatography after previous derivatization. Thus a novel reversed-phase HPLC method was developed to simplify the evaluation of pharmacopoeial impurity F of ibuprofen. Favourable properties of zirconia stationary phases were employed for this purpose. The HPLC separation was achieved on a Zr-CARB column (150 mm x 4.6mm i.d., 5 microm) using the mobile phase acetonitrile-phosphate buffer (pH 3.5, 25 mM) (38:62, v/v), temperature 80 degrees C and the flow rate 1.2 ml min(-1). The fluorescence detection was employed to enhance the sensitivity of the method. Optimal detection parameters were chosen on the basis of fluorescence spectra of the analytes. The excitation and emission wavelengths were 220 nm and 285 nm, respectively. The analysis was completed within 25 min. The subsequent validation of the method confirmed the applicability of method for the analytical assay of impurity F.

Fluorous tagging strategy for solution-phase synthesis of small molecules, peptides and oligosaccharides

PubMed Central

Zhang, Wei

2005-01-01

The purification of reaction mixtures is a slow process in organic synthesis, especially during the production of large numbers of analogs and compound libraries. Phase-tag methods such as solid-phase synthesis and fluorous synthesis, provide efficient ways of addressing the separation issue. Fluorous synthesis employs functionalized perfluoroalkyl groups attached to substrates or reagents. The separation of the resulting fluorous molecules can be achieved using strong and selective fluorous liquid-liquid extraction, fluorous silica gel-based solid-phase extraction or high-performance liquid chromatography. Fluorous technology is a novel solution-phase method, which has the advantages of fast reaction times in homogeneous environments, being readily adaptable to literature conditions, having easy intermediate analysis, and having flexibility in reaction scale and scope. In principle, any synthetic methods that use a solid-support could be conducted in solution-phase by replacing the polymer linker with a corresponding fluorous tag. This review summarizes the progress of fluorous tags in solution-phase synthesis of small molecules, peptides and oligosaccharides. PMID:15595439

Microvolume trace environmental analysis using peak-focusing online solid-phase extraction-nano-liquid chromatography-high-resolution mass spectrometry.

PubMed

Stravs, Michael A; Mechelke, Jonas; Ferguson, P Lee; Singer, Heinz; Hollender, Juliane

2016-03-01

Online solid-phase extraction was combined with nano-liquid chromatography coupled to high-resolution mass spectrometry (HRMS) for the analysis of micropollutants in environmental samples from small volumes. The method was validated in surface water, Microcystis aeruginosa cell lysate, and spent Microcystis growth medium. For 41 analytes, quantification limits of 0.1-28 ng/L (surface water) and 0.1-32 ng/L (growth medium) were obtained from only 88 μL of sample. In cell lysate, quantification limits ranged from 0.1-143 ng/L or 0.33-476 ng/g dry weight from a sample of 88 μL, or 26 μg dry weight, respectively. The method matches the sensitivity of established online and offline solid-phase extraction-liquid chromatography-mass spectrometry methods but requires only a fraction of the sample used by those techniques, and is among the first applications of nano-LC-MS for environmental analysis. The method was applied to the determination of bioconcentration in Microcystis aeruginosa in a laboratory experiment, and the benefit of coupling to HRMS was demonstrated in a transformation product screening.

Analysis of iodinated haloacetic acids in drinking water by reversed-phase liquid chromatography/electrospray ionization/tandem mass spectrometry with large volume direct aqueous injection.

PubMed

Li, Yongtao; Whitaker, Joshua S; McCarty, Christina L

2012-07-06

A large volume direct aqueous injection method was developed for the analysis of iodinated haloacetic acids in drinking water by using reversed-phase liquid chromatography/electrospray ionization/tandem mass spectrometry in the negative ion mode. Both the external and internal standard calibration methods were studied for the analysis of monoiodoacetic acid, chloroiodoacetic acid, bromoiodoacetic acid, and diiodoacetic acid in drinking water. The use of a divert valve technique for the mobile phase solvent delay, along with isotopically labeled analogs used as internal standards, effectively reduced and compensated for the ionization suppression typically caused by coexisting common inorganic anions. Under the optimized method conditions, the mean absolute and relative recoveries resulting from the replicate fortified deionized water and chlorinated drinking water analyses were 83-107% with a relative standard deviation of 0.7-11.7% and 84-111% with a relative standard deviation of 0.8-12.1%, respectively. The method detection limits resulting from the external and internal standard calibrations, based on seven fortified deionized water replicates, were 0.7-2.3 ng/L and 0.5-1.9 ng/L, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Method optimization for non-equilibrium solid phase microextraction sampling of HAPs for GC/MS analysis

NASA Astrophysics Data System (ADS)

Zawadowicz, M. A.; Del Negro, L. A.

2010-12-01

Hazardous air pollutants (HAPs) are usually present in the atmosphere at pptv-level, requiring measurements with high sensitivity and minimal contamination. Commonly used evacuated canister methods require an overhead in space, money and time that often is prohibitive to primarily-undergraduate institutions. This study optimized an analytical method based on solid-phase microextraction (SPME) of ambient gaseous matrix, which is a cost-effective technique of selective VOC extraction, accessible to an unskilled undergraduate. Several approaches to SPME extraction and sample analysis were characterized and several extraction parameters optimized. Extraction time, temperature and laminar air flow velocity around the fiber were optimized to give highest signal and efficiency. Direct, dynamic extraction of benzene from a moving air stream produced better precision (±10%) than sampling of stagnant air collected in a polymeric bag (±24%). Using a low-polarity chromatographic column in place of a standard (5%-Phenyl)-methylpolysiloxane phase decreased the benzene detection limit from 2 ppbv to 100 pptv. The developed method is simple and fast, requiring 15-20 minutes per extraction and analysis. It will be field-validated and used as a field laboratory component of various undergraduate Chemistry and Environmental Studies courses.

Aqueous nitrite ion determination by selective reduction and gas phase nitric oxide chemiluminescence

NASA Technical Reports Server (NTRS)

Dunham, A. J.; Barkley, R. M.; Sievers, R. E.; Clarkson, T. W. (Principal Investigator)

1995-01-01

An improved method of flow injection analysis for aqueous nitrite ion exploits the sensitivity and selectivity of the nitric oxide (NO) chemilluminescence detector. Trace analysis of nitrite ion in a small sample (5-160 microL) is accomplished by conversion of nitrite ion to NO by aqueous iodide in acid. The resulting NO is transported to the gas phase through a semipermeable membrane and subsequently detected by monitoring the photoemission of the reaction between NO and ozone (O3). Chemiluminescence detection is selective for measurement of NO, and, since the detection occurs in the gas-phase, neither sample coloration nor turbidity interfere. The detection limit for a 100-microL sample is 0.04 ppb of nitrite ion. The precision at the 10 ppb level is 2% relative standard deviation, and 60-180 samples can be analyzed per hour. Samples of human saliva and food extracts were analyzed; the results from a standard colorimetric measurement are compared with those from the new chemiluminescence method in order to further validate the latter method. A high degree of selectivity is obtained due to the three discriminating steps in the process: (1) the nitrite ion to NO conversion conditions are virtually specific for nitrite ion, (2) only volatile products of the conversion will be swept to the gas phase (avoiding turbidity or color in spectrophotometric methods), and (3) the NO chemiluminescence detector selectively detects the emission from the NO + O3 reaction. The method is free of interferences, offers detection limits of low parts per billion of nitrite ion, and allows the analysis of up to 180 microL-sized samples per hour, with little sample preparation and no chromatographic separation. Much smaller samples can be analyzed by this method than in previously reported batch analysis methods, which typically require 5 mL or more of sample and often need chromatographic separations as well.

Digital Speckle Photography of Subpixel Displacements of Speckle Structures Based on Analysis of Their Spatial Spectra

NASA Astrophysics Data System (ADS)

Maksimova, L. A.; Ryabukho, P. V.; Mysina, N. Yu.; Lyakin, D. V.; Ryabukho, V. P.

2018-04-01

We have investigated the capabilities of the method of digital speckle interferometry for determining subpixel displacements of a speckle structure formed by a displaceable or deformable object with a scattering surface. An analysis of spatial spectra of speckle structures makes it possible to perform measurements with a subpixel accuracy and to extend the lower boundary of the range of measurements of displacements of speckle structures to the range of subpixel values. The method is realized on the basis of digital recording of the images of undisplaced and displaced speckle structures, their spatial frequency analysis using numerically specified constant phase shifts, and correlation analysis of spatial spectra of speckle structures. Transformation into the frequency range makes it possible to obtain quantities to be measured with a subpixel accuracy from the shift of the interference-pattern minimum in the diffraction halo by introducing an additional phase shift into the complex spatial spectrum of the speckle structure or from the slope of the linear plot of the function of accumulated phase difference in the field of the complex spatial spectrum of the displaced speckle structure. The capabilities of the method have been investigated in natural experiment.

Mediating the Cognitive Walkthrough with Patient Groups to achieve Personalized Health in Chronic Disease Self-Management System Evaluation.

PubMed

Georgsson, Mattias; Kushniruk, Andre

2016-01-01

The cognitive walkthrough (CW) is a task-based, expert inspection usability evaluation method involving benefits such as cost effectiveness and efficiency. A drawback of the method is that it doesn't involve the user perspective from real users but instead is based on experts' predictions about the usability of the system and how users interact. In this paper, we propose a way of involving the user in an expert evaluation method by modifying the CW with patient groups as mediators. This along with other modifications include a dual domain session facilitator, specific patient groups and three different phases: 1) a preparation phase where suitable tasks are developed by a panel of experts and patients, validated through the content validity index 2) a patient user evaluation phase including an individual and collaborative process part 3) an analysis and coding phase where all data is digitalized and synthesized making use of Qualitative Data Analysis Software (QDAS) to determine usability deficiencies. We predict that this way of evaluating will utilize the benefits of the expert methods, also providing a way of including the patient user of these self-management systems. Results from this prospective study should provide evidence of the usefulness of this method modification.

From expert-derived user needs to user-perceived ease of use and usefulness: a two-phase mixed-methods evaluation framework.

PubMed

Boland, Mary Regina; Rusanov, Alexander; So, Yat; Lopez-Jimenez, Carlos; Busacca, Linda; Steinman, Richard C; Bakken, Suzanne; Bigger, J Thomas; Weng, Chunhua

2014-12-01

Underspecified user needs and frequent lack of a gold standard reference are typical barriers to technology evaluation. To address this problem, this paper presents a two-phase evaluation framework involving usability experts (phase 1) and end-users (phase 2). In phase 1, a cross-system functionality alignment between expert-derived user needs and system functions was performed to inform the choice of "the best available" comparison system to enable a cognitive walkthrough in phase 1 and a comparative effectiveness evaluation in phase 2. During phase 2, five quantitative and qualitative evaluation methods are mixed to assess usability: time-motion analysis, software log, questionnaires - System Usability Scale and the Unified Theory of Acceptance of Use of Technology, think-aloud protocols, and unstructured interviews. Each method contributes data for a unique measure (e.g., time motion analysis contributes task-completion-time; software log contributes action transition frequency). The measures are triangulated to yield complementary insights regarding user-perceived ease-of-use, functionality integration, anxiety during use, and workflow impact. To illustrate its use, we applied this framework in a formative evaluation of a software called Integrated Model for Patient Care and Clinical Trials (IMPACT). We conclude that this mixed-methods evaluation framework enables an integrated assessment of user needs satisfaction and user-perceived usefulness and usability of a novel design. This evaluation framework effectively bridges the gap between co-evolving user needs and technology designs during iterative prototyping and is particularly useful when it is difficult for users to articulate their needs for technology support due to the lack of a baseline. Copyright © 2013 Elsevier Inc. All rights reserved.

Fractionated-combustion analysis of carbonate-containing phases in composite materials of the hydroxyapatite-calcium carbonate system

NASA Astrophysics Data System (ADS)

Goldberg, M. A.; Shibaeva, T. V.; Smirnov, V. V.; Kutsev, S. V.; Barinov, S. M.; Grigorovich, K. V.

2012-12-01

Materials in the hydroxyapatite (HA)-calcium carbonate (CC) system were synthesized by a precipitation method from aqueous solutions. According to the data of X-ray phase analysis and IR spectroscopy, the powders consisted of CC and AB-type carbonate-substituted HA (CHA). In order to determine the content of carbonate-containing phases in materials, the temperature-temporal mode of fractionated-combustion analysis of carbon was developed. The quantitative phase ratios and the degree of substitution of carbonate groups in CHA were determined. It was shown that the degree of substitution of carbonate groups in CHA increased from 2.47 to 5.31 wt % as the CC content increased from 13.50 to 88.33 wt %.

Quantification of susceptibility change at high-concentrated SPIO-labeled target by characteristic phase gradient recognition.

PubMed

Zhu, Haitao; Nie, Binbin; Liu, Hua; Guo, Hua; Demachi, Kazuyuki; Sekino, Masaki; Shan, Baoci

2016-05-01

Phase map cross-correlation detection and quantification may produce highlighted signal at superparamagnetic iron oxide nanoparticles, and distinguish them from other hypointensities. The method may quantify susceptibility change by performing least squares analysis between a theoretically generated magnetic field template and an experimentally scanned phase image. Because characteristic phase recognition requires the removal of phase wrap and phase background, additional steps of phase unwrapping and filtering may increase the chance of computing error and enlarge the inconsistence among algorithms. To solve problem, phase gradient cross-correlation and quantification method is developed by recognizing characteristic phase gradient pattern instead of phase image because phase gradient operation inherently includes unwrapping and filtering functions. However, few studies have mentioned the detectable limit of currently used phase gradient calculation algorithms. The limit may lead to an underestimation of large magnetic susceptibility change caused by high-concentrated iron accumulation. In this study, mathematical derivation points out the value of maximum detectable phase gradient calculated by differential chain algorithm in both spatial and Fourier domain. To break through the limit, a modified quantification method is proposed by using unwrapped forward differentiation for phase gradient generation. The method enlarges the detectable range of phase gradient measurement and avoids the underestimation of magnetic susceptibility. Simulation and phantom experiments were used to quantitatively compare different methods. In vivo application performs MRI scanning on nude mice implanted by iron-labeled human cancer cells. Results validate the limit of detectable phase gradient and the consequent susceptibility underestimation. Results also demonstrate the advantage of unwrapped forward differentiation compared with differential chain algorithms for susceptibility quantification at high-concentrated iron accumulation. Copyright © 2015 Elsevier Inc. All rights reserved.

Freud: a software suite for high-throughput simulation analysis

NASA Astrophysics Data System (ADS)

Harper, Eric; Spellings, Matthew; Anderson, Joshua; Glotzer, Sharon

Computer simulation is an indispensable tool for the study of a wide variety of systems. As simulations scale to fill petascale and exascale supercomputing clusters, so too does the size of the data produced, as well as the difficulty in analyzing these data. We present Freud, an analysis software suite for efficient analysis of simulation data. Freud makes no assumptions about the system being analyzed, allowing for general analysis methods to be applied to nearly any type of simulation. Freud includes standard analysis methods such as the radial distribution function, as well as new methods including the potential of mean force and torque and local crystal environment analysis. Freud combines a Python interface with fast, parallel C + + analysis routines to run efficiently on laptops, workstations, and supercomputing clusters. Data analysis on clusters reduces data transfer requirements, a prohibitive cost for petascale computing. Used in conjunction with simulation software, Freud allows for smart simulations that adapt to the current state of the system, enabling the study of phenomena such as nucleation and growth, intelligent investigation of phases and phase transitions, and determination of effective pair potentials.

Single and two-shot quantitative phase imaging using Hilbert-Huang Transform based fringe pattern analysis

NASA Astrophysics Data System (ADS)

Trusiak, Maciej; Micó, Vicente; Patorski, Krzysztof; García-Monreal, Javier; Sluzewski, Lukasz; Ferreira, Carlos

2016-08-01

In this contribution we propose two Hilbert-Huang Transform based algorithms for fast and accurate single-shot and two-shot quantitative phase imaging applicable in both on-axis and off-axis configurations. In the first scheme a single fringe pattern containing information about biological phase-sample under study is adaptively pre-filtered using empirical mode decomposition based approach. Further it is phase demodulated by the Hilbert Spiral Transform aided by the Principal Component Analysis for the local fringe orientation estimation. Orientation calculation enables closed fringes efficient analysis and can be avoided using arbitrary phase-shifted two-shot Gram-Schmidt Orthonormalization scheme aided by Hilbert-Huang Transform pre-filtering. This two-shot approach is a trade-off between single-frame and temporal phase shifting demodulation. Robustness of the proposed techniques is corroborated using experimental digital holographic microscopy studies of polystyrene micro-beads and red blood cells. Both algorithms compare favorably with the temporal phase shifting scheme which is used as a reference method.

Method Development for the Analysis of 1,4-Dioxane in Drinking Water Using Solid Phase Extraction and Gas Chromatography/Mass Spectrometry

EPA Science Inventory

1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of...

Biomechanical analysis using FEA and experiments of a standard plate method versus three cable methods for fixing acetabular fractures with simultaneous THA.

PubMed

Aziz, Mina S R; Dessouki, Omar; Samiezadeh, Saeid; Bougherara, Habiba; Schemitsch, Emil H; Zdero, Radovan

2017-08-01

Acetabular fractures potentially account for up to half of all pelvic fractures, while pelvic fractures potentially account for over one-tenth of all human bone fractures. This is the first biomechanical study to assess acetabular fracture fixation using plates versus cables in the presence of a total hip arthroplasty, as done for the elderly. In Phase 1, finite element (FE) models compared a standard plate method versus 3 cable methods for repairing an acetabular fracture (type: anterior column plus posterior hemi-transverse) subjected to a physiological-type compressive load of 2207N representing 3 x body weight for a 75kg person during walking. FE stress maps were compared to choose the most mechanically stable cable method, i.e. lowest peak bone stress. In Phase 2, mechanical tests were then done in artificial hemipelvises to compare the standard plate method versus the optimal cable method selected from Phase 1. FE analysis results showed peak bone stresses of 255MPa (Plate method), 205MPa (Mears cable method), 250MPa (Kang cable method), and 181MPa (Mouhsine cable method). Mechanical tests then showed that the Plate method versus the Mouhsine cable method selected from Phase 1 had higher stiffness (662versus 385N/mm, p=0.001), strength (3210versus 2060N, p=0.009), and failure energy (8.8versus 6.2J, p=0.002), whilst they were statistically equivalent for interfragmentary sliding (p≥0.179) and interfragmentary gapping (p≥0.08). The Plate method had superior mechanical properties, but the Mouhsine cable method may be a reasonable alternative if osteoporosis prevents good screw thread interdigitation during plating. Copyright © 2017 IPEM. Published by Elsevier Ltd. All rights reserved.

Modifications Of Discrete Ordinate Method For Computations With High Scattering Anisotropy: Comparative Analysis

NASA Technical Reports Server (NTRS)

Korkin, Sergey V.; Lyapustin, Alexei I.; Rozanov, Vladimir V.

2012-01-01

A numerical accuracy analysis of the radiative transfer equation (RTE) solution based on separation of the diffuse light field into anisotropic and smooth parts is presented. The analysis uses three different algorithms based on the discrete ordinate method (DOM). Two methods, DOMAS and DOM2+, that do not use the truncation of the phase function, are compared against the TMS-method. DOMAS and DOM2+ use the Small-Angle Modification of RTE and the single scattering term, respectively, as an anisotropic part. The TMS method uses Delta-M method for truncation of the phase function along with the single scattering correction. For reference, a standard discrete ordinate method, DOM, is also included in analysis. The obtained results for cases with high scattering anisotropy show that at low number of streams (16, 32) only DOMAS provides an accurate solution in the aureole area. Outside of the aureole, the convergence and accuracy of DOMAS, and TMS is found to be approximately similar: DOMAS was found more accurate in cases with coarse aerosol and liquid water cloud models, except low optical depth, while the TMS showed better results in case of ice cloud.

Development of a sensitive and rapid method for rifampicin impurity analysis using supercritical fluid chromatography.

PubMed

Li, Wei; Wang, Jun; Yan, Zheng-Yu

2015-10-10

A novel simple, fast and efficient supercritical fluid chromatography (SFC) method was developed and compared with RPLC method for the separation and determination of impurities in rifampicin. The separation was performed using a packed diol column and a mobile phase B (modifier) consisting of methanol with 0.1% ammonium formate (w/v) and 2% water (v/v). Overall satisfactory resolutions and peak shapes for rifampicin quinone (RQ), rifampicin (RF), rifamycin SV (RSV), rifampicin N-oxide (RNO) and 3-formylrifamycinSV (3-FR) were obtained by optimization of the chromatography system. With gradient elution of mobile phase, all of the impurities and the active were separated within 4 min. Taking full advantage of features of SFC (such as particular selectivity, non-sloping baseline in gradient elution, and without injection solvent effects), the method was successfully used for determination of impurities in rifampicin, with more impurity peaks detected, better resolution achieved and much less analysis time needed compared with conventional reversed-phase liquid chromatography (RPLC) methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative characterization of the spatial distribution of particles in materials: Application to materials processing

NASA Technical Reports Server (NTRS)

Parse, Joseph B.; Wert, J. A.

1991-01-01

Inhomogeneities in the spatial distribution of second phase particles in engineering materials are known to affect certain mechanical properties. Progress in this area has been hampered by the lack of a convenient method for quantitative description of the spatial distribution of the second phase. This study intends to develop a broadly applicable method for the quantitative analysis and description of the spatial distribution of second phase particles. The method was designed to operate on a desktop computer. The Dirichlet tessellation technique (geometrical method for dividing an area containing an array of points into a set of polygons uniquely associated with the individual particles) was selected as the basis of an analysis technique implemented on a PC. This technique is being applied to the production of Al sheet by PM processing methods; vacuum hot pressing, forging, and rolling. The effect of varying hot working parameters on the spatial distribution of aluminum oxide particles in consolidated sheet is being studied. Changes in distributions of properties such as through-thickness near-neighbor distance correlate with hot-working reduction.

Weighted least squares phase unwrapping based on the wavelet transform

NASA Astrophysics Data System (ADS)

Chen, Jiafeng; Chen, Haiqin; Yang, Zhengang; Ren, Haixia

2007-01-01

The weighted least squares phase unwrapping algorithm is a robust and accurate method to solve phase unwrapping problem. This method usually leads to a large sparse linear equation system. Gauss-Seidel relaxation iterative method is usually used to solve this large linear equation. However, this method is not practical due to its extremely slow convergence. The multigrid method is an efficient algorithm to improve convergence rate. However, this method needs an additional weight restriction operator which is very complicated. For this reason, the multiresolution analysis method based on the wavelet transform is proposed. By applying the wavelet transform, the original system is decomposed into its coarse and fine resolution levels and an equivalent equation system with better convergence condition can be obtained. Fast convergence in separate coarse resolution levels speeds up the overall system convergence rate. The simulated experiment shows that the proposed method converges faster and provides better result than the multigrid method.

Polarization-phase tomography of biological fluids polycrystalline structure

NASA Astrophysics Data System (ADS)

Dubolazov, A. V.; Vanchuliak, O. Ya.; Garazdiuk, M.; Sidor, M. I.; Motrich, A. V.; Kostiuk, S. V.

2013-12-01

Our research is aimed at designing an experimental method of Fourier's laser polarization phasometry of the layers of human effusion for an express diagnostics during surgery and a differentiation of the degree of severity (acute - gangrenous) appendectomy by means of statistical, correlation and fractal analysis of the coherent scattered field. A model of generalized optical anisotropy of polycrystal networks of albumin and globulin of the effusion of appendicitis has been suggested and the method of Fourier's phasometry of linear (a phase shift between the orthogonal components of the laser wave amplitude) and circular (the angle of rotation of the polarization plane) birefringence with a spatial-frequency selection of the coordinate distributions for the differentiation of acute and gangrenous conditions have been analytically substantiated. Comparative studies of the efficacy of the methods of direct mapping of phase distributions and Fourier's phasometry of a laser radiation field transformed by the dendritic and spherolitic networks of albumin and globulin of the layers of effusion of appendicitis on the basis of complex statistical, correlation and fractal analysis of the structure of phase maps.

Using the Image Analysis Method for Describing Soil Detachment by a Single Water Drop Impact

PubMed Central

Ryżak, Magdalena; Bieganowski, Andrzej

2012-01-01

The aim of the present work was to develop a method based on image analysis for describing soil detachment caused by the impact of a single water drop. The method consisted of recording tracks made by splashed particles on blotting paper under an optical microscope. The analysis facilitated division of the recorded particle tracks on the paper into drops, “comets” and single particles. Additionally, the following relationships were determined: (i) the distances of splash; (ii) the surface areas of splash tracks into relation to distance; (iii) the surface areas of the solid phase transported over a given distance; and (iv) the ratio of the solid phase to the splash track area in relation to distance. Furthermore, the proposed method allowed estimation of the weight of soil transported by a single water drop splash in relation to the distance of the water drop impact. It was concluded that the method of image analysis of splashed particles facilitated analysing the results at very low water drop energy and generated by single water drops.

Purification of Derivatized Oligosaccharides by Solid Phase Extraction for Glycomic Analysis

PubMed Central

Zhang, Qiwei; Li, Henghui; Feng, Xiaojun; Liu, Bi-Feng; Liu, Xin

2014-01-01

Profiling of glycans released from proteins is very complex and important. To enhance the detection sensitivity, chemical derivatization is required for the analysis of carbohydrates. Due to the interference of excess reagents, a simple and reliable purification method is usually necessary for the derivatized oligosaccharides. Various SPE based methods have been applied for the clean-up process. To demonstrate the differences among these methods, seven types of self-packed SPE cartridges were systematically compared in this study. The optimized conditions were determined for each type of cartridge and it was found that microcrystalline cellulose was the most appropriate SPE material for the purification of derivatized oligosaccharide. Normal phase HPLC analysis of the derivatized maltoheptaose was realized with a detection limit of 0.12 pmol (S N−1 = 3) and a recovery over 70%. With the optimized SPE method, relative quantification analysis of N-glycans from model glycoproteins were carried out accurately and over 40 N-glycans from human serum samples were determined regardless of the isomers. Due to the high stability and sensitivity, microcrystalline cellulose cartridge showed potential applications in glycomics analysis. PMID:24705408

A numerical analysis of phase-change problems including natural convection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cao, Y.; Faghri, A.

1990-08-01

Fixed grid solutions for phase-change problems remove the need to satisfy conditions at the phase-change front and can be easily extended to multidimensional problems. The two most important and widely used methods are enthalpy methods and temperature-based equivalent heat capacity methods. Both methods in this group have advantages and disadvantages. Enthalpy methods (Shamsundar and Sparrow, 1975; Voller and Prakash, 1987; Cao et al., 1989) are flexible and can handle phase-change problems occurring both at a single temperature and over a temperature range. The drawback of this method is that although the predicted temperature distributions and melting fronts are reasonable, themore » predicted time history of the temperature at a typical grid point may have some oscillations. The temperature-based fixed grid methods (Morgan, 1981; Hsiao and Chung, 1984) have no such time history problems and are more convenient with conjugate problems involving an adjacent wall, but have to deal with the severe nonlinearity of the governing equations when the phase-change temperature range is small. In this paper, a new temperature-based fixed-grid formulation is proposed, and the reason that the original equivalent heat capacity model is subject to such restrictions on the time step, mesh size, and the phase-change temperature range will also be discussed.« less

A simple method for plasma total vitamin C analysis suitable for routine clinical laboratory use.

PubMed

Robitaille, Line; Hoffer, L John

2016-04-21

In-hospital hypovitaminosis C is highly prevalent but almost completely unrecognized. Medical awareness of this potentially important disorder is hindered by the inability of most hospital laboratories to determine plasma vitamin C concentrations. The availability of a simple, reliable method for analyzing plasma vitamin C could increase opportunities for routine plasma vitamin C analysis in clinical medicine. Plasma vitamin C can be analyzed by high performance liquid chromatography (HPLC) with electrochemical (EC) or ultraviolet (UV) light detection. We modified existing UV-HPLC methods for plasma total vitamin C analysis (the sum of ascorbic and dehydroascorbic acid) to develop a simple, constant-low-pH sample reduction procedure followed by isocratic reverse-phase HPLC separation using a purely aqueous low-pH non-buffered mobile phase. Although EC-HPLC is widely recommended over UV-HPLC for plasma total vitamin C analysis, the two methods have never been directly compared. We formally compared the simplified UV-HPLC method with EC-HPLC in 80 consecutive clinical samples. The simplified UV-HPLC method was less expensive, easier to set up, required fewer reagents and no pH adjustments, and demonstrated greater sample stability than many existing methods for plasma vitamin C analysis. When compared with the gold-standard EC-HPLC method in 80 consecutive clinical samples exhibiting a wide range of plasma vitamin C concentrations, it performed equivalently. The easy set up, simplicity and sensitivity of the plasma vitamin C analysis method described here could make it practical in a normally equipped hospital laboratory. Unlike any prior UV-HPLC method for plasma total vitamin C analysis, it was rigorously compared with the gold-standard EC-HPLC method and performed equivalently. Adoption of this method could increase the availability of plasma vitamin C analysis in clinical medicine.

Simultaneous separation by reversed-phase high-performance liquid chromatography and mass spectral identification of anthocyanins and flavonols in Shiraz grape skin.

PubMed

Downey, Mark O; Rochfort, Simone

2008-08-01

A limitation of large-scale viticultural trials is the time and cost of comprehensive compositional analysis of the fruit by high-performance liquid chromatography (HPLC). In addition, separate methods have generally been required to identify and quantify different classes of metabolites. To address these shortcomings a reversed-phase HPLC method was developed to simultaneously separate the anthocyanins and flavonols present in grape skins. The method employs a methanol and water gradient acidified with 10% formic acid with a run-time of 48 min including re-equilibration. Identity of anthocyanins and flavonols in Shiraz (Vitis vinifera L.) skin was confirmed by mass spectral analysis.

An accurate cost effective DFT approach to study the sensing behaviour of polypyrrole towards nitrate ions in gas and aqueous phases.

PubMed

Wasim, Fatima; Mahmood, Tariq; Ayub, Khurshid

2016-07-28

Density functional theory (DFT) calculations have been performed to study the response of polypyrrole towards nitrate ions in gas and aqueous phases. First, an accurate estimate of interaction energies is obtained by methods calibrated against the gold standard CCSD(T) method. Then, a number of low cost DFT methods are also evaluated for their ability to accurately estimate the binding energies of polymer-nitrate complexes. The low cost methods evaluated here include dispersion corrected potential (DCP), Grimme's D3 correction, counterpoise correction of the B3LYP method, and Minnesota functionals (M05-2X). The interaction energies calculated using the counterpoise (CP) correction and DCP methods at the B3LYP level are in better agreement with the interaction energies calculated using the calibrated methods. The interaction energies of an infinite polymer (polypyrrole) with nitrate ions are calculated by a variety of low cost methods in order to find the associated errors. The electronic and spectroscopic properties of polypyrrole oligomers nPy (where n = 1-9) and nPy-NO3(-) complexes are calculated, and then extrapolated for an infinite polymer through a second degree polynomial fit. Charge analysis, frontier molecular orbital (FMO) analysis and density of state studies also reveal the sensing ability of polypyrrole towards nitrate ions. Interaction energies, charge analysis and density of states analyses illustrate that the response of polypyrrole towards nitrate ions is considerably reduced in the aqueous medium (compared to the gas phase).

Harmonic reduction of Direct Torque Control of six-phase induction motor.

PubMed

Taheri, A

2016-07-01

In this paper, a new switching method in Direct Torque Control (DTC) of a six-phase induction machine for reduction of current harmonics is introduced. Selecting a suitable vector in each sampling period is an ordinal method in the ST-DTC drive of a six-phase induction machine. The six-phase induction machine has 64 voltage vectors and divided further into four groups. In the proposed DTC method, the suitable voltage vectors are selected from two vector groups. By a suitable selection of two vectors in each sampling period, the harmonic amplitude is decreased more, in and various comparison to that of the ST-DTC drive. The harmonics loss is greater reduced, while the electromechanical energy is decreased with switching loss showing a little increase. Spectrum analysis of the phase current in the standard and new switching table DTC of the six-phase induction machine and determination for the amplitude of each harmonics is proposed in this paper. The proposed method has a less sampling time in comparison to the ordinary method. The Harmonic analyses of the current in the low and high speed shows the performance of the presented method. The simplicity of the proposed method and its implementation without any extra hardware is other advantages of the proposed method. The simulation and experimental results show the preference of the proposed method. Copyright © 2016 ISA. Published by Elsevier Ltd. All rights reserved.

A combined long-range phasing and long haplotype imputation method to impute phase for SNP genotypes

PubMed Central

2011-01-01

Background Knowing the phase of marker genotype data can be useful in genome-wide association studies, because it makes it possible to use analysis frameworks that account for identity by descent or parent of origin of alleles and it can lead to a large increase in data quantities via genotype or sequence imputation. Long-range phasing and haplotype library imputation constitute a fast and accurate method to impute phase for SNP data. Methods A long-range phasing and haplotype library imputation algorithm was developed. It combines information from surrogate parents and long haplotypes to resolve phase in a manner that is not dependent on the family structure of a dataset or on the presence of pedigree information. Results The algorithm performed well in both simulated and real livestock and human datasets in terms of both phasing accuracy and computation efficiency. The percentage of alleles that could be phased in both simulated and real datasets of varying size generally exceeded 98% while the percentage of alleles incorrectly phased in simulated data was generally less than 0.5%. The accuracy of phasing was affected by dataset size, with lower accuracy for dataset sizes less than 1000, but was not affected by effective population size, family data structure, presence or absence of pedigree information, and SNP density. The method was computationally fast. In comparison to a commonly used statistical method (fastPHASE), the current method made about 8% less phasing mistakes and ran about 26 times faster for a small dataset. For larger datasets, the differences in computational time are expected to be even greater. A computer program implementing these methods has been made available. Conclusions The algorithm and software developed in this study make feasible the routine phasing of high-density SNP chips in large datasets. PMID:21388557

Dehydration of detomidine hydrochloride monohydrate.

PubMed

Veldre, K; Actiņš, A; Jaunbergs, J

2011-10-09

The thermodynamic stability of detomidine hydrochloride monohydrate has been evaluated on the basis of phase transition kinetics in solid state. A method free of empirical models was used for the treatment of kinetic data, and compared to several known solid state kinetic data processing methods. Phase transitions were monitored by powder X-ray diffraction (PXRD) and thermal analysis. Full PXRD profiles were used for determining the phase content instead of single reflex intensity measurements, in order to minimize the influence of particle texture. We compared the applicability of isothermal and nonisothermal methods to our investigation of detomidine hydrochlorine monohydrate dehydration. Copyright © 2011 Elsevier B.V. All rights reserved.

Optomechanical design and analysis of a self-adaptive mounting method for optimizing phase matching of large potassium dihydrogen phosphate converter

NASA Astrophysics Data System (ADS)

Zhang, Zheng; Tian, Menjiya; Quan, Xusong; Pei, Guoqing; Wang, Hui; Liu, Tianye; Long, Kai; Xiong, Zhao; Rong, Yiming

2017-11-01

Surface control and phase matching of large laser conversion optics are urgent requirements and huge challenges in high-power solid-state laser facilities. A self-adaptive, nanocompensating mounting configuration of a large aperture potassium dihydrogen phosphate (KDP) frequency doubler is proposed based on a lever-type surface correction mechanism. A mechanical, numerical, and optical model is developed and employed to evaluate comprehensive performance of this mounting method. The results validate the method's advantages of surface adjustment and phase matching improvement. In addition, the optimal value of the modulation force is figured out through a series of simulations and calculations.

Development and Validation of an HPLC Method for Karanjin in Pongamia pinnata linn. Leaves.

PubMed

Katekhaye, S; Kale, M S; Laddha, K S

2012-01-01

A rapid, simple and specific reversed-phase HPLC method has been developed for analysis of karanjin in Pongamia pinnata Linn. leaves. HPLC analysis was performed on a C(18) column using an 85:13.5:1.5 (v/v) mixtures of methanol, water and acetic acid as isocratic mobile phase at a flow rate of 1 ml/min. UV detection was at 300 nm. The method was validated for accuracy, precision, linearity, specificity. Validation revealed the method is specific, accurate, precise, reliable and reproducible. Good linear correlation coefficients (r(2)>0.997) were obtained for calibration plots in the ranges tested. Limit of detection was 4.35 μg and limit of quantification was 16.56 μg. Intra and inter-day RSD of retention times and peak areas was less than 1.24% and recovery was between 95.05 and 101.05%. The established HPLC method is appropriate enabling efficient quantitative analysis of karanjin in Pongamia pinnata leaves.

Development and Validation of an HPLC Method for Karanjin in Pongamia pinnata linn. Leaves

PubMed Central

Katekhaye, S; Kale, M. S.; Laddha, K. S.

2012-01-01

A rapid, simple and specific reversed-phase HPLC method has been developed for analysis of karanjin in Pongamia pinnata Linn. leaves. HPLC analysis was performed on a C18 column using an 85:13.5:1.5 (v/v) mixtures of methanol, water and acetic acid as isocratic mobile phase at a flow rate of 1 ml/min. UV detection was at 300 nm. The method was validated for accuracy, precision, linearity, specificity. Validation revealed the method is specific, accurate, precise, reliable and reproducible. Good linear correlation coefficients (r2>0.997) were obtained for calibration plots in the ranges tested. Limit of detection was 4.35 μg and limit of quantification was 16.56 μg. Intra and inter-day RSD of retention times and peak areas was less than 1.24% and recovery was between 95.05 and 101.05%. The established HPLC method is appropriate enabling efficient quantitative analysis of karanjin in Pongamia pinnata leaves. PMID:23204626

Topologically Close-packed Phase Formation in High Entropy Alloys: A Review of Calphad and Experimental Results

NASA Astrophysics Data System (ADS)

Guruvidyathri, K.; Hari Kumar, K. C.; Yeh, J. W.; Murty, B. S.

2017-11-01

One of the major challenges in high entropy alloy (HEA) research is to obtain single-phase solid solutions by proper selection of components and processing techniques. Often one encounters situations where topologically close-packed (TCP) phases are present in the HEA microstructures. TCP phases are a class of intermetallic phases that are in general considered undesirable. The ability to predict these phases in HEAs using the Calphad (CALculation of PHAse Diagrams) method has been shown to accelerate the identification of promising compositions. In this review, an analysis of the reported Calphad studies and corresponding microstructural information on HEAs is done to evaluate the success of the Calphad method for TCP phases. A total of 52 alloys with 123 post-heat treatment microstructures reported so far have been compared. Challenges and issues in experiments and calculations are brought out with a possible way forward.

Inferring cardiac phase response curve in vivo

NASA Astrophysics Data System (ADS)

Pikovsky, Arkady; Kralemann, Bjoern; Fruehwirth, Matthias; Rosenblum, Michael; Kenner, Thomas; Schaefer, Jochen; Moser, Maximilian

2014-03-01

Characterizing properties of biological oscillators with phase response cirves (PRC) is one of main theoretical tools in neuroscience, cardio-respiratory physiology, and chronobiology. We present a technique that allows the extraction of the PRC from a non-invasive observation of a system consisting of two interacting oscillators, in this case heartbeat and respiration, in its natural environment and under free-running conditions. We use this method to obtain the phase coupling functions describing cardio-respiratory interactions and the phase response curve of 17 healthy humans. We show at which phase the cardiac beat is susceptible to respiratory drive and extract the respiratory-related component of heart rate variability. This non-invasive method of bivariate data analysis for the determination of phase response curves of coupled oscillators may find application in other biological and physical systems.

A Two-Radius Circular Array Method: Extracting Independent Information on Phase Velocities of Love Waves From Microtremor Records From a Simple Seismic Array

NASA Astrophysics Data System (ADS)

Tada, T.; Cho, I.; Shinozaki, Y.

2005-12-01

We have invented a Two-Radius (TR) circular array method of microtremor exploration, an algorithm that enables to estimate phase velocities of Love waves by analyzing horizontal-component records of microtremors that are obtained with an array of seismic sensors placed around circumferences of two different radii. The data recording may be done either simultaneously around the two circles or in two separate sessions with sensors distributed around each circle. Both Rayleigh and Love waves are present in the horizontal components of microtremors, but in the data processing of our TR method, all information on the Rayleigh waves ends up cancelled out, and information on the Love waves alone are left to be analyzed. Also, unlike the popularly used frequency-wavenumber spectral (F-K) method, our TR method does not resolve individual plane-wave components arriving from different directions and analyze their "vector" phase velocities, but instead directly evaluates their "scalar" phase velocities --- phase velocities that contain no information on the arrival direction of waves --- through a mathematical procedure which involves azimuthal averaging. The latter feature leads us to expect that, with our TR method, it is possible to conduct phase velocity analysis with smaller numbers of sensors, with higher stability, and up to longer-wavelength ranges than with the F-K method. With a view to investigating the capabilities and limitations of our TR method in practical implementation to real data, we have deployed circular seismic arrays of different sizes at a test site in Japan where the underground structure is well documented through geophysical exploration. Ten seismic sensors were placed equidistantly around two circumferences, five around each circle, with varying combinations of radii ranging from several meters to several tens of meters, and simultaneous records of microtremors around circles of two different radii were analyzed with our TR method to produce estimates for the phase velocities of Love waves. The estimates were then checked against "model" phase velocities that are derived from theoretical calculations. We have also conducted a check of the estimated spectral ratios against the "model" spectral ratios, where we mean by "spectral ratio" an intermediary quantity that is calculated from observed records prior to the estimation of the phase velocity in the data analysis procedure of our TR method. In most cases, the estimated phase velocities coincided well with the model phase velocities within a wavelength range extending roughly from 3r to 6r (r: array radius). It was found out that, outside the upper and lower resolution limits of the TR method, the discrepancy between the estimated and model phase velocities, as well as the discrepancy between the estimated and model spectral ratios, were accounted for satisfactorily by theoretical consideration of three factors: the presence of higher surface-wave modes, directional aliasing effects related to the finite number of sensors in the seismic array, and the presence of incoherent noise.

Prospects for the application of radiometric methods in the measurement of two-phase flows

NASA Astrophysics Data System (ADS)

Zych, Marcin

2018-06-01

The article constitutes an overview of the application of radiometric methods in the research of two-phase flows: liquid-solid particles and liquid-gas flows. The methods which were used were described on the basis of the experiments which were conducted in the Water Laboratory of the Wrocław University of Environmental and Life Sciences and in the Sedimentological Laboratory of the Faculty of Geology, Geophysics and Environmental Protection, AGH-UST in Kraków. The advanced mathematical methods for the analysis of signals from scintillation probes that were applied enable the acquisition of a number of parameters associated with the flowing two-phase mixture, such as: average velocities of the particular phases, concentration of the solid phase, and void fraction for a liquid-gas mixture. Despite the fact that the application of radioactive sources requires considerable carefulness and a number of state permits, in many cases these sources become useful in the experiments which are presented.

[Absorption spectrum of Quasi-continuous laser modulation demodulation method].

PubMed

Shao, Xin; Liu, Fu-Gui; Du, Zhen-Hui; Wang, Wei

2014-05-01

A software phase-locked amplifier demodulation method is proposed in order to demodulate the second harmonic (2f) signal of quasi-continuous laser wavelength modulation spectroscopy (WMS) properly, based on the analysis of its signal characteristics. By judging the effectiveness of the measurement data, filter, phase-sensitive detection, digital filtering and other processing, the method can achieve the sensitive detection of quasi-continuous signal The method was verified by using carbon dioxide detection experiments. The WMS-2f signal obtained by the software phase-locked amplifier and the high-performance phase-locked amplifier (SR844) were compared simultaneously. The results show that the Allan variance of WMS-2f signal demodulated by the software phase-locked amplifier is one order of magnitude smaller than that demodulated by SR844, corresponding two order of magnitude lower of detection limit. And it is able to solve the unlocked problem caused by the small duty cycle of quasi-continuous modulation signal, with a small signal waveform distortion.

Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

USDA-ARS?s Scientific Manuscript database

A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was appli...

Development and validation of reverse phase high performance liquid chromatography for citral analysis from essential oils.

PubMed

Gaonkar, Roopa; Yallappa, S; Dhananjaya, B L; Hegde, Gurumurthy

2016-11-15

Citral is a widely used monoterpene aldehyde in aromatherapy, food and pesticide industries. A new validated reverse phase high performance liquid chromatography (RP - HPLC) procedure for the detection and quantification of cis-trans isomers of citral was developed. The RP-HPLC analysis was carried out using Enable C - 18G column (250×4.6mm, 5μ), with acetonitrile and water (70: 30) mobile phase in isocratic mode at 1mL/min flow. A photodiode array (PDA) detector was set at 233nm for the detection of citral. The method showed linearity, selectivity and accuracy for citral in the range of 3-100μg/mL. In order to compare the new RP-HPLC method with the available methods, one of the commercially available essential oil from Cymbopogon flexuosus was analyzed using new RP-HPLC method and the same was analyzed using GC-MS for the comparison of the method for the detection of citral. The GC-MS analysis was done using mass selective detector (MSD) showed citral content to be of 72.76%; wherein the new method showed to contain that same at 74.98%. To prove the application of the new method, essential oils were extracted from lemongrass, lemon leaves and mosambi peels by steam distillation. The citral content present in the essential and also in the condensate was analyzed. The method was found to be suitable for the analysis of citral in essential oils and water based citral formulations with a very good resolution of its components geranial and neral. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of Michelson interferometer based spatial phase-shift digital shearography

NASA Astrophysics Data System (ADS)

Xie, Xin

Digital shearography is a non-contact, full field, optical measurement method, which has the capability of directly measuring the gradient of deformation. For high measurement sensitivity, phase evaluation method has to be introduced into digital shearography by phase-shift technique. Catalog by phase-shift method, digital phase-shift shearography can be divided into Temporal Phase-Shift Digital Shearography (TPS-DS) and Spatial Phase-Shift Digital Shearography (SPS-DS). TPS-DS is the most widely used phase-shift shearography system, due to its simple algorithm, easy operation and good phase-map quality. However, the application of TPS-DS is only limited in static/step-by-step loading measurement situation, due to its multi-step shifting process. In order to measure the strain under dynamic/continuous loading situation, a SPS-DS system has to be developed. This dissertation aims to develop a series of Michelson Interferometer based SPS-DS measurement methods to achieve the strain measurement by using only a single pair of speckle pattern images. The Michelson Interferometer based SPS-DS systems utilize special designed optical setup to introduce extra carrier frequency into the laser wavefront. The phase information corresponds to the strain field can be separated on the Fourier domain using a Fourier Transform and can further be evaluated with a Windowed Inverse Fourier Transform. With different optical setups and carrier frequency arrangements, the Michelson Interferometer based SPS-DS method is capable to achieve a variety of measurement tasks using only single pair of speckle pattern images. Catalog by the aimed measurand, these capable measurement tasks can be divided into five categories: 1) measurement of out-of-plane strain field with small shearing amount; 2) measurement of relative out-of-plane deformation field with big shearing amount; 3) simultaneous measurement of relative out-of-plane deformation field and deformation gradient field by using multiple carrier frequencies; 4) simultaneous measurement of two directional strain field using dual measurement channels 5) measurement of pure in-plane strain and pure out-of-plane strain with multiple carrier frequencies. The basic theory, optical path analysis, preliminary studies, results analysis and research plan are shown in detail in this dissertation.

Modelling of Hydrophilic Interaction Liquid Chromatography Stationary Phases Using Chemometric Approaches

PubMed Central

Ortiz-Villanueva, Elena; Tauler, Romà

2017-01-01

Metabolomics is a powerful and widely used approach that aims to screen endogenous small molecules (metabolites) of different families present in biological samples. The large variety of compounds to be determined and their wide diversity of physical and chemical properties have promoted the development of different types of hydrophilic interaction liquid chromatography (HILIC) stationary phases. However, the selection of the most suitable HILIC stationary phase is not straightforward. In this work, four different HILIC stationary phases have been compared to evaluate their potential application for the analysis of a complex mixture of metabolites, a situation similar to that found in non-targeted metabolomics studies. The obtained chromatographic data were analyzed by different chemometric methods to explore the behavior of the considered stationary phases. ANOVA-simultaneous component analysis (ASCA), principal component analysis (PCA) and partial least squares regression (PLS) were used to explore the experimental factors affecting the stationary phase performance, the main similarities and differences among chromatographic conditions used (stationary phase and pH) and the molecular descriptors most useful to understand the behavior of each stationary phase. PMID:29064436

Extraction and determination of biogenic amines in fermented sausages and other meat products using reversed-phase-HPLC.

PubMed

Straub, B; Schollenberger, M; Kicherer, M; Luckas, B; Hammes, W P

1993-09-01

A convenient method is described for the analysis of biogenic amines (BA) by means of reversed-phase-HPLC. The method is characterized by multi-channel UV detection (diodearray), subsequent post-column derivatization with o-phthaldialdehyde and 3-mercaptopropionic acid, and fluorescence detection. For the analysis of meat products and especially fermented sausages an optimized perchloric acid extraction process was introduced to determine putrescine, cadaverine, histamine, tyramine and 2-phenylethylamine. BA recoveries from meat ranged between 96 and 113% with a detection limit for amines of 0.5 mg/kg.

Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Selvaraj, Mahalakshmi; Department of Material Science, School of Chemistry, Madurai Kamaraj University, Tamilnadu Madurai-625 021; Venkatachalapathy, V.

2015-11-15

Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO{sub 3}) nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C) employing barium dichloride (BaCl{sub 2}) and titanium tetrachloride (TiCl{sub 4}) as precursors and sodium hydroxide (NaOH) as mineralizer for synthesis of BaTiO{sub 3} nanopowders. The as-prepared BaTiO{sub 3} powders were investigated for structural characteristics using x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phasemore » directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula). SEM and TEM analysis verified that the BaTiO{sub 3} nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED) shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric) phases of undoped BaTiO{sub 3} nanopowders can be stabilized by the sol-hydrothermal method.« less

Fluorescence recovery after photo-bleaching as a method to determine local diffusion coefficient in the stratum corneum.

PubMed

Anissimov, Yuri G; Zhao, Xin; Roberts, Michael S; Zvyagin, Andrei V

2012-10-01

Fluorescence recovery after photo-bleaching experiments were performed in human stratum corneum in vitro. Fluorescence multiphoton tomography was used, which allowed the dimensions of the photobleached volume to be at the micron scale and located fully within the lipid phase of the stratum corneum. Analysis of the fluorescence recovery data with simplified mathematical models yielded the diffusion coefficient of small molecular weight organic fluorescent dye Rhodamine B in the stratum corneum lipid phase of about (3-6) × 10(-9)cm(2) s(-1). It was concluded that the presented method can be used for detailed analysis of localised diffusion coefficients in the stratum corneum phases for various fluorescent probes. Copyright © 2012 Elsevier B.V. All rights reserved.

Online and unsupervised face recognition for continuous video stream

NASA Astrophysics Data System (ADS)

Huo, Hongwen; Feng, Jufu

2009-10-01

We present a novel online face recognition approach for video stream in this paper. Our method includes two stages: pre-training and online training. In the pre-training phase, our method observes interactions, collects batches of input data, and attempts to estimate their distributions (Box-Cox transformation is adopted here to normalize rough estimates). In the online training phase, our method incrementally improves classifiers' knowledge of the face space and updates it continuously with incremental eigenspace analysis. The performance achieved by our method shows its great potential in video stream processing.

Development and validation of a reversed phase liquid chromatographic method for analysis of oxytetracycline and related impurities.

PubMed

Kahsay, Getu; Shraim, Fairouz; Villatte, Philippe; Rotger, Jacques; Cassus-Coussère, Céline; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

2013-03-05

A simple, robust and fast high-performance liquid chromatographic method is described for the analysis of oxytetracycline and its related impurities. The principal peak and impurities are all baseline separated in 20 min using an Inertsil C₈ (150 mm × 4.6 mm, 5 μm) column kept at 50 °C. The mobile phase consists of a gradient mixture of mobile phases A (0.05% trifluoroacetic acid in water) and B (acetonitrile-methanol-tetrahydrofuran, 80:15:5, v/v/v) pumped at a flow rate of 1.3 ml/min. UV detection was performed at 254 nm. The developed method was validated for its robustness, sensitivity, precision and linearity in the range from limit of quantification (LOQ) to 120%. The limits of detection (LOD) and LOQ were found to be 0.08 μg/ml and 0.32 μg/ml, respectively. This method allows the separation of oxytetracycline from all known and 5 unknown impurities, which is better than previously reported in the literature. Moreover, the simple mobile phase composition devoid of non-volatile buffers made the method suitable to interface with mass spectrometry for further characterization of unknown impurities. The developed method has been applied for determination of related substances in oxytetracycline bulk samples available from four manufacturers. The validation results demonstrate that the method is reliable for quantification of oxytetracycline and its impurities. Copyright © 2012 Elsevier B.V. All rights reserved.

Complex amplitude reconstruction by iterative amplitude-phase retrieval algorithm with reference

NASA Astrophysics Data System (ADS)

Shen, Cheng; Guo, Cheng; Tan, Jiubin; Liu, Shutian; Liu, Zhengjun

2018-06-01

Multi-image iterative phase retrieval methods have been successfully applied in plenty of research fields due to their simple but efficient implementation. However, there is a mismatch between the measurement of the first long imaging distance and the sequential interval. In this paper, an amplitude-phase retrieval algorithm with reference is put forward without additional measurements or priori knowledge. It gets rid of measuring the first imaging distance. With a designed update formula, it significantly raises the convergence speed and the reconstruction fidelity, especially in phase retrieval. Its superiority over the original amplitude-phase retrieval (APR) method is validated by numerical analysis and experiments. Furthermore, it provides a conceptual design of a compact holographic image sensor, which can achieve numerical refocusing easily.

A novel method to optimize the mode spectrum of the dynamic resonant magnetic perturbation on the J-TEXT tokamak.

PubMed

Yi, B; Rao, B; Ding, Y H; Li, M; Xu, H Y; Zhang, M; Zhuang, G; Pan, Y

2014-11-01

The dynamic resonant magnetic perturbation (DRMP) system has been developed for the J-TEXT tokamak to study the interaction between the rotating perturbation magnetic field and the plasma. When the DRMP coils are energized by two phase sinusoidal currents with the same frequency, a 2/1 rotating resonant magnetic perturbation component will be generated. But at the same time, a small perturbation component rotating in the opposite direction is also produced because of the control error of the currents. This small component has bad influence on the experiment investigations. Actually, the mode spectrum of the generated DRMP can be optimized with an accurate control of phase difference between the two currents. In this paper, a new phase control method based on a novel all-digital phase-locked loop (ADPLL) is proposed. The proposed method features accurate phase control and flexible phase adjustment. Modeling and analysis of the proposed ADPLL is presented to guide the design of the parameters of the phase controller in order to obtain a better performance. Testing results verify the effectiveness of the ADPLL and validity of the method applying to the DRMP system.

A novel method to optimize the mode spectrum of the dynamic resonant magnetic perturbation on the J-TEXT tokamak

NASA Astrophysics Data System (ADS)

Yi, B.; Rao, B.; Ding, Y. H.; Li, M.; Xu, H. Y.; Zhang, M.; Zhuang, G.; Pan, Y.

2014-11-01

The dynamic resonant magnetic perturbation (DRMP) system has been developed for the J-TEXT tokamak to study the interaction between the rotating perturbation magnetic field and the plasma. When the DRMP coils are energized by two phase sinusoidal currents with the same frequency, a 2/1 rotating resonant magnetic perturbation component will be generated. But at the same time, a small perturbation component rotating in the opposite direction is also produced because of the control error of the currents. This small component has bad influence on the experiment investigations. Actually, the mode spectrum of the generated DRMP can be optimized with an accurate control of phase difference between the two currents. In this paper, a new phase control method based on a novel all-digital phase-locked loop (ADPLL) is proposed. The proposed method features accurate phase control and flexible phase adjustment. Modeling and analysis of the proposed ADPLL is presented to guide the design of the parameters of the phase controller in order to obtain a better performance. Testing results verify the effectiveness of the ADPLL and validity of the method applying to the DRMP system.

Dual-domain point diffraction interferometer

DOEpatents

Naulleau, Patrick P.; Goldberg, Kenneth Alan

2000-01-01

A hybrid spatial/temporal-domain point diffraction interferometer (referred to as the dual-domain PS/PDI) that is capable of suppressing the scattered-reference-light noise that hinders the conventional PS/PDI is provided. The dual-domain PS/PDI combines the separate noise-suppression capabilities of the widely-used phase-shifting and Fourier-transform fringe pattern analysis methods. The dual-domain PS/PDI relies on both a more restrictive implementation of the image plane PS/PDI mask and a new analysis method to be applied to the interferograms generated and recorded by the modified PS/PDI. The more restrictive PS/PDI mask guarantees the elimination of spatial-frequency crosstalk between the signal and the scattered-light noise arising from scattered-reference-light interfering with the test beam. The new dual-domain analysis method is then used to eliminate scattered-light noise arising from both the scattered-reference-light interfering with the test beam and the scattered-reference-light interfering with the "true" pinhole-diffracted reference light. The dual-domain analysis method has also been demonstrated to provide performance enhancement when using the non-optimized standard PS/PDI design. The dual-domain PS/PDI is essentially a three-tiered filtering system composed of lowpass spatial-filtering the test-beam electric field using the more restrictive PS/PDI mask, bandpass spatial-filtering the individual interferogram irradiance frames making up the phase-shifting series, and bandpass temporal-filtering the phase-shifting series as a whole.

Finite element techniques in computational time series analysis of turbulent flows

NASA Astrophysics Data System (ADS)

Horenko, I.

2009-04-01

In recent years there has been considerable increase of interest in the mathematical modeling and analysis of complex systems that undergo transitions between several phases or regimes. Such systems can be found, e.g., in weather forecast (transitions between weather conditions), climate research (ice and warm ages), computational drug design (conformational transitions) and in econometrics (e.g., transitions between different phases of the market). In all cases, the accumulation of sufficiently detailed time series has led to the formation of huge databases, containing enormous but still undiscovered treasures of information. However, the extraction of essential dynamics and identification of the phases is usually hindered by the multidimensional nature of the signal, i.e., the information is "hidden" in the time series. The standard filtering approaches (like f.~e. wavelets-based spectral methods) have in general unfeasible numerical complexity in high-dimensions, other standard methods (like f.~e. Kalman-filter, MVAR, ARCH/GARCH etc.) impose some strong assumptions about the type of the underlying dynamics. Approach based on optimization of the specially constructed regularized functional (describing the quality of data description in terms of the certain amount of specified models) will be introduced. Based on this approach, several new adaptive mathematical methods for simultaneous EOF/SSA-like data-based dimension reduction and identification of hidden phases in high-dimensional time series will be presented. The methods exploit the topological structure of the analysed data an do not impose severe assumptions on the underlying dynamics. Special emphasis will be done on the mathematical assumptions and numerical cost of the constructed methods. The application of the presented methods will be first demonstrated on a toy example and the results will be compared with the ones obtained by standard approaches. The importance of accounting for the mathematical assumptions used in the analysis will be pointed up in this example. Finally, applications to analysis of meteorological and climate data will be presented.

Application of Concepts from Cross-Recurrence Analysis in Speech Production: An Overview and Comparison with Other Nonlinear Methods

ERIC Educational Resources Information Center

Lancia, Leonardo; Fuchs, Susanne; Tiede, Mark

2014-01-01

Purpose: The aim of this article was to introduce an important tool, cross-recurrence analysis, to speech production applications by showing how it can be adapted to evaluate the similarity of multivariate patterns of articulatory motion. The method differs from classical applications of cross-recurrence analysis because no phase space…

Auto correlation analysis of coda waves from local earthquakes for detecting temporal changes in shallow subsurface structures - The 2011 Tohoku-Oki, Japan, earthquake -

NASA Astrophysics Data System (ADS)

Nakahara, H.

2013-12-01

For monitoring temporal changes in subsurface structures, I propose to use auto correlation functions of coda waves from local earthquakes recorded at surface receivers, which probably contain more body waves than surface waves. Because the use of coda waves requires earthquakes, time resolution for monitoring decreases. But at regions with high seismicity, it may be possible to monitor subsurface structures in sufficient time resolutions. Studying the 2011 Tohoku-Oki (Mw 9.0), Japan, earthquake for which velocity changes have been already reported by previous studies, I try to validate the method. KiK-net stations in northern Honshu are used in the analysis. For each moderate earthquake, normalized auto correlation functions of surface records are stacked with respect to time windows in S-wave coda. Aligning the stacked normalized auto correlation functions with time, I search for changes in arrival times of phases. The phases at lag times of less than 1s are studied because changes at shallow depths are focused. Based on the stretching method, temporal variations in the arrival times are measured at the stations. Clear phase delays are found to be associated with the mainshock and to gradually recover with time. Amounts of the phase delays are in the order of 10% on average with the maximum of about 50% at some stations. For validation, the deconvolution analysis using surface and subsurface records at the same stations are conducted. The results show that the phase delays from the deconvolution analysis are slightly smaller than those from the auto correlation analysis, which implies that the phases on the auto correlations are caused by larger velocity changes at shallower depths. The auto correlation analysis seems to have an accuracy of about several percents, which is much larger than methods using earthquake doublets and borehole array data. So this analysis might be applicable to detect larger changes. In spite of these disadvantages, this analysis is still attractive because it can be applied to many records on the surface in regions where no boreholes are available. Acknowledgements: Seismograms recorded by KiK-net managed by National Research Institute for Earth Science and Disaster Prevention (NIED) were used in this study. This study was partially supported by JST J-RAPID program and JSPS KAKENHI Grant Numbers 24540449 and 23540449.

Compound Specific Concentration and Stable Isotope Ratio Measurements of Atmospheric Particulate Organic Matter and Gas Phase Nitrophenols

NASA Astrophysics Data System (ADS)

Busca, R.; Saccon, M.; Moukhtar, S.; Rudolph, J.

2009-05-01

Atmospheric particulate organic matter (POM) adversely affects health and climate. One of the still poorly understood sources of secondary organic matter (SOM) is the formation of secondary POM from the photo- oxidation of atmospheric volatile organic compounds (VOC). Nitrophenols, which are toxic semi-volatile compounds, are formed in the atmosphere by OH-radical initiated photo-oxidation of aromatic hydrocarbons, such as toluene. A method was developed to determine concentrations and stable carbon isotope ratios of particulate methyl nitrophenols in the atmosphere. This method has been used to quantify methyl nitrophenols, specifically 2-methyl-4-nitrophenol and 4-methyl-2-nitrophenol, found in atmospheric PM samples in trace quantities. Using this method, we conducted measurements of methyl nitrophenols in atmospheric PM in rural and suburban areas in Southern Ontario. The results of these measurements showed that the concentration of methyl nitrophenols in atmospheric PM is much lower than expected from the extrapolation of laboratory experiments and measured atmospheric toluene concentrations. In order to better understand the reasons for these findings, an analytical method for the analysis of nitrophenols in the gas phase is currently being developed. Similarly, the measurement technique is modified to allow analysis of other phenolic products of the oxidation of aromatic hydrocarbons in PM as well as in the gas phase. In this poster, sampling techniques for collection and GC-MS analysis of nitrophenols in gas phase and PM will be presented along with preliminary results from summer 2008 and spring 2009 studies.

Leukotriene B4 catabolism: quantitation of leukotriene B4 and its omega-oxidation products by reversed-phase high-performance liquid chromatography.

PubMed

Shak, S

1987-01-01

LTB4 and its omega-oxidation products may be rapidly, sensitively, and specifically quantitated by the methods of solid-phase extraction and reversed-phase high-performance liquid chromatography (HPLC), which are described in this chapter. Although other techniques, such as radioimmunoassay or gas chromatography-mass spectrometry, may be utilized for quantitative analysis of the lipoxygenase products of arachidonic acid, only the technique of reversed-phase HPLC can quantitate as many as 10 metabolites in a single analysis, without prior derivatization. In this chapter, we also reviewed the chromatographic theory which we utilized in order to optimize reversed-phase HPLC analysis of LTB4 and its omega-oxidation products. With this information and a gradient HPLC system, it is possible for any investigator to develop a powerful assay for the potent inflammatory mediator, LTB4, or for any other lipoxygenase product of arachidonic acid.

Two-phase electromembrane extraction followed by gas chromatography-mass spectrometry analysis.

PubMed

Davarani, Saied Saeed Hosseiny; Morteza-Najarian, Amin; Nojavan, Saeed; Pourahadi, Ahmad; Abbassi, Mojtaba Beigzadeh

2013-02-01

A two-phase electromembrane extraction (EME) was developed and directly coupled with gas chromatography mass spectrometry (GC-MS) analysis. The proposed method was successfully applied to the simultaneous determination of imipramine, desipramine, citalopram and sertraline. The model compounds were extracted from neutral aqueous sample solutions into the organic phase filled in the lumen of the hollow fiber. This method was accomplished with 1-heptanol as organic phase, by means of 60 V applied voltage and with the extraction time of 15 min. Experiments reported recoveries in the range of 69-87% from 1.2 mL neutral sample solution. The compounds were quantified by GC-MS instrument, with acceptable linearity ranging from 1 to 500 ng mL(-1) (R(2) in the range of 0.989 to 0.998), and repeatability (RSD) ranging between 7.5 and 11.5% (n = 5). The estimated detection limits (S/N ratio of 3:1) were less than 0.25 ng mL(-1). This novel approach based on two-phase EME brought advantages such as simplicity, low-costing, low detection limit and fast extraction with a total analysis time less than 25 min. These experimental findings were highly interesting and demonstrated the possibility of solving ionic species in the organic phase at the presence of electrical potential. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

How little data is enough? Phase-diagram analysis of sparsity-regularized X-ray computed tomography

PubMed Central

Jørgensen, J. S.; Sidky, E. Y.

2015-01-01

We introduce phase-diagram analysis, a standard tool in compressed sensing (CS), to the X-ray computed tomography (CT) community as a systematic method for determining how few projections suffice for accurate sparsity-regularized reconstruction. In CS, a phase diagram is a convenient way to study and express certain theoretical relations between sparsity and sufficient sampling. We adapt phase-diagram analysis for empirical use in X-ray CT for which the same theoretical results do not hold. We demonstrate in three case studies the potential of phase-diagram analysis for providing quantitative answers to questions of undersampling. First, we demonstrate that there are cases where X-ray CT empirically performs comparably with a near-optimal CS strategy, namely taking measurements with Gaussian sensing matrices. Second, we show that, in contrast to what might have been anticipated, taking randomized CT measurements does not lead to improved performance compared with standard structured sampling patterns. Finally, we show preliminary results of how well phase-diagram analysis can predict the sufficient number of projections for accurately reconstructing a large-scale image of a given sparsity by means of total-variation regularization. PMID:25939620

How little data is enough? Phase-diagram analysis of sparsity-regularized X-ray computed tomography.

PubMed

Jørgensen, J S; Sidky, E Y

2015-06-13

We introduce phase-diagram analysis, a standard tool in compressed sensing (CS), to the X-ray computed tomography (CT) community as a systematic method for determining how few projections suffice for accurate sparsity-regularized reconstruction. In CS, a phase diagram is a convenient way to study and express certain theoretical relations between sparsity and sufficient sampling. We adapt phase-diagram analysis for empirical use in X-ray CT for which the same theoretical results do not hold. We demonstrate in three case studies the potential of phase-diagram analysis for providing quantitative answers to questions of undersampling. First, we demonstrate that there are cases where X-ray CT empirically performs comparably with a near-optimal CS strategy, namely taking measurements with Gaussian sensing matrices. Second, we show that, in contrast to what might have been anticipated, taking randomized CT measurements does not lead to improved performance compared with standard structured sampling patterns. Finally, we show preliminary results of how well phase-diagram analysis can predict the sufficient number of projections for accurately reconstructing a large-scale image of a given sparsity by means of total-variation regularization.

Fully automated method for the liquid chromatographic determination of cyproterone acetate in plasma using restricted access material for sample pre-treatment.

PubMed

Christiaens, B; Chiap, P; Rbeida, O; Cello, D; Crommen, J; Hubert, Ph

2003-09-25

A new fully automated method for the quantitative analysis of an antiandrogenic substance, cyproterone acetate (CPA), in plasma samples has been developed using on-line solid-phase extraction (SPE) prior to the determination by reversed-phase liquid chromatography (LC). The automated method was based on the use of a precolumn packed with an internal-surface reversed-phase packing material (LiChrospher RP-4 ADS) for sample clean-up coupled to LC analysis on an octadecyl stationary phase using a column-switching system. A 200-microL volume of plasma sample was injected directly on the precolumn packed with restricted access material using a mixture of water-acetonitrile (90:10, v/v) as washing liquid. The analyte was then eluted in the back-flush mode with the LC mobile phase which consisted of a mixture of phosphate buffer, pH 7.0-acetonitrile (54:46, v/v). The elution profiles of CPA and blank plasma samples on the precolumn and the time needed for analyte transfer from the precolumn to the analytical column were determined. Different compositions of washing liquid and mobile phase were tested to reduce the interference of plasma endogenous components. UV detection was achieved at 280 nm. Finally, the developed method was validated using a new approach, namely the application of the accuracy profile based on the interval confidence at 90% of the total measurement error (bias+standard deviation). The limit of quantification of cyproterone acetate in plasma was determined at 15 ng mL(-1). The validated method should be applicable to the determination of CPA in patients treated by at least 50 mg day(-1).

[Improvement of the determination method of benzene, toluene, ethylbenzene and xylene(BTEX) in water using activated carbon fiber solid-phase microextraction/gas chromatography-mass spectrometry(GC-MS)].

PubMed

Jia, Jin-ping; Feng, Xue; Fang, Neng-hu; Huang, Jia-liang

2002-01-01

The methods of direct injection, carbon disulfide extraction and activated carbon fiber solid-phase microextraction/GC-MS, usually used in the determination of BTEX in water matrix, are compared and discussed. Experimental data of linearity, precision and limit of detection illustrate that the last one is better than the two other methods. This method was tested by the practical sample experiments and expected to be a simple and sensitive new method for the analysis of BTEX in water.

Talker Localization Based on Interference between Transmitted and Reflected Audible Sound

NASA Astrophysics Data System (ADS)

Nakayama, Masato; Nakasako, Noboru; Shinohara, Toshihiro; Uebo, Tetsuji

In many engineering fields, distance to targets is very important. General distance measurement method uses a time delay between transmitted and reflected waves, but it is difficult to estimate the short distance. On the other hand, the method using phase interference to measure the short distance has been known in the field of microwave radar. Therefore, we have proposed the distance estimation method based on interference between transmitted and reflected audible sound, which can measure the distance between microphone and target with one microphone and one loudspeaker. In this paper, we propose talker localization method based on distance estimation using phase interference. We expand the distance estimation method using phase interference into two microphones (microphone array) in order to estimate talker position. The proposed method can estimate talker position by measuring the distance and direction between target and microphone array. In addition, talker's speech is regarded as a noise in the proposed method. Therefore, we also propose combination of the proposed method and CSP (Cross-power Spectrum Phase analysis) method which is one of the DOA (Direction Of Arrival) estimation methods. We evaluated the performance of talker localization in real environments. The experimental result shows the effectiveness of the proposed method.

Airflow and Particle Transport Through Human Airways: A Systematic Review

NASA Astrophysics Data System (ADS)

Kharat, S. B.; Deoghare, A. B.; Pandey, K. M.

2017-08-01

This paper describes review of the relevant literature about two phase analysis of air and particle flow through human airways. An emphasis of the review is placed on elaborating the steps involved in two phase analysis, which are Geometric modelling methods and Mathematical models. The first two parts describes various approaches that are followed for constructing an Airway model upon which analysis are conducted. Broad two categories of geometric modelling viz. Simplified modelling and Accurate modelling using medical scans are discussed briefly. Ease and limitations of simplified models, then examples of CT based models are discussed. In later part of the review different mathematical models implemented by researchers for analysis are briefed. Mathematical models used for Air and Particle phases are elaborated separately.

First derivative ratio spectrophotometric, HPTLC-densitometric, and HPLC determination of nicergoline in presence of its hydrolysis-induced degradation product.

PubMed

Ahmad, Abdel Kader S; Kawy, M Abdel; Nebsen, M

2002-10-15

Three methods are presented for the determination of Nicergoline in presence of its hydrolysis-induced degradation product. The first method was based on measurement of the first derivative of ratio spectra amplitude of Nicergoline at 291 nm. The second method was based on separation of Nicergoline from its degradation product followed by densitometric measurement of the spots at 287 nm. The separation was carried out on HPTLC silica gel F(254) plates, using methanol-ethyl acetate-glacial acetic acid (5:7:3, v/v/v) as mobile phase. The third method was based on high performance liquid chromatographic (HPLC) separation and determination of Nicergoline from its degradation product on a reversed phase, nucloesil C(18) column using a mobile phase of methanol-water-glacial acetic acid (80:20:0.1, v/v/v) with UV detection at 280 nm. Chlorpromazine hydrochloride was used as internal standard. Laboratory prepared mixtures containing different percentages of the degradation product were analysed by the proposed methods and satisfactory results were obtained. These methods have been successfully applied to the analysis of Nicergoline in Sermion tablets. The validities of these methods were ascertained by applying standard addition technique, the mean percentage recovery +/- R.S.D.% was found to be 99.47 +/- 0.752, 100.01 +/- 0.940, 99.75 +/- 0.740 for the first derivative of ratio spectra method, the HPTLC method and the HPLC method, respectively. The proposed methods were statistically compared with the manufacturer's HPLC method of analysis of Nicergoline and no significant difference was found with respect to both precision and accuracy. They have the advantage of being stability indicating. Therefore, they can be used for routine analysis of the drug in quality control laboratories. Copyright 2002 Elsevier Science B.V.

The diagnostic performance of dental maturity for identification of the circumpubertal growth phases: a meta-analysis.

PubMed

Perinetti, Giuseppe; Westphalen, Graziela H; Biasotto, Matteo; Salgarello, Stefano; Contardo, Luca

2013-05-23

The present meta-analysis initially evaluates the reliability of dental maturation in the identification of the circumpubertal growth phases, essentially for determining treatment timing in orthodontics. A literature survey was performed using the Medline, LILACS and SciELO databases, and the Cochrane Library (2000 to 2011). Studies of the correlation between dental and cervical vertebral maturation methods were considered. The mandibular canine, the first and second premolars, and the second molar were investigated. After the selection, six articles qualified for the final analysis. The overall correlation coefficients were all significant, ranging from 0.57 to 0.73. Five of these studies suggested the use of dental maturation as an indicator of the growth phase. However, the diagnostic performance analysis uncovered limited reliability only for the identification of the pre-pubertal growth phase. The determination of dental maturity for the assessment of treatment timing in orthodontics is not recommended.

Flow Pattern Phenomena in Two-Phase Flow in Microchannels

NASA Astrophysics Data System (ADS)

Keska, Jerry K.; Simon, William E.

2004-02-01

Space transportation systems require high-performance thermal protection and fluid management techniques for systems ranging from cryogenic fluid management devices to primary structures and propulsion systems exposed to extremely high temperatures, as well as for other space systems such as cooling or environment control for advanced space suits and integrated circuits. Although considerable developmental effort is being expended to bring potentially applicable technologies to a readiness level for practical use, new and innovative methods are still needed. One such method is the concept of Advanced Micro Cooling Modules (AMCMs), which are essentially compact two-phase heat exchangers constructed of microchannels and designed to remove large amounts of heat rapidly from critical systems by incorporating phase transition. The development of AMCMs requires fundamental technological advancement in many areas, including: (1) development of measurement methods/systems for flow-pattern measurement/identification for two-phase mixtures in microchannels; (2) development of a phenomenological model for two-phase flow which includes the quantitative measure of flow patterns; and (3) database development for multiphase heat transfer/fluid dynamics flows in microchannels. This paper focuses on the results of experimental research in the phenomena of two-phase flow in microchannels. The work encompasses both an experimental and an analytical approach to incorporating flow patterns for air-water mixtures flowing in a microchannel, which are necessary tools for the optimal design of AMCMs. Specifically, the following topics are addressed: (1) design and construction of a sensitive test system for two-phase flow in microchannels, one which measures ac and dc components of in-situ physical mixture parameters including spatial concentration using concomitant methods; (2) data acquisition and analysis in the amplitude, time, and frequency domains; and (3) analysis of results including evaluation of data acquisition techniques and their validity for application in flow pattern determination.

Chapter 5: Modulation Excitation Spectroscopy with Phase-Sensitive Detection for Surface Analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shulda, Sarah; Richards, Ryan M.

Advancements in in situ spectroscopic techniques have led to significant progress being made in elucidating heterogeneous reaction mechanisms. The potential of these progressive methods is often limited only by the complexity of the system and noise in the data. Short-lived intermediates can be challenging, if not impossible, to identify with conventional spectra analysis means. Often equally difficult is separating signals that arise from active and inactive species. Modulation excitation spectroscopy combined with phase-sensitive detection analysis is a powerful tool for removing noise from the data while simultaneously revealing the underlying kinetics of the reaction. A stimulus is applied at amore » constant frequency to the reaction system, for example, a reactant cycled with an inert phase. Through mathematical manipulation of the data, any signal contributing to the overall spectra but not oscillating with the same frequency as the stimulus will be dampened or removed. With phase-sensitive detection, signals oscillating with the stimulus frequency but with various lag times are amplified providing valuable kinetic information. In this chapter, some examples are provided from the literature that have successfully used modulation excitation spectroscopy with phase-sensitive detection to uncover previously unobserved reaction intermediates and kinetics. Examples from a broad range of spectroscopic methods are included to provide perspective to the reader.« less

Comparison of core-shell and totally porous ultra high performance liquid chromatographic stationary phases based on their selectivity towards alfuzosin compounds.

PubMed

Szulfer, Jarosław; Plenis, Alina; Bączek, Tomasz

2014-06-13

This paper focuses on the application of a column classification system based on the Katholieke Universiteit Leuven for the characterization of physicochemical properties of core-shell and ultra-high performance liquid chromatographic stationary phases, followed by the verification of the reliability of the obtained column classification in pharmaceutical practice. In the study, 7 stationary phases produced in core-shell technology and 18 ultra-high performance liquid chromatographic columns were chromatographically tested, and ranking lists were built on the FKUL-values calculated against two selected reference columns. In the column performance test, an analysis of alfuzosin in the presence of related substances was carried out using the brands of the stationary phases with the highest ranking positions. Next, a system suitability test as described by the European Pharmacopoeia monograph was performed. Moreover, a study was also performed to achieve a purposeful shortening of the analysis time of the compounds of interest using the selected stationary phases. Finally, it was checked whether methods using core-shell and ultra-high performance liquid chromatographic columns can be an interesting alternative to the high-performance liquid chromatographic method for the analysis of alfuzosin in pharmaceutical practice. Copyright © 2014 Elsevier B.V. All rights reserved.

Characterization of carbon silica hybrid fillers obtained by pyrolysis of waste green tires by the STEM–EDX method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Al-Hartomy, Omar A.; Department of Physics, Faculty of Science, University of Tabuk, Tabuk 71491; Al-Ghamdi, Ahmed A.

2015-03-15

Dual phase carbon–silica hybrid fillers obtained by pyrolysis-cum-water vapor of waste green tires have been characterized by energy dispersive X-ray spectroscopy in a scanning transmission electron microscope, silicate analysis, weight analysis, atomic absorption spectroscopy and by inductively coupled plasma–optical emission spectroscopy. The results achieved have shown that the location and distribution of the phases in the carbon silica hybrid fillers as well as their most essential characteristics are influenced by the pyrolysis conditions. The carbon phase of the filler thus obtained is located predominantly in the space among silica aggregates which have already been existing while it has been formedmore » by elastomer destruction in the course of pyrolysis. The presence of ZnS also has been found in the hybrid fillers investigated. - Highlights: • Dual phase fillers obtained by pyrolysis of waste green tires have been characterized. • The STEM–EDX method was used for characterization. • The phase distributions in the fillers are influenced by the pyrolysis conditions.« less

Improving Quality of Seal Leak Test Product using Six Sigma

NASA Astrophysics Data System (ADS)

Luthfi Malik, Abdullah; Akbar, Muhammad; Irianto, Dradjad

2016-02-01

Seal leak test part is a polyurethane material-based product. Based on past data, defect level of this product was 8%, higher than the target of 5%. Quality improvement effort was done using six sigma method that included phases of define, measure, analyse, improve, and control. In the design phase, a Delphi method was used to identify factors that were critical to quality. In the measure phase, stability and process capability was measured. Fault tree analysis (FTA) and failure mode and effect analysis (FMEA) were used in the next phase to analize the root cause and to determine the priority issues. Improve phase was done by compiling, selecting, and designing alternative repair. Some improvement efforts were identified, i.e. (i) making a checklist for maintenance schedules, (ii) making written reminder form, (iii) modifying the SOP more detail, and (iv) performing a major service to the vacuum machine. To ensure the continuity of improvement efforts, some control activities were executed, i.e. (i) controlling, monitoring, documenting, and setting target frequently, (ii) implementing reward and punishment system, (iii) adding cleaning tool, and (iv) building six sigma organizational structure.

Influence of OPD in wavelength-shifting interferometry

NASA Astrophysics Data System (ADS)

Wang, Hongjun; Tian, Ailing; Liu, Bingcai; Dang, Juanjuan

2009-12-01

Phase-shifting interferometry is a powerful tool for high accuracy optical measurement. It operates by change the optical path length in the reference arm or test arm. This method practices by move optical device. So it has much problem when the optical device is very large and heavy. For solve this problem, the wavelength-shifting interferometry was put forwarded. In wavelength-shifting interferometry, the phase shifting angle was achieved by change the wavelength of optical source. The phase shifting angle was decided by wavelength and OPD (Optical Path Difference) between test and reference wavefront. So the OPD is an important factor to measure results. But in measurement, because the positional error and profile error of under testing optical element is exist, the phase shifting angle is different in different test point when wavelength scanning, it will introduce phase shifting angle error, so it will introduce optical surface measure error. For analysis influence of OPD on optical surface error, the relation between surface error and OPD was researched. By simulation, the relation between phase shifting error and OPD was established. By analysis, the error compensation method was put forward. After error compensation, the measure results can be improved to great extend.

Influence of OPD in wavelength-shifting interferometry

NASA Astrophysics Data System (ADS)

Wang, Hongjun; Tian, Ailing; Liu, Bingcai; Dang, Juanjuan

2010-03-01

Phase-shifting interferometry is a powerful tool for high accuracy optical measurement. It operates by change the optical path length in the reference arm or test arm. This method practices by move optical device. So it has much problem when the optical device is very large and heavy. For solve this problem, the wavelength-shifting interferometry was put forwarded. In wavelength-shifting interferometry, the phase shifting angle was achieved by change the wavelength of optical source. The phase shifting angle was decided by wavelength and OPD (Optical Path Difference) between test and reference wavefront. So the OPD is an important factor to measure results. But in measurement, because the positional error and profile error of under testing optical element is exist, the phase shifting angle is different in different test point when wavelength scanning, it will introduce phase shifting angle error, so it will introduce optical surface measure error. For analysis influence of OPD on optical surface error, the relation between surface error and OPD was researched. By simulation, the relation between phase shifting error and OPD was established. By analysis, the error compensation method was put forward. After error compensation, the measure results can be improved to great extend.

Determination of esters in glycerol phase after transesterification of vegetable oil.

PubMed

Hájek, Martin; Skopal, Frantisek; Kwiecien, Jirí; Cernoch, Michal

2010-06-30

In biodiesel production, glycerol is formed as a side product and it is contained in the glycerol phase. This phase contains (besides glycerol): water, soaps, alcohol, traces of catalyst and glycerides and the remaining esters. In this paper, a new method for the determination of esters in the glycerol phase is introduced. The determination enables the minimization of the losses of biodiesel within the production process. It is based on the gradient RP-LC method (water and acetonitrile) with refractometric detection. The analysis is easy and the samples do not need any treatment (only dilution by water) and has a low detection limit. The results of this method were compared with the results of two other published methods: isocratic HPLC and GC. The disadvantage of these two methods is that they need extensive treatment of the sample, which takes many hours, and they are able to determine only the sum of esters. The new method is reliable, much faster and able to differentiate esters of almost each higher fatty acid (e.g. linoleic, linolenic, strearic alkyl ester) in the glycerol phase. Copyright 2010 Elsevier B.V. All rights reserved.

Evaluation of Wet Chemical ICP-AES Elemental Analysis Methods usingSimulated Hanford Waste Samples-Phase I Interim Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Coleman, Charles J.; Edwards, Thomas B.

2005-04-30

The wet chemistry digestion method development for providing process control elemental analyses of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Melter Feed Preparation Vessel (MFPV) samples is divided into two phases: Phase I consists of: (1) optimizing digestion methods as a precursor to elemental analyses by ICP-AES techniques; (2) selecting methods with the desired analytical reliability and speed to support the nine-hour or less turnaround time requirement of the WTP; and (3) providing baseline comparison to the laser ablation (LA) sample introduction technique for ICP-AES elemental analyses that is being developed at the Savannah River National Laboratory (SRNL).more » Phase II consists of: (1) Time-and-Motion study of the selected methods from Phase I with actual Hanford waste or waste simulants in shielded cell facilities to ensure that the methods can be performed remotely and maintain the desired characteristics; and (2) digestion of glass samples prepared from actual Hanford Waste tank sludge for providing comparative results to the LA Phase II study. Based on the Phase I testing discussed in this report, a tandem digestion approach consisting of sodium peroxide fusion digestions carried out in nickel crucibles and warm mixed-acid digestions carried out in plastic bottles has been selected for Time-and-Motion study in Phase II. SRNL experience with performing this analytical approach in laboratory hoods indicates that well-trained cell operator teams will be able to perform the tandem digestions in five hours or less. The selected approach will produce two sets of solutions for analysis by ICP-AES techniques. Four hours would then be allocated for performing the ICP-AES analyses and reporting results to meet the nine-hour or less turnaround time requirement. The tandem digestion approach will need to be performed in two separate shielded analytical cells by two separate cell operator teams in order to achieve the nine-hour or less turnaround time. Because of the simplicity of the warm mixed-acid method, a well-trained cell operator team may in time be able to perform both sets of digestions. However, having separate shielded cells for each of the methods is prudent to avoid overcrowding problems that would impede a minimal turnaround time.« less

Multimodal pressure-flow method to assess dynamics of cerebral autoregulation in stroke and hypertension

PubMed Central

Novak, Vera; Yang, Albert CC; Lepicovsky, Lukas; Goldberger, Ary L; Lipsitz, Lewis A; Peng, Chung-Kang

2004-01-01

Background This study evaluated the effects of stroke on regulation of cerebral blood flow in response to fluctuations in systemic blood pressure (BP). The autoregulatory dynamics are difficult to assess because of the nonstationarity and nonlinearity of the component signals. Methods We studied 15 normotensive, 20 hypertensive and 15 minor stroke subjects (48.0 ± 1.3 years). BP and blood flow velocities (BFV) from middle cerebral arteries (MCA) were measured during the Valsalva maneuver (VM) using transcranial Doppler ultrasound. Results A new technique, multimodal pressure-flow analysis (MMPF), was implemented to analyze these short, nonstationary signals. MMPF analysis decomposes complex BP and BFV signals into multiple empirical modes, representing their instantaneous frequency-amplitude modulation. The empirical mode corresponding to the VM BP profile was used to construct the continuous phase diagram and to identify the minimum and maximum values from the residual BP (BPR) and BFV (BFVR) signals. The BP-BFV phase shift was calculated as the difference between the phase corresponding to the BPR and BFVR minimum (maximum) values. BP-BFV phase shifts were significantly different between groups. In the normotensive group, the BFVR minimum and maximum preceded the BPR minimum and maximum, respectively, leading to large positive values of BP-BFV shifts. Conclusion In the stroke and hypertensive groups, the resulting BP-BFV phase shift was significantly smaller compared to the normotensive group. A standard autoregulation index did not differentiate the groups. The MMPF method enables evaluation of autoregulatory dynamics based on instantaneous BP-BFV phase analysis. Regulation of BP-BFV dynamics is altered with hypertension and after stroke, rendering blood flow dependent on blood pressure. PMID:15504235

Obtaining reliable phase-gradient delays from otoacoustic emission data.

PubMed

Shera, Christopher A; Bergevin, Christopher

2012-08-01

Reflection-source otoacoustic emission phase-gradient delays are widely used to obtain noninvasive estimates of cochlear function and properties, such as the sharpness of mechanical tuning and its variation along the length of the cochlear partition. Although different data-processing strategies are known to yield different delay estimates and trends, their relative reliability has not been established. This paper uses in silico experiments to evaluate six methods for extracting delay trends from reflection-source otoacoustic emissions (OAEs). The six methods include both previously published procedures (e.g., phase smoothing, energy-weighting, data exclusion based on signal-to-noise ratio) and novel strategies (e.g., peak-picking, all-pass factorization). Although some of the methods perform well (e.g., peak-picking), others introduce substantial bias (e.g., phase smoothing) and are not recommended. In addition, since standing waves caused by multiple internal reflection can complicate the interpretation and compromise the application of OAE delays, this paper develops and evaluates two promising signal-processing strategies, the first based on time-frequency filtering using the continuous wavelet transform and the second on cepstral analysis, for separating the direct emission from its subsequent reflections. Altogether, the results help to resolve previous disagreements about the frequency dependence of human OAE delays and the sharpness of cochlear tuning while providing useful analysis methods for future studies.

Isolation and quantification of Quillaja saponaria Molina saponins and lipids in iscom-matrix and iscoms.

PubMed

Behboudi, S; Morein, B; Rönnberg, B

1995-12-01

In the iscom, multiple copies of antigen are attached by hydrophobic interaction to a matrix which is built up by Quillaja triterpenoid saponins and lipids. Thus, the iscom presents antigen in multimeric form in a small particle with a built-in adjuvant resulting in a highly immunogenic antigen formulation. We have designed a chloroform-methanol-water extraction procedure to isolate the triterpenoid saponins and lipids incorporated into iscom-matrix and iscoms. The triterpenoids in the triterpenoid phase were quantitated using orcinol sulfuric acid detecting their carbohydrate chains and by HPLC. The cholesterol and phosphatidylcholine in the lipid phase were quantitated by HPLC and a commercial colorimetric method for the cholesterol. The quantitative methods showed an almost total separation and recovery of triterpenoids and lipids in their respective phases, while protein was detected in all phases after extraction. The protein content was determined by the method of Lowry and by amino acid analysis. Amino acid analysis was shown to be the reliable method of the two to quantitate proteins in iscoms. In conclusion, simple, reproducible and efficient procedures have been designed to isolate and quantitate the triterpenoids and lipids added for preparation of iscom-matrix and iscoms. The procedures described should also be useful to adequately define constituents in prospective vaccines.

Wave transmission approach based on modal analysis for embedded mechanical systems

NASA Astrophysics Data System (ADS)

Cretu, Nicolae; Nita, Gelu; Ioan Pop, Mihail

2013-09-01

An experimental method for determining the phase velocity in small solid samples is proposed. The method is based on measuring the resonant frequencies of a binary or ternary solid elastic system comprising the small sample of interest and a gauge material of manageable size. The wave transmission matrix of the combined system is derived and the theoretical values of its eigenvalues are used to determine the expected eigenfrequencies that, equated with the measured values, allow for the numerical estimation of the phase velocities in both materials. The known phase velocity of the gauge material is then used to asses the accuracy of the method. Using computer simulation and the experimental values for phase velocities, the theoretical values for the eigenfrequencies of the eigenmodes of the embedded elastic system are obtained, to validate the method. We conclude that the proposed experimental method may be reliably used to determine the elastic properties of small solid samples whose geometries do not allow a direct measurement of their resonant frequencies.

Microfluidic and nanofluidic phase behaviour characterization for industrial CO2, oil and gas.

PubMed

Bao, Bo; Riordon, Jason; Mostowfi, Farshid; Sinton, David

2017-08-08

Microfluidic systems that leverage unique micro-scale phenomena have been developed to provide rapid, accurate and robust analysis, predominantly for biomedical applications. These attributes, in addition to the ability to access high temperatures and pressures, have motivated recent expanded applications in phase measurements relevant to industrial CO 2 , oil and gas applications. We here present a comprehensive review of this exciting new field, separating microfluidic and nanofluidic approaches. Microfluidics is practical, and provides similar phase properties analysis to established bulk methods with advantages in speed, control and sample size. Nanofluidic phase behaviour can deviate from bulk measurements, which is of particular relevance to emerging unconventional oil and gas production from nanoporous shale. In short, microfluidics offers a practical, compelling replacement of current bulk phase measurement systems, whereas nanofluidics is not practical, but uniquely provides insight into phase change phenomena at nanoscales. Challenges, trends and opportunities for phase measurements at both scales are highlighted.

Analysis of digital communication signals and extraction of parameters

NASA Astrophysics Data System (ADS)

Al-Jowder, Anwar

1994-12-01

The signal classification performance of four types of electronics support measure (ESM) communications detection systems is compared from the standpoint of the unintended receiver (interceptor). Typical digital communication signals considered include binary phase shift keying (BPSK), quadrature phase shift keying (QPSK), frequency shift keying (FSK), and on-off keying (OOK). The analysis emphasizes the use of available signal processing software. Detection methods compared include broadband energy detection, FFT-based narrowband energy detection, and two correlation methods which employ the fast Fourier transform (FFT). The correlation methods utilize modified time-frequency distributions, where one of these is based on the Wigner-Ville distribution (WVD). Gaussian white noise is added to the signal to simulate various signal-to-noise ratios (SNR's).

A multi-residue method for the analysis of pesticides and pesticide degradates in water using HLB solid-phase extraction and gas chromatography-ion trap mass spectrometry

USGS Publications Warehouse

Hladik, M.L.; Smalling, K.L.; Kuivila, K.M.

2008-01-01

A method was developed for the analysis of over 60 pesticides and degradates in water by HLB solid-phase extraction and gas-chromatography/mass spectrometry. Method recoveries and detection limits were determined using two surface waters with different dissolved organic carbon (DOC) concentrations. In the lower DOC water, recoveries and detection limits were 80%-108% and 1-12 ng/L, respectively. In the higher DOC water, the detection limits were slightly higher (1-15 ng/L). Additionally, surface water samples from four sites were analyzed and 14 pesticides were detected with concentrations ranging from 4 to 1,200 ng/L. ?? 2008 Springer Science+Business Media, LLC.

Methods of chemical and phase composition analysis of gallstones

NASA Astrophysics Data System (ADS)

Suvorova, E. I.; Pantushev, V. V.; Voloshin, A. E.

2017-11-01

This review presents the instrumental methods used for chemical and phase composition investigation of gallstones. A great body of data has been collected in the literature on the presence of elements and their concentrations, obtained by fluorescence microscopy, X-ray fluorescence spectroscopy, neutron activation analysis, proton (particle) induced X-ray emission, atomic absorption spectroscopy, high-resolution gamma-ray spectrometry, electron paramagnetic resonance. Structural methods—powder X-ray diffraction, infrared spectroscopy, Raman spectroscopy—provide information about organic and inorganic phases in gallstones. Stone morphology was studied at the macrolevel with optical microscopy. Results obtained by analytical scanning and transmission electron microscopy with X-ray energy dispersive spectrometry are discussed. The chemical composition and structure of gallstones determine the strategy of removing stone from the body and treatment of patients: surgery or dissolution in the body. Therefore one chapter of the review describes the potential of dissolution methods. Early diagnosis and appropriate treatment of the disease depend on the development of clinical methods for in vivo investigation, which gave grounds to present the main characteristics and potential of ultrasonography (ultrasound scanning), magnetic resonance imaging, and X-ray computed tomography.

A two phase Mach number description of the equilibrium flow of nitrogen in ducts

NASA Technical Reports Server (NTRS)

Bursik, J. W.; Hall, R. M.; Adcock, J. B.

1979-01-01

Some additional thermodynamic properties of the usual two-phase form which is linear in the moisture fraction are derived which are useful in the analysis of many kinds of duct flow. The method used is based on knowledge of the vapor pressure and Gibbs function as functions of temperature. With these, additional two-phase functions linear in moisture fraction are generated, which ultimately reveal that the squared ratio of mixture specific volume to mixture sound speed depends on liquid mass fraction and temperature in the same manner as do many weighted mean two-phase properties. This leads to a simple method of calculating two-phase Mach numbers for various duct flows. The matching of one- and two-phase flows at a saturated vapor point with discontinuous Mach number is also discussed.

High sensitivity phase retrieval method in grating-based x-ray phase contrast imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Zhao; Gao, Kun; Chen, Jian

2015-02-15

Purpose: Grating-based x-ray phase contrast imaging is considered as one of the most promising techniques for future medical imaging. Many different methods have been developed to retrieve phase signal, among which the phase stepping (PS) method is widely used. However, further practical implementations are hindered, due to its complex scanning mode and high radiation dose. In contrast, the reverse projection (RP) method is a novel fast and low dose extraction approach. In this contribution, the authors present a quantitative analysis of the noise properties of the refraction signals retrieved by the two methods and compare their sensitivities. Methods: Using themore » error propagation formula, the authors analyze theoretically the signal-to-noise ratios (SNRs) of the refraction images retrieved by the two methods. Then, the sensitivities of the two extraction methods are compared under an identical exposure dose. Numerical experiments are performed to validate the theoretical results and provide some quantitative insight. Results: The SNRs of the two methods are both dependent on the system parameters, but in different ways. Comparison between their sensitivities reveals that for the refraction signal, the RP method possesses a higher sensitivity, especially in the case of high visibility and/or at the edge of the object. Conclusions: Compared with the PS method, the RP method has a superior sensitivity and provides refraction images with a higher SNR. Therefore, one can obtain highly sensitive refraction images in grating-based phase contrast imaging. This is very important for future preclinical and clinical implementations.« less

DBR, Sub-wavelength grating, and Photonic crystal slab Fabry-Perot cavity design using phase analysis by FDTD.

PubMed

Kim, Jae Hwan Eric; Chrostowski, Lukas; Bisaillon, Eric; Plant, David V

2007-08-06

We demonstrate a Finite-Difference Time-Domain (FDTD) phase methodology to estimate resonant wavelengths in Fabry-Perot (FP) cavity structures. We validate the phase method in a conventional Vertical-Cavity Surface-Emitting Laser (VCSEL) structure using a transfer-matrix method, and compare results with a FDTD reflectance method. We extend this approach to a Sub-Wavelength Grating (SWG) and a Photonic Crystal (Phc) slab, either of which may replace one of the Distributed Bragg Reflectors (DBRs) in the VCSEL, and predict resonant conditions with varying lithographic parameters. Finally, we compare the resonant tunabilities of three different VCSEL structures, taking quality factors into account.

A rapid hydrolysis method and DABS-Cl derivatization for complete amino acid analysis of octreotide acetate by reversed phase HPLC.

PubMed

Akhlaghi, Yousef; Ghaffari, Solmaz; Attar, Hossein; Alamir Hoor, Amir

2015-11-01

Octreotide as a synthetic cyclic octapeptide is a somatostatin analog with longer half-life and more selectivity for inhibition of the growth hormone. The acetate salt of octreotide is currently used for medical treatment of somatostatin-related disorders such as endocrine and carcinoid tumors, acromegaly, and gigantism. Octreotide contains both cysteine and tryptophan residues which make the hydrolysis part of its amino acid analysis procedure very challenging. The current paper introduces a fast and additive-free method which preserves tryptophan and cysteine residues during the hydrolysis. Using only 6 M HCl, this hydrolysis process is completed in 30 min at 150 °C. This fast hydrolysis method followed by pre-column derivatization of the released amino acids with 4-N,N-dimethylaminoazobenzene-4'-sulfonyl chloride (DABS-Cl) which takes only 20 min, makes it possible to do the complete amino acid analysis of an octreotide sample in a few hours. The highly stable-colored DABS-Cl derivatives can be detected in 436 nm in a reversed phase chromatographic system, which eliminates spectral interferences to a great extent. The amino acid analysis of octreotide acetate including hydrolysis, derivatization, and reversed phase HPLC determination was validated according to International Conference of Harmonization (ICH) guidelines.

Simultaneous determination of water-soluble vitamins in beverages and dietary supplements by LC-MS/MS.

PubMed

Kakitani, Ayano; Inoue, Tomonori; Matsumoto, Keiko; Watanabe, Jun; Nagatomi, Yasushi; Mochizuki, Naoki

2014-01-01

An LC-MS/MS method was developed for the simultaneous determination of 15 water-soluble vitamins that are widely used as additives in beverages and dietary supplements. This combined method involves the following simple pre-treatment procedures: dietary supplement samples were prepared by centrifugation and filtration after an extraction step, whereas beverage samples were diluted prior to injection. Chromatographic analysis in this method utilised a multi-mode ODS column, which provided reverse-phase, anion- and cation-exchange capacities, and therefore improved the retention of highly polar analytes such as water-soluble vitamins. Additionally, the multi-mode ODS column did not require adding ion pair reagents to the mobile phase. We optimised the chromatographic separation of 15 water-soluble vitamins by adjusting the mobile phase pH and the organic solvent. We also conducted an analysis of a NIST Standard Reference Material (SRM 3280 Multi-vitamin/Multi-element tablets) using this method to verify its accuracy. In addition, the method was applied to identify the vitamins in commercial beverages and dietary supplements. By comparing results with the label values and results obtained by official methods, it was concluded that the method could be used for quality control and to compose nutrition labels for vitamin-enriched products.

Development of high-throughput multi-residue method for non-steroidal anti-inflammatory drugs monitoring in swine muscle by LC-MS/MS.

PubMed

Castilhos, Tamara S; Barreto, Fabiano; Meneghini, Leonardo; Bergold, Ana Maria

2016-07-01

A reliable and simple method for the detection and quantification of residues of 14 non-steroidal anti-inflammatory drugs and a metamizole metabolite in swine muscle was developed using liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The samples were extracted with acetonitrile (ACN) in solid-liquid extraction followed by a low-temperature partitioning (LLE-LTP) process at -20 ± 2°C. After evaporation to dryness, the residue was reconstituted with hexane and a mixture of water:acetonitrile (1:1). LC separation was achieved on a reversed-phase (RP18) column with gradient elution using water (phase A) and ACN (phase B) both containing 1 mmol l(-)(1) ammonium acetate (NH4COO) with 0.025% acetic acid. Analysis was carried out on a triple-quadrupole tandem mass spectrometer (LC-MS/MS) in multiple reaction monitoring mode using an electrospray interface in negative and positive mode in a single run. Method validation was performed according to the criteria of Commission Decision No. 2002/657/EC. The matrix effect and linearity were evaluated. Decision limit (CCα), detection capability (CCβ), accuracy and repeatability of the method are also reported. The proposed method proved to be simple, easy and adequate for high-throughput analysis and was applied to routine analysis by the Brazilian Ministry of Agriculture, Livestock and Food Supply.

Phase retrieval with the reverse projection method in the presence of object's scattering

NASA Astrophysics Data System (ADS)

Wang, Zhili; Gao, Kun; Wang, Dajiang

2017-08-01

X-ray grating interferometry can provide substantially increased contrast over traditional attenuation-based techniques in biomedical applications, and therefore novel and complementary information. Recently, special attention has been paid to quantitative phase retrieval in X-ray grating interferometry, which is mandatory to perform phase tomography, to achieve material identification, etc. An innovative approach, dubbed ;Reverse Projection; (RP), has been developed for quantitative phase retrieval. The RP method abandons grating scanning completely, and is thus advantageous in terms of higher efficiency and reduced radiation damage. Therefore, it is expected that this novel method would find its potential in preclinical and clinical implementations. Strictly speaking, the reverse projection method is applicable for objects exhibiting only absorption and refraction. In this contribution, we discuss the phase retrieval with the reverse projection method for general objects with absorption, refraction and scattering simultaneously. Especially, we investigate the influence of the object's scattering on the retrieved refraction signal. Both theoretical analysis and numerical experiments are performed. The results show that the retrieved refraction signal is the product of object's refraction and scattering signals for small values. In the case of a strong scattering, the reverse projection method cannot provide reliable phase retrieval. Those presented results will guide the use of the reverse projection method for future practical applications, and help to explain some possible artifacts in the retrieved images and/or reconstructed slices.

A Unified Approach to Genotype Imputation and Haplotype-Phase Inference for Large Data Sets of Trios and Unrelated Individuals

PubMed Central

Browning, Brian L.; Browning, Sharon R.

2009-01-01

We present methods for imputing data for ungenotyped markers and for inferring haplotype phase in large data sets of unrelated individuals and parent-offspring trios. Our methods make use of known haplotype phase when it is available, and our methods are computationally efficient so that the full information in large reference panels with thousands of individuals is utilized. We demonstrate that substantial gains in imputation accuracy accrue with increasingly large reference panel sizes, particularly when imputing low-frequency variants, and that unphased reference panels can provide highly accurate genotype imputation. We place our methodology in a unified framework that enables the simultaneous use of unphased and phased data from trios and unrelated individuals in a single analysis. For unrelated individuals, our imputation methods produce well-calibrated posterior genotype probabilities and highly accurate allele-frequency estimates. For trios, our haplotype-inference method is four orders of magnitude faster than the gold-standard PHASE program and has excellent accuracy. Our methods enable genotype imputation to be performed with unphased trio or unrelated reference panels, thus accounting for haplotype-phase uncertainty in the reference panel. We present a useful measure of imputation accuracy, allelic R2, and show that this measure can be estimated accurately from posterior genotype probabilities. Our methods are implemented in version 3.0 of the BEAGLE software package. PMID:19200528

Industrial application of green chromatography--I. Separation and analysis of niacinamide in skincare creams using pure water as the mobile phase.

PubMed

Yang, Yu; Strickland, Zackary; Kapalavavi, Brahmam; Marple, Ronita; Gamsky, Chris

2011-03-15

In this work, chromatographic separation of niacin and niacinamide using pure water as the sole component in the mobile phase has been investigated. The separation and analysis of niacinamide have been optimized using three columns at different temperatures and various flow rates. Our results clearly demonstrate that separation and analysis of niacinamide from skincare products can be achieved using pure water as the eluent at 60°C on a Waters XTerra MS C18 column, a Waters XBridge C18 column, or at 80°C on a Hamilton PRP-1 column. The separation efficiency, quantification quality, and analysis time of this new method are at least comparable with those of the traditional HPLC methods. Compared with traditional HPLC, the major advantage of this newly developed green chromatography technique is the elimination of organic solvents required in the HPLC mobile phase. In addition, the pure water chromatography separations described in this work can be directly applied in industrial plant settings without further modification of the existing HPLC equipment. Copyright © 2011 Elsevier B.V. All rights reserved.

A Review of Content and Task Analysis Methodology. Technical Report No. 2.

ERIC Educational Resources Information Center

Gibbons, Andrew S.

A review of the literature related to methods for analyzing content or tasks prior to instructional development is presented. The review classifies methods according to a two-dimensional matrix. The first dimension differentiates phases of analysis, each dealing with content and tasks of a particular scope and each generating certain…

Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

2016-11-01

A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phase unwrapping methods of corner reflector DInSAR monitoring slow ground deformation

NASA Astrophysics Data System (ADS)

Fu, Wenxue; Guo, Xiaofang; Tian, Qingjiu

2007-06-01

Difference interferometric Synthetic aperture radar (DInSAR) has turned out to be a very powerful technique for the measurement of land deformations, but it requires the observed area to be correlated, and coherence degradation will seriously affect the quality of interferogram. Corner reflector DInSAR (CRDInSAR) is a new technique in recently years, which can compensate for the limitation of the classical DInSAR. Due to the stable amplitude and phase performance of the reflector, the interferometric phase difference of the reflector can be used to monitor or measure the small and slowly ground deformation for the cases of large geometrical baseline and large time interval between acquisitions. Phase unwrapping is the process where the absolute phase is reconstructed from its principal value as accurately as possible. It is a key step in the analysis of DInSAR. The classical phase unwrapping methods are either of path following type or of minimum-norm type. However, if the coherence of the two images is very low, the both methods will get error result. In application of CRDInSAR, due to the scattered points, the phase unwrapping of corner reflectors is only dealt with on a sparse grid, so all the reflectors are connected with Delaunay triangulation firstly, which can be used to define neighboring points and elementary cycles. When the monitoring ground deformation is slow, that is unwrapped neighboring-CR phase gradients are supposed to equal their wrapped-phase counterparts, then path-following method and Phase unwrapping using Coefficient of Elevation-Phase-Relation can be used to phase unwrapping. However, in the cases of unwrapped gradients exceeding one-half cycle, minimum cost flow (MCF) method can be used to unwrap the interferogram.

A sensitive and accurate method for the determination of perfluoroalkyl and polyfluoroalkyl substances in human serum using a high performance liquid chromatography-online solid phase extraction-tandem mass spectrometry.

PubMed

Yu, Chang Ho; Patel, Bhupendra; Palencia, Marilou; Fan, Zhihua Tina

2017-01-13

A selective, sensitive, and accurate analytical method for the measurement of perfluoroalkyl and polyfluoroalkyl substances (PFASs) in human serum, utilizing LC-MS/MS (liquid chromatography-tandem mass spectrometry), was developed and validated according to the Centers for Disease Control and Prevention (CDC) guidelines for biological sample analysis. Tests were conducted to determine the optimal analytical column, mobile phase composition and pH, gradient program, and cleaning procedure. The final analytical column selected for analysis was an extra densely bonded silica-packed reverse-phase column (Agilent XDB-C 8 , 3.0×100mm, 3.5μm). Mobile phase A was an aqueous buffer solution containing 10mM ammonium acetate (pH=4.3). Mobile phase B was a mixture of methanol and acetonitrile (1:1, v/v). The gradient program was programmed by initiating a fast elution (%B, from 40 to 65%) between 1.0 and 1.5min, followed by a slow elution (%B: 65-80%) in the period of 1.5-7.5min. The cleanup procedures were augmented by cleaning with (1) various solvents (isopropyl alcohol, methanol, acetonitrile, and reverse osmosis-purified water); (2) extensive washing steps for the autosampler and solid phase extraction (SPE) cartridge; and (3) a post-analysis cleaning step for the whole system. Under the above conditions, the resolution and sensitivity were significantly improved. Twelve target PFASs were baseline-separated (2.5-7.0min) within a 10-min of acquisition time. The limits of detection (LODs) were 0.01ng/mL or lower for all of the target compounds, making this method 5 times more sensitive than previously published methods. The newly developed method was validated in the linear range of 0.01-50ng/mL, and the accuracy (recovery between 80 and 120%) and precision (RSD<20%) were acceptable at three spiked levels (0.25, 2.5, and 25ng/mL). The method development and validation results demonstrated that this method was precise, accurate, and robust, with high-throughput (∼10min per sample); thus suitable for large-scale epidemiological studies. Published by Elsevier B.V.

An improved principal component analysis based region matching method for fringe direction estimation

NASA Astrophysics Data System (ADS)

He, A.; Quan, C.

2018-04-01

The principal component analysis (PCA) and region matching combined method is effective for fringe direction estimation. However, its mask construction algorithm for region matching fails in some circumstances, and the algorithm for conversion of orientation to direction in mask areas is computationally-heavy and non-optimized. We propose an improved PCA based region matching method for the fringe direction estimation, which includes an improved and robust mask construction scheme, and a fast and optimized orientation-direction conversion algorithm for the mask areas. Along with the estimated fringe direction map, filtered fringe pattern by automatic selective reconstruction modification and enhanced fast empirical mode decomposition (ASRm-EFEMD) is used for Hilbert spiral transform (HST) to demodulate the phase. Subsequently, windowed Fourier ridge (WFR) method is used for the refinement of the phase. The robustness and effectiveness of proposed method are demonstrated by both simulated and experimental fringe patterns.

Validated LC–MS-MS Method for Multiresidual Analysis of 13 Illicit Phenethylamines in Amniotic Fluid

PubMed Central

Burrai, Lucia; Nieddu, Maria; Carta, Antonio; Trignano, Claudia; Sanna, Raimonda; Boatto, Gianpiero

2016-01-01

A multi-residue analytical method was developed for the determination in amniotic fluid (AF) of 13 illicit phenethylamines, including 12 compounds never investigated in this matrix before. Samples were subject to solid-phase extraction using; hydrophilic–lipophilic balance cartridges which gave good recoveries and low matrix effects on analysis of the extracts. The quantification was performed by liquid chromatography electrospray tandem mass spectrometry. The water–acetonitrile mobile phase containing 0.1% formic acid, used with a C18 reversed phase column, provided adequate separation, resolution and signal-to-noise ratio for the analytes and the internal standard. The final optimized method was validated according to international guidelines. A monitoring campaign to assess fetal exposure to these 13 substances of abuse has been performed on AF test samples obtained from pregnant women. All mothers (n = 194) reported no use of drugs of abuse during pregnancy, and this was confirmed by the analytical data. PMID:26755540

Solid-phase microextraction and chiral HPLC analysis of ibuprofen in urine.

PubMed

de Oliveira, Anderson Rodrigo Moraes; Cesarino, Evandro José; Bonato, Pierina Sueli

2005-04-25

A simple and rapid solid-phase microextraction method was developed for the enantioselective analysis of ibuprofen in urine. The sampling was made with a polydimethylsiloxane-divinylbenzene coated fiber immersed in the liquid sample. After desorptioning from the fiber, ibuprofen enantiomers were analyzed by HPLC using a Chiralpak AD-RH column and UV detection. The mobile phase was made of methanol-pH 3.0 phosphoric acid solution (75:25, v/v), at a flow rate of 0.45 mL/min. The mean recoveries of SPME were 19.8 and 19.1% for (-)-R-ibuprofen and (+)-(S)-ibuprofen, respectively. The method was linear at the range of 0.25-25 microg/mL. Within-day and between-day assay precision and accuracy were below 15% for both ibuprofen enantiomers at concentrations of 0.75, 7.5 and 20 microg/mL. The method was tested with urine quality control samples and human urine fractions after administration of 200 mg rac-ibuprofen.

Single-phase power distribution system power flow and fault analysis

NASA Technical Reports Server (NTRS)

Halpin, S. M.; Grigsby, L. L.

1992-01-01

Alternative methods for power flow and fault analysis of single-phase distribution systems are presented. The algorithms for both power flow and fault analysis utilize a generalized approach to network modeling. The generalized admittance matrix, formed using elements of linear graph theory, is an accurate network model for all possible single-phase network configurations. Unlike the standard nodal admittance matrix formulation algorithms, the generalized approach uses generalized component models for the transmission line and transformer. The standard assumption of a common node voltage reference point is not required to construct the generalized admittance matrix. Therefore, truly accurate simulation results can be obtained for networks that cannot be modeled using traditional techniques.

Generating a Multiphase Equation of State with Swarm Intelligence

NASA Astrophysics Data System (ADS)

Cox, Geoffrey

2017-06-01

Hydrocode calculations require knowledge of the variation of pressure of a material with density and temperature, which is given by the equation of state. An accurate model needs to account for discontinuities in energy, density and properties of a material across a phase boundary. When generating a multiphase equation of state the modeller attempts to balance the agreement between the available data for compression, expansion and phase boundary location. However, this can prove difficult because minor adjustments in the equation of state for a single phase can have a large impact on the overall phase diagram. Recently, Cox and Christie described a method for combining statistical-mechanics-based condensed matter physics models with a stochastic analysis technique called particle swarm optimisation. The models produced show good agreement with experiment over a wide range of pressure-temperature space. This talk details the general implementation of this technique, shows example results, and describes the types of analysis that can be performed with this method.

"Observation Obscurer" - Time Series Viewer, Editor and Processor

NASA Astrophysics Data System (ADS)

Andronov, I. L.

The program is described, which contains a set of subroutines suitable for East viewing and interactive filtering and processing of regularly and irregularly spaced time series. Being a 32-bit DOS application, it may be used as a default fast viewer/editor of time series in any compute shell ("commander") or in Windows. It allows to view the data in the "time" or "phase" mode, to remove ("obscure") or filter outstanding bad points; to make scale transformations and smoothing using few methods (e.g. mean with phase binning, determination of the statistically opti- mal number of phase bins; "running parabola" (Andronov, 1997, As. Ap. Suppl, 125, 207) fit and to make time series analysis using some methods, e.g. correlation, autocorrelation and histogram analysis: determination of extrema etc. Some features have been developed specially for variable star observers, e.g. the barycentric correction, the creation and fast analysis of "OC" diagrams etc. The manual for "hot keys" is presented. The computer code was compiled with a 32-bit Free Pascal (www.freepascal.org).

Swept-frequency feedback interferometry using terahertz frequency QCLs: a method for imaging and materials analysis.

PubMed

Rakić, Aleksandar D; Taimre, Thomas; Bertling, Karl; Lim, Yah Leng; Dean, Paul; Indjin, Dragan; Ikonić, Zoran; Harrison, Paul; Valavanis, Alexander; Khanna, Suraj P; Lachab, Mohammad; Wilson, Stephen J; Linfield, Edmund H; Davies, A Giles

2013-09-23

The terahertz (THz) frequency quantum cascade laser (QCL) is a compact source of high-power radiation with a narrow intrinsic linewidth. As such, THz QCLs are extremely promising sources for applications including high-resolution spectroscopy, heterodyne detection, and coherent imaging. We exploit the remarkable phase-stability of THz QCLs to create a coherent swept-frequency delayed self-homodyning method for both imaging and materials analysis, using laser feedback interferometry. Using our scheme we obtain amplitude-like and phase-like images with minimal signal processing. We determine the physical relationship between the operating parameters of the laser under feedback and the complex refractive index of the target and demonstrate that this coherent detection method enables extraction of complex refractive indices with high accuracy. This establishes an ultimately compact and easy-to-implement THz imaging and materials analysis system, in which the local oscillator, mixer, and detector are all combined into a single laser.

Analysis of gene expression levels in individual bacterial cells without image segmentation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kwak, In Hae; Son, Minjun; Hagen, Stephen J., E-mail: sjhagen@ufl.edu

2012-05-11

Highlights: Black-Right-Pointing-Pointer We present a method for extracting gene expression data from images of bacterial cells. Black-Right-Pointing-Pointer The method does not employ cell segmentation and does not require high magnification. Black-Right-Pointing-Pointer Fluorescence and phase contrast images of the cells are correlated through the physics of phase contrast. Black-Right-Pointing-Pointer We demonstrate the method by characterizing noisy expression of comX in Streptococcus mutans. -- Abstract: Studies of stochasticity in gene expression typically make use of fluorescent protein reporters, which permit the measurement of expression levels within individual cells by fluorescence microscopy. Analysis of such microscopy images is almost invariably based on amore » segmentation algorithm, where the image of a cell or cluster is analyzed mathematically to delineate individual cell boundaries. However segmentation can be ineffective for studying bacterial cells or clusters, especially at lower magnification, where outlines of individual cells are poorly resolved. Here we demonstrate an alternative method for analyzing such images without segmentation. The method employs a comparison between the pixel brightness in phase contrast vs fluorescence microscopy images. By fitting the correlation between phase contrast and fluorescence intensity to a physical model, we obtain well-defined estimates for the different levels of gene expression that are present in the cell or cluster. The method reveals the boundaries of the individual cells, even if the source images lack the resolution to show these boundaries clearly.« less

Development and validation of a rapid ultra-high performance liquid chromatography method for the assay of benzalkonium chloride using a quality-by-design approach.

PubMed

Mallik, Rangan; Raman, Srividya; Liang, Xiaoli; Grobin, Adam W; Choudhury, Dilip

2015-09-25

A rapid robust reversed-phase UHPLC method has been developed for the analysis of total benzalkonium chloride in preserved drug formulation. A systematic Quality-by-Design (QbD) method development approach using commercial, off the shelf software (Fusion AE(®)) has been used to optimize the column, mobile phases, gradient time, and other HPLC conditions. Total benzalkonium chloride analysis involves simple sample preparation. The method uses gradient elution from an ACE Excel 2 C18-AR column (50mm×2.1mm, 2.0μm particle size), ammonium phosphate buffer (pH 3.3; 10mM) as aqueous mobile phase and methanol/acetonitrile (85/15, v/v) as the organic mobile phase with UV detection at 214nm. Using these conditions, major homologs of the benzalkonium chloride (C12 and C14) have been separated in less than 2.0min. The validation results confirmed that the method is precise, accurate and linear at concentrations ranging from 0.025mg/mL to 0.075mg/mL for total benzalkonium chloride. The recoveries ranged from 99% to 103% at concentrations from 0.025mg/mL to 0.075mg/mL for total benzalkonium chloride. The validation results also confirmed the robustness of the method as predicted by Fusion AE(®). Copyright © 2015 Elsevier B.V. All rights reserved.

Diagnosis of the three-phase induction motor using thermal imaging

NASA Astrophysics Data System (ADS)

Glowacz, Adam; Glowacz, Zygfryd

2017-03-01

Three-phase induction motors are used in the industry commonly for example woodworking machines, blowers, pumps, conveyors, elevators, compressors, mining industry, automotive industry, chemical industry and railway applications. Diagnosis of faults is essential for proper maintenance. Faults may damage a motor and damaged motors generate economic losses caused by breakdowns in production lines. In this paper the authors develop fault diagnostic techniques of the three-phase induction motor. The described techniques are based on the analysis of thermal images of three-phase induction motor. The authors analyse thermal images of 3 states of the three-phase induction motor: healthy three-phase induction motor, three-phase induction motor with 2 broken bars, three-phase induction motor with faulty ring of squirrel-cage. In this paper the authors develop an original method of the feature extraction of thermal images MoASoID (Method of Areas Selection of Image Differences). This method compares many training sets together and it selects the areas with the biggest changes for the recognition process. Feature vectors are obtained with the use of mentioned MoASoID and image histogram. Next 3 methods of classification are used: NN (the Nearest Neighbour classifier), K-means, BNN (the back-propagation neural network). The described fault diagnostic techniques are useful for protection of three-phase induction motor and other types of rotating electrical motors such as: DC motors, generators, synchronous motors.

Shear-wave velocity and site-amplification factors for 50 Australian sites determined by the spectral analysis of surface waves method

USGS Publications Warehouse

Kayen, Robert E.; Carkin, Bradley A.; Allen, Trevor; Collins, Clive; McPherson, Andrew; Minasian, Diane L.

2015-01-01

One-dimensional shear-wave velocity (VS ) profiles are presented at 50 strong motion sites in New South Wales and Victoria, Australia. The VS profiles are estimated with the spectral analysis of surface waves (SASW) method. The SASW method is a noninvasive method that indirectly estimates the VS at depth from variations in the Rayleigh wave phase velocity at the surface.

Analysis of verbal communication during teaching in the operating room and the potentials for surgical training.

PubMed

Blom, E M; Verdaasdonk, E G G; Stassen, L P S; Stassen, H G; Wieringa, P A; Dankelman, J

2007-09-01

Verbal communication in the operating room during surgical procedures affects team performance, reflects individual skills, and is related to the complexity of the operation process. During the procedural training of surgeons (residents), feedback and guidance is given through verbal communication. A classification method based on structural analysis of the contents was developed to analyze verbal communication. This study aimed to evaluate whether a classification method for the contents of verbal communication in the operating room could provide insight into the teaching processes. Eight laparoscopic cholecystectomies were videotaped. Two entire cholecystectomies and the dissection phase of six additional procedures were analyzed by categorization of the communication in terms of type (4 categories: commanding, explaining, questioning, and miscellaneous) and content (9 categories: operation method, location, direction, instrument handling, visualization, anatomy and pathology, general, private, undefinable). The operation was divided into six phases: start, dissection, clipping, separating, control, closing. Classification of the communication during two entire procedures showed that each phase of the operation was dominated by different kinds of communication. A high percentage of explaining anatomy and pathology was found throughout the whole procedure except for the control and closing phases. In the dissection phases, 60% of verbal communication concerned explaining. These explaining communication events were divided as follows: 27% operation method, 19% anatomy and pathology, 25% location (positioning of the instrument-tissue interaction), 15% direction (direction of tissue manipulation), 11% instrument handling, and 3% other nonclassified instructions. The proposed classification method is feasible for analyzing verbal communication during surgical procedures. Communication content objectively reflects the interaction between surgeon and resident. This information can potentially be used to specify training needs, and may contribute to the evaluation of different training methods.

An introduction to wavelet analysis in oceanography and meteorology - With application to the dispersion of Yanai waves

NASA Technical Reports Server (NTRS)

Meyers, Steven D.; Kelly, B. G.; O'Brien, J. J.

1993-01-01

Wavelet analysis is a relatively new technique that is an important addition to standard signal analysis methods. Unlike Fourier analysis that yields an average amplitude and phase for each harmonic in a dataset, the wavelet transform produces an instantaneous estimate or local value for the amplitude and phase of each harmonic. This allows detailed study of nonstationary spatial or time-dependent signal characteristics. The wavelet transform is discussed, examples are given, and some methods for preprocessing data for wavelet analysis are compared. By studying the dispersion of Yanai waves in a reduced gravity equatorial model, the usefulness of the transform is demonstrated. The group velocity is measured directly over a finite range of wavenumbers by examining the time evolution of the transform. The results agree well with linear theory at higher wavenumber but the measured group velocity is reduced at lower wavenumbers, possibly due to interaction with the basin boundaries.

Exhaled breath condensate – from an analytical point of view

PubMed Central

Dodig, Slavica; Čepelak, Ivana

2013-01-01

Over the past three decades, the goal of many researchers is analysis of exhaled breath condensate (EBC) as noninvasively obtained sample. A total quality in laboratory diagnostic processes in EBC analysis was investigated: pre-analytical (formation, collection, storage of EBC), analytical (sensitivity of applied methods, standardization) and post-analytical (interpretation of results) phases. EBC analysis is still used as a research tool. Limitations referred to pre-analytical, analytical, and post-analytical phases of EBC analysis are numerous, e.g. low concentrations of EBC constituents, single-analyte methods lack in sensitivity, and multi-analyte has not been fully explored, and reference values are not established. When all, pre-analytical, analytical and post-analytical requirements are met, EBC biomarkers as well as biomarker patterns can be selected and EBC analysis can hopefully be used in clinical practice, in both, the diagnosis and in the longitudinal follow-up of patients, resulting in better outcome of disease. PMID:24266297

Use of Probabilistic Engineering Methods in the Detailed Design and Development Phases of the NASA Ares Launch Vehicle

NASA Technical Reports Server (NTRS)

Fayssal, Safie; Weldon, Danny

2008-01-01

The United States National Aeronautics and Space Administration (NASA) is in the midst of a space exploration program called Constellation to send crew and cargo to the international Space Station, to the moon, and beyond. As part of the Constellation program, a new launch vehicle, Ares I, is being developed by NASA Marshall Space Flight Center. Designing a launch vehicle with high reliability and increased safety requires a significant effort in understanding design variability and design uncertainty at the various levels of the design (system, element, subsystem, component, etc.) and throughout the various design phases (conceptual, preliminary design, etc.). In a previous paper [1] we discussed a probabilistic functional failure analysis approach intended mainly to support system requirements definition, system design, and element design during the early design phases. This paper provides an overview of the application of probabilistic engineering methods to support the detailed subsystem/component design and development as part of the "Design for Reliability and Safety" approach for the new Ares I Launch Vehicle. Specifically, the paper discusses probabilistic engineering design analysis cases that had major impact on the design and manufacturing of the Space Shuttle hardware. The cases represent important lessons learned from the Space Shuttle Program and clearly demonstrate the significance of probabilistic engineering analysis in better understanding design deficiencies and identifying potential design improvement for Ares I. The paper also discusses the probabilistic functional failure analysis approach applied during the early design phases of Ares I and the forward plans for probabilistic design analysis in the detailed design and development phases.

Applying time-frequency analysis to assess cerebral autoregulation during hypercapnia.

PubMed

Placek, Michał M; Wachel, Paweł; Iskander, D Robert; Smielewski, Peter; Uryga, Agnieszka; Mielczarek, Arkadiusz; Szczepański, Tomasz A; Kasprowicz, Magdalena

2017-01-01

Classic methods for assessing cerebral autoregulation involve a transfer function analysis performed using the Fourier transform to quantify relationship between fluctuations in arterial blood pressure (ABP) and cerebral blood flow velocity (CBFV). This approach usually assumes the signals and the system to be stationary. Such an presumption is restrictive and may lead to unreliable results. The aim of this study is to present an alternative method that accounts for intrinsic non-stationarity of cerebral autoregulation and the signals used for its assessment. Continuous recording of CBFV, ABP, ECG, and end-tidal CO2 were performed in 50 young volunteers during normocapnia and hypercapnia. Hypercapnia served as a surrogate of the cerebral autoregulation impairment. Fluctuations in ABP, CBFV, and phase shift between them were tested for stationarity using sphericity based test. The Zhao-Atlas-Marks distribution was utilized to estimate the time-frequency coherence (TFCoh) and phase shift (TFPS) between ABP and CBFV in three frequency ranges: 0.02-0.07 Hz (VLF), 0.07-0.20 Hz (LF), and 0.20-0.35 Hz (HF). TFPS was estimated in regions locally validated by statistically justified value of TFCoh. The comparison of TFPS with spectral phase shift determined using transfer function approach was performed. The hypothesis of stationarity for ABP and CBFV fluctuations and the phase shift was rejected. Reduced TFPS was associated with hypercapnia in the VLF and the LF but not in the HF. Spectral phase shift was also decreased during hypercapnia in the VLF and the LF but increased in the HF. Time-frequency method led to lower dispersion of phase estimates than the spectral method, mainly during normocapnia in the VLF and the LF. The time-frequency method performed no worse than the classic one and yet may offer benefits from lower dispersion of phase shift as well as a more in-depth insight into the dynamic nature of cerebral autoregulation.

DETERMINATION OF VENLAFAXINE, VILAZODONE AND THEIR MAIN ACTIVE METABOLITES IN HUMAN SERUM BY HPLC-DAD AND HPLC-MS.

PubMed

Petruczynik, Anna; Wroblewski, Karol; Szultka-Mlynska, Malgorzata; Buszewsk, Boguslaw; Karakula-Juchnowicz, Hanna; Gajewski, Jacek; Morylowska-Topolska, Justyna; Waksmundzka-Hajnosi, Monika

2017-05-01

A high performance liquid chromatography (HPLC) method for simultaneous analysis of venlafaxine and its major metabolite 0-desmethylvenlafaxine and vilazodone and its methabolite M10 have been devel- oped and validated. Chromatography was performed on the Phenyl-Hexyl column with mobile phase containing methanol, acetate buffer at pH 3.5 and diethylamine. The application of stationary phase with 7r-7c moieties and mobile phase containing diethylamine as silanol blocker lets to obtain double protection against silanols and thus very high theoretical plate numbers were obtained. The good separation selectivity, good peaks' symmetry and very high systems efficiency for all investigated compounds were obtained in applied chromatographic system. The method is very efficient and suitable for the analysis of investigated drugs and their metabolites in human serum for patients' pharmacotherapy control.

Flow-gated radial phase-contrast imaging in the presence of weak flow.

PubMed

Peng, Hsu-Hsia; Huang, Teng-Yi; Wang, Fu-Nien; Chung, Hsiao-Wen

2013-01-01

To implement a flow-gating method to acquire phase-contrast (PC) images of carotid arteries without use of an electrocardiography (ECG) signal to synchronize the acquisition of imaging data with pulsatile arterial flow. The flow-gating method was realized through radial scanning and sophisticated post-processing methods including downsampling, complex difference, and correlation analysis to improve the evaluation of flow-gating times in radial phase-contrast scans. Quantitatively comparable results (R = 0.92-0.96, n = 9) of flow-related parameters, including mean velocity, mean flow rate, and flow volume, with conventional ECG-gated imaging demonstrated that the proposed method is highly feasible. The radial flow-gating PC imaging method is applicable in carotid arteries. The proposed flow-gating method can potentially avoid the setting up of ECG-related equipment for brain imaging. This technique has potential use in patients with arrhythmia or weak ECG signals.

Multiple velocity encoding in the phase of an MRI signal

NASA Astrophysics Data System (ADS)

Benitez-Read, E. E.

2017-01-01

The measurement of fluid velocity by encoding it in the phase of a magnetic resonance imaging (MRI) signal could allow the discrimination of the stationary spins signals from those of moving spins. This results in a wide variety of applications i.e. in medicine, in order to obtain more than angiograms, blood velocity images of veins, arteries and other vessels without having static tissue perturbing the signal of fluid in motion. The work presented in this paper is a theoretical analysis of some novel methods for multiple fluid velocity encoding in the phase of an MRI signal. These methods are based on a tripolar gradient (TPG) and can be an alternative to the conventional methods based on a bipolar gradient (BPG) and could be more suitable for multiple velocity encoding in the phase of an MRI signal.

On the relation between phase-field crack approximation and gradient damage modelling

NASA Astrophysics Data System (ADS)

Steinke, Christian; Zreid, Imadeddin; Kaliske, Michael

2017-05-01

The finite element implementation of a gradient enhanced microplane damage model is compared to a phase-field model for brittle fracture. Phase-field models and implicit gradient damage models share many similarities despite being conceived from very different standpoints. In both approaches, an additional differential equation and a length scale are introduced. However, while the phase-field method is formulated starting from the description of a crack in fracture mechanics, the gradient method starts from a continuum mechanics point of view. At first, the scope of application for both models is discussed to point out intersections. Then, the analysis of the employed mathematical methods and their rigorous comparison are presented. Finally, numerical examples are introduced to illustrate the findings of the comparison which are summarized in a conclusion at the end of the paper.

Hydrophilic interaction liquid chromatographic analysis of aminohydroxyphenylalanines from melanin pigments.

PubMed

Nezirević, Dzeneta; Arstrand, Kerstin; Kågedal, Bertil

2007-09-07

Malignant melanomas are more often seen in subjects with light colored skin who tan poorly than in persons who tan more rapidly. This has been attributed to the structure of their pigment, pheomelanin, which differs markedly from the eumelanin of persons with darker skin. To study the hydrolysis products of pheomelanin pigments a new method was developed for analysis of 4-amino-3-hydroxyphenylalanine (4-AHP) and 3-amino-4-hydroxyphenylalanine (3-AHP). Pheomelanin samples were hydrolyzed and extracted with solid-phase extraction columns using strong cation-exchange (SCX) cartridges. Separation of 4-AHP and 3-AHP was achieved on a ZIC-HILIC column (150 mm x 2.1mm I.D.) with a mobile phase consisting of acetonitrile: 0.1 M ammonium acetate buffer, pH 4.5 (82:18, v/v). Detection was performed with an electrochemical detector at +400 mV. Run time was 30 min. The limits of detection were 73 pg and 51 pg for 4-AHP and 3-AHP respectively, using 2 microl injections. Good linearity was found within the range 0.05-5.0 microg/ml. Absolute recovery was 70% and relative recovery was 100%. The AHPs were stable for 1 year in the hydrolyzed samples, for 4 days in the eluates from solid-phase sorbents stored in the refrigerator, and for 2 days diluted with mobile phase and stored in the autosampler at 10 degrees C. The within-day imprecision was <5% and the between-day imprecision was <7% for the two analytes. The method, applied to the analysis of pheomelanin in urine from human melanoma patients, allows the analysis of 30 samples in one set and is suitable for routine work with human hair and melanoma cells. By using the ZIC-HILIC stationary phase, ion-pairing reagents could be avoided, which makes the method suitable to further analysis of degradation products from pheomelanins using mass spectrometric detection.

Research on effects of phase error in phase-shifting interferometer

NASA Astrophysics Data System (ADS)

Wang, Hongjun; Wang, Zhao; Zhao, Hong; Tian, Ailing; Liu, Bingcai

2007-12-01

Referring to phase-shifting interferometry technology, the phase shifting error from the phase shifter is the main factor that directly affects the measurement accuracy of the phase shifting interferometer. In this paper, the resources and sorts of phase shifting error were introduction, and some methods to eliminate errors were mentioned. Based on the theory of phase shifting interferometry, the effects of phase shifting error were analyzed in detail. The Liquid Crystal Display (LCD) as a new shifter has advantage as that the phase shifting can be controlled digitally without any mechanical moving and rotating element. By changing coded image displayed on LCD, the phase shifting in measuring system was induced. LCD's phase modulation characteristic was analyzed in theory and tested. Based on Fourier transform, the effect model of phase error coming from LCD was established in four-step phase shifting interferometry. And the error range was obtained. In order to reduce error, a new error compensation algorithm was put forward. With this method, the error can be obtained by process interferogram. The interferogram can be compensated, and the measurement results can be obtained by four-step phase shifting interferogram. Theoretical analysis and simulation results demonstrate the feasibility of this approach to improve measurement accuracy.

Regional fringe analysis for improving depth measurement in phase-shifting fringe projection profilometry

NASA Astrophysics Data System (ADS)

Chien, Kuang-Che Chang; Tu, Han-Yen; Hsieh, Ching-Huang; Cheng, Chau-Jern; Chang, Chun-Yen

2018-01-01

This study proposes a regional fringe analysis (RFA) method to detect the regions of a target object in captured shifted images to improve depth measurement in phase-shifting fringe projection profilometry (PS-FPP). In the RFA method, region-based segmentation is exploited to segment the de-fringed image of a target object, and a multi-level fuzzy-based classification with five presented features is used to analyze and discriminate the regions of an object from the segmented regions, which were associated with explicit fringe information. Then, in the experiment, the performance of the proposed method is tested and evaluated on 26 test cases made of five types of materials. The qualitative and quantitative results demonstrate that the proposed RFA method can effectively detect the desired regions of an object to improve depth measurement in the PS-FPP system.

Bayesian Analysis of Evolutionary Divergence with Genomic Data under Diverse Demographic Models.

PubMed

Chung, Yujin; Hey, Jody

2017-06-01

We present a new Bayesian method for estimating demographic and phylogenetic history using population genomic data. Several key innovations are introduced that allow the study of diverse models within an Isolation-with-Migration framework. The new method implements a 2-step analysis, with an initial Markov chain Monte Carlo (MCMC) phase that samples simple coalescent trees, followed by the calculation of the joint posterior density for the parameters of a demographic model. In step 1, the MCMC sampling phase, the method uses a reduced state space, consisting of coalescent trees without migration paths, and a simple importance sampling distribution without the demography of interest. Once obtained, a single sample of trees can be used in step 2 to calculate the joint posterior density for model parameters under multiple diverse demographic models, without having to repeat MCMC runs. Because migration paths are not included in the state space of the MCMC phase, but rather are handled by analytic integration in step 2 of the analysis, the method is scalable to a large number of loci with excellent MCMC mixing properties. With an implementation of the new method in the computer program MIST, we demonstrate the method's accuracy, scalability, and other advantages using simulated data and DNA sequences of two common chimpanzee subspecies: Pan troglodytes (P. t.) troglodytes and P. t. verus. © The Author 2017. Published by Oxford University Press on behalf of the Society for Molecular Biology and Evolution. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Pseudotargeted MS Method for the Sensitive Analysis of Protein Phosphorylation in Protein Complexes.

PubMed

Lyu, Jiawen; Wang, Yan; Mao, Jiawei; Yao, Yating; Wang, Shujuan; Zheng, Yong; Ye, Mingliang

2018-05-15

In this study, we presented an enrichment-free approach for the sensitive analysis of protein phosphorylation in minute amounts of samples, such as purified protein complexes. This method takes advantage of the high sensitivity of parallel reaction monitoring (PRM). Specifically, low confident phosphopeptides identified from the data-dependent acquisition (DDA) data set were used to build a pseudotargeted list for PRM analysis to allow the identification of additional phosphopeptides with high confidence. The development of this targeted approach is very easy as the same sample and the same LC-system were used for the discovery and the targeted analysis phases. No sample fractionation or enrichment was required for the discovery phase which allowed this method to analyze minute amount of sample. We applied this pseudotargeted MS method to quantitatively examine phosphopeptides in affinity purified endogenous Shc1 protein complexes at four temporal stages of EGF signaling and identified 82 phospho-sites. To our knowledge, this is the highest number of phospho-sites identified from the protein complexes. This pseudotargeted MS method is highly sensitive in the identification of low abundance phosphopeptides and could be a powerful tool to study phosphorylation-regulated assembly of protein complex.

Validated chromatographic and spectrophotometric methods for analysis of some amoebicide drugs in their combined pharmaceutical preparation.

PubMed

Abdelaleem, Eglal Adelhamid; Abdelwahab, Nada Sayed

2013-01-01

This work is concerned with development and validation of chromatographic and spectrophotometric methods for analysis of mebeverine HCl (MEH), diloxanide furoate (DF) and metronidazole (MET) in Dimetrol® tablets - spectrophotometric and RP-HPLC methods using UV detection. The developed spectrophotometric methods depend on determination of MEH and DF in the combined dosage form using the successive derivative ratio spectra method which depends on derivatization of the obtained ratio spectra in two steps using methanol as a solvent and measuring MEH at 226.4-232.2 nm (peak to peak) and DF at 260.6-264.8 nm (peak to peak). While MET concentrations were determined using first derivative (1D) at λ = 327 nm using the same solvent. The chromatographic method depends on HPLC separation on ODS column and elution with a mobile phase consisting water: methanol: triethylamine (25: 75: 0.5, by volume, orthophosphoric acid to pH =4). Pumping the mobile phase at 0.7 ml min-1 with UV at 230 nm. Factors affecting the developed methods were studied and optimized, moreover, they have been validated as per ICH guideline and the results demonstrated that the suggested methods are reproducible, reliable and can be applied for routine use with short time of analysis. Statistical analysis of the two developed methods with each other using F and student's-t tests showed no significant difference.

Relaxation mode analysis of a peptide system: comparison with principal component analysis.

PubMed

Mitsutake, Ayori; Iijima, Hiromitsu; Takano, Hiroshi

2011-10-28

This article reports the first attempt to apply the relaxation mode analysis method to a simulation of a biomolecular system. In biomolecular systems, the principal component analysis is a well-known method for analyzing the static properties of fluctuations of structures obtained by a simulation and classifying the structures into some groups. On the other hand, the relaxation mode analysis has been used to analyze the dynamic properties of homopolymer systems. In this article, a long Monte Carlo simulation of Met-enkephalin in gas phase has been performed. The results are analyzed by the principal component analysis and relaxation mode analysis methods. We compare the results of both methods and show the effectiveness of the relaxation mode analysis.

Thermodynamic analysis of fuels in gas phase: ethanol, gasoline and ethanol - gasoline predicted by DFT method.

PubMed

Neto, A F G; Lopes, F S; Carvalho, E V; Huda, M N; Neto, A M J C; Machado, N T

2015-10-01

This paper presents a theoretical study using density functional theory to calculate thermodynamics properties of major molecules compounds at gas phase of fuels like gasoline, ethanol, and gasoline-ethanol mixture in thermal equilibrium on temperature range up to 1500 K. We simulated a composition of gasoline mixture with ethanol for a thorough study of thermal energy, enthalpy, Gibbs free energy, entropy, heat capacity at constant pressure with respect to temperature in order to study the influence caused by ethanol as an additive to gasoline. We used semi-empirical computational methods as well in order to know the efficiency of other methods to simulate fuels through this methodology. In addition, the ethanol influence through the changes in percentage fractions of chemical energy released in combustion reaction and the variations on thermal properties for autoignition temperatures of fuels was analyzed. We verified how ethanol reduces the chemical energy released by gasoline combustion and how at low temperatures the gas phase fuels in thermal equilibrium have similar thermodynamic behavior. Theoretical results were compared with experimental data, when available, and showed agreement. Graphical Abstract Thermodynamic analysis of fuels in gas phase.

Structure identification methods for atomistic simulations of crystalline materials

DOE PAGES

Stukowski, Alexander

2012-05-28

Here, we discuss existing and new computational analysis techniques to classify local atomic arrangements in large-scale atomistic computer simulations of crystalline solids. This article includes a performance comparison of typical analysis algorithms such as common neighbor analysis (CNA), centrosymmetry analysis, bond angle analysis, bond order analysis and Voronoi analysis. In addition we propose a simple extension to the CNA method that makes it suitable for multi-phase systems. Finally, we introduce a new structure identification algorithm, the neighbor distance analysis, which is designed to identify atomic structure units in grain boundaries.

Phase noise in oscillators as differential-algebraic systems with colored noise sources

NASA Astrophysics Data System (ADS)

Demir, Alper

2004-05-01

Oscillators are key components of many kinds of systems, particularly electronic and opto-electronic systems. Undesired perturbations, i.e. noise, in practical systems adversely affect the spectral and timing properties of the signals generated by oscillators resulting in phase noise and timing jitter, which are key performance limiting factors, being major contributors to bit-error-rate (BER) of RF and possibly optical communication systems, and creating synchronization problems in clocked and sampled-data electronic systems. In this paper, we review our work on the theory and numerical methods for nonlinear perturbation and noise analysis of oscillators described by a system of differential-algebraic equations (DAEs) with white and colored noise sources. The bulk of the work reviewed in this paper first appeared in [1], then in [2] and [3]. Prior to the work mentioned above, we developed a theory and numerical methods for nonlinear perturbation and noise analysis of oscillators described by a system of ordinary differential equations (ODEs) with white noise sources only [4, 5]. In this paper, we also discuss some open problems and issues in the modeling and analysis of phase noise both in free running oscillators and in phase/injection-locked ones.

Photometric geodesy of main-belt asteroids. IV - An updated analysis of lightcurves for poles, periods, and shapes

NASA Technical Reports Server (NTRS)

Drummond, J. D.; Weidenschilling, S. J.; Chapman, C. R.; Davis, D. R.

1991-01-01

The Drummond et al. (1988) analysis of main-belt asteroids is presently extended, using three independent methods to derive poles, periods, phase functions, and triaxial ellipsoid shapes from lightcurve maxima and minima. This group of 26 asteroids is also reinvestigated with a view to the distributions of triaxial shapes and obliquity distributions. Poles weakly tend to avoid asteroid orbital planes; a rough-smooth dichotomization appears to be justified by the persistence of two solar phase angle-amplitude relations. Seven of the objects may be Jacobi ellipsoids if axial ratios are slightly exaggerated by a systematic effect of the analytical method employed.

Structural Phase Evolution in Ultrasonic-Assisted Friction Stir Welded 2195 Aluminum Alloy Joints

NASA Astrophysics Data System (ADS)

Eliseev, A. A.; Fortuna, S. V.; Kalashnikova, T. A.; Chumaevskii, A. V.; Kolubaev, E. A.

2017-10-01

The authors examined the structural and phase state of fixed joints produced by method of friction stir welding (FSW) and ultrasonic-assisted friction stir welding (UAFSW) from extruded profile of aluminum alloy AA2195. In order to identify the role of ultrasonic application in the course of welding, such characteristics, as volume fraction and average size of secondary particles are compared in the base material and stir zones of FSW and UAFSW joints. By applying the methods of SEM and TEM analysis, researchers established the complex character of phase transitions as a result of ultrasonic application.

Model mismatch analysis and compensation for modal phase measuring deflectometry

DOE PAGES

Huang, Lei; Xue, Junpeng; Gao, Bo; ...

2017-01-11

The correspondence residuals due to the discrepancy between the reality and the shape model in use are analyzed for the modal phase measuring deflectometry. Slope residuals are calculated from these discrepancies between the modal estimation and practical acquisition. Since the shape mismatch mainly occurs locally, zonal integration methods which are good at dealing with local variations are used to reconstruct the height residual for compensation. Finally, results of both simulation and experiment indicate the proposed height compensation method is effective, which can be used as a post-complement for the modal phase measuring deflectometry.

A mid-layer model for human reliability analysis : understanding the cognitive causes of human failure events.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Song-Hua; Chang, James Y. H.; Boring,Ronald L.

2010-03-01

The Office of Nuclear Regulatory Research (RES) at the US Nuclear Regulatory Commission (USNRC) is sponsoring work in response to a Staff Requirements Memorandum (SRM) directing an effort to establish a single human reliability analysis (HRA) method for the agency or guidance for the use of multiple methods. As part of this effort an attempt to develop a comprehensive HRA qualitative approach is being pursued. This paper presents a draft of the method's middle layer, a part of the qualitative analysis phase that links failure mechanisms to performance shaping factors. Starting with a Crew Response Tree (CRT) that has identifiedmore » human failure events, analysts identify potential failure mechanisms using the mid-layer model. The mid-layer model presented in this paper traces the identification of the failure mechanisms using the Information-Diagnosis/Decision-Action (IDA) model and cognitive models from the psychological literature. Each failure mechanism is grouped according to a phase of IDA. Under each phase of IDA, the cognitive models help identify the relevant performance shaping factors for the failure mechanism. The use of IDA and cognitive models can be traced through fault trees, which provide a detailed complement to the CRT.« less

Semi-automatic tracking, smoothing and segmentation of hyoid bone motion from videofluoroscopic swallowing study.

PubMed

Kim, Won-Seok; Zeng, Pengcheng; Shi, Jian Qing; Lee, Youngjo; Paik, Nam-Jong

2017-01-01

Motion analysis of the hyoid bone via videofluoroscopic study has been used in clinical research, but the classical manual tracking method is generally labor intensive and time consuming. Although some automatic tracking methods have been developed, masked points could not be tracked and smoothing and segmentation, which are necessary for functional motion analysis prior to registration, were not provided by the previous software. We developed software to track the hyoid bone motion semi-automatically. It works even in the situation where the hyoid bone is masked by the mandible and has been validated in dysphagia patients with stroke. In addition, we added the function of semi-automatic smoothing and segmentation. A total of 30 patients' data were used to develop the software, and data collected from 17 patients were used for validation, of which the trajectories of 8 patients were partly masked. Pearson correlation coefficients between the manual and automatic tracking are high and statistically significant (0.942 to 0.991, P-value<0.0001). Relative errors between automatic tracking and manual tracking in terms of the x-axis, y-axis and 2D range of hyoid bone excursion range from 3.3% to 9.2%. We also developed an automatic method to segment each hyoid bone trajectory into four phases (elevation phase, anterior movement phase, descending phase and returning phase). The semi-automatic hyoid bone tracking from VFSS data by our software is valid compared to the conventional manual tracking method. In addition, the ability of automatic indication to switch the automatic mode to manual mode in extreme cases and calibration without attaching the radiopaque object is convenient and useful for users. Semi-automatic smoothing and segmentation provide further information for functional motion analysis which is beneficial to further statistical analysis such as functional classification and prognostication for dysphagia. Therefore, this software could provide the researchers in the field of dysphagia with a convenient, useful, and all-in-one platform for analyzing the hyoid bone motion. Further development of our method to track the other swallowing related structures or objects such as epiglottis and bolus and to carry out the 2D curve registration may be needed for a more comprehensive functional data analysis for dysphagia with big data.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

Purification of inkjet ink from water using liquid phase, electric discharge polymerization and cellulosic membrane filtration.

PubMed

Jordan, Alexander T; Hsieh, Jeffery S; Lee, Daniel T

2013-01-01

A method to separate inkjet ink from water was developed using a liquid phase, electric discharge process. The liquid phase, electric discharge process with filtration or sedimentation was shown to remove 97% of inkjet ink from solutions containing between 0.1-0.8 g/L and was consistent over a range of treatment conditions. Additionally, particle size analysis of treated allyl alcohol and treated propanol confirmed the electric discharge treatment has a polymerization mechanism, and small molecule analysis of treated methanol using gas chromatography and mass spectroscopy confirmed the mechanism was free radical initiated polymerization.

Self-Tuning Threshold Method for Real-Time Gait Phase Detection Based on Ground Contact Forces Using FSRs.

PubMed

Tang, Jing; Zheng, Jianbin; Wang, Yang; Yu, Lie; Zhan, Enqi; Song, Qiuzhi

2018-02-06

This paper presents a novel methodology for detecting the gait phase of human walking on level ground. The previous threshold method (TM) sets a threshold to divide the ground contact forces (GCFs) into on-ground and off-ground states. However, the previous methods for gait phase detection demonstrate no adaptability to different people and different walking speeds. Therefore, this paper presents a self-tuning triple threshold algorithm (STTTA) that calculates adjustable thresholds to adapt to human walking. Two force sensitive resistors (FSRs) were placed on the ball and heel to measure GCFs. Three thresholds (i.e., high-threshold, middle-threshold andlow-threshold) were used to search out the maximum and minimum GCFs for the self-adjustments of thresholds. The high-threshold was the main threshold used to divide the GCFs into on-ground and off-ground statuses. Then, the gait phases were obtained through the gait phase detection algorithm (GPDA), which provides the rules that determine calculations for STTTA. Finally, the STTTA reliability is determined by comparing the results between STTTA and Mariani method referenced as the timing analysis module (TAM) and Lopez-Meyer methods. Experimental results show that the proposed method can be used to detect gait phases in real time and obtain high reliability when compared with the previous methods in the literature. In addition, the proposed method exhibits strong adaptability to different wearers walking at different walking speeds.

Direct determination of one-dimensional interphase structures using normalized crystal truncation rod analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kawaguchi, Tomoya; Liu, Yihua; Reiter, Anthony

Here, a one-dimensional non-iterative direct method was employed for normalized crystal truncation rod analysis. The non-iterative approach, utilizing the Kramers–Kronig relation, avoids the ambiguities due to an improper initial model or incomplete convergence in the conventional iterative methods. The validity and limitations of the present method are demonstrated through both numerical simulations and experiments with Pt(111) in a 0.1 M CsF aqueous solution. The present method is compared with conventional iterative phase-retrieval methods.

Direct determination of one-dimensional interphase structures using normalized crystal truncation rod analysis

DOE PAGES

Kawaguchi, Tomoya; Liu, Yihua; Reiter, Anthony; ...

2018-04-20

Here, a one-dimensional non-iterative direct method was employed for normalized crystal truncation rod analysis. The non-iterative approach, utilizing the Kramers–Kronig relation, avoids the ambiguities due to an improper initial model or incomplete convergence in the conventional iterative methods. The validity and limitations of the present method are demonstrated through both numerical simulations and experiments with Pt(111) in a 0.1 M CsF aqueous solution. The present method is compared with conventional iterative phase-retrieval methods.

Statistical analysis of gravity waves characteristics observed by airglow imaging at Syowa Station (69S, 39E), Antarctica

NASA Astrophysics Data System (ADS)

Matsuda, Takashi S.; Nakamura, Takuji; Shiokawa, Kazuo; Tsutsumi, Masaki; Suzuki, Hidehiko; Ejiri, Mitsumu K.; Taguchi, Makoto

Atmospheric gravity waves (AGWs), which are generated in the lower atmosphere, transport significant amount of energy and momentum into the mesosphere and lower thermosphere and cause the mean wind accelerations in the mesosphere. This momentum deposit drives the general circulation and affects the temperature structure. Among many parameters to characterize AGWs, horizontal phase velocity is very important to discuss the vertical propagation. Airglow imaging is a useful technique for investigating the horizontal structures of AGWs at around 90 km altitude. Recently, there are many reports about statistical characteristics of AGWs observed by airglow imaging. However, comparison of these results obtained at various locations is difficult because each research group uses its own method for extracting and analyzing AGW events. We have developed a new statistical analysis method for obtaining the power spectrum in the horizontal phase velocity domain from airglow image data, so as to deal with huge amounts of imaging data obtained on different years and at various observation sites, without bias caused by different event extraction criteria for the observer. This method was applied to the data obtained at Syowa Station, Antarctica, in 2011 and compared with a conventional event analysis in which the phase fronts were traced manually in order to estimate horizontal characteristics. This comparison shows that our new method is adequate to deriving the horizontal phase velocity characteristics of AGWs observed by airglow imaging technique. We plan to apply this method to airglow imaging data observed at Syowa Station in 2002 and between 2008 and 2013, and also to the data observed at other stations in Antarctica (e.g. Rothera Station (67S, 68W) and Halley Station (75S, 26W)), in order to investigate the behavior of AGWs propagation direction and source distribution in the MLT region over Antarctica. In this presentation, we will report interim analysis result of the data at Syowa Station.

RP-HPLC×HILIC chromatography for quantifying ertapenem sodium with a look at green chemistry.

PubMed

Pedroso, Tahisa M; Medeiros, Ana C D; Salgado, Herida R N

2016-11-01

Ertapenem sodium is a polar and ionizable compound; therefore, it has little retention on traditional C18 columns in reverse-phase high-performance liquid chromatography, even using a highly-aqueous mobile phase that can result in dewetting in the stationary phase. Thus, the most coherent process for ERTM is to develop a method for Hydrophilic Interaction Chromatography. However, for the traditional methods in HILIC, the use of a highly organic mobile phase is necessary; usually an amount exceeding 80% acetonitrile is necessary. On the other hand, the RP-HPLC mode is considered for the analysis technique, which is more often used for quantification of substances, and new columns are often introduced to analyze different groups of compounds. Two new analytical methods have been developed for routine analysis. The proposed chromatographic method was adequate and advantageous by presenting simplicity, linearity, precision, accuracy, robustness, detection limits, and satisfactory quantification. Analytical methods are constantly undergoing changes and improvements. Researchers worldwide are rapidly adopting Green Chemistry. The development of new pharmaceutical methods based in Green chemistry has been encouraged by universities and the pharmaceutical industry. Issues related to green chemistry are in evidence and they have been featured in international journals of high impact. The methods described here have economic advantages and they feature an eco-friendly focus, which is discussed in this work. This work was developed with an environmental conscience, always looking to minimize the possible generated organic waste. Therefore, discussion on this aspect is included. Copyright © 2016 Elsevier B.V. All rights reserved.

Finite element methods for the biomechanics of soft hydrated tissues: nonlinear analysis and adaptive control of meshes.

PubMed

Spilker, R L; de Almeida, E S; Donzelli, P S

1992-01-01

This chapter addresses computationally demanding numerical formulations in the biomechanics of soft tissues. The theory of mixtures can be used to represent soft hydrated tissues in the human musculoskeletal system as a two-phase continuum consisting of an incompressible solid phase (collagen and proteoglycan) and an incompressible fluid phase (interstitial water). We first consider the finite deformation of soft hydrated tissues in which the solid phase is represented as hyperelastic. A finite element formulation of the governing nonlinear biphasic equations is presented based on a mixed-penalty approach and derived using the weighted residual method. Fluid and solid phase deformation, velocity, and pressure are interpolated within each element, and the pressure variables within each element are eliminated at the element level. A system of nonlinear, first-order differential equations in the fluid and solid phase deformation and velocity is obtained. In order to solve these equations, the contributions of the hyperelastic solid phase are incrementally linearized, a finite difference rule is introduced for temporal discretization, and an iterative scheme is adopted to achieve equilibrium at the end of each time increment. We demonstrate the accuracy and adequacy of the procedure using a six-node, isoparametric axisymmetric element, and we present an example problem for which independent numerical solution is available. Next, we present an automated, adaptive environment for the simulation of soft tissue continua in which the finite element analysis is coupled with automatic mesh generation, error indicators, and projection methods. Mesh generation and updating, including both refinement and coarsening, for the two-dimensional examples examined in this study are performed using the finite quadtree approach. The adaptive analysis is based on an error indicator which is the L2 norm of the difference between the finite element solution and a projected finite element solution. Total stress, calculated as the sum of the solid and fluid phase stresses, is used in the error indicator. To allow the finite difference algorithm to proceed in time using an updated mesh, solution values must be transferred to the new nodal locations. This rezoning is accomplished using a projected field for the primary variables. The accuracy and effectiveness of this adaptive finite element analysis is demonstrated using a linear, two-dimensional, axisymmetric problem corresponding to the indentation of a thin sheet of soft tissue. The method is shown to effectively capture the steep gradients and to produce solutions in good agreement with independent, converged, numerical solutions.

Thermal decomposition in thermal desorption instruments: importance of thermogram measurements for analysis of secondary organic aerosol

NASA Astrophysics Data System (ADS)

Stark, H.; Yatavelli, R. L. N.; Thompson, S.; Kang, H.; Krechmer, J. E.; Kimmel, J.; Palm, B. B.; Hu, W.; Hayes, P.; Day, D. A.; Campuzano Jost, P.; Ye, P.; Canagaratna, M. R.; Jayne, J. T.; Worsnop, D. R.; Jimenez, J. L.

2017-12-01

Understanding the chemical composition of secondary organic aerosol (SOA) is crucial for explaining sources and fate of this important aerosol class in tropospheric chemistry. Further, determining SOA volatility is key in predicting its atmospheric lifetime and fate, due to partitioning from and to the gas phase. We present three analysis approaches to determine SOA volatility distributions from two field campaigns in areas with strong biogenic emissions, a Ponderosa pine forest in Colorado, USA, from the BEACHON-RoMBAS campaign, and a mixed forest in Alabama, USA, from the SOAS campaign. We used a high-resolution-time-of-flight chemical ionization mass spectrometer (CIMS) for both campaigns, equipped with a micro-orifice volatilization impactor (MOVI) inlet for BEACHON and a filter inlet for gases and aerosols (FIGAERO) for SOAS. These inlets allow near simultaneous analysis of particle and gas-phase species by the CIMS. While gas-phase species are directly measured without heating, particles undergo thermal desorption prior to analysis. Volatility distributions can be estimated in three ways: (1) analysis of the thermograms (signal vs. temperature); (2) via partitioning theory using the gas- and particle-phase measurements; (3) from measured chemical formulas via a group contribution model. Comparison of the SOA volatility distributions from the three methods shows large discrepancies for both campaigns. Results from the thermogram method are the most consistent of the methods when compared with independent AMS-thermal denuder measurements. The volatility distributions estimated from partitioning measurements are very narrow, likely due to signal-to-noise limits in the measurements. The discrepancy between the formula and the thermogram methods indicates large-scale thermal decomposition of the SOA species. We will also show results of citric acid thermal decomposition, where, in addition to the mass spectra, measurements of CO, CO2 and H2O were made, showing thermal decomposition of up to 65% of the citric acid molecules.

Fast analysis of capsaicinoids in Naga Jolokia extracts (Capsicum chinense) by high-performance liquid chromatography using fused core columns.

PubMed

Stipcovich, Tea; Barbero, Gerardo F; Ferreiro-González, Marta; Palma, Miguel; Barroso, Carmelo G

2018-01-15

A rapid high-performance liquid chromatography method with a C18 reverse-phase fused-core column has been developed for the determination and quantification of the main capsaicinoids (nornordihydrocapsaicin, nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin and homodihydrocapsaicin) present in Naga Jolokia peppers. A fused-core Kinetex™ C18 column (50×2.1mm i.d.; 2.6μm) was used for the analysis. The chromatographic separation was obtained with a gradient method in which the mobile phase was water (0.1% acetic acid) as solvent A and acetonitrile (0.1% acetic acid) as solvent B. The separation of all compounds was achieved in less than 3min with a total analysis time (sample-to-sample) of 10min. The robustness of the method was evaluated. The method showed excellent repeatability and intermediate precision expressed as coefficient of variance of less than 2%. The developed method was employed for the quantification of the major capsaicinoids present in different peppers and commercial products containing chilli peppers. Copyright © 2017 Elsevier Ltd. All rights reserved.

Can matrix solid phase dispersion (MSPD) be more simplified? Application of solventless MSPD sample preparation method for GC-MS and GC-FID analysis of plant essential oil components.

PubMed

Wianowska, Dorota; Dawidowicz, Andrzej L

2016-05-01

This paper proposes and shows the analytical capabilities of a new variant of matrix solid phase dispersion (MSPD) with the solventless blending step in the chromatographic analysis of plant volatiles. The obtained results prove that the use of a solvent is redundant as the sorption ability of the octadecyl brush is sufficient for quantitative retention of volatiles from 9 plants differing in their essential oil composition. The extraction efficiency of the proposed simplified MSPD method is equivalent to the efficiency of the commonly applied variant of MSPD with the organic dispersing liquid and pressurized liquid extraction, which is a much more complex, technically advanced and highly efficient technique of plant extraction. The equivalency of these methods is confirmed by the variance analysis. The proposed solventless MSPD method is precise, accurate, and reproducible. The recovery of essential oil components estimated by the MSPD method exceeds 98%, which is satisfactory for analytical purposes. Copyright © 2016 Elsevier B.V. All rights reserved.

Spectral analysis and quantum chemical studies of chair and twist-boat conformers of cycloheximide in gas and solution phases

NASA Astrophysics Data System (ADS)

Tokatli, A.; Ucun, F.; Sütçü, K.; Osmanoğlu, Y. E.; Osmanoğlu, Ş.

2018-02-01

In this study the conformational behavior of cycloheximide in the gas and solution (CHCl3) phases has theoretically been investigated by spectroscopic and quantum chemical properties using density functional theory (wB97X-D) method with 6-31++G(d,p) basis set, for the first time. The calculated IR results reveal that in the ground state the molecule exits as a mixture of the chair and twist-boat conformers in the gas phase, while the calculated NMR results reveal that it only exits as the chair conformer in the solution phase. In order to obtain the contributions coming from intramolecular interactions to the stability of the conformers in the gas and solution phases, the quantum theory of atoms in molecules (QTAIM), noncovalent interactions (NCI) method, and natural bond orbital analysis (NBO) have been employed. The QTAIM and NCI methods indicated that by intramolecular interactions with bond critical point (BCP) the twist-boat conformer is more stabilized than the chair conformer, while by steric interactions it is more destabilized. Considering that these interactions balance each other, the stabilities of the conformers are understood to be dictated by the van der Waals interactions. The NBO analyses show that the hyperconjugative and steric effects play an important role in the stabilization in the gas and solution phases. Furthermore, to get a better understanding of the chemical behavior of this important antibiotic drug we have evaluated and, commented the global and local reactivity descriptors of the both conformers. Finally, the EPR analysis of γ-irradiated cycloheximide has been done. The comparison of the experimental and calculated data have showed the inducement of a radical structure of (CH2)2ĊCH2 in the molecule. The experimental EPR spectrum has also confirmed that the molecule simultaneously exists in the chair and twist-boat conformers in the solid phase.

Discrimination between biologically relevant calcium phosphate phases by surface-analytical techniques

NASA Astrophysics Data System (ADS)

Kleine-Boymann, Matthias; Rohnke, Marcus; Henss, Anja; Peppler, Klaus; Sann, Joachim; Janek, Juergen

2014-08-01

The spatially resolved phase identification of biologically relevant calcium phosphate phases (CPPs) in bone tissue is essential for the elucidation of bone remodeling mechanisms and for the diagnosis of bone diseases. Analytical methods with high spatial resolution for the discrimination between chemically quite close phases are rare. Therefore the applicability of state-of-the-art ToF-SIMS, XPS and EDX as chemically specific techniques was investigated. The eight CPPs hydroxyapatite (HAP), β-tricalcium phosphate (β-TCP), α-tricalcium phosphate (α-TCP), octacalcium phosphate (OCP), dicalcium phosphate dihydrate (DCPD), dicalcium phosphate (DCP), monocalcium phosphate (MCP) and amorphous calcium phosphate (ACP) were either commercial materials in high purity or synthesized by ourselves. The phase purity was proven by XRD analysis. All of the eight CPPs show different mass spectra and the phases can be discriminated by applying the principal component analysis method to the mass spectrometric data. The Ca/P ratios of all phosphates were determined by XPS and EDX. With both methods some CPPs can be distinguished, but the obtained Ca/P ratios deviate systematically from their theoretical values. It is necessary in any case to determine a calibration curve, respectively the ZAF values, from appropriate standards. In XPS also the O(1s)-satellite signals are correlated to the CPPs composition. Angle resolved and long-term XPS measurements of HAP clearly prove that there is no phosphate excess at the surface. Decomposition due to X-ray irradiation has not been observed.

Full-Field Calibration of Color Camera Chromatic Aberration using Absolute Phase Maps.

PubMed

Liu, Xiaohong; Huang, Shujun; Zhang, Zonghua; Gao, Feng; Jiang, Xiangqian

2017-05-06

The refractive index of a lens varies for different wavelengths of light, and thus the same incident light with different wavelengths has different outgoing light. This characteristic of lenses causes images captured by a color camera to display chromatic aberration (CA), which seriously reduces image quality. Based on an analysis of the distribution of CA, a full-field calibration method based on absolute phase maps is proposed in this paper. Red, green, and blue closed sinusoidal fringe patterns are generated, consecutively displayed on an LCD (liquid crystal display), and captured by a color camera from the front viewpoint. The phase information of each color fringe is obtained using a four-step phase-shifting algorithm and optimum fringe number selection method. CA causes the unwrapped phase of the three channels to differ. These pixel deviations can be computed by comparing the unwrapped phase data of the red, blue, and green channels in polar coordinates. CA calibration is accomplished in Cartesian coordinates. The systematic errors introduced by the LCD are analyzed and corrected. Simulated results show the validity of the proposed method and experimental results demonstrate that the proposed full-field calibration method based on absolute phase maps will be useful for practical software-based CA calibration.

Analysis of nanoscale two-phase flow of argon using molecular dynamics

NASA Astrophysics Data System (ADS)

Verma, Abhishek Kumar; Kumar, Rakesh

2014-12-01

Two phase flows through micro and nanochannels have attracted a lot of attention because of their immense applicability to many advanced fields such as MEMS/NEMS, electronic cooling, bioengineering etc. In this work, a molecular dynamics simulation method is employed to study the condensation process of superheated argon vapor force driven flow through a nanochannel combining fluid flow and heat transfer. A simple and effective particle insertion method is proposed to model phase change of argon based on non-periodic boundary conditions in the simulation domain. Starting from a crystalline solid wall of channel, the condensation process evolves from a transient unsteady state where we study the influence of different wall temperatures and fluid wall interactions on interfacial and heat transport properties of two phase flows. Subsequently, we analyzed transient temperature, density and velocity fields across the channel and their dependency on varying wall temperature and fluid wall interaction, after a dynamic equilibrium is achieved in phase transition. Quasi-steady nonequilibrium temperature profile, heat flux and interfacial thermal resistance were analyzed. The results demonstrate that the molecular dynamics method, with the proposed particle insertion method, effectively solves unsteady nonequilibrium two phase flows at nanoscale resolutions whose interphase between liquid and vapor phase is typically of the order of a few molecular diameters.

Single particle analysis based on Zernike phase contrast transmission electron microscopy.

PubMed

Danev, Radostin; Nagayama, Kuniaki

2008-02-01

We present the first application of Zernike phase-contrast transmission electron microscopy to single-particle 3D reconstruction of a protein, using GroEL chaperonin as the test specimen. We evaluated the performance of the technique by comparing 3D models derived from Zernike phase contrast imaging, with models from conventional underfocus phase contrast imaging. The same resolution, about 12A, was achieved by both imaging methods. The reconstruction based on Zernike phase contrast data required about 30% fewer particles. The advantages and prospects of each technique are discussed.

Optimization of propagation-based x-ray phase-contrast tomography for breast cancer imaging

NASA Astrophysics Data System (ADS)

Baran, P.; Pacile, S.; Nesterets, Y. I.; Mayo, S. C.; Dullin, C.; Dreossi, D.; Arfelli, F.; Thompson, D.; Lockie, D.; McCormack, M.; Taba, S. T.; Brun, F.; Pinamonti, M.; Nickson, C.; Hall, C.; Dimmock, M.; Zanconati, F.; Cholewa, M.; Quiney, H.; Brennan, P. C.; Tromba, G.; Gureyev, T. E.

2017-03-01

The aim of this study was to optimise the experimental protocol and data analysis for in-vivo breast cancer x-ray imaging. Results are presented of the experiment at the SYRMEP beamline of Elettra Synchrotron using the propagation-based phase-contrast mammographic tomography method, which incorporates not only absorption, but also x-ray phase information. In this study the images of breast tissue samples, of a size corresponding to a full human breast, with radiologically acceptable x-ray doses were obtained, and the degree of improvement of the image quality (from the diagnostic point of view) achievable using propagation-based phase-contrast image acquisition protocols with proper incorporation of x-ray phase retrieval into the reconstruction pipeline was investigated. Parameters such as the x-ray energy, sample-to-detector distance and data processing methods were tested, evaluated and optimized with respect to the estimated diagnostic value using a mastectomy sample with a malignant lesion. The results of quantitative evaluation of images were obtained by means of radiological assessment carried out by 13 experienced specialists. A comparative analysis was performed between the x-ray and the histological images of the specimen. The results of the analysis indicate that, within the investigated range of parameters, both the objective image quality characteristics and the subjective radiological scores of propagation-based phase-contrast images of breast tissues monotonically increase with the strength of phase contrast which in turn is directly proportional to the product of the radiation wavelength and the sample-to-detector distance. The outcomes of this study serve to define the practical imaging conditions and the CT reconstruction procedures appropriate for low-dose phase-contrast mammographic imaging of live patients at specially designed synchrotron beamlines.

Determination of partition coefficient and analysis of nitrophenols by three-phase liquid-phase microextraction coupled with capillary electrophoresis.

PubMed

Sanagi, Mohd Marsin; Miskam, Mazidatulakmam; Wan Ibrahim, Wan Aini; Hermawan, Dadan; Aboul-Enein, Hassan Y

2010-07-01

A three-phase hollow fiber liquid-phase microextraction method coupled with CE was developed and used for the determination of partition coefficients and analysis of selected nitrophenols in water samples. The selected nitrophenols were extracted from 14 mL of aqueous solution (donor solution) with the pH adjusted to pH 3 into an organic phase (1-octanol) immobilized in the pores of the hollow fiber and finally backextracted into 40.0 microL of the acceptor phase (NaOH) at pH 12.0 located inside the lumen of the hollow fiber. The extractions were carried out under the following optimum conditions: donor solution, 0.05 M H(3)PO(4), pH 3.0; organic solvent, 1-octanol; acceptor solution, 40 microL of 0.1 M NaOH, pH 12.0; agitation rate, 1050 rpm; extraction time, 15 min. Under optimized conditions, the calibration curves for the analytes were linear in the range of 0.05-0.30 mg/L with r(2)>0.9900 and LODs were in the range of 0.01-0.04 mg/L with RSDs of 1.25-2.32%. Excellent enrichment factors of up to 398-folds were obtained. It was found that the partition coefficient (K(a/d)) values were high for 2-nitrophenol, 3-nitrophenol, 4-nitrophenol, 2,4-dinitrophenol and 2,6-dinitrophenol and that the individual partition coefficients (K(org/d) and K(a/org)) promoted efficient simultaneous extraction from the donor through the organic phase and further into the acceptor phase. The developed method was successfully applied for the analysis of water samples.

Rapid analysis of dissolved methane, ethylene, acetylene and ethane using partition coefficients and headspace-gas chromatography.

PubMed

Lomond, Jasmine S; Tong, Anthony Z

2011-01-01

Analysis of dissolved methane, ethylene, acetylene, and ethane in water is crucial in evaluating anaerobic activity and investigating the sources of hydrocarbon contamination in aquatic environments. A rapid chromatographic method based on phase equilibrium between water and its headspace is developed for these analytes. The new method requires minimal sample preparation and no special apparatus except those associated with gas chromatography. Instead of Henry's Law used in similar previous studies, partition coefficients are used for the first time to calculate concentrations of dissolved hydrocarbon gases, which considerably simplifies the calculation involved. Partition coefficients are determined to be 128, 27.9, 1.28, and 96.3 at 30°C for methane, ethylene, acetylene, and ethane, respectively. It was discovered that the volume ratio of gas-to-liquid phase is critical to the accuracy of the measurements. The method performance can be readily improved by reducing the volume ratio of the two phases. Method validation shows less than 6% variation in accuracy and precision except at low levels of methane where interferences occur in ambient air. Method detection limits are determined to be in the low ng/L range for all analytes. The performance of the method is further tested using environmental samples collected from various sites in Nova Scotia.

Method of LSD profile asymmetry for estimating the center of mass velocities of pulsating stars

NASA Astrophysics Data System (ADS)

Britavskiy, Nikolay; Pancino, Elena; Romano, Donatella; Tsymbal, Vadim

2015-08-01

We present radial velocity analysis for 20 solar neighborhood RR Lyrae and 3 Population II Cepheids. High-resolution spectra were observed with either TNG/SARG or VLT/UVES over varying phases. To estimate the center of mass (barycentric) velocities of the program stars, we utilized two independent methods. First, the 'classic' method was employed, which is based on RR Lyrae radial velocity curve templates. Second, we provide the new method that used absorption line profile asymmetry to determine both the pulsation and the barycentric velocities even with a low number of high-resolution spectra and in cases where the phase of the observations is uncertain. This new method is based on a Least Squares Deconvolution (LSD) of the line profiles in order to analyze line asymmetry that occurs in the spectra of pulsating stars. By applying this method to our sample stars we attain accurate measurements (± 1 km/s) of the pulsation component of the radial velocity. This results in determination of the barycentric velocity to within 5 km/s even with a low number of high-resolution spectra. A detailed investigation of LSD profile asymmetry shows the variable nature of the project factor at different pulsation phases, which should be taken into account in the detailed spectroscopic analysis of pulsating stars.

Method of LSD profile asymmetry for estimating the center of mass velocities of pulsating stars

NASA Astrophysics Data System (ADS)

Britavskiy, N.; Pancino, E.; Tsymbal, V.; Romano, D.; Cacciari, C.; Clementini, C.

2016-05-01

We present radial velocity analysis for 20 solar neighborhood RR Lyrae and 3 Population II Cepheids. High-resolution spectra were observed with either TNG/SARG or VLT/UVES over varying phases. To estimate the center of mass (barycentric) velocities of the program stars, we utilized two independent methods. First, the 'classic' method was employed, which is based on RR Lyrae radial velocity curve templates. Second, we provide the new method that used absorption line profile asymmetry to determine both the pulsation and the barycentric velocities even with a low number of high-resolution spectra and in cases where the phase of the observations is uncertain. This new method is based on a least squares deconvolution (LSD) of the line profiles in order to an- alyze line asymmetry that occurs in the spectra of pulsating stars. By applying this method to our sample stars we attain accurate measurements (+- 2 kms^-1) of the pulsation component of the radial velocity. This results in determination of the barycentric velocity to within 5 kms^-1 even with a low number of high- resolution spectra. A detailed investigation of LSD profile asymmetry shows the variable nature of the project factor at different pulsation phases, which should be taken into account in the detailed spectroscopic analysis of pulsating stars.

Development and optimisation of an HPLC-DAD-ESI-Q-ToF method for the determination of phenolic acids and derivatives.

PubMed

Restivo, Annalaura; Degano, Ilaria; Ribechini, Erika; Colombini, Maria Perla

2014-01-01

A method for the HPLC-MS/MS analysis of phenols, including phenolic acids and naphtoquinones, using an amide-embedded phase column was developed and compared to the literature methods based on classical C18 stationary phase columns. RP-Amide is a recently developed polar embedded stationary phase, whose wetting properties mean that up to 100% water can be used as an eluent. The increased retention and selectivity for polar compounds and the possibility of working in 100% water conditions make this column particularly interesting for the HPLC analysis of phenolic acids and derivatives. In this study, the chromatographic separation was optimised on an HPLC-DAD, and was used to separate 13 standard phenolic acids and derivatives. The method was validated on an HPLC-ESI-Q-ToF. The acquisition was performed in negative polarity and MS/MS target mode. Ionisation conditions and acquisition parameters for the Q-ToF detector were investigated by working on collision energies and fragmentor potentials. The performance of the method was fully evaluated on standards. Moreover, several raw materials containing phenols were analysed: walnut, gall, wine, malbec grape, French oak, red henna and propolis. Our method allowed us to characterize the phenolic composition in a wide range of matrices and to highlight possible matrix effects.

Bandwidth and Detection of Packet Length Covert Channels

DTIC Science & Technology

2011-03-01

Shared Resource Matrix ( SRM ): Develop a matrix of all resources on one side and on the other all the processes. Then, determine which process uses which...system calls. This method is similar to that of the SRM . Covert channels have also been created by modulating packet timing, data and headers of net- work...analysis, noninterference analysis, SRM method, and the covert flow tree method [4]. These methods can be used during the design phase of a system. Less

Community-Involved Learning to Expand Possibilities for Vulnerable Children: A Critical Communicative, Sen's Capability, and Action Research Approach

ERIC Educational Resources Information Center

Kim, Kyung Hi

2014-01-01

This research, based on a case study of vulnerable children in Korea, used a mixed methods transformative approach to explore strategies to support and help disadvantaged children. The methodological approach includes three phases: a mixed methods contextual analysis, a qualitative dominant analysis based on Sen's capability approach and critical…

Formative Research on the Simplifying Conditions Method (SCM) for Task Analysis and Sequencing.

ERIC Educational Resources Information Center

Kim, YoungHwan; Reigluth, Charles M.

The Simplifying Conditions Method (SCM) is a set of guidelines for task analysis and sequencing of instructional content under the Elaboration Theory (ET). This article introduces the fundamentals of SCM and presents the findings from a formative research study on SCM. It was conducted in two distinct phases: design and instruction. In the first…

Analysis of High School English Curriculum Materials through Rasch Measurement Model and Maxqda

ERIC Educational Resources Information Center

Batdi, Veli; Elaldi, Senel

2016-01-01

The purpose of the study is to analyze high school English curriculum materials (ECM) through FACETS analysis and MAXQDA-11 programs. The mixed methods approach, both quantitative and qualitative methods, were used in three samples including English teachers in Elazig during the 2014-2015 academic year. While the quantitative phase of the study…

Identifying What Student Affairs Professionals Value: A Mixed Methods Analysis of Professional Competencies Listed in Job Descriptions

ERIC Educational Resources Information Center

Hoffman, John L.; Bresciani, Marilee J.

2012-01-01

This mixed method study explored the professional competencies that administrators expect from entry-, mid-, and senior-level professionals as reflected in 1,759 job openings posted in 2008. Knowledge, skill, and dispositional competencies were identified during the qualitative phase of the study. Statistical analysis of the prevalence of…

Industrial application of green chromatography - II. Separation and analysis of preservatives in skincare products using subcritical water chromatography.

PubMed

Yang, Y; Kapalavavi, B; Gujjar, L; Hadrous, S; Marple, R; Gamsky, C

2012-10-01

Several high-temperature liquid chromatography (HTLC) and subcritical water chromatography (SBWC) methods have been successfully developed in this study for separation and analysis of preservatives contained in Olay skincare creams. Efficient separation and quantitative analysis of preservatives have been achieved on four commercially available ZirChrom and Waters XBridge columns at temperatures ranging from 100 to 200°C. The quantification results obtained by both HTLC and SBWC methods developed for preservatives analysis are accurate and reproducible. A large number of replicate HTLC and SBWC runs also indicate no significant system building-up or interference for skincare cream analysis. Compared with traditional HPLC separation carried out at ambient temperature, the HTLC methods can save up to 90% methanol required in the HPLC mobile phase. However, the SBWC methods developed in this project completely eliminated the use of toxic organic solvents required in the HPLC mobile phase, thus saving a significant amount of money and making the environment greener. Although both homemade and commercial systems can accomplish SBWC separations, the SBWC methods using the commercial system for preservative analysis are recommended for industrial applications because they can be directly applied in industrial plant settings. © 2012 The Authors ICS © 2012 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Testing for Granger Causality in the Frequency Domain: A Phase Resampling Method.

PubMed

Liu, Siwei; Molenaar, Peter

2016-01-01

This article introduces phase resampling, an existing but rarely used surrogate data method for making statistical inferences of Granger causality in frequency domain time series analysis. Granger causality testing is essential for establishing causal relations among variables in multivariate dynamic processes. However, testing for Granger causality in the frequency domain is challenging due to the nonlinear relation between frequency domain measures (e.g., partial directed coherence, generalized partial directed coherence) and time domain data. Through a simulation study, we demonstrate that phase resampling is a general and robust method for making statistical inferences even with short time series. With Gaussian data, phase resampling yields satisfactory type I and type II error rates in all but one condition we examine: when a small effect size is combined with an insufficient number of data points. Violations of normality lead to slightly higher error rates but are mostly within acceptable ranges. We illustrate the utility of phase resampling with two empirical examples involving multivariate electroencephalography (EEG) and skin conductance data.

Preparation of thermally stable nanocrystalline hydroxyapatite by hydrothermal method.

PubMed

Prakash Parthiban, S; Elayaraja, K; Girija, E K; Yokogawa, Y; Kesavamoorthy, R; Palanichamy, M; Asokan, K; Narayana Kalkura, S

2009-12-01

Thermally stable hydroxyapatite (HAp) was synthesized by hydrothermal method in the presence of malic acid. X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscopy (SEM), differential thermal analysis (DTA), thermogravimetric analysis (TGA) was done on the synthesized powders. These analyses confirmed the sample to be free from impurities and other phases of calcium phosphates, and were of rhombus morphology along with nanosized particles. IR and Raman analyses indicated the adsorption of malic acid on HAp. Thermal stability of the synthesized HAp was confirmed by DTA and TGA. The synthesized powders were thermally stable upto 1,400 degrees C and showed no phase change. The proposed method might be useful for producing thermally stable HAp which is a necessity for high temperature coating applications.

Analysis of alternative coordination methods at border ports of entry between the United States and Mexico.

DOT National Transportation Integrated Search

2001-12-01

Phase 1: To identify the intersectorial coordination problems between public agencies in Mexico, the problems that originate from the lack of Bi-national Coordination at the Border Ports of Entry, and the costs derived from these problems. Phase 2: T...

Toward Improved Methods of Estimating Attenuation, Phase and Group velocity of surface waves observed on Shallow Seismic Records

NASA Astrophysics Data System (ADS)

Diallo, M. S.; Holschneider, M.; Kulesh, M.; Scherbaum, F.; Ohrnberger, M.; Lück, E.

2004-05-01

This contribution is concerned with the estimate of attenuation and dispersion characteristics of surface waves observed on a shallow seismic record. The analysis is based on a initial parameterization of the phase and attenuation functions which are then estimated by minimizing a properly defined merit function. To minimize the effect of random noise on the estimates of dispersion and attenuation we use cross-correlations (in Fourier domain) of preselected traces from some region of interest along the survey line. These cross-correlations are then expressed in terms of the parameterized attenuation and phase functions and the auto-correlation of the so-called source trace or reference trace. Cross-corelation that enter the optimization are selected so as to provide an average estimate of both the attenuation function and the phase (group) velocity of the area under investigation. The advantage of the method over the standard two stations method using Fourier technique is that uncertainties related to the phase unwrapping and the estimate of the number of 2π cycle skip in the phase phase are eliminated. However when mutliple modes arrival are observed, its become merely impossible to obtain reliable estimate the dipsersion curves for the different modes using optimization method alone. To circumvent this limitations we using the presented approach in conjunction with the wavelet propagation operator (Kulesh et al., 2003) which allows the application of band pass filtering in (ω -t) domain, to select a particular mode for the minimization. Also by expressing the cost function in the wavelet domain the optimization can be performed either with respect to the phase, the modulus of the transform or a combination of both. This flexibility in the design of the cost function provides an additional mean of constraining the optimization results. Results from the application of this dispersion and attenuation analysis method are shown for both synthetic and real 2D shallow seismic data sets. M. Kulesh, M. Holschneider, M. S. Diallo, Q. Xie and F. Scherbaum, Modeling of Wave Dispersion Using Wavelet Transfrom (Submitted to Pure and Applied Geophysics).

High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids.

PubMed

Lue, Bena-Marie; Guo, Zheng; Xu, Xuebing

2008-07-11

Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method developed was successfully applied for primary screening of RTILs (>20), with in depth evaluation of substrates in 10 RTILs, for their evaluation as reaction media.

Method and apparatus for measuring the mass flow rate of a fluid

DOEpatents

Evans, Robert P.; Wilkins, S. Curtis; Goodrich, Lorenzo D.; Blotter, Jonathan D.

2002-01-01

A non invasive method and apparatus is provided to measure the mass flow rate of a multi-phase fluid. An accelerometer is attached to a pipe carrying a multi-phase fluid. Flow related measurements in pipes are sensitive to random velocity fluctuations whose magnitude is proportional to the mean mass flow rate. An analysis of the signal produced by the accelerometer shows a relationship between the mass flow of a fluid and the noise component of the signal of an accelerometer. The noise signal, as defined by the standard deviation of the accelerometer signal allows the method and apparatus of the present invention to non-intrusively measure the mass flow rate of a multi-phase fluid.

Symplocin A, a Linear Peptide from the Bahamian Cyanobacterium Symploca sp. Configurational Analysis of N,N-Dimethylamino Acids by Chiral-Phase HPLC of Naphthacyl Esters†

PubMed Central

Molinski, Tadeusz F.; Reynolds, Kirk A.; Morinaka, Brandon I.

2012-01-01

The absolute stereostructures of the components of symplocin A (3), a new N,N-dimethyl-terminated peptide from the Bahamian cyanobacterium, Symploca sp., were assigned from spectroscopic analysis, including MS and 2D NMR and Marfey’s analysis. The complete absolute configuration of symplocin A, including the unexpected D-configurations of the terminal N,N-dimethylisoleucine and valic acid residues, were assigned by chiral-phase HPLC of the corresponding 2-naphthacyl esters, a highly sensitive, complementary strategy for assignment of N-blocked peptide residues where Marfey’s method is ineffectual, or other methods fall short. Symplocin A exhibited potent activity as an inhibitor of cathepsin E (IC50 300 pM). PMID:22360587

Validated reversed phase LC method for quantitative analysis of polymethoxyflavones in citrus peel extracts.

PubMed

Wang, Zhenyu; Li, Shiming; Ferguson, Stephen; Goodnow, Robert; Ho, Chi-Tang

2008-01-01

Polymethoxyflavones (PMFs), which exist exclusively in the citrus genus, have biological activities including anti-inflammatory, anticarcinogenic, and antiatherogenic properties. A validated RPLC method was developed for quantitative analysis of six major PMFs, namely nobiletin, tangeretin, sinensetin, 5,6,7,4'-tetramethoxyflavone, 3,5,6,7,3',4'-hexamethoxyflavone, and 3,5,6,7,8,3',4'-heptamethoxyflavone. The polar embedded LC stationary phase was able to fully resolve the six analogues. The developed method was fully validated in terms of linearity, accuracy, precision, sensitivity, and system suitability. The LOD of the method was calculated as 0.15 microg/mL and the recovery rate was between 97.0 and 105.1%. This analytical method was successfully applied to quantify the individual PMFs in four commercially available citrus peel extracts (CPEs). Each extract shows significant difference in the PMF composition and concentration. This method may provide a simple, rapid, and reliable tool to help reveal the correlation between the bioactivity of the PMF extracts and the individual PMF content.

The Intramolecular Hydrogen Bond N-H···S in 2,2'-Diaminodiphenyl Disulfide: Experimental and Computational Thermochemistry.

PubMed

Ramos, Fernando; Flores, Henoc; Hernández-Pérez, Julio M; Sandoval-Lira, Jacinto; Camarillo, E Adriana

2018-01-11

The intramolecular hydrogen bond of the N-H···S type has been investigated sparingly by thermochemical and computational methods. In order to study this interaction, the standard molar enthalpies of formation in gaseous phase of diphenyl disulfide, 2,2'-diaminodiphenyl disulfide and 4,4'-diaminodiphenyl disulfide at T = 298.15 K were determined by experimental thermochemical methods and computational calculations. The experimental enthalpies of formation in gas-phase were obtained from enthalpies of formation in crystalline phase and enthalpies of sublimation. Enthalpies of formation in crystalline phase were obtained using rotatory bomb combustion calorimetry. By thermogravimetry, enthalpies of vaporization were obtained, and by combining them with enthalpies of fusion, the enthalpies of sublimation were calculated. The Gaussian-4 procedure and the atomization method were applied to obtain enthalpies of formation in gas-phase of the compounds under study. Theoretical and experimental values are in good agreement. Through natural bond orbital (NBO) analysis and a topological analysis of the electronic density, the intramolecular hydrogen bridge (N-H···S) in the 2,2'-diaminodiphenyl disulfide was confirmed. Finally, an enthalpic difference of 11.8 kJ·mol -1 between the 2,2'-diaminodiphenyl disulfide and 4,4'-diaminodiphenyl disulfide was found, which is attributed to the intramolecular N-H···S interaction.

Development and optimization of SPECT gated blood pool cluster analysis for the prediction of CRT outcome

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lalonde, Michel, E-mail: mlalonde15@rogers.com; Wassenaar, Richard; Wells, R. Glenn

2014-07-15

Purpose: Phase analysis of single photon emission computed tomography (SPECT) radionuclide angiography (RNA) has been investigated for its potential to predict the outcome of cardiac resynchronization therapy (CRT). However, phase analysis may be limited in its potential at predicting CRT outcome as valuable information may be lost by assuming that time-activity curves (TAC) follow a simple sinusoidal shape. A new method, cluster analysis, is proposed which directly evaluates the TACs and may lead to a better understanding of dyssynchrony patterns and CRT outcome. Cluster analysis algorithms were developed and optimized to maximize their ability to predict CRT response. Methods: Aboutmore » 49 patients (N = 27 ischemic etiology) received a SPECT RNA scan as well as positron emission tomography (PET) perfusion and viability scans prior to undergoing CRT. A semiautomated algorithm sampled the left ventricle wall to produce 568 TACs from SPECT RNA data. The TACs were then subjected to two different cluster analysis techniques, K-means, and normal average, where several input metrics were also varied to determine the optimal settings for the prediction of CRT outcome. Each TAC was assigned to a cluster group based on the comparison criteria and global and segmental cluster size and scores were used as measures of dyssynchrony and used to predict response to CRT. A repeated random twofold cross-validation technique was used to train and validate the cluster algorithm. Receiver operating characteristic (ROC) analysis was used to calculate the area under the curve (AUC) and compare results to those obtained for SPECT RNA phase analysis and PET scar size analysis methods. Results: Using the normal average cluster analysis approach, the septal wall produced statistically significant results for predicting CRT results in the ischemic population (ROC AUC = 0.73;p < 0.05 vs. equal chance ROC AUC = 0.50) with an optimal operating point of 71% sensitivity and 60% specificity. Cluster analysis results were similar to SPECT RNA phase analysis (ROC AUC = 0.78, p = 0.73 vs cluster AUC; sensitivity/specificity = 59%/89%) and PET scar size analysis (ROC AUC = 0.73, p = 1.0 vs cluster AUC; sensitivity/specificity = 76%/67%). Conclusions: A SPECT RNA cluster analysis algorithm was developed for the prediction of CRT outcome. Cluster analysis results produced results equivalent to those obtained from Fourier and scar analysis.« less

A novel technique for phase synchrony measurement from the complex motor imaginary potential of combined body and limb action

NASA Astrophysics Data System (ADS)

Zhou, Zhong-xing; Wan, Bai-kun; Ming, Dong; Qi, Hong-zhi

2010-08-01

In this study, we proposed and evaluated the use of the empirical mode decomposition (EMD) technique combined with phase synchronization analysis to investigate the human brain synchrony of the supplementary motor area (SMA) and primary motor area (M1) during complex motor imagination of combined body and limb action. We separated the EEG data of the SMA and M1 into intrinsic mode functions (IMFs) using the EMD method and determined the characteristic IMFs by power spectral density (PSD) analysis. Thereafter, the instantaneous phases of the characteristic IMFs were obtained by the Hilbert transformation, and the single-trial phase-locking value (PLV) features for brain synchrony measurement between the SMA and M1 were investigated separately. The classification performance suggests that the proposed approach is effective for phase synchronization analysis and is promising for the application of a brain-computer interface in motor nerve reconstruction of the lower limbs.

Sparsity-driven coupled imaging and autofocusing for interferometric SAR

NASA Astrophysics Data System (ADS)

Zengin, Oǧuzcan; Khwaja, Ahmed Shaharyar; ćetin, Müjdat

2018-04-01

We propose a sparsity-driven method for coupled image formation and autofocusing based on multi-channel data collected in interferometric synthetic aperture radar (IfSAR). Relative phase between SAR images contains valuable information. For example, it can be used to estimate the height of the scene in SAR interferometry. However, this relative phase could be degraded when independent enhancement methods are used over SAR image pairs. Previously, Ramakrishnan et al. proposed a coupled multi-channel image enhancement technique, based on a dual descent method, which exhibits better performance in phase preservation compared to independent enhancement methods. Their work involves a coupled optimization formulation that uses a sparsity enforcing penalty term as well as a constraint tying the multichannel images together to preserve the cross-channel information. In addition to independent enhancement, the relative phase between the acquisitions can be degraded due to other factors as well, such as platform location uncertainties, leading to phase errors in the data and defocusing in the formed imagery. The performance of airborne SAR systems can be affected severely by such errors. We propose an optimization formulation that combines Ramakrishnan et al.'s coupled IfSAR enhancement method with the sparsity-driven autofocus (SDA) approach of Önhon and Çetin to alleviate the effects of phase errors due to motion errors in the context of IfSAR imaging. Our method solves the joint optimization problem with a Lagrangian optimization method iteratively. In our preliminary experimental analysis, we have obtained results of our method on synthetic SAR images and compared its performance to existing methods.

Multi-mode phase speed measurements with array-based analysis: Application to the North American continent

NASA Astrophysics Data System (ADS)

Matsuzawa, H.; Yoshizawa, K.

2017-12-01

Recent high-density broad-band seismic networks allow us to construct improved 3-D upper mantle models with unprecedented horizontal resolution using surface waves. Such dispersion measurements have been primarily based on the analysis of fundamental mode. Higher-mode information can be of help in enhancing vertical resolution of 3-D models, but their dispersion analysis is intrinsically difficult, since wave-packets of several modes are overlapped each other in an observed seismogram. In this study, we measure phase dispersion of multi-mode surface waves with an array-based analysis. Our method is modeled on a one-dimensional frequency-wavenumber method originally developed by Nolet (1975, GRL), which can be applied to a set of broadband seismic records observed in a linear array along a great circle path. Through this analysis, we can obtain a spectrogram in c-T (phase speed - period) domain, which is characterized by mode-branch dispersion curves and relative spectral powers for each mode. Synthetic experiments indicate that we can separate the modal contribution using a long linear array with typical array length of about 2000 to 4000 km. The method is applied to a large data set from USArray using nearly 400 seismic events in 2007 - 2014 with Mw 6.5 or greater. Our phase-speed maps for the fundamental-mode Love and Rayleigh waves and the first higher-mode Rayleigh waves match well with the earlier models. The phase speed maps reflect typical large-scale features of regional seismic structure in North America, but smaller-scale variations are less constrained in our model, since our measured phase speeds represent path-average features over a long path (about a few thousands kilometers). Our multi-mode dispersion measurements can also be used for the extraction of mode-branch waveforms for the first a few modes. This can be done by applying a narrow filter around the dispersion curves of a target mode in c-T spectrogram. The mode-branch waveforms can then be reconstructed based on a linear Radon transform (e.g., Luo et al., 2015, GJI). Synthetic experiments suggest that we can successfully retrieve the mode-branch waveforms for several mode branches, which can be used in the secondary analysis for constraining local-scale heterogeneity with enhanced depth resolution.

Carrier recovery methods for a dual-mode modem: A design approach

NASA Technical Reports Server (NTRS)

Richards, C. W.; Wilson, S. G.

1984-01-01

A dual mode model with selectable QPSK or 16-QASK modulation schemes is discussed. The theoretical reasoning as well as the practical trade-offs made during the development of a modem are presented, with attention given to the carrier recovery method used for coherent demodulation. Particular attention is given to carrier recovery methods that can provide little degradation due to phase error for both QPSK and 16-QASK, while being insensitive to the amplitude characteristic of a 16-QASK modulation scheme. A computer analysis of the degradation is symbol error rate (SER) for QPSK and 16-QASK due to phase error is prresented. Results find that an energy increase of roughly 4 dB is needed to maintain a SER of 1X10(-5) for QPSK with 20 deg of phase error and 16-QASK with 7 deg phase error.

Critical assessment of three high performance liquid chromatography analytical methods for food carotenoid quantification.

PubMed

Dias, M Graça; Oliveira, Luísa; Camões, M Filomena G F C; Nunes, Baltazar; Versloot, Pieter; Hulshof, Paul J M

2010-05-21

Three sets of extraction/saponification/HPLC conditions for food carotenoid quantification were technically and economically compared. Samples were analysed for carotenoids alpha-carotene, beta-carotene, beta-cryptoxanthin, lutein, lycopene, and zeaxanthin. All methods demonstrated good performance in the analysis of a composite food standard reference material for the analytes they are applicable to. Methods using two serial connected C(18) columns and a mobile phase based on acetonitrile, achieved a better carotenoid separation than the method using a mobile phase based on methanol and one C(18)-column. Carotenoids from leafy green vegetable matrices appeared to be better extracted with a mixture of methanol and tetrahydrofuran than with tetrahydrofuran alone. Costs of carotenoid determination in foods were lower for the method with mobile phase based on methanol. However for some food matrices and in the case of E-Z isomer separations, this was not technically satisfactory. Food extraction with methanol and tetrahydrofuran with direct evaporation of these solvents, and saponification (when needed) using pyrogallol as antioxidant, combined with a HPLC system using a slight gradient mobile phase based on acetonitrile and a stationary phase composed by two serial connected C(18) columns was the most technically and economically favourable method. 2010. Published by Elsevier B.V.

New approaches for the analysis of confluent cell layers with quantitative phase digital holographic microscopy

NASA Astrophysics Data System (ADS)

Pohl, L.; Kaiser, M.; Ketelhut, S.; Pereira, S.; Goycoolea, F.; Kemper, Björn

2016-03-01

Digital holographic microscopy (DHM) enables high resolution non-destructive inspection of technical surfaces and minimally-invasive label-free live cell imaging. However, the analysis of confluent cell layers represents a challenge as quantitative DHM phase images in this case do not provide sufficient information for image segmentation, determination of the cellular dry mass or calculation of the cell thickness. We present novel strategies for the analysis of confluent cell layers with quantitative DHM phase contrast utilizing a histogram based-evaluation procedure. The applicability of our approach is illustrated by quantification of drug induced cell morphology changes and it is shown that the method is capable to quantify reliable global morphology changes of confluent cell layers.

Quality Analysis of Chlorogenic Acid and Hyperoside in Crataegi fructus

PubMed Central

Weon, Jin Bae; Jung, Youn Sik; Ma, Choong Je

2016-01-01

Background: Crataegi fructus is a herbal medicine for strong stomach, sterilization, and alcohol detoxification. Chlorogenic acid and hyperoside are the major compounds in Crataegi fructus. Objective: In this study, we established novel high-performance liquid chromatography (HPLC)-diode array detection analysis method of chlorogenic acid and hyperoside for quality control of Crataegi fructus. Materials and Methods: HPLC analysis was achieved on a reverse-phase C18 column (5 μm, 4.6 mm × 250 mm) using water and acetonitrile as mobile phase with gradient system. The method was validated for linearity, precision, and accuracy. About 31 batches of Crataegi fructus samples collected from Korea and China were analyzed by using HPLC fingerprint of developed HPLC method. Then, the contents of chlorogenic acid and hyperoside were compared for quality evaluation of Crataegi fructus. Results: The results have shown that the average contents (w/w %) of chlorogenic acid and hyperoside in Crataegi fructus collected from Korea were 0.0438% and 0.0416%, respectively, and the average contents (w/w %) of 0.0399% and 0.0325%, respectively. Conclusion: In conclusion, established HPLC analysis method was stable and could provide efficient quality evaluation for monitoring of commercial Crataegi fructus. SUMMARY Quantitative analysis method of chlorogenic acid and hyperoside in Crataegi fructus is developed by high.performance liquid chromatography.(HPLC).diode array detectionEstablished HPLC analysis method is validated with linearity, precision, and accuracyThe developed method was successfully applied for quantitative analysis of Crataegi fructus sample collected from Korea and China. Abbreviations used: HPLC: High-performance liquid chromatography, GC: Gas chromatography, MS: Mass spectrometer, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation, RRT: Relative retention time, RPA: Relation peak area. PMID:27076744

Open Vehicle Sketch Pad Aircraft Modeling Strategies

NASA Technical Reports Server (NTRS)

Hahn, Andrew S.

2013-01-01

Geometric modeling of aircraft during the Conceptual design phase is very different from that needed for the Preliminary or Detailed design phases. The Conceptual design phase is characterized by the rapid, multi-disciplinary analysis of many design variables by a small engineering team. The designer must walk a line between fidelity and productivity, picking tools and methods with the appropriate balance of characteristics to achieve the goals of the study, while staying within the available resources. Identifying geometric details that are important, and those that are not, is critical to making modeling and methodology choices. This is true for both the low-order analysis methods traditionally used in Conceptual design as well as the highest-order analyses available. This paper will highlight some of Conceptual design's characteristics that drive the designer s choices as well as modeling examples for several aircraft configurations using the open source version of the Vehicle Sketch Pad (Open VSP) aircraft Conceptual design geometry modeler.

Spatial Phase Imaging

NASA Technical Reports Server (NTRS)

2006-01-01

Frequently, scientists grow crystals by dissolving a protein in a specific liquid solution, and then allowing that solution to evaporate. The methods used next have been, variously, invasive (adding a dye that is absorbed by the protein), destructive (crushing protein/salt-crystal mixtures and observing differences between the crushing of salt and protein), or costly and time-consuming (X-ray crystallography). In contrast to these methods, a new technology for monitoring protein growth, developed in part through NASA Small Business Innovation Research (SBIR) funding from Marshall Space Flight Center, is noninvasive, nondestructive, rapid, and more cost effective than X-ray analysis. The partner for this SBIR, Photon-X, Inc., of Huntsville, Alabama, developed spatial phase imaging technology that can monitor crystal growth in real time and in an automated mode. Spatial phase imaging scans for flaws quickly and produces a 3-D structured image of a crystal, showing volumetric growth analysis for future automated growth.

Systems and methods for analyzing liquids under vacuum

DOEpatents

Yu, Xiao-Ying; Yang, Li; Cowin, James P.; Iedema, Martin J.; Zhu, Zihua

2013-10-15

Systems and methods for supporting a liquid against a vacuum pressure in a chamber can enable analysis of the liquid surface using vacuum-based chemical analysis instruments. No electrical or fluid connections are required to pass through the chamber walls. The systems can include a reservoir, a pump, and a liquid flow path. The reservoir contains a liquid-phase sample. The pump drives flow of the sample from the reservoir, through the liquid flow path, and back to the reservoir. The flow of the sample is not substantially driven by a differential between pressures inside and outside of the liquid flow path. An aperture in the liquid flow path exposes a stable portion of the liquid-phase sample to the vacuum pressure within the chamber. The radius, or size, of the aperture is less than or equal to a critical value required to support a meniscus of the liquid-phase sample by surface tension.

Large Area Crop Inventory Experiment (LACIE). Phase 2 evaluation report

NASA Technical Reports Server (NTRS)

1977-01-01

Documentation of the activities of the Large Area Crop Inventory Experiment during the 1976 Northern Hemisphere crop year is presented. A brief overview of the experiment is included as well as phase two area, yield, and production estimates for the United States Great Plains, Canada, and the Union of Soviet Socialist Republics spring winter wheat regions. The accuracies of these estimates are compared with independent government estimates. Accuracy assessment of the United States Great Plains yardstick region based on a through blind sight analysis is given, and reasons for variations in estimating performance are discussed. Other phase two technical activities including operations, exploratory analysis, reporting, methods of assessment, phase three and advanced system design, technical issues, and developmental activities are also included.

Identification of atypical flight patterns

NASA Technical Reports Server (NTRS)

Statler, Irving C. (Inventor); Ferryman, Thomas A. (Inventor); Amidan, Brett G. (Inventor); Whitney, Paul D. (Inventor); White, Amanda M. (Inventor); Willse, Alan R. (Inventor); Cooley, Scott K. (Inventor); Jay, Joseph Griffith (Inventor); Lawrence, Robert E. (Inventor); Mosbrucker, Chris (Inventor)

2005-01-01

Method and system for analyzing aircraft data, including multiple selected flight parameters for a selected phase of a selected flight, and for determining when the selected phase of the selected flight is atypical, when compared with corresponding data for the same phase for other similar flights. A flight signature is computed using continuous-valued and discrete-valued flight parameters for the selected flight parameters and is optionally compared with a statistical distribution of other observed flight signatures, yielding atypicality scores for the same phase for other similar flights. A cluster analysis is optionally applied to the flight signatures to define an optimal collection of clusters. A level of atypicality for a selected flight is estimated, based upon an index associated with the cluster analysis.

Approximation and Numerical Analysis of Nonlinear Equations of Evolution.

DTIC Science & Technology

1980-01-31

dominant convective terms, or Stefan type problems such as the flow of fluids through porous media or the melting and freezing of ice. Such problems...means of formulating time-dependent Stefan problems was initiated. Classes of problems considered here include the one-phase and two-phase Stefan ...some new numerical methods were 2 developed for two dimensional, two-phase Stefan problems with time dependent boundary conditions. A variety of example

Structure and electrical properties of intergrowth bismuth layer-structured Bi4Ti3O12-CaBi4Ti4O15 ferroelectric ceramics

NASA Astrophysics Data System (ADS)

Choi, Gi Ppeum; Cho, Sam Yeon; Bu, Sang Don

2016-09-01

Pb-free ferroelectric Bi4Ti3O12-CaBi4Ti4O15 (BIT-CBT) ceramics were manufactured using a solid-state reaction method. Structural analysis by using X-ray diffraction confirmed the presence of a second phase of Bi2Ti2O7, and the surface depth X-ray diffraction analysis revealed that this phase existed only on the surface. This second phase appears to have been caused by the volatilization of Bi ions at high sintering temperatures. For resolution of the issue of volatilization of Bi ions and manufacture of BIT-CBT ceramics with a single phase, Bi2O3 powder was added to the BIT-CBT mixture, and a powder-bed method, in which pellets were covered with BIT-CBT powder, was used to manufacture the ceramic. The piezoelectric coefficient of the single-phase BIT-CBT ceramics was 12.4 pC/N while the residual polarization and the coercive electric field were 11.3 μC/cm2, and 125 kV/cm, respectively. The results suggest that single-phase BIT-CBT ceramics are suitable for the manufacture of elements incorporating these electrical characteristics.

Instrumental Analysis in Environmental Chemistry - Liquid and Solid Phase Detection Systems

ERIC Educational Resources Information Center

Stedman, Donald H.; Meyers, Philip A.

1974-01-01

This is the second of two reviews dealing with analytical methods applicable to environmental chemistry. Methods are discussed under gas, liquid, or solid depending upon the state of the analyte during detection. (RH)

Methods for magnetic resonance analysis using magic angle technique

DOEpatents

Hu, Jian Zhi [Richland, WA; Wind, Robert A [Kennewick, WA; Minard, Kevin R [Kennewick, WA; Majors, Paul D [Kennewick, WA

2011-11-22

Methods of performing a magnetic resonance analysis of a biological object are disclosed that include placing the object in a main magnetic field (that has a static field direction) and in a radio frequency field; rotating the object at a frequency of less than about 100 Hz around an axis positioned at an angle of about 54.degree.44' relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a phase-corrected magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. In particular embodiments the method includes pulsing the radio frequency to provide at least two of a spatially selective read pulse, a spatially selective phase pulse, and a spatially selective storage pulse. Further disclosed methods provide pulse sequences that provide extended imaging capabilities, such as chemical shift imaging or multiple-voxel data acquisition.

Method development for the analysis of N-nitrosodimethylamine and other N-nitrosamines in drinking water at low nanogram/liter concentrations using solid-phase extraction and gas chromatography with chemical ionization tandem mass spectrometry.

PubMed

Munch, Jean W; Bassett, Margarita V

2006-01-01

N-nitrosodimethylamine (NDMA) is a probable human carcinogen of concern that has been identified as a drinking water contaminant. U.S. Environmental Protection Agency Method 521 has been developed for the analysis of NDMA and 6 additional N-nitrosamines in drinking water at low ng/L concentrations. The method uses solid-phase extraction with coconut charcoal as the sorbent and dichloromethane as the eluent to concentrate 0.50 L water samples to 1 mL. The extracts are analyzed by gas chromatography-chemical ionization tandem mass spectrometry using large-volume injection. Method performance was evaluated in 2 laboratories. Typical analyte recoveries of 87-104% were demonstrated for fortified reagent water samples, and recoveries of 77-106% were demonstrated for fortified drinking water samples. All relative standard deviations on replicate analyses were < 11%.

Random-Phase Approximation Methods

NASA Astrophysics Data System (ADS)

Chen, Guo P.; Voora, Vamsee K.; Agee, Matthew M.; Balasubramani, Sree Ganesh; Furche, Filipp

2017-05-01

Random-phase approximation (RPA) methods are rapidly emerging as cost-effective validation tools for semilocal density functional computations. We present the theoretical background of RPA in an intuitive rather than formal fashion, focusing on the physical picture of screening and simple diagrammatic analysis. A new decomposition of the RPA correlation energy into plasmonic modes leads to an appealing visualization of electron correlation in terms of charge density fluctuations. Recent developments in the areas of beyond-RPA methods, RPA correlation potentials, and efficient algorithms for RPA energy and property calculations are reviewed. The ability of RPA to approximately capture static correlation in molecules is quantified by an analysis of RPA natural occupation numbers. We illustrate the use of RPA methods in applications to small-gap systems such as open-shell d- and f-element compounds, radicals, and weakly bound complexes, where semilocal density functional results exhibit strong functional dependence.

Comparative study viruses with computer-aided phase microscope AIRYSCAN

NASA Astrophysics Data System (ADS)

Tychinsky, Vladimir P.; Koufal, Georgy E.; Perevedentseva, Elena V.; Vyshenskaia, Tatiana V.

1996-12-01

Traditionally viruses are studied with scanning electron microscopy (SEM) after complicated procedure of sample preparation without the possibility to study it under natural conditions. We obtained images of viruses (Vaccinia virus, Rotavirus) and rickettsias (Rickettsia provazekii, Coxiella burnetti) in native state with computer-aided phase microscope airyscan -- the interference microscope of Linnik layout with phase modulation of the reference wave with dissector image tube as coordinate-sensitive photodetector and computer processing of phase image. A light source was the He-Ne laser. The main result is coincidence of dimensions and shape of phase images with available information concerning their morphology obtained with SEM and other methods. The fine structure of surface and nuclei is observed. This method may be applied for virus recognition and express identification, investigation of virus structure and the analysis of cell-virus interaction.

Evaluation of mechanical dyssynchrony and myocardial perfusion using phase analysis of gated SPECT imaging in patients with left ventricular dysfunction

PubMed Central

Trimble, Mark A.; Borges-Neto, Salvador; Honeycutt, Emily F.; Shaw, Linda K.; Pagnanelli, Robert; Chen, Ji; Iskandrian, Ami E.; Garcia, Ernest V.; Velazquez, Eric J.

2010-01-01

Background Using phase analysis of gated single photon emission computed tomography (SPECT) imaging, we examined the relation between myocardial perfusion, degree of electrical dyssynchrony, and degree of SPECT-derived mechanical dyssynchrony in patients with left ventricular (LV) dysfunction. Methods and Results We retrospectively examined 125 patients with LV dysfunction and ejection fraction of 35% or lower. Fourier analysis converts regional myocardial counts into a continuous thickening function, allowing resolution of phase of onset of myocardial thickening. The SD of LV phase distribution (phase SD) and histogram bandwidth describe LV phase dispersion as a measure of dyssynchrony. Heart failure (HF) patients with perfusion abnormalities ities have higher degrees of dyssynchrony measured by median phase SD (45.5° vs 27.7°, P < .0001) and bandwidth (117.0° vs 73.0°, P = .0006). HF patients with prolonged QRS durations have higher degrees of dyssynchrony measured by median phase SD (54.1° vs 34.7°, P < .0001) and bandwidth (136.5° vs 99.0°, P = .0005). Mild to moderate correlations exist between QRS duration and phase analysis indices of phase SD (r = 0.50) and bandwidth (r = 0.40). Mechanical dyssynchrony (phase SD >43°) was 43.2%. Conclusions HF patients with perfusion abnormalities or prolonged QRS durations QRS durations have higher degrees of mechanical dyssynchrony. Gated SPECT myocardial perfusion imaging can quantify myocardial function, perfusion, and dyssynchrony and may help in evaluating patients for cardiac resynchronization therapy. PMID:18761269

Mathematical Development and Computational Analysis of Harmonic Phase-Magnetic Resonance Imaging (HARP-MRI) Based on Bloch Nuclear Magnetic Resonance (NMR) Diffusion Model for Myocardial Motion.

PubMed

Dada, Michael O; Jayeoba, Babatunde; Awojoyogbe, Bamidele O; Uno, Uno E; Awe, Oluseyi E

2017-09-13

Harmonic Phase-Magnetic Resonance Imaging (HARP-MRI) is a tagged image analysis method that can measure myocardial motion and strain in near real-time and is considered a potential candidate to make magnetic resonance tagging clinically viable. However, analytical expressions of radially tagged transverse magnetization in polar coordinates (which is required to appropriately describe the shape of the heart) have not been explored because the physics required to directly connect myocardial deformation of tagged Nuclear Magnetic Resonance (NMR) transverse magnetization in polar geometry and the appropriate harmonic phase parameters are not yet available. The analytical solution of Bloch NMR diffusion equation in spherical geometry with appropriate spherical wave tagging function is important for proper analysis and monitoring of heart systolic and diastolic deformation with relevant boundary conditions. In this study, we applied Harmonic Phase MRI method to compute the difference between tagged and untagged NMR transverse magnetization based on the Bloch NMR diffusion equation and obtained radial wave tagging function for analysis of myocardial motion. The analytical solution of the Bloch NMR equations and the computational simulation of myocardial motion as developed in this study are intended to significantly improve healthcare for accurate diagnosis, prognosis and treatment of cardiovascular related deceases at the lowest cost because MRI scan is still one of the most expensive anywhere. The analysis is fundamental and significant because all Magnetic Resonance Imaging techniques are based on the Bloch NMR flow equations.

Brightness analysis of an electron beam with a complex profile

NASA Astrophysics Data System (ADS)

Maesaka, Hirokazu; Hara, Toru; Togawa, Kazuaki; Inagaki, Takahiro; Tanaka, Hitoshi

2018-05-01

We propose a novel analysis method to obtain the core bright part of an electron beam with a complex phase-space profile. This method is beneficial to evaluate the performance of simulation data of a linear accelerator (linac), such as an x-ray free electron laser (XFEL) machine, since the phase-space distribution of a linac electron beam is not simple, compared to a Gaussian beam in a synchrotron. In this analysis, the brightness of undulator radiation is calculated and the core of an electron beam is determined by maximizing the brightness. We successfully extracted core electrons from a complex beam profile of XFEL simulation data, which was not expressed by a set of slice parameters. FEL simulations showed that the FEL intensity was well remained even after extracting the core part. Consequently, the FEL performance can be estimated by this analysis without time-consuming FEL simulations.

Analysis of Multi-Antenna GNSS Receiver Performance under Jamming Attacks.

PubMed

Vagle, Niranjana; Broumandan, Ali; Lachapelle, Gérard

2016-11-17

Although antenna array-based Global Navigation Satellite System (GNSS) receivers can be used to mitigate both narrowband and wideband electronic interference sources, measurement distortions induced by array processing methods are not suitable for high precision applications. The measurement distortions have an adverse effect on the carrier phase ambiguity resolution, affecting the navigation solution. Depending on the array attitude information availability and calibration parameters, different spatial processing methods can be implemented although they distort carrier phase measurements in some cases. This paper provides a detailed investigation of the effect of different array processing techniques on array-based GNSS receiver measurements and navigation performance. The main novelty of the paper is to provide a thorough analysis of array-based GNSS receivers employing different beamforming techniques from tracking to navigation solution. Two beamforming techniques, namely Power Minimization (PM) and Minimum Power Distortionless Response (MPDR), are being investigated. In the tracking domain, the carrier Doppler, Phase Lock Indicator (PLI), and Carrier-to-Noise Ratio (C/N₀) are analyzed. Pseudorange and carrier phase measurement distortions and carrier phase position performance are also evaluated. Performance analyses results from simulated GNSS signals and field tests are provided.

Preparation of fine powdered composite for latent heat storage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fořt, Jan, E-mail: jan.fort.1@fsv.cvut.cz; Trník, Anton, E-mail: anton.trnik@fsv.cvut.cz; Pavlíková, Milena, E-mail: milena.pavlikova@fsv.cvut.cz

Application of latent heat storage building envelope systems using phase-change materials represents an attractive method of storing thermal energy and has the advantages of high-energy storage density and the isothermal nature of the storage process. This study deals with a preparation of a new type of powdered phase change composite material for thermal energy storage. The idea of a composite is based upon the impregnation of a natural silicate material by a reasonably priced commercially produced pure phase change material and forming the homogenous composite powdered structure. For the preparation of the composite, vacuum impregnation method is used. The particlemore » size distribution accessed by the laser diffraction apparatus proves that incorporation of the organic phase change material into the structure of inorganic siliceous pozzolana does not lead to the clustering of the particles. The compatibility of the prepared composite is characterized by the Fourier transformation infrared analysis (FTIR). Performed DSC analysis shows potential of the developed composite for thermal energy storage that can be easily incorporated into the cement-based matrix of building materials. Based on the obtained results, application of the developed phase change composite can be considered with a great promise.« less

Phase progression of γ-Al2O3 nanoparticles synthesized in a solvent-deficient environment.

PubMed

Smith, Stacey J; Amin, Samrat; Woodfield, Brian F; Boerio-Goates, Juliana; Campbell, Branton J

2013-04-15

Our simple and uniquely cost-effective solvent-deficient synthetic method produces 3-5 nm Al2O3 nanoparticles which show promise as improved industrial catalyst-supports. While catalytic applications are sensitive to the details of the atomic structure, a diffraction analysis of alumina nanoparticles is challenging because of extreme size/microstrain-related peak broadening and the similarity of the diffraction patterns of various transitional Al2O3 phases. Here, we employ a combination of X-ray pair-distribution function (PDF) and Rietveld methods, together with solid-state NMR and thermogravimetry/differential thermal analysis-mass spectrometry (TG/DTA-MS), to characterize the alumina phase-progression in our nanoparticles as a function of calcination temperature between 300 and 1200 °C. In the solvent-deficient synthetic environment, a boehmite precursor phase forms which transitions to γ-Al2O3 at an extraordinarily low temperature (below 300 °C), but this γ-Al2O3 is initially riddled with boehmite-like stacking-fault defects that steadily disappear during calcination in the range from 300 to 950 °C. The healing of these defects accounts for many of the most interesting and widely reported properties of the γ-phase.

A low bioimpedance phase angle predicts a higher mortality and lower nutritional status in chronic dialysis patients

NASA Astrophysics Data System (ADS)

Dumler Md, Francis

2010-04-01

Bioelectrical impedance analysis is an established technique for body composition analysis. The phase angle parameter, an index of body cell mass, tissue hydration, and membrane integrity, makes it suitable for assessing nutritional status and survivability. We evaluated the significance of a low phase angle value on nutritional status and mortality in 285 chronic dialysis patients during a longitudinal prospective observational study. Patients in the lower phase angle tertile had decreased body weight, body mass index, fat free mass, body cell mass, and lower serum albumin concentrations than those in the higher tertile (P<001). In addition, mortality rates were significantly lower (P=0.05) in the highest tertile patients. In conclusion, the phase angle is a useful method for identifying dialysis patients at high risk for malnutrition and increased mortality.

Ethanol- and trifluoroethanol-induced changes in phase states of DPPC membranes. Prodan emission-excitation fluorescence spectroscopy supported by PARAFAC analysis

NASA Astrophysics Data System (ADS)

Horochowska, Martyna; Cieślik-Boczula, Katarzyna; Rospenk, Maria

2018-03-01

It has been shown that Prodan emission-excitation fluorescence spectroscopy supported by Parallel Factor (PARAFAC) analysis is a fast, simple and sensitive method used in the study of the phase transition from the noninterdigitated gel (Lβ‧) state to the interdigitated gel (LβI) phase, triggered by ethanol and 2,2,2-trifluoroethanol (TFE) molecules in dipalmitoylphosphatidylcholines (DPPC) membranes. The relative contribution of lipid phases with spectral characteristics of each pure phase component has been presented as a function of an increase in alcohol concentration. It has been stated that both alcohol molecules can induce a formation of the LβI phase, but TFE is over six times stronger inducer of the interdigitated phase in DPPC membranes than ethanol molecules. Moreover, in the TFE-mixed DPPC membranes, the transition from the Lβ‧ to LβI phase is accompanied by a formation of the fluid phase, which most probably serves as a boundary phase between the Lβ‧ and LβI regions. Contrary to the three phase-state model of TFE-mixed DPPC membranes, in ethanol-mixed DPPC membranes only the two phase-state model has been detected.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haslam, J J; Wall, M A; Johnson, D L

We have measured and modeled the change in electrical resistivity due to partial transformation to the martensitic {alpha}{prime}-phase in a {delta}-phase Pu-Ga matrix. The primary objective is to relate the change in resistance, measured with a 4-probe technique during the transformation, to the volume fraction of the {alpha}{prime} phase created in the microstructure. Analysis by finite element methods suggests that considerable differences in the resistivity may be anticipated depending on the orientational and morphological configurations of the {alpha}{prime} particles. Finite element analysis of the computed resistance of an assembly of lenticular shaped particles indicates that series resistor or parallel resistormore » approximations are inaccurate and can lead to an underestimation of the predicted amount of {alpha}{prime} in the sample by 15% or more. Comparison of the resistivity of a simulated network of partially transformed grains or portions of grains suggests that a correction to the measured resistivity allows quantification of the amount of {alpha}{prime} phase in the microstructure with minimal consideration of how the {alpha}{prime} morphology may evolve. It is found that the average of the series and parallel resistor approximations provide the most accurate relationship between the measured resistivity and the amount of {alpha}{prime} phase. The methods described here are applicable to any evolving two-phase microstructure in which the resistance difference between the two phases is measurable.« less

New materials through a variety of sintering methods

NASA Astrophysics Data System (ADS)

Jaworska, L.; Cyboroń, J.; Cygan, S.; Laszkiewicz-Łukasik, J.; Podsiadło, M.; Novak, P.; Holovenko, Y.

2018-03-01

New sintering techniques make it possible to obtain materials with special properties that are impossible to obtain by conventional sintering techniques. This issue is especially important for ceramic materials for application under extreme conditions. Following the tendency to limit critical materials in manufacturing processes, the use of W, Si, B, Co, Cr should be limited, also. One of the cheapest and widely available materials is aluminum oxide, which shows differences in phase composition, grain size, hardness, strain and fracture toughness of the same type of powder, sintered via various methods. In this paper the alumina was sintered using the conventional free sintering process, microwave sintering, Spark Plasma Sintering (SPS), high pressure-high temperature method (HP-HT) and High Pressure Spark Plasma Sintering (HP SPS). Phase composition analysis, by X-ray diffraction of the alumina materials sintered using various methods, was carried out. For the conventional sintering method, compacts are composed of α-Al2O3 and θ-Al2O3. For compacts sintered using SPS, microwave and HP-HT methods, χ-Al2O3 and γ-Al2O3 phases were additionally present. Mechanical and physical properties of the obtained materials were compared between the methods of sintering. On the basis of images from scanning electron microscope quantitative analysis was performed to determine the degree of grain growth of alumina after sintering.

Bioanalytical method for the estimation of co-administered esomeprazole, leflunomide and ibuprofen in human plasma and in pharmaceutical dosage forms using micellar liquid chromatography.

PubMed

Talaat, Wael

2017-05-01

The present study represents a connection between basic science and clinical applied science through providing a bioanalytical method for the analysis of certain co-administered drugs used for the treatment of rheumatoid arthritis. The studied drugs are esomeprazole, leflunomide and ibuprofen. The proposed bioanalytical method is a simple reversed phase high performance liquid chromatographic method using micellar mobile phase. The method is conducted using a Shim-pack VP-ODS (150 mm × 4.6 mm ID) stainless steel column at ambient temperature with ultraviolet detection at 285 nm. The micellar mobile phase consisted of 0.1 m sodium dodecyl sulfate, 10% n-propanol, 0.3% triethylamine in 0.02 m orthophosphoric acid (pH 3.5) and is pumped at a flow rate of 1.0 mL/min. The calibration curve was rectilinear over the concentration range of 0.1-5.0, 0.5-10.0 and 1.0-20.0 μg/mL for esomeprazole, leflunomide and ibuprofen respectively. The proposed method was successfully applied to the analysis of these drugs in dosage forms. The method is extended to the in-vitro, in-vivo determination of these drugs in spiked and real human plasma samples. Copyright © 2016 John Wiley & Sons, Ltd.

Method development for speciation analysis of nanoparticle and ionic forms of gold in biological samples by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Malejko, Julita; Świerżewska, Natalia; Bajguz, Andrzej; Godlewska-Żyłkiewicz, Beata

2018-04-01

A new method based on coupling high performance liquid chromatography (HPLC) to inductively coupled plasma mass spectrometry (ICP MS) has been developed for the speciation analysis of gold nanoparticles (AuNPs) and dissolved gold species (Au(III)) in biological samples. The column type, the composition and the flow rate of the mobile phase were carefully investigated in order to optimize the separation conditions. The usefulness of two polymeric reversed phase columns (PLRP-S with 100 nm and 400 nm pore size) to separate gold species were investigated for the first time. Under the optimal conditions (PLRP-S400 column, 10 mmol L-1 SDS and 5% methanol as the mobile phase, 0.5 mL min-1 flow rate), detection limits of 2.2 ng L-1 for Au(III), 2.8 ng L-1 for 10 nm AuNPs and 3.7 ng L-1 for 40 nm AuNPs were achieved. The accuracy of the method was proved by analysis of reference material RM 8011 (NIST) of gold nanoparticles of nominal diameter of 10 nm. The HPLC-ICP MS method has been successfully applied to the detection and size characterization of gold species in lysates of green algae Acutodesmus obliquus, typical representative of phytoplankton flora, incubated with 10 nm AuNPs or Au(III).

A Comparison of Phasing Algorithms for Trios and Unrelated Individuals

PubMed Central

Marchini, Jonathan; Cutler, David; Patterson, Nick; Stephens, Matthew; Eskin, Eleazar; Halperin, Eran; Lin, Shin; Qin, Zhaohui S.; Munro, Heather M.; Abecasis, Gonçalo R.; Donnelly, Peter

2006-01-01

Knowledge of haplotype phase is valuable for many analysis methods in the study of disease, population, and evolutionary genetics. Considerable research effort has been devoted to the development of statistical and computational methods that infer haplotype phase from genotype data. Although a substantial number of such methods have been developed, they have focused principally on inference from unrelated individuals, and comparisons between methods have been rather limited. Here, we describe the extension of five leading algorithms for phase inference for handling father-mother-child trios. We performed a comprehensive assessment of the methods applied to both trios and to unrelated individuals, with a focus on genomic-scale problems, using both simulated data and data from the HapMap project. The most accurate algorithm was PHASE (v2.1). For this method, the percentages of genotypes whose phase was incorrectly inferred were 0.12%, 0.05%, and 0.16% for trios from simulated data, HapMap Centre d'Etude du Polymorphisme Humain (CEPH) trios, and HapMap Yoruban trios, respectively, and 5.2% and 5.9% for unrelated individuals in simulated data and the HapMap CEPH data, respectively. The other methods considered in this work had comparable but slightly worse error rates. The error rates for trios are similar to the levels of genotyping error and missing data expected. We thus conclude that all the methods considered will provide highly accurate estimates of haplotypes when applied to trio data sets. Running times differ substantially between methods. Although it is one of the slowest methods, PHASE (v2.1) was used to infer haplotypes for the 1 million–SNP HapMap data set. Finally, we evaluated methods of estimating the value of r2 between a pair of SNPs and concluded that all methods estimated r2 well when the estimated value was ⩾0.8. PMID:16465620

A new method of measuring centre-of-mass velocities of radially pulsating stars from high-resolution spectroscopy

NASA Astrophysics Data System (ADS)

Britavskiy, N.; Pancino, E.; Tsymbal, V.; Romano, D.; Fossati, L.

2018-03-01

We present a radial velocity analysis of 20 solar neighbourhood RR Lyrae and three Population II Cepheid variables. We obtained high-resolution, moderate-to-high signal-to-noise ratio spectra for most stars; these spectra covered different pulsation phases for each star. To estimate the gamma (centre-of-mass) velocities of the programme stars, we use two independent methods. The first, `classic' method is based on RR Lyrae radial velocity curve templates. The second method is based on the analysis of absorption-line profile asymmetry to determine both pulsational and gamma velocities. This second method is based on the least-squares deconvolution (LSD) technique applied to analyse the line asymmetry that occurs in the spectra. We obtain measurements of the pulsation component of the radial velocity with an accuracy of ±3.5 km s-1. The gamma velocity was determined with an accuracy of ±10 km s-1, even for those stars having a small number of spectra. The main advantage of this method is the possibility of obtaining an estimation of gamma velocity even from one spectroscopic observation with uncertain pulsation phase. A detailed investigation of LSD profile asymmetry shows that the projection factor p varies as a function of the pulsation phase - this is a key parameter, which converts observed spectral line radial velocity variations into photospheric pulsation velocities. As a by-product of our study, we present 41 densely spaced synthetic grids of LSD profile bisectors based on atmospheric models of RR Lyr covering all pulsation phases.

Comparative analysis of autofocus functions in digital in-line phase-shifting holography.

PubMed

Fonseca, Elsa S R; Fiadeiro, Paulo T; Pereira, Manuela; Pinheiro, António

2016-09-20

Numerical reconstruction of digital holograms relies on a precise knowledge of the original object position. However, there are a number of relevant applications where this parameter is not known in advance and an efficient autofocusing method is required. This paper addresses the problem of finding optimal focusing methods for use in reconstruction of digital holograms of macroscopic amplitude and phase objects, using digital in-line phase-shifting holography in transmission mode. Fifteen autofocus measures, including spatial-, spectral-, and sparsity-based methods, were evaluated for both synthetic and experimental holograms. The Fresnel transform and the angular spectrum reconstruction methods were compared. Evaluation criteria included unimodality, accuracy, resolution, and computational cost. Autofocusing under angular spectrum propagation tends to perform better with respect to accuracy and unimodality criteria. Phase objects are, generally, more difficult to focus than amplitude objects. The normalized variance, the standard correlation, and the Tenenbaum gradient are the most reliable spatial-based metrics, combining computational efficiency with good accuracy and resolution. A good trade-off between focus performance and computational cost was found for the Fresnelet sparsity method.

Highly concentrated, ring-shaped phase conversion laser-induced breakdown spectroscopy technology for liquid sample analysis.

PubMed

Lin, Qingyu; Wei, Zhimei; Guo, Hongli; Wang, Shuai; Guo, Guangmeng; Zhang, Zhi; Duan, Yixiang

2017-06-10

A highly concentrated, ring-shaped phase conversion (RSPC) method was developed for liquid sample analysis using the laser-induced breakdown spectroscopy (LIBS) technique. In this work, test samples were prepared by mixing the metal particles with polyvinyl alcohol (PVA) supporter in liquid phase. With heat, the PVA solution solidified inside a modified glass petri dish, forming a metal-enriched polymer ring film. Distinguished from other traditional liquid-to-solid conversing methods, the proposed new method takes advantage of enhanced homogeneity for the target elements inside the ring film. The modified glass petri dish was used to control the ring-shaped concentration. Due to the specially designed circular groove at the bottom of this dish, where the PVA solution and liquid sample mixture accumulated, the target elements were concentrated in this small ring, which is beneficial for enhancing and stabilizing the plasma signals compared to the direct liquid sample analysis using LIBS. The limits of detection for Ag, Cu, Cr, and Ba obtained with the RSPC-LIBS technology were 0.098  μg·mL -1 , 0.18  μg·mL -1 , 0.83  μg·mL -1 , and 0.046  μg·mL -1 , respectively, which provided greater improvement than the direct bulk liquid analysis using LIBS.

Analysis of PBDEs in soil, dust, spiked lake water, and human serum samples by hollow fiber-liquid phase microextraction combined with GC-ICP-MS.

PubMed

Xiao, Qin; Hu, Bin; Duan, Jiankun; He, Man; Zu, Wanqing

2007-10-01

A novel method for the analysis of four polybrominated diphenyl ethers (PBDEs) in environmental and human serum samples based on hollow fiber-liquid phase microextraction (HF-LPME) followed by gas chromatography-inductively coupled plasma mass spectrometric (GC-ICP-MS) detection has been developed. The organic solvent in the porous hollow fiber was first dipped into the sample for extraction at a given time, and the retracted organic phase was introduced into the GC-ICP-MS for analysis. The addition of methanol has a strong effect on the HF-LPME extraction efficiency. Other significant parameters affecting the extraction efficiency of HF-LPME were also studied. HF-LPME was effective to isolate the analytes from the complex matrix. Under the optimized conditions, the detection limits of the proposed method varied from 15.2 to 40.5 ng/L. In general, the relative standard deviations (RSDs) were less than 10%. Good linearity was obtained with the correlation coefficients all better than 0.999. The proposed method is simple, quick, few microliters of organic solvent required, and is especially suitable for the analysis of the real sample with small amount available. The overall process of HF-LPME with GC-ICP-MS was applied successfully for the determination of polybrominated diphenyl ethers (PBDEs) in environmental and spiked human serum samples, and the results were satisfactory.

Analysis of non-esterified fatty acids in human samples by solid-phase-extraction and gas chromatography/mass spectrometry.

PubMed

Kopf, Thomas; Schmitz, Gerd

2013-11-01

The determination of the fatty acid (FA) profile of lipid classes is essential for lipidomic analysis. We recently developed a GC/MS-method for the analysis of the FA profile of total FAs, i.e. the totality of bound and unbound FAs, in any given biological sample (TOFAs). Here, we present a method for the analysis of non-esterified fatty acids (NEFAs) in biological samples, i.e. the fraction that is present as extractable free fatty acids. Lipid extraction is performed according to Dole using 80/20 2-propanol/n-hexane (v/v), with 0.1% H2SO4. The fatty acid-species composition of this NEFA-fraction is determined as FAME after derivatization with our GC/MS-method on a BPX column (Shimadzu). Validation of the NEFA-method presented was performed in human plasma samples. The validated method has been used with human plasma, cells and tissues, as well as mammalian body fluids and tissue samples. The newly developed solid-phase-extraction (SPE)-GC-MS method allows the rapid separation of the NEFA-fraction from a neutral lipid extract of plasma samples. As a major advantage compared to G-FID-methods, GC-MS allows the use of stable isotope labeled fatty acid precursors to monitor fatty acid metabolism. Copyright © 2013 Elsevier B.V. All rights reserved.

Surfactant/detergent titration analysis method and apparatus for machine working fluids, surfactant-containing wastewater and the like

DOEpatents

Smith, Douglas D.; Hiller, John M.

1998-01-01

The present invention is an improved method and related apparatus for quantitatively analyzing machine working fluids and other aqueous compositions such as wastewater which contain various mixtures of cationic, neutral, and/or anionic surfactants, soluble soaps, and the like. The method utilizes a single-phase, non-aqueous, reactive titration composition containing water insoluble bismuth nitrate dissolved in glycerol for the titration reactant. The chemical reaction of the bismuth ion and glycerol with the surfactant in the test solutions results in formation of micelles, changes in micelle size, and the formation of insoluble bismuth soaps. These soaps are quantified by physical and chemical changes in the aqueous test solution. Both classical potentiometric analysis and turbidity measurements have been used as sensing techniques to determine the quantity of surfactant present in test solutions. This method is amenable to the analysis of various types of new, in-use, dirty or decomposed surfactants and detergents. It is a quick and efficient method utilizing a single-phase reaction without needing a separate extraction from the aqueous solution. It is adaptable to automated control with simple and reliable sensing methods. The method is applicable to a variety of compositions with concentrations from about 1% to about 10% weight. It is also applicable to the analysis of waste water containing surfactants with appropriate pre-treatments for concentration.

Surfactant/detergent titration analysis method and apparatus for machine working fluids, surfactant-containing wastewater and the like

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, D.D.; Hiller, J.M.

1998-02-24

The present invention is an improved method and related apparatus for quantitatively analyzing machine working fluids and other aqueous compositions such as wastewater which contain various mixtures of cationic, neutral, and/or anionic surfactants, soluble soaps, and the like. The method utilizes a single-phase, non-aqueous, reactive titration composition containing water insoluble bismuth nitrate dissolved in glycerol for the titration reactant. The chemical reaction of the bismuth ion and glycerol with the surfactant in the test solutions results in formation of micelles, changes in micelle size, and the formation of insoluble bismuth soaps. These soaps are quantified by physical and chemical changesmore » in the aqueous test solution. Both classical potentiometric analysis and turbidity measurements have been used as sensing techniques to determine the quantity of surfactant present in test solutions. This method is amenable to the analysis of various types of new, in-use, dirty or decomposed surfactants and detergents. It is a quick and efficient method utilizing a single-phase reaction without needing a separate extraction from the aqueous solution. It is adaptable to automated control with simple and reliable sensing methods. The method is applicable to a variety of compositions with concentrations from about 1% to about 10% weight. It is also applicable to the analysis of waste water containing surfactants with appropriate pre-treatments for concentration. 1 fig.« less

Surfactant/detergent titration analysis method and apparatus for machine working fluids, surfactant-containing wastewater and the like

DOEpatents

Smith, D.D.; Hiller, J.M.

1998-02-24

The present invention is an improved method and related apparatus for quantitatively analyzing machine working fluids and other aqueous compositions such as wastewater which contain various mixtures of cationic, neutral, and/or anionic surfactants, soluble soaps, and the like. The method utilizes a single-phase, non-aqueous, reactive titration composition containing water insoluble bismuth nitrate dissolved in glycerol for the titration reactant. The chemical reaction of the bismuth ion and glycerol with the surfactant in the test solutions results in formation of micelles, changes in micelle size, and the formation of insoluble bismuth soaps. These soaps are quantified by physical and chemical changes in the aqueous test solution. Both classical potentiometric analysis and turbidity measurements have been used as sensing techniques to determine the quantity of surfactant present in test solutions. This method is amenable to the analysis of various types of new, in-use, dirty or decomposed surfactants and detergents. It is a quick and efficient method utilizing a single-phase reaction without needing a separate extraction from the aqueous solution. It is adaptable to automated control with simple and reliable sensing methods. The method is applicable to a variety of compositions with concentrations from about 1% to about 10% weight. It is also applicable to the analysis of waste water containing surfactants with appropriate pre-treatments for concentration. 1 fig.

Solid Phase Extraction (SPE) for Biodiesel Processing and Analysis

DTIC Science & Technology

2017-12-13

1 METHODS ...sources. There are several methods than can be applied to development of separation techniques that may replace necessary water wash steps in...biodiesel refinement. Unfortunately, the most common methods are poorly suited or face high costs when applied to diesel purification. Distillation is

Wavelength modulation spectroscopy--digital detection of gas absorption harmonics based on Fourier analysis.

PubMed

Mei, Liang; Svanberg, Sune

2015-03-20

This work presents a detailed study of the theoretical aspects of the Fourier analysis method, which has been utilized for gas absorption harmonic detection in wavelength modulation spectroscopy (WMS). The lock-in detection of the harmonic signal is accomplished by studying the phase term of the inverse Fourier transform of the Fourier spectrum that corresponds to the harmonic signal. The mathematics and the corresponding simulation results are given for each procedure when applying the Fourier analysis method. The present work provides a detailed view of the WMS technique when applying the Fourier analysis method.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE--COMPENDIUM OF METHODS FOR ANALYSIS OF METALS, PESTICIDES, AND VOCS IN WATER (EPA-COMPENDIUM)

EPA Science Inventory

This compendium includes descriptions of methods for analyzing metals, pesticides and volatile organic compounds (VOCs) in water. The individual methods covered are these: (1) Method 200.8: determination of trace elements in waters and wastes by inductively coupled plasma-mass s...

A Phase-Only technique for enhancing the high-frequency MASW method

USDA-ARS?s Scientific Manuscript database

For soil exploration in the vadose zone, a high-frequency multi-channel analysis of surface waves (HF-MASW) method has been developed. In the study, several practical techniques were applied to enhance the overtone image of the HF-MASW method. They included (1) the self-adaptive MASW method using a ...

Time Domain Radar Laboratory Operating System Development and Transient EM Analysis.

DTIC Science & Technology

1981-09-01

polarization of the return, arg used. Other similar methods use amplitude and phase differences or special properties of Rayleigh region scattering. All these...3ptias Inverse Scattering ... 19 2. "!xact" Inverse Scattering !Nethod .. 20 3. Other Methods ................... 21 C. REVIEW OF TDRL PROGRESS AT SPS...explicit independant variable in.most methods . In the past, frequency domain analysis has been the primary means of analyzing aan-monochromatic EM

Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

1992-01-01

A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

Application of Solid Phase Microextraction with Gas Chromatography-Mass Spectrometry as a Rapid, Reliable, and Safe Method for Field Sampling and Analysis of Chemical Warfare Agent Precursors

DTIC Science & Technology

2005-03-01

in hair samples with analysis by GC-MS [41,42]. The research discussed here examined a polydimethylsiloxane polymer with 10% activated charcoal (PDMS...Field Sampling and Analysis of Chemical Warfare Agent Precursors” Name of Candidate: LT Douglas Parrish Doctor of Philosophy, Environmental...Microextraction with Gas Chromatography-Mass Spectrometry as a Rapid, Reliable, and Safe Method for Field Sampling and Analysis of Chemical Warfare

Quantifying the similarity of seismic polarizations

NASA Astrophysics Data System (ADS)

Jones, Joshua P.; Eaton, David W.; Caffagni, Enrico

2016-02-01

Assessing the similarities of seismic attributes can help identify tremor, low signal-to-noise (S/N) signals and converted or reflected phases, in addition to diagnosing site noise and sensor misalignment in arrays. Polarization analysis is a widely accepted method for studying the orientation and directional characteristics of seismic phases via computed attributes, but similarity is ordinarily discussed using qualitative comparisons with reference values or known seismic sources. Here we introduce a technique for quantitative polarization similarity that uses weighted histograms computed in short, overlapping time windows, drawing on methods adapted from the image processing and computer vision literature. Our method accounts for ambiguity in azimuth and incidence angle and variations in S/N ratio. Measuring polarization similarity allows easy identification of site noise and sensor misalignment and can help identify coherent noise and emergent or low S/N phase arrivals. Dissimilar azimuths during phase arrivals indicate misaligned horizontal components, dissimilar incidence angles during phase arrivals indicate misaligned vertical components and dissimilar linear polarization may indicate a secondary noise source. Using records of the Mw = 8.3 Sea of Okhotsk earthquake, from Canadian National Seismic Network broad-band sensors in British Columbia and Yukon Territory, Canada, and a vertical borehole array at Hoadley gas field, central Alberta, Canada, we demonstrate that our method is robust to station spacing. Discrete wavelet analysis extends polarization similarity to the time-frequency domain in a straightforward way. Time-frequency polarization similarities of borehole data suggest that a coherent noise source may have persisted above 8 Hz several months after peak resource extraction from a `flowback' type hydraulic fracture.

An interactive graphics system to facilitate finite element structural analysis

NASA Technical Reports Server (NTRS)

Burk, R. C.; Held, F. H.

1973-01-01

The characteristics of an interactive graphics systems to facilitate the finite element method of structural analysis are described. The finite element model analysis consists of three phases: (1) preprocessing (model generation), (2) problem solution, and (3) postprocessing (interpretation of results). The advantages of interactive graphics to finite element structural analysis are defined.

Electromagnetic phenomena analysis in brushless DC motor with speed control using PWM method

NASA Astrophysics Data System (ADS)

Ciurys, Marek Pawel

2017-12-01

Field-circuit model of a brushless DC motor with speed control using PWM method was developed. Waveforms of electrical and mechanical quantities of the designed motor with a high pressure vane pump built in a rotor of the motor were computed. Analysis of electromagnetic phenomena in the system: single phase AC network - converter - BLDC motor was carried out.

NHEXAS PHASE I REGION 5 STUDY--STANDARD OPERATING PROCEDURE--COMPENDIUM OF METHOD SUMMARIES FOR COLLECTION AND ANALYSIS OF METALS AND VOCS IN BLOOD AND URINE (CDC-COMPENDIUM)

EPA Science Inventory

This compendium includes method summaries provided by the Centers for Disease Control and Prevention/National Center for Environmental Health (CDC/NCEH) for collection and shipping of blood and urine samples for analysis of metals and volatile organic compounds (VOCs). It provide...

NHEXAS PHASE I MARYLAND STUDY--STANDARD OPERATING PROCEDURE--COMPENDIUM OF METHOD SUMMARIES FOR COLLECTION AND ANALYSIS OF METALS, PESTICIDE METABOLITES, AND VOCS IN BLOOD AND URINE (CDC-COMPENDIUM)

EPA Science Inventory

This compendium includes method summaries provided by the Centers for Disease Control and Prevention/National Center for Environmental Health (CDC/NCEH) for the collection and shipping of blood and urine samples for analysis of metals and volatile organic compounds (VOCs). It pro...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE--COMPENDIUM OF METHODS FOR ANALYSIS OF TRACE METALS AND PESTICIDES IN DIETARY SAMPLES USING TOTAL DIET STUDY PROCEDURES (FDA-COMPENDIUM)

EPA Science Inventory

This compendium contains seven SOPs developed by Food and Drug Administration (FDA) laboratories for methods of analyzing trace metals in dietary samples collected using Total Diet study procedures. The SOPs include the following: (1) Quality Control for Analysis of NHEXAS Food o...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE--COMPENDIUM OF METHOD SUMMARIES FOR COLLECTION AND ANALYSIS OF METALS, PESTICIDE METABOLITES, AND VOC IN BLOOD AND URINE (CDC-COMPENDIUM)

EPA Science Inventory

This compendium includes method summaries provided by the Centers for Disease Control and Prevention/National Center for Environmental Health (CDC/NCEH) for the collection and shipping of blood and urine samples for analysis of metals and volatile organic compounds (VOCs). It pro...

Birefringence measurement of retinal nerve fiber layer using polarization-sensitive spectral domain optical coherence tomography with Jones matrix based analysis

NASA Astrophysics Data System (ADS)

Yamanari, Masahiro; Miura, Masahiro; Makita, Shuichi; Yatagai, Toyohiko; Yasuno, Yoshiaki

2007-02-01

Birefringence of retinal nerve fiber layer is measured by polarization-sensitive spectral domain optical coherence tomography using the B-scan-oriented polarization modulation method. Birefringence of the optical fiber and the cornea is compensated by Jones matrix based analysis. Three-dimensional phase retardation map around the optic nerve head and en-face phase retardation map of the retinal nerve fiber layer are shown. Unlike scanning laser polarimetry, our system can measure the phase retardation quantitatively without using bow-tie pattern of the birefringence in the macular region, which enables diagnosis of glaucoma even if the patients have macular disease.

Simulation of anisoplanatic imaging through optical turbulence using numerical wave propagation with new validation analysis

NASA Astrophysics Data System (ADS)

Hardie, Russell C.; Power, Jonathan D.; LeMaster, Daniel A.; Droege, Douglas R.; Gladysz, Szymon; Bose-Pillai, Santasri

2017-07-01

We present a numerical wave propagation method for simulating imaging of an extended scene under anisoplanatic conditions. While isoplanatic simulation is relatively common, few tools are specifically designed for simulating the imaging of extended scenes under anisoplanatic conditions. We provide a complete description of the proposed simulation tool, including the wave propagation method used. Our approach computes an array of point spread functions (PSFs) for a two-dimensional grid on the object plane. The PSFs are then used in a spatially varying weighted sum operation, with an ideal image, to produce a simulated image with realistic optical turbulence degradation. The degradation includes spatially varying warping and blurring. To produce the PSF array, we generate a series of extended phase screens. Simulated point sources are numerically propagated from an array of positions on the object plane, through the phase screens, and ultimately to the focal plane of the simulated camera. Note that the optical path for each PSF will be different, and thus, pass through a different portion of the extended phase screens. These different paths give rise to a spatially varying PSF to produce anisoplanatic effects. We use a method for defining the individual phase screen statistics that we have not seen used in previous anisoplanatic simulations. We also present a validation analysis. In particular, we compare simulated outputs with the theoretical anisoplanatic tilt correlation and a derived differential tilt variance statistic. This is in addition to comparing the long- and short-exposure PSFs and isoplanatic angle. We believe this analysis represents the most thorough validation of an anisoplanatic simulation to date. The current work is also unique that we simulate and validate both constant and varying Cn2(z) profiles. Furthermore, we simulate sequences with both temporally independent and temporally correlated turbulence effects. Temporal correlation is introduced by generating even larger extended phase screens and translating this block of screens in front of the propagation area. Our validation analysis shows an excellent match between the simulation statistics and the theoretical predictions. Thus, we think this tool can be used effectively to study optical anisoplanatic turbulence and to aid in the development of image restoration methods.

Excitation power quantities in phase resonance testing of nonlinear systems with phase-locked-loop excitation

NASA Astrophysics Data System (ADS)

Peter, Simon; Leine, Remco I.

2017-11-01

Phase resonance testing is one method for the experimental extraction of nonlinear normal modes. This paper proposes a novel method for nonlinear phase resonance testing. Firstly, the issue of appropriate excitation is approached on the basis of excitation power considerations. Therefore, power quantities known from nonlinear systems theory in electrical engineering are transferred to nonlinear structural dynamics applications. A new power-based nonlinear mode indicator function is derived, which is generally applicable, reliable and easy to implement in experiments. Secondly, the tuning of the excitation phase is automated by the use of a Phase-Locked-Loop controller. This method provides a very user-friendly and fast way for obtaining the backbone curve. Furthermore, the method allows to exploit specific advantages of phase control such as the robustness for lightly damped systems and the stabilization of unstable branches of the frequency response. The reduced tuning time for the excitation makes the commonly used free-decay measurements for the extraction of backbone curves unnecessary. Instead, steady-state measurements for every point of the curve are obtained. In conjunction with the new mode indicator function, the correlation of every measured point with the associated nonlinear normal mode of the underlying conservative system can be evaluated. Moreover, it is shown that the analysis of the excitation power helps to locate sources of inaccuracies in the force appropriation process. The method is illustrated by a numerical example and its functionality in experiments is demonstrated on a benchmark beam structure.

Determination of pterins in urine by HPLC with UV and fluorescent detection using different types of chromatographic stationary phases (HILIC, RP C8, RP C18).

PubMed

Kośliński, Piotr; Jarzemski, Piotr; Markuszewski, Michał J; Kaliszan, Roman

2014-03-01

Pterins are a class of potential cancer biomarkers. New methods involving hydrophilic interaction liquid chromatography (HILIC) and reversed phase (RP) high-performance liquid chromatography have been developed for analysis of eight pterin compounds: 6,7-dimethylpterin, pterin, 6-OH-methylpterin, biopterin, isoxanthopterin, neopterin, xanthopterin, and pterin-6-carboxylic acid. The effect of mobile phase composition, buffer type, pH and concentration on retention using HILIC, C8 and C18 RP stationary phases were examined. Separation of pterins on RP and HILIC stationary phase was performed and optimized. Eight pterins were successfully separated on HILIC Luna diol-bonded phases, Aquasil C18 RP column and LiChrospher C8 RP column. Determination and separation of the pterins from urine samples were performed on HILIC Luna and LiChrospher C8 RP columns which were chosen as the most appropriate ones. Finally, LiChrospher C8 RP column with fluorescence detection was selected for further validation of the method. The optimum chromatographic condition was mobile phase methanol (A)/phosphoric buffer pH 7, 10mM (B), isocratic elution 0-15min 5% A flow=0.5ml/min 15-17min. 5% A, flow=0.5-1ml/min the linearity (R(2)>0.997) and retention time repeatability (RSD%<1) were at satisfactory level. The precision of peak areas expressed as RSD in % was between 0.55 and 14. Pterins detection limits varied from 0.041ng/ml to 2.9ng/ml. Finally, HPLC method was used for the analysis of pterins in urine samples with two different oxidation procedures. Concentration levels of pterin compounds in bladder cancer patients and healthy subjects were compared. Copyright © 2013 Elsevier B.V. All rights reserved.

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mathematic model analysis of Gaussian beam propagation through an arbitrary thickness random phase screen.

PubMed

Tian, Yuzhen; Guo, Jin; Wang, Rui; Wang, Tingfeng

2011-09-12

In order to research the statistical properties of Gaussian beam propagation through an arbitrary thickness random phase screen for adaptive optics and laser communication application in the laboratory, we establish mathematic models of statistical quantities, which are based on the Rytov method and the thin phase screen model, involved in the propagation process. And the analytic results are developed for an arbitrary thickness phase screen based on the Kolmogorov power spectrum. The comparison between the arbitrary thickness phase screen and the thin phase screen shows that it is more suitable for our results to describe the generalized case, especially the scintillation index.

Quality evaluation of moluodan concentrated pill using high-performance liquid chromatography fingerprinting coupled with chemometrics.

PubMed

Tao, Lingyan; Zhang, Qing; Wu, Yongjiang; Liu, Xuesong

2016-12-01

In this study, a fast and effective high-performance liquid chromatography method was developed to obtain a fingerprint chromatogram and quantitative analysis simultaneously of four indexes including gallic acid, chlorogenic acid, albiflorin and paeoniflorin of the traditional Chinese medicine Moluodan Concentrated Pill. The method was performed by using a Waters X-bridge C 18 reversed phase column on an Agilent 1200S high-performance liquid chromatography system coupled with diode array detection. The mobile phase of the high-performance liquid chromatography method was composed of 20 mmol/L phosphate solution and acetonitrile with a 1 mL/min eluent velocity, under a detection temperature of 30°C and a UV detection wavelength of 254 nm. After the methodology validation, 16 batches of Moluodan Concentrated Pill were analyzed by this high-performance liquid chromatography method and both qualitative and quantitative evaluation results were achieved by similarity analysis, principal component analysis and hierarchical cluster analysis. The results of these three chemometrics were in good agreement and all indicated that batch 10 and batch 16 showed significant differences with the other 14 batches. This suggested that the developed high-performance liquid chromatography method could be applied in the quality evaluation of Moluodan Concentrated Pill. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Automated measurement and classification of pulmonary blood-flow velocity patterns using phase-contrast MRI and correlation analysis.

PubMed

van Amerom, Joshua F P; Kellenberger, Christian J; Yoo, Shi-Joon; Macgowan, Christopher K

2009-01-01

An automated method was evaluated to detect blood flow in small pulmonary arteries and classify each as artery or vein, based on a temporal correlation analysis of their blood-flow velocity patterns. The method was evaluated using velocity-sensitive phase-contrast magnetic resonance data collected in vitro with a pulsatile flow phantom and in vivo in 11 human volunteers. The accuracy of the method was validated in vitro, which showed relative velocity errors of 12% at low spatial resolution (four voxels per diameter), but was reduced to 5% at increased spatial resolution (16 voxels per diameter). The performance of the method was evaluated in vivo according to its reproducibility and agreement with manual velocity measurements by an experienced radiologist. In all volunteers, the correlation analysis was able to detect and segment peripheral pulmonary vessels and distinguish arterial from venous velocity patterns. The intrasubject variability of repeated measurements was approximately 10% of peak velocity, or 2.8 cm/s root-mean-variance, demonstrating the high reproducibility of the method. Excellent agreement was obtained between the correlation analysis and radiologist measurements of pulmonary velocities, with a correlation of R2=0.98 (P<.001) and a slope of 0.99+/-0.01.

Improved sample preparation of glyphosate and methylphosphonic acid by EPA method 6800A and time-of-flight mass spectrometry using novel solid-phase extraction.

PubMed

Wagner, Rebecca; Wetzel, Stephanie J; Kern, John; Kingston, H M Skip

2012-02-01

The employment of chemical weapons by rogue states and/or terrorist organizations is an ongoing concern in the United States. The quantitative analysis of nerve agents must be rapid and reliable for use in the private and public sectors. Current methods describe a tedious and time-consuming derivatization for gas chromatography-mass spectrometry and liquid chromatography in tandem with mass spectrometry. Two solid-phase extraction (SPE) techniques for the analysis of glyphosate and methylphosphonic acid are described with the utilization of isotopically enriched analytes for quantitation via atmospheric pressure chemical ionization-quadrupole time-of-flight mass spectrometry (APCI-Q-TOF-MS) that does not require derivatization. Solid-phase extraction-isotope dilution mass spectrometry (SPE-IDMS) involves pre-equilibration of a naturally occurring sample with an isotopically enriched standard. The second extraction method, i-Spike, involves loading an isotopically enriched standard onto the SPE column before the naturally occurring sample. The sample and the spike are then co-eluted from the column enabling precise and accurate quantitation via IDMS. The SPE methods in conjunction with IDMS eliminate concerns of incomplete elution, matrix and sorbent effects, and MS drift. For accurate quantitation with IDMS, the isotopic contribution of all atoms in the target molecule must be statistically taken into account. This paper describes two newly developed sample preparation techniques for the analysis of nerve agent surrogates in drinking water as well as statistical probability analysis for proper molecular IDMS. The methods described in this paper demonstrate accurate molecular IDMS using APCI-Q-TOF-MS with limits of quantitation as low as 0.400 mg/kg for glyphosate and 0.031 mg/kg for methylphosphonic acid. Copyright © 2012 John Wiley & Sons, Ltd.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jo, J.C.; Shin, W.K.; Choi, C.Y.

Transient heat transfer problems with phase changes (Stefan problems) occur in many engineering situations, including potential core melting and solidification during pressurized-water-reactor severe accidents, ablation of thermal shields, melting and solidification of alloys, and many others. This article addresses the numerical analysis of nonlinear transient heat transfer with melting or solidification. An effective and simple procedure is presented for the simulation of the motion of the boundary and the transient temperature field during the phase change process. To accomplish this purpose, an iterative implicit solution algorithm has been developed by employing the dual-reciprocity boundary-element method. The dual-reciprocity boundary-element approach providedmore » in this article is much simpler than the usual boundary-element method in applying a reciprocity principle and an available technique for dealing with the domain integral of the boundary element formulation simultaneously. In this article, attention is focused on two-dimensional melting (ablation)/solidification problems for simplicity. The accuracy and effectiveness of the present analysis method have been illustrated through comparisons of the calculation results of some examples of one-phase ablation/solidification problems with their known semianalytical or numerical solutions where available.« less

HPLC separation of acetaminophen and its impurities using a mixed-mode reversed-phase/cation exchange stationary phase.

PubMed

Călinescu, Octavian; Badea, Irinel A; Vlădescu, Luminiţa; Meltzer, Viorica; Pincu, Elena

2012-04-01

Determination of acetaminophen and its main impurities: 4-nitrophenol, 4'-chloroacetanilide, as well as 4-aminophenol and its degradation products, p-benzoquinone and hydroquinone has been developed and validated by a new high-performance liquid chromatography method. Chromatographic separation has been obtained on a Hypersil Duet C18/SCX column, using gradient elution, with a mixture of phosphate buffer (pH = 4.88) and methanol as a mobile phase. Analysis time did not exceed 14.5 min and good resolutions, peak shapes and asymmetries have resulted. The linearity of the method has been tested in the range of 5.0-60 µg/mL for acetaminophen and 0.5-6 µg/mL for the other compounds. The limits of detection and quantification have been also established to be lower than 0.1 µg/mL and 0.5 µg/mL, respectively. The method has been successfully applied for the analysis of commercial acetaminophen preparations. © The Author [2012]. Published by Oxford University Press. All rights reserved.

Validated LC-MS-MS Method for Multiresidual Analysis of 13 Illicit Phenethylamines in Amniotic Fluid.

PubMed

Burrai, Lucia; Nieddu, Maria; Carta, Antonio; Trignano, Claudia; Sanna, Raimonda; Boatto, Gianpiero

2016-04-01

A multi-residue analytical method was developed for the determination in amniotic fluid (AF) of 13 illicit phenethylamines, including 12 compounds never investigated in this matrix before. Samples were subject to solid-phase extraction using; hydrophilic-lipophilic balance cartridges which gave good recoveries and low matrix effects on analysis of the extracts. The quantification was performed by liquid chromatography electrospray tandem mass spectrometry. The water-acetonitrile mobile phase containing 0.1% formic acid, used with a C18 reversed phase column, provided adequate separation, resolution and signal-to-noise ratio for the analytes and the internal standard. The final optimized method was validated according to international guidelines. A monitoring campaign to assess fetal exposure to these 13 substances of abuse has been performed on AF test samples obtained from pregnant women. All mothers (n = 194) reported no use of drugs of abuse during pregnancy, and this was confirmed by the analytical data. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Regional water-quality analysis of 2,4-D and dicamba in river water using gas chromatography-isotope dilution mass spectrometry

USGS Publications Warehouse

Thurman, E.M.; Zimmerman, L.R.; Aga, D.S.; Gilliom, R.J.

2001-01-01

Gas chromatography with isotope dilution mass spectrometry (GC-MS) and enzyme-linked immunosorbent assay (ELISA) were used in regional National Water Quality Assessment studies of the herbicides, 2,4-D and dicamba, in river water across the United States. The GC-MS method involved solid-phase extraction, derivatized with deutemted 2,4-D, and analysis by selected ion monitoring. The ELISA method was applied after preconcentration with solid-phase extraction. The ELISA method was unreliable because of interference from humic substances that were also isolated by solid-phase extraction. Therefore, GC-MS was used to analyzed 80 samples from river water from 14 basins. The frequency of detection of dicamba (28%) was higher than that for 2,4-D (16%). Concentrations were higher for dicamba than for 2,4-D, ranging from less than the detection limit (<0.05 ??g/L) to 3.77 ??g/L, in spite of 5 times more annual use of 2,4-D as compared to dicamba. These results suggest that 2,4-D degrades more rapidly in the environment than dicamba.

Direct numerical simulation of reactor two-phase flows enabled by high-performance computing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fang, Jun; Cambareri, Joseph J.; Brown, Cameron S.

Nuclear reactor two-phase flows remain a great engineering challenge, where the high-resolution two-phase flow database which can inform practical model development is still sparse due to the extreme reactor operation conditions and measurement difficulties. Owing to the rapid growth of computing power, the direct numerical simulation (DNS) is enjoying a renewed interest in investigating the related flow problems. A combination between DNS and an interface tracking method can provide a unique opportunity to study two-phase flows based on first principles calculations. More importantly, state-of-the-art high-performance computing (HPC) facilities are helping unlock this great potential. This paper reviews the recent researchmore » progress of two-phase flow DNS related to reactor applications. The progress in large-scale bubbly flow DNS has been focused not only on the sheer size of those simulations in terms of resolved Reynolds number, but also on the associated advanced modeling and analysis techniques. Specifically, the current areas of active research include modeling of sub-cooled boiling, bubble coalescence, as well as the advanced post-processing toolkit for bubbly flow simulations in reactor geometries. A novel bubble tracking method has been developed to track the evolution of bubbles in two-phase bubbly flow. Also, spectral analysis of DNS database in different geometries has been performed to investigate the modulation of the energy spectrum slope due to bubble-induced turbulence. In addition, the single-and two-phase analysis results are presented for turbulent flows within the pressurized water reactor (PWR) core geometries. The related simulations are possible to carry out only with the world leading HPC platforms. These simulations are allowing more complex turbulence model development and validation for use in 3D multiphase computational fluid dynamics (M-CFD) codes.« less

Multi-Scale Computational Modeling of Two-Phased Metal Using GMC Method

NASA Technical Reports Server (NTRS)

Moghaddam, Masoud Ghorbani; Achuthan, A.; Bednacyk, B. A.; Arnold, S. M.; Pineda, E. J.

2014-01-01

A multi-scale computational model for determining plastic behavior in two-phased CMSX-4 Ni-based superalloys is developed on a finite element analysis (FEA) framework employing crystal plasticity constitutive model that can capture the microstructural scale stress field. The generalized method of cells (GMC) micromechanics model is used for homogenizing the local field quantities. At first, GMC as stand-alone is validated by analyzing a repeating unit cell (RUC) as a two-phased sample with 72.9% volume fraction of gamma'-precipitate in the gamma-matrix phase and comparing the results with those predicted by finite element analysis (FEA) models incorporating the same crystal plasticity constitutive model. The global stress-strain behavior and the local field quantity distributions predicted by GMC demonstrated good agreement with FEA. High computational saving, at the expense of some accuracy in the components of local tensor field quantities, was obtained with GMC. Finally, the capability of the developed multi-scale model linking FEA and GMC to solve real life sized structures is demonstrated by analyzing an engine disc component and determining the microstructural scale details of the field quantities.

Simultaneous analysis of different classes of phytohormones in coconut (Cocos nucifera L.) water using high-performance liquid chromatography and liquid chromatography-tandem mass spectrometry after solid-phase extraction.

PubMed

Ma, Zhen; Ge, Liya; Lee, Anna S Y; Yong, Jean Wan Hong; Tan, Swee Ngin; Ong, Eng Shi

2008-03-10

Coconut (Cocos nucifera L.) water, which contains many uncharacterized phytohormones is extensively used as a growth promoting supplement in plant tissue culture. In this paper, a high-performance liquid chromatography (HPLC) method was developed for the simultaneous determination of various classes phytohormones, including indole-3-acetic acid (IAA), indole-3-butyric acid (IBA), abscisic acid (ABA), gibberellic acid (GA), zeatin (Z), N(6)-benzyladenine (BA), alpha-naphthaleneacetic acid (NAA) and 2,4-dichlorophenoxyacetic acid (2,4-D) in young coconut water (CW). The analysis was carried out using a reverse-phase HPLC gradient elution, with an aqueous mobile phase (containing 0.1% formic acid, pH adjusted to 3.2 with triethylamine (TEA)) modified by methanol, and solute detection made at 265 nm wavelength. The method was validated for specificity, quantification, accuracy and precision. After preconcentration of putative endogenous phytohormones in CW using C(18) solid-phase extraction (SPE) cartridges, the HPLC method was able to screen for putative endogenous phytohormones present in CW. Finally, the identities of the putative phytohormones present in CW were further confirmed using independent liquid chromatography-tandem mass spectrometry (LC-MS/MS) equipped with an electrospray ionization (ESI) interface.

From atomistic interfaces to dendritic patterns

NASA Astrophysics Data System (ADS)

Galenko, P. K.; Alexandrov, D. V.

2018-01-01

Transport processes around phase interfaces, together with thermodynamic properties and kinetic phenomena, control the formation of dendritic patterns. Using the thermodynamic and kinetic data of phase interfaces obtained on the atomic scale, one can analyse the formation of a single dendrite and the growth of a dendritic ensemble. This is the result of recent progress in theoretical methods and computational algorithms calculated using powerful computer clusters. Great benefits can be attained from the development of micro-, meso- and macro-levels of analysis when investigating the dynamics of interfaces, interpreting experimental data and designing the macrostructure of samples. The review and research articles in this theme issue cover the spectrum of scales (from nano- to macro-length scales) in order to exhibit recently developing trends in the theoretical analysis and computational modelling of dendrite pattern formation. Atomistic modelling, the flow effect on interface dynamics, the transition from diffusion-limited to thermally controlled growth existing at a considerable driving force, two-phase (mushy) layer formation, the growth of eutectic dendrites, the formation of a secondary dendritic network due to coalescence, computational methods, including boundary integral and phase-field methods, and experimental tests for theoretical models-all these themes are highlighted in the present issue. This article is part of the theme issue `From atomistic interfaces to dendritic patterns'.

Principles of Micellar Electrokinetic Capillary Chromatography Applied in Pharmaceutical Analysis

PubMed Central

Hancu, Gabriel; Simon, Brigitta; Rusu, Aura; Mircia, Eleonora; Gyéresi, Árpád

2013-01-01

Since its introduction capillary electrophoresis has shown great potential in areas where electrophoretic techniques have rarely been used before, including here the analysis of pharmaceutical substances. The large majority of pharmaceutical substances are neutral from electrophoretic point of view, consequently separations by the classic capillary zone electrophoresis; where separation is based on the differences between the own electrophoretic mobilities of the analytes; are hard to achieve. Micellar electrokinetic capillary chromatography, a hybrid method that combines chromatographic and electrophoretic separation principles, extends the applicability of capillary electrophoretic methods to neutral analytes. In micellar electrokinetic capillary chromatography, surfactants are added to the buffer solution in concentration above their critical micellar concentrations, consequently micelles are formed; micelles that undergo electrophoretic migration like any other charged particle. The separation is based on the differential partitioning of an analyte between the two-phase system: the mobile aqueous phase and micellar pseudostationary phase. The present paper aims to summarize the basic aspects regarding separation principles and practical applications of micellar electrokinetic capillary chromatography, with particular attention to those relevant in pharmaceutical analysis. PMID:24312804

Multifractality and Network Analysis of Phase Transition

PubMed Central

Li, Wei; Yang, Chunbin; Han, Jihui; Su, Zhu; Zou, Yijiang

2017-01-01

Many models and real complex systems possess critical thresholds at which the systems shift dramatically from one sate to another. The discovery of early-warnings in the vicinity of critical points are of great importance to estimate how far the systems are away from the critical states. Multifractal Detrended Fluctuation analysis (MF-DFA) and visibility graph method have been employed to investigate the multifractal and geometrical properties of the magnetization time series of the two-dimensional Ising model. Multifractality of the time series near the critical point has been uncovered from the generalized Hurst exponents and singularity spectrum. Both long-term correlation and broad probability density function are identified to be the sources of multifractality. Heterogeneous nature of the networks constructed from magnetization time series have validated the fractal properties. Evolution of the topological quantities of the visibility graph, along with the variation of multifractality, serve as new early-warnings of phase transition. Those methods and results may provide new insights about the analysis of phase transition problems and can be used as early-warnings for a variety of complex systems. PMID:28107414

Meta-analysis of PECS with individuals with ASD: investigation of targeted versus non-targeted outcomes, participant characteristics, and implementation phase.

PubMed

Ganz, Jennifer B; Davis, John L; Lund, Emily M; Goodwyn, Fara D; Simpson, Richard L

2012-01-01

The Picture Exchange Communication System (PECS) is a widely used picture/icon aided augmentative communication system designed for learners with autism and other developmental disorders. This meta-analysis analyzes the extant empirical literature for PECS relative to targeted (functional communication) and non-targeted concomitant outcomes (behavior, social skills, and speech) for learners with autism, learners with autism and intellectual disabilities and those with autism and multiple disabilities. Effect size analyses were done using the Improvement Rate Difference method, an advanced metric. Effect sizes were independently analyzed for targeted and non-targeted outcomes, student age, learner disability, and number of phases in the PECS protocol acquired by learners. Results supported the judgment that PECS is a promising intervention method. Analysis also revealed that functional communication outcomes associated with the PECS protocol were most impacted, that preschool children and those with autism generally showed the strongest training effects, and that in general students who advanced through the most PECS protocol phases had the best outcomes. Copyright © 2011 Elsevier Ltd. All rights reserved.

Improved method for the extraction and chromatographic analysis on a fused-core column of ellagitannins found in oak-aged wine.

PubMed

Navarro, María; Kontoudakis, Nikolaos; Canals, Joan Miquel; García-Romero, Esteban; Gómez-Alonso, Sergio; Zamora, Fernando; Hermosín-Gutiérrez, Isidro

2017-07-01

A new method for the analysis of ellagitannins observed in oak-aged wine is proposed, exhibiting interesting advantages with regard to previously reported analytical methods. The necessary extraction of ellagitannins from wine was simplified to a single step of solid phase extraction (SPE) using size exclusion chromatography with Sephadex LH-20 without the need for any previous SPE of phenolic compounds using reversed-phase materials. The quantitative recovery of wine ellagitannins requires a combined elution with methanol and ethyl acetate, especially for increasing the recovery of the less polar acutissimins. The chromatographic method was performed using a fused-core C18 column, thereby avoiding the coelution of main ellagitannins, such as vescalagin and roburin E. However, the very polar ellagitannins, namely, the roburins A, B and C, still partially coeluted, and their quantification was assisted by the MS detector. This methodology also enabled the analysis of free gallic and ellagic acids in the same chromatographic run. Copyright © 2017 Elsevier Ltd. All rights reserved.

Application of Haddon's matrix in qualitative research methodology: an experience in burns epidemiology.

PubMed

Deljavan, Reza; Sadeghi-Bazargani, Homayoun; Fouladi, Nasrin; Arshi, Shahnam; Mohammadi, Reza

2012-01-01

Little has been done to investigate the application of injury specific qualitative research methods in the field of burn injuries. The aim of this study was to use an analytical tool (Haddon's matrix) through qualitative research methods to better understand people's perceptions about burn injuries. This study applied Haddon's matrix as a framework and an analytical tool for a qualitative research methodology in burn research. Both child and adult burn injury victims were enrolled into a qualitative study conducted using focus group discussion. Haddon's matrix was used to develop an interview guide and also through the analysis phase. The main analysis clusters were pre-event level/human (including risky behaviors, belief and cultural factors, and knowledge and education), pre-event level/object, pre-event phase/environment and event and post-event phase (including fire control, emergency scald and burn wound management, traditional remedies, medical consultation, and severity indicators). This research gave rise to results that are possibly useful both for future injury research and for designing burn injury prevention plans. Haddon's matrix is applicable in a qualitative research methodology both at data collection and data analysis phases. The study using Haddon's matrix through a qualitative research methodology yielded substantially rich information regarding burn injuries that may possibly be useful for prevention or future quantitative research.

Liquid and vapour-phase antifungal activities of selected essential oils against candida albicans: microscopic observations and chemical characterization of cymbopogon citratus

PubMed Central

2010-01-01

Background Use of essential oils for controlling Candida albicans growth has gained significance due to the resistance acquired by pathogens towards a number of widely-used drugs. The aim of this study was to test the antifungal activity of selected essential oils against Candida albicans in liquid and vapour phase and to determine the chemical composition and mechanism of action of most potent essential oil. Methods Minimum Inhibitory concentration (MIC) of different essential oils in liquid phase, assayed through agar plate dilution, broth dilution & 96-well micro plate dilution method and vapour phase activity evaluated through disc volatilization method. Reduction of C. albicans cells with vapour exposure was estimated by kill time assay. Morphological alteration in treated/untreated C. albicans cells was observed by the Scanning electron microscopy (SEM)/Atomic force microscopy (AFM) and chemical analysis of the strongest antifungal agent/essential oil has been done by GC, GC-MS. Results Lemon grass (Cymbopogon citratus) essential oil exhibited the strongest antifungal effect followed by mentha (Mentha piperita) and eucalyptus (Eucalyptus globulus) essential oil. The MIC of lemon grass essential oil in liquid phase (288 mg/l) was significantly higher than that in the vapour phase (32.7 mg/l) and a 4 h exposure was sufficient to cause 100% loss in viability of C. albicans cells. SEM/AFM of C. albicans cells treated with lemon grass essential oil at MIC level in liquid and vapour phase showed prominent shrinkage and partial degradation, respectively, confirming higher efficacy of vapour phase. GC-MS analysis revealed that lemon grass essential oil was dominated by oxygenated monoterpenes (78.2%); α-citral or geranial (36.2%) and β-citral or neral (26.5%), monoterpene hydrocarbons (7.9%) and sesquiterpene hydrocarbons (3.8%). Conclusion Lemon grass essential oil is highly effective in vapour phase against C. albicans, leading to deleterious morphological changes in cellular structures and cell surface alterations. PMID:21067604

Histopathological image analysis of chemical-induced hepatocellular hypertrophy in mice.

PubMed

Asaoka, Yoshiji; Togashi, Yuko; Mutsuga, Mayu; Imura, Naoko; Miyoshi, Tomoya; Miyamoto, Yohei

2016-04-01

Chemical-induced hepatocellular hypertrophy is frequently observed in rodents, and is mostly caused by the induction of phase I and phase II drug metabolic enzymes and peroxisomal lipid metabolic enzymes. Liver weight is a sensitive and commonly used marker for detecting hepatocellular hypertrophy, but is also increased by a number of other factors. Histopathological observations subjectively detect changes such as hepatocellular hypertrophy based on the size of a hepatocyte. Therefore, quantitative microscopic observations are required to evaluate histopathological alterations objectively. In the present study, we developed a novel quantitative method for an image analysis of hepatocellular hypertrophy using liver sections stained with hematoxylin and eosin, and demonstrated its usefulness for evaluating hepatocellular hypertrophy induced by phenobarbital (a phase I and phase II enzyme inducer) and clofibrate (a peroxisomal enzyme inducer) in mice. The algorithm of this imaging analysis was designed to recognize an individual hepatocyte through a combination of pixel-based and object-based analyses. Hepatocellular nuclei and the surrounding non-hepatocellular cells were recognized by the pixel-based analysis, while the areas of the recognized hepatocellular nuclei were then expanded until they ran against their expanding neighboring hepatocytes and surrounding non-hepatocellular cells by the object-based analysis. The expanded area of each hepatocellular nucleus was regarded as the size of an individual hepatocyte. The results of this imaging analysis showed that changes in the sizes of hepatocytes corresponded with histopathological observations in phenobarbital and clofibrate-treated mice, and revealed a correlation between hepatocyte size and liver weight. In conclusion, our novel image analysis method is very useful for quantitative evaluations of chemical-induced hepatocellular hypertrophy. Copyright © 2015 Elsevier GmbH. All rights reserved.

Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Neuefiend, J.; Weber, H.-P.; Proffen, T.; VonDreele, R.; Palosz, W.;

Structure function monitor

DOEpatents

McGraw, John T [Placitas, NM; Zimmer, Peter C [Albuquerque, NM; Ackermann, Mark R [Albuquerque, NM

2012-01-24

Methods and apparatus for a structure function monitor provide for generation of parameters characterizing a refractive medium. In an embodiment, a structure function monitor acquires images of a pupil plane and an image plane and, from these images, retrieves the phase over an aperture, unwraps the retrieved phase, and analyzes the unwrapped retrieved phase. In an embodiment, analysis yields atmospheric parameters measured at spatial scales from zero to the diameter of a telescope used to collect light from a source.

Development of Conductivity Sensors for Multi-Phase Flow Local Measurements at the Polytechnic University of Valencia (UPV) and University Jaume I of Castellon (UJI).

PubMed

Muñoz-Cobo, José Luis; Chiva, Sergio; Méndez, Santos; Monrós, Guillem; Escrivá, Alberto; Cuadros, José Luis

2017-05-10

This paper describes all the procedures and methods currently used at UPV (Universitat Politécnica de Valencia) and UJI (University Jaume I) for the development and use of sensors for multi-phase flow analysis in vertical pipes. This paper also describes the methods that we use to obtain the values of the two-phase flow magnitudes from the sensor signals and the validation and cross-verification methods developed to check the consistency of the results obtained for these magnitudes with the sensors. First, we provide information about the procedures used to build the multi-sensor conductivity probes and some of the tests performed with different materials to avoid sensor degradation issues. In addition, we provide information about the characteristics of the electric circuits that feed the sensors. Then the data acquisition of the conductivity probe, the signal conditioning and the data processing including the device that have been designed to automatize all the measurement process of moving the sensors inside the channels by means of stepper electric motors controlled by computer are shown in operation. Then, we explain the methods used for bubble identification and categorization. Finally, we describe the methodology used to obtain the two-phase flow information from the sensor signals. This includes the following items: void fraction, gas velocity, Sauter mean diameter and interfacial area concentration. The last part of this paper is devoted to the conductance probes developed for the annular flow analysis, which includes the analysis of the interfacial waves produced in annular flow and that requires a different type of sensor.

Development of Conductivity Sensors for Multi-Phase Flow Local Measurements at the Polytechnic University of Valencia (UPV) and University Jaume I of Castellon (UJI)

PubMed Central

Muñoz-Cobo, José Luis; Chiva, Sergio; Méndez, Santos; Monrós, Guillem; Escrivá, Alberto; Cuadros, José Luis

2017-01-01

This paper describes all the procedures and methods currently used at UPV (Universitat Politécnica de Valencia) and UJI (University Jaume I) for the development and use of sensors for multi-phase flow analysis in vertical pipes. This paper also describes the methods that we use to obtain the values of the two-phase flow magnitudes from the sensor signals and the validation and cross-verification methods developed to check the consistency of the results obtained for these magnitudes with the sensors. First, we provide information about the procedures used to build the multi-sensor conductivity probes and some of the tests performed with different materials to avoid sensor degradation issues. In addition, we provide information about the characteristics of the electric circuits that feed the sensors. Then the data acquisition of the conductivity probe, the signal conditioning and the data processing including the device that have been designed to automatize all the measurement process of moving the sensors inside the channels by means of stepper electric motors controlled by computer are shown in operation. Then, we explain the methods used for bubble identification and categorization. Finally, we describe the methodology used to obtain the two-phase flow information from the sensor signals. This includes the following items: void fraction, gas velocity, Sauter mean diameter and interfacial area concentration. The last part of this paper is devoted to the conductance probes developed for the annular flow analysis, which includes the analysis of the interfacial waves produced in annular flow and that requires a different type of sensor. PMID:28489035

Simultaneous analysis and retention behavior of major isoflavonoids in Radix Puerariae lobatae and Radix Puerariae thomsonii by high performance liquid chromatography with cyclodextrins as a mobile phase modifier.

PubMed

Zeng, Aiguo; Xing, Jianfeng; Wang, Changhe; Song, Jie; Li, Cong; Yang, Xin; Yang, Guangde

2012-01-27

In order to differentiate two species of Radix Puerariae (Radix Puerariae lobatae and Radix Puerariae thomsonii) and to determine major isoflavonoids (puerarin, daidzin, daidzein and genistein) in the samples, a simple high performance liquid chromatography (HPLC) method with isocratic elution employing cyclodextrins (CDs) as mobile phase additives was developed. Various factors affecting the retention of isoflavonoids in the C(18) reversed-phase column, such as the nature of CDs, the concentration of hydroxypropyl-β-cyclodextrin (HP-β-CD) and the methanol percentage in the mobile phase, were studied. Experimental results confirmed that HP-β-CD, as a very effective mobile phase additive, could markedly reduce the retention of isoflavonoids, especially daidzein and genistein. The elution of four isoflavonoids could be achieved on a Kromasil(®) C(18) column within 56 min by using the methanol-water contained 5 mM HP-β-CD (25/75, v/v) mixture as the mobile phase. The formation of the inclusion complexes between isoflavonoids and HP-β-CD explained the modification of the retention of analytes. The apparent formation constants determined by HPLC confirmed that the stoichiometry of HP-β-CD-isoflavonoid complexes was 1:1, and the stability of the complexes depended on the size and property of isoflavonoids. The optimized method was successfully applied for the simultaneous determination of major isoflavonoids in P. lobatae and P. thomsonii samples. This work provides a useful method for the analysis of traditional Chinese herbs. Copyright © 2011 Elsevier B.V. All rights reserved.

Ab initio phasing by molecular averaging in real space with new criteria: application to structure determination of a betanodavirus.

PubMed

Yoshimura, Masato; Chen, Nai Chi; Guan, Hong Hsiang; Chuankhayan, Phimonphan; Lin, Chien Chih; Nakagawa, Atsushi; Chen, Chun Jung

2016-07-01

Molecular averaging, including noncrystallographic symmetry (NCS) averaging, is a powerful method for ab initio phase determination and phase improvement. Applications of the cross-crystal averaging (CCA) method have been shown to be effective for phase improvement after initial phasing by molecular replacement, isomorphous replacement, anomalous dispersion or combinations of these methods. Here, a two-step process for phase determination in the X-ray structural analysis of a new coat protein from a betanodavirus, Grouper nervous necrosis virus, is described in detail. The first step is ab initio structure determination of the T = 3 icosahedral virus-like particle using NCS averaging (NCSA). The second step involves structure determination of the protrusion domain of the viral molecule using cross-crystal averaging. In this method, molecular averaging and solvent flattening constrain the electron density in real space. To quantify these constraints, a new, simple and general indicator, free fraction (ff), is introduced, where ff is defined as the ratio of the volume of the electron density that is freely changed to the total volume of the crystal unit cell. This indicator is useful and effective to evaluate the strengths of both NCSA and CCA. Under the condition that a mask (envelope) covers the target molecule well, an ff value of less than 0.1, as a new rule of thumb, gives sufficient phasing power for the successful construction of new structures.

Fiber-based polarization-sensitive OCT of the human retina with correction of system polarization distortions

PubMed Central

Braaf, Boy; Vermeer, Koenraad A.; de Groot, Mattijs; Vienola, Kari V.; de Boer, Johannes F.

2014-01-01

In polarization-sensitive optical coherence tomography (PS-OCT) the use of single-mode fibers causes unpredictable polarization distortions which can result in increased noise levels and erroneous changes in calculated polarization parameters. In the current paper this problem is addressed by a new Jones matrix analysis method that measures and corrects system polarization distortions as a function of wavenumber by spectral analysis of the sample surface polarization state and deeper located birefringent tissue structures. This method was implemented on a passive-component depth-multiplexed swept-source PS-OCT system at 1040 nm which was theoretically modeled using Jones matrix calculus. High-resolution B-scan images are presented of the double-pass phase retardation, diattenuation, and relative optic axis orientation to show the benefits of the new analysis method for in vivo imaging of the human retina. The correction of system polarization distortions yielded reduced phase retardation noise, and better estimates of the diattenuation and the relative optic axis orientation in weakly birefringent tissues. The clinical potential of the system is shown by en face visualization of the phase retardation and optic axis orientation of the retinal nerve fiber layer in a healthy volunteer and a glaucoma patient with nerve fiber loss. PMID:25136498

Calculating the Bending Modulus for Multicomponent Lipid Membranes in Different Thermodynamic Phases

PubMed Central

2013-01-01

We establish a computational approach to extract the bending modulus, KC, for lipid membranes from relatively small-scale molecular simulations. Fluctuations in the splay of individual pairs of lipids faithfully inform on KC in multicomponent membranes over a large range of rigidities in different thermodynamic phases. Predictions are validated by experiments even where the standard spectral analysis-based methods fail. The local nature of this method potentially allows its extension to calculations of KC in protein-laden membranes. PMID:24039553

A Review on the Nonlinear Dynamical System Analysis of Electrocardiogram Signal

PubMed Central

Mohapatra, Biswajit

2018-01-01

Electrocardiogram (ECG) signal analysis has received special attention of the researchers in the recent past because of its ability to divulge crucial information about the electrophysiology of the heart and the autonomic nervous system activity in a noninvasive manner. Analysis of the ECG signals has been explored using both linear and nonlinear methods. However, the nonlinear methods of ECG signal analysis are gaining popularity because of their robustness in feature extraction and classification. The current study presents a review of the nonlinear signal analysis methods, namely, reconstructed phase space analysis, Lyapunov exponents, correlation dimension, detrended fluctuation analysis (DFA), recurrence plot, Poincaré plot, approximate entropy, and sample entropy along with their recent applications in the ECG signal analysis. PMID:29854361

A Review on the Nonlinear Dynamical System Analysis of Electrocardiogram Signal.

PubMed

Nayak, Suraj K; Bit, Arindam; Dey, Anilesh; Mohapatra, Biswajit; Pal, Kunal

2018-01-01

Electrocardiogram (ECG) signal analysis has received special attention of the researchers in the recent past because of its ability to divulge crucial information about the electrophysiology of the heart and the autonomic nervous system activity in a noninvasive manner. Analysis of the ECG signals has been explored using both linear and nonlinear methods. However, the nonlinear methods of ECG signal analysis are gaining popularity because of their robustness in feature extraction and classification. The current study presents a review of the nonlinear signal analysis methods, namely, reconstructed phase space analysis, Lyapunov exponents, correlation dimension, detrended fluctuation analysis (DFA), recurrence plot, Poincaré plot, approximate entropy, and sample entropy along with their recent applications in the ECG signal analysis.

Subway Subsidence Monitoring and Analysis in Beijing through Envisat-Asar and Terrasar-X DATA

NASA Astrophysics Data System (ADS)

Duan, G.; Gong, H.; Chen, B.; Li, X.

2014-12-01

Subway plays a significant role in public transport in Beijing, China. The safe operation of such underground rail transports are serious threatened by ground subsidence that mainly caused by groundwater over-exploitation. It is necessary to carry out a continuous observation and analysis of the surface deformation along the newly built rails. The paper mainly studied four subways which were built in different periods(see attachment). Envisat-ASAR and Terrasar-X images of the study area were selected to measure the ground deformation. Interferometric Point Target Analysis method was gathered to process the SAR data. The method is developed based on the idea of the Permanent Scatterers SAR Interferometry method which can overcome the decorrelation and atmospheric effect to gain more precise estimation of the ground deformation. The master image can be selected according to the perpendicular, Doppler and temporal baselines to minimize the potential decorrelation. After the registration of all slave images to the master image, the PS candidates would be detected on the basis of the scattering properties of the images. A complex operation of the PSs was conducted to obtain the interferometric phase which was composed of terrain phase, atmospheric phase, deformation phase and noise. A model used for the evaluation of the contribution of each component was built by means of the least squares method. The deformation phase would be the remaining of the interferometric phase minus disturbance terms. Deformation information that came from two different kinds of data was jointly analyzed to reveal the temporal character of the rails before, during and after they were built. The regional LOS(line-of-sight) velocity around a special subway station shows that the rail has suffered from a serious uneven settlement along the rail during the observation period. In addition, time series data revealed the characteristic stages of each PS point. There is a clear accelerating trend of settlement in the construction period of the subway, and the sedimentation velocity would remain very high after a period of the opening of the line. Overall, ground subsidence had a certain delay when compared to the construction and operation of the subway.

An Isotopic Dilution Experiment Using Liquid Scintillation: A Simple Two-System, Two-Phase Analysis.

ERIC Educational Resources Information Center

Moehs, Peter J.; Levine, Samuel

1982-01-01

A simple isotonic, dilution analysis whose principles apply to methods of more complex radioanalyses is described. Suitable for clinical and instrumental analysis chemistry students, experimental manipulations are kept to a minimum involving only aqueous extraction before counting. Background information, procedures, and results are discussed.…

Multimodal pressure-flow method to assess dynamics of cerebral autoregulation in stroke and hypertension.

PubMed

Novak, Vera; Yang, Albert C C; Lepicovsky, Lukas; Goldberger, Ary L; Lipsitz, Lewis A; Peng, Chung-Kang

2004-10-25

This study evaluated the effects of stroke on regulation of cerebral blood flow in response to fluctuations in systemic blood pressure (BP). The autoregulatory dynamics are difficult to assess because of the nonstationarity and nonlinearity of the component signals. We studied 15 normotensive, 20 hypertensive and 15 minor stroke subjects (48.0 +/- 1.3 years). BP and blood flow velocities (BFV) from middle cerebral arteries (MCA) were measured during the Valsalva maneuver (VM) using transcranial Doppler ultrasound. A new technique, multimodal pressure-flow analysis (MMPF), was implemented to analyze these short, nonstationary signals. MMPF analysis decomposes complex BP and BFV signals into multiple empirical modes, representing their instantaneous frequency-amplitude modulation. The empirical mode corresponding to the VM BP profile was used to construct the continuous phase diagram and to identify the minimum and maximum values from the residual BP (BPR) and BFV (BFVR) signals. The BP-BFV phase shift was calculated as the difference between the phase corresponding to the BPR and BFVR minimum (maximum) values. BP-BFV phase shifts were significantly different between groups. In the normotensive group, the BFVR minimum and maximum preceded the BPR minimum and maximum, respectively, leading to large positive values of BP-BFV shifts. In the stroke and hypertensive groups, the resulting BP-BFV phase shift was significantly smaller compared to the normotensive group. A standard autoregulation index did not differentiate the groups. The MMPF method enables evaluation of autoregulatory dynamics based on instantaneous BP-BFV phase analysis. Regulation of BP-BFV dynamics is altered with hypertension and after stroke, rendering blood flow dependent on blood pressure.

Direct injection analysis of fatty and resin acids in papermaking process waters by HPLC/MS.

PubMed

Valto, Piia; Knuutinen, Juha; Alén, Raimo

2011-04-01

A novel HPLC-atmospheric pressure chemical ionization/MS (HPLC-APCI/MS) method was developed for the rapid analysis of selected fatty and resin acids typically present in papermaking process waters. A mixture of palmitic, stearic, oleic, linolenic, and dehydroabietic acids was separated by a commercial HPLC column (a modified stationary C(18) phase) using gradient elution with methanol/0.15% formic acid (pH 2.5) as a mobile phase. The internal standard (myristic acid) method was used to calculate the correlation coefficients and in the quantitation of the results. In the thorough quality parameters measurement, a mixture of these model acids in aqueous media as well as in six different paper machine process waters was quantitatively determined. The measured quality parameters, such as selectivity, linearity, precision, and accuracy, clearly indicated that, compared with traditional gas chromatographic techniques, the simple method developed provided a faster chromatographic analysis with almost real-time monitoring of these acids. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fault detection and classification in electrical power transmission system using artificial neural network.

PubMed

Jamil, Majid; Sharma, Sanjeev Kumar; Singh, Rajveer

2015-01-01

This paper focuses on the detection and classification of the faults on electrical power transmission line using artificial neural networks. The three phase currents and voltages of one end are taken as inputs in the proposed scheme. The feed forward neural network along with back propagation algorithm has been employed for detection and classification of the fault for analysis of each of the three phases involved in the process. A detailed analysis with varying number of hidden layers has been performed to validate the choice of the neural network. The simulation results concluded that the present method based on the neural network is efficient in detecting and classifying the faults on transmission lines with satisfactory performances. The different faults are simulated with different parameters to check the versatility of the method. The proposed method can be extended to the Distribution network of the Power System. The various simulations and analysis of signals is done in the MATLAB(®) environment.

Text grouping in patent analysis using adaptive K-means clustering algorithm

NASA Astrophysics Data System (ADS)

Shanie, Tiara; Suprijadi, Jadi; Zulhanif

2017-03-01

Patents are one of the Intellectual Property. Analyzing patent is one requirement in knowing well the development of technology in each country and in the world now. This study uses the patent document coming from the Espacenet server about Green Tea. Patent documents related to the technology in the field of tea is still widespread, so it will be difficult for users to information retrieval (IR). Therefore, it is necessary efforts to categorize documents in a specific group of related terms contained therein. This study uses titles patent text data with the proposed Green Tea in Statistical Text Mining methods consists of two phases: data preparation and data analysis stage. The data preparation phase uses Text Mining methods and data analysis stage is done by statistics. Statistical analysis in this study using a cluster analysis algorithm, the Adaptive K-Means Clustering Algorithm. Results from this study showed that based on the maximum value Silhouette, generate 87 clusters associated fifteen terms therein that can be utilized in the process of information retrieval needs.

A phase match based frequency estimation method for sinusoidal signals

NASA Astrophysics Data System (ADS)

Shen, Yan-Lin; Tu, Ya-Qing; Chen, Lin-Jun; Shen, Ting-Ao

2015-04-01

Accurate frequency estimation affects the ranging precision of linear frequency modulated continuous wave (LFMCW) radars significantly. To improve the ranging precision of LFMCW radars, a phase match based frequency estimation method is proposed. To obtain frequency estimation, linear prediction property, autocorrelation, and cross correlation of sinusoidal signals are utilized. The analysis of computational complex shows that the computational load of the proposed method is smaller than those of two-stage autocorrelation (TSA) and maximum likelihood. Simulations and field experiments are performed to validate the proposed method, and the results demonstrate the proposed method has better performance in terms of frequency estimation precision than methods of Pisarenko harmonic decomposition, modified covariance, and TSA, which contribute to improving the precision of LFMCW radars effectively.

DOT/NASA comparative assessment of Brayton engines for guideway vehicles and busses. Volume 2: Analysis and results

NASA Technical Reports Server (NTRS)

1975-01-01

Gas turbine engines were assessed for application to hear duty transportation. A summary of the assumptions, applications, and methods of analysis is included along with a discussion of the approach taken, the technical program flow chart, and weighting criteria used for performance evaluation. The various engines are compared on the bases of weight, performance, emissions and noise, technology status, and growth potential. The results of the engine screening phase and the conceptual design phase are presented.

Advances in silver ion chromatography for the analysis of fatty acids and triacylglycerols-2001 to 2011.

PubMed

Momchilova, Svetlana M; Nikolova-Damyanova, Boryana M

2012-01-01

An effort is made to critically present the achievements in silver ion chromatography during the last decade. Novelties in columns, mobile-phase compositions and detectors are described. Recent applications of silver ion chromatography in the analysis of fatty acids and triacylglycerols are presented while stressing novel analytical strategies or new objects. The tendencies in the application of the method in complementary ways with reversed-phase chromatography, chiral chromatography and, especially, mass detection are outlined.

An improved method for the analysis of sennosides in Cassia angustifolia by high-performance liquid chromatography.

PubMed

Bala, S; Uniyal, G C; Dubey, T; Singh, S P

2001-01-01

A reversed-phase column liquid chromatographic method for the analysis of sennosides A and B present in leaf and pod extracts of Cassia angustifolia has been developed using a Symmetry C18 column and a linear binary gradient profile. The method can be utilised for the quantitative determination of other sennosides as a baseline resolution for most of the constituents was achieved. The method is economical in terms of the time taken and the amount of solvent used (25 mL) for each analysis. The validity of the method with respect to analysis was confirmed by comparing the UV spectra of each peak with those of reference compounds using a photodiode array detector.

Understanding and scaffolding Danish schoolteachers’ motivation for using classroom-based physical activity: study protocol for a mixed methods study

PubMed Central

Skovgaard, Thomas; Bredahl, Thomas

2018-01-01

Introduction The benefits of physical activity for children’s health, both mental and physical, and its positive effects on academic achievement are well established. Research also emphasises that schools could provide a natural setting for regular physical activity. There is, however, a limited amount of knowledge about teachers’ views when it comes to integrating physical activity as part of teaching. The aim of this study is to understand teachers’ motivation for integrating physical activity as part of teaching and to assess their need for guidance and support. Methods and analysis The study uses an explanatory sequential mixed-methods design. Schools from across Denmark are included in the sample. The design comprises two separated phases—a quantitative and qualitative phase. The quantitative phase is guided by the self-determination theory where teachers’ motivation will be measured using the Work Task Motivation Scale for Teachers. The theory of scaffolding guides the qualitative phase, which consists of in-depth interviews with participants selected from the quantitative phase based on levels of motivation and on demographic information. In accordance with the study aims, the analysis of data will identify teachers’ internal and external levels of motivation. The purpose of the qualitative phase is to enhance understanding of teachers’ motivation and of their need for support in the use of physical activity in teaching. Ethics and dissemination All relevant ethics approvals have been acquired. All participants in this study will provide written informed consent prior to data collection. All data emerging from the quantitative and qualitative phase will be anonymised for analysis. Ethics approval was requested from the Regional Committee on Health Research Ethics for Southern Denmark approval ID S-20162000–40 and the Danish Data Protection Agency approval ID 16/15491). The study was deemed not notifiable by both authorities. Trial registration number NCT02894346; Pre-results. PMID:29540419

National survey of availability of physical rehabilitation services in Iran: A mixed methods study

PubMed Central

Shirazikhah, Marzieh; Mirabzadeh, Arash; Sajadi, Homeira; Joghataei, Mohammad Taghi; Biglarian, Akbar; Mousavi, Tahmineh; Shahboulaghi, Farahnaz Mohammadi

2017-01-01

Background The prevalence of disability in Iran has increased due to ageing of the population and the presence of chronic diseases. However, little is known about the availability of rehabilitation services in Iran. Objective To study the availability of physical rehabilitation services in Iran. Methods This was a mixed method study. In the first phase, a qualitative design was conducted for designing an instrument with focus groups based on Service Availability and Readiness Assessment (SARA) instrument (developed by World Health Organization). Content analysis was used for data analysis. Then, in the second phase, a cross-sectional study was performed to collect the data with census method in Iran. This study was formed from June to October 2015, and samples consisted of all governmental, public non-governmental and private facilities established for rehabilitation centers affiliated with the Ministry of Health and Medical Education, Ministry of Labor, Cooperative and Social Welfare and the Iranian Red Crescent Society. Data analyses were performed using SPSS software (version 16). Descriptive statistical analysis (percentage and frequency) were calculated for quantitative data. Results In the first phase, the content analysis of qualitative data identified a Master Facilities List (MFL) of rehabilitation services and service providers in Iran. Results of the second phase showed that the rate of inpatient, outpatient, community-based and long-term care centers per 1,000,000 populations in Iran were 1.68, 89.24, 66.21 and 3.6, respectively. Also, that the rate of rehabilitation professionals including physical medicine and rehabilitation specialists, physiotherapists, occupational therapists, speech therapists, and audiologists were 3.90, 64.65, 22.09, 22.83 and 24.18 per 1,000,000 populations, respectively. Conclusion There is a need to increase the availability of rehabilitation services and to promote rehabilitation referrals by using an interdisciplinary team approach. PMID:29403619

A Hybrid Method for Endocardial Contour Extraction of Right Ventricle in 4-Slices from 3D Echocardiography Dataset.

PubMed

Dawood, Faten A; Rahmat, Rahmita W; Kadiman, Suhaini B; Abdullah, Lili N; Zamrin, Mohd D

2014-01-01

This paper presents a hybrid method to extract endocardial contour of the right ventricular (RV) in 4-slices from 3D echocardiography dataset. The overall framework comprises four processing phases. In Phase I, the region of interest (ROI) is identified by estimating the cavity boundary. Speckle noise reduction and contrast enhancement were implemented in Phase II as preprocessing tasks. In Phase III, the RV cavity region was segmented by generating intensity threshold which was used for once for all frames. Finally, Phase IV is proposed to extract the RV endocardial contour in a complete cardiac cycle using a combination of shape-based contour detection and improved radial search algorithm. The proposed method was applied to 16 datasets of 3D echocardiography encompassing the RV in long-axis view. The accuracy of experimental results obtained by the proposed method was evaluated qualitatively and quantitatively. It has been done by comparing the segmentation results of RV cavity based on endocardial contour extraction with the ground truth. The comparative analysis results show that the proposed method performs efficiently in all datasets with overall performance of 95% and the root mean square distances (RMSD) measure in terms of mean ± SD was found to be 2.21 ± 0.35 mm for RV endocardial contours.

An autonomous surface discontinuity detection and quantification method by digital image correlation and phase congruency

NASA Astrophysics Data System (ADS)

Cinar, A. F.; Barhli, S. M.; Hollis, D.; Flansbjer, M.; Tomlinson, R. A.; Marrow, T. J.; Mostafavi, M.

2017-09-01

Digital image correlation has been routinely used to measure full-field displacements in many areas of solid mechanics, including fracture mechanics. Accurate segmentation of the crack path is needed to study its interaction with the microstructure and stress fields, and studies of crack behaviour, such as the effect of closure or residual stress in fatigue, require data on its opening displacement. Such information can be obtained from any digital image correlation analysis of cracked components, but it collection by manual methods is quite onerous, particularly for massive amounts of data. We introduce the novel application of Phase Congruency to detect and quantify cracks and their opening. Unlike other crack detection techniques, Phase Congruency does not rely on adjustable threshold values that require user interaction, and so allows large datasets to be treated autonomously. The accuracy of the Phase Congruency based algorithm in detecting cracks is evaluated and compared with conventional methods such as Heaviside function fitting. As Phase Congruency is a displacement-based method, it does not suffer from the noise intensification to which gradient-based methods (e.g. strain thresholding) are susceptible. Its application is demonstrated to experimental data for cracks in quasi-brittle (Granitic rock) and ductile (Aluminium alloy) materials.

Modeling of Bulk Evaporation and Condensation

NASA Technical Reports Server (NTRS)

Anghaie, S.; Ding, Z.

1996-01-01

This report describes the modeling and mathematical formulation of the bulk evaporation and condensation involved in liquid-vapor phase change processes. An internal energy formulation, for these phase change processes that occur under the constraint of constant volume, was studied. Compared to the enthalpy formulation, the internal energy formulation has a more concise and compact form. The velocity and time scales of the interface movement were obtained through scaling analysis and verified by performing detailed numerical experiments. The convection effect induced by the density change was analyzed and found to be negligible compared to the conduction effect. Two iterative methods for updating the value of the vapor phase fraction, the energy based (E-based) and temperature based (T-based) methods, were investigated. Numerical experiments revealed that for the evaporation and condensation problems the E-based method is superior to the T-based method in terms of computational efficiency. The internal energy formulation and the E-based method were used to compute the bulk evaporation and condensation processes under different conditions. The evolution of the phase change processes was investigated. This work provided a basis for the modeling of thermal performance of multi-phase nuclear fuel elements under variable gravity conditions, in which the buoyancy convection due to gravity effects and internal heating are involved.

Application of Jacobian-free Newton–Krylov method in implicitly solving two-fluid six-equation two-phase flow problems: Implementation, validation and benchmark

DOE PAGES

Zou, Ling; Zhao, Haihua; Zhang, Hongbin

2016-03-09

This work represents a first-of-its-kind successful application to employ advanced numerical methods in solving realistic two-phase flow problems with two-fluid six-equation two-phase flow model. These advanced numerical methods include high-resolution spatial discretization scheme with staggered grids (high-order) fully implicit time integration schemes, and Jacobian-free Newton–Krylov (JFNK) method as the nonlinear solver. The computer code developed in this work has been extensively validated with existing experimental flow boiling data in vertical pipes and rod bundles, which cover wide ranges of experimental conditions, such as pressure, inlet mass flux, wall heat flux and exit void fraction. Additional code-to-code benchmark with the RELAP5-3Dmore » code further verifies the correct code implementation. The combined methods employed in this work exhibit strong robustness in solving two-phase flow problems even when phase appearance (boiling) and realistic discrete flow regimes are considered. Transitional flow regimes used in existing system analysis codes, normally introduced to overcome numerical difficulty, were completely removed in this work. As a result, this in turn provides the possibility to utilize more sophisticated flow regime maps in the future to further improve simulation accuracy.« less

Gait Analysis Using Wearable Sensors

PubMed Central

Tao, Weijun; Liu, Tao; Zheng, Rencheng; Feng, Hutian

2012-01-01

Gait analysis using wearable sensors is an inexpensive, convenient, and efficient manner of providing useful information for multiple health-related applications. As a clinical tool applied in the rehabilitation and diagnosis of medical conditions and sport activities, gait analysis using wearable sensors shows great prospects. The current paper reviews available wearable sensors and ambulatory gait analysis methods based on the various wearable sensors. After an introduction of the gait phases, the principles and features of wearable sensors used in gait analysis are provided. The gait analysis methods based on wearable sensors is divided into gait kinematics, gait kinetics, and electromyography. Studies on the current methods are reviewed, and applications in sports, rehabilitation, and clinical diagnosis are summarized separately. With the development of sensor technology and the analysis method, gait analysis using wearable sensors is expected to play an increasingly important role in clinical applications. PMID:22438763

Development of the IBSAL-SimMOpt Method for the Optimization of Quality in a Corn Stover Supply Chain

DOE PAGES

Chavez, Hernan; Castillo-Villar, Krystel; Webb, Erin

2017-08-01

Variability on the physical characteristics of feedstock has a relevant effect on the reactor’s reliability and operating cost. Most of the models developed to optimize biomass supply chains have failed to quantify the effect of biomass quality and preprocessing operations required to meet biomass specifications on overall cost and performance. The Integrated Biomass Supply Analysis and Logistics (IBSAL) model estimates the harvesting, collection, transportation, and storage cost while considering the stochastic behavior of the field-to-biorefinery supply chain. This paper proposes an IBSAL-SimMOpt (Simulation-based Multi-Objective Optimization) method for optimizing the biomass quality and costs associated with the efforts needed to meetmore » conversion technology specifications. The method is developed in two phases. For the first phase, a SimMOpt tool that interacts with the extended IBSAL is developed. For the second phase, the baseline IBSAL model is extended so that the cost for meeting and/or penalization for failing in meeting specifications are considered. The IBSAL-SimMOpt method is designed to optimize quality characteristics of biomass, cost related to activities intended to improve the quality of feedstock, and the penalization cost. A case study based on 1916 farms in Ontario, Canada is considered for testing the proposed method. Analysis of the results demonstrates that this method is able to find a high-quality set of non-dominated solutions.« less

Development and Optimisation of an HPLC-DAD-ESI-Q-ToF Method for the Determination of Phenolic Acids and Derivatives

PubMed Central

Restivo, Annalaura; Degano, Ilaria; Ribechini, Erika; Colombini, Maria Perla

2014-01-01

A method for the HPLC-MS/MS analysis of phenols, including phenolic acids and naphtoquinones, using an amide-embedded phase column was developed and compared to the literature methods based on classical C18 stationary phase columns. RP-Amide is a recently developed polar embedded stationary phase, whose wetting properties mean that up to 100% water can be used as an eluent. The increased retention and selectivity for polar compounds and the possibility of working in 100% water conditions make this column particularly interesting for the HPLC analysis of phenolic acids and derivatives. In this study, the chromatographic separation was optimised on an HPLC-DAD, and was used to separate 13 standard phenolic acids and derivatives. The method was validated on an HPLC-ESI-Q-ToF. The acquisition was performed in negative polarity and MS/MS target mode. Ionisation conditions and acquisition parameters for the Q-ToF detector were investigated by working on collision energies and fragmentor potentials. The performance of the method was fully evaluated on standards. Moreover, several raw materials containing phenols were analysed: walnut, gall, wine, malbec grape, French oak, red henna and propolis. Our method allowed us to characterize the phenolic composition in a wide range of matrices and to highlight possible matrix effects. PMID:24551158

Development of the IBSAL-SimMOpt Method for the Optimization of Quality in a Corn Stover Supply Chain

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chavez, Hernan; Castillo-Villar, Krystel; Webb, Erin

Variability on the physical characteristics of feedstock has a relevant effect on the reactor’s reliability and operating cost. Most of the models developed to optimize biomass supply chains have failed to quantify the effect of biomass quality and preprocessing operations required to meet biomass specifications on overall cost and performance. The Integrated Biomass Supply Analysis and Logistics (IBSAL) model estimates the harvesting, collection, transportation, and storage cost while considering the stochastic behavior of the field-to-biorefinery supply chain. This paper proposes an IBSAL-SimMOpt (Simulation-based Multi-Objective Optimization) method for optimizing the biomass quality and costs associated with the efforts needed to meetmore » conversion technology specifications. The method is developed in two phases. For the first phase, a SimMOpt tool that interacts with the extended IBSAL is developed. For the second phase, the baseline IBSAL model is extended so that the cost for meeting and/or penalization for failing in meeting specifications are considered. The IBSAL-SimMOpt method is designed to optimize quality characteristics of biomass, cost related to activities intended to improve the quality of feedstock, and the penalization cost. A case study based on 1916 farms in Ontario, Canada is considered for testing the proposed method. Analysis of the results demonstrates that this method is able to find a high-quality set of non-dominated solutions.« less

Separation and quantitation of three acidic herbicide residues in tobacco and soil by dispersive solid-phase extraction and UPLC-MS/MS.

PubMed

Xiong, Wei; Tao, Xiaoqiu; Pang, Su; Yang, Xue; Tang, GangLing; Bian, Zhaoyang

2014-01-01

A method for the determination of three acidic herbicides, dicamba, 2,4-dichlorophenoxyacetic acid (2,4-D) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) in tobacco and soil has been developed based on the use of liquid-liquid extraction and dispersive solid-phase extraction (dispersive-SPE) followed by UPLC-MS/MS. Two percentage of (v/v) formic acid in acetonitrile as the extraction helped partitioning of analytes into the acetonitrile phase. The extract was then cleaned up by dispersive-SPE using primary secondary amine as selective sorbents. Quantitative analysis was done in the multiple-reaction monitoring mode using stable isotope-labeled internal standards for each compound. A separate internal standard for each analyte is required to minimize sample matrix effects on each analyte, which can lead to poor analyte recoveries and decreases in method accuracy and precision. The total analysis time was <4 min. The linear range of the method was from 1 to 100 ng mL(-1) with a limit of detection of each herbicide varied from 0.012 to 0.126 ng g(-1). The proposed method is faster, more sensitive and selective than the traditional methods and more accurate and robust than the published LC-MS/MS methods. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

In-line phase contrast micro-CT reconstruction for biomedical specimens.

PubMed

Fu, Jian; Tan, Renbo

2014-01-01

X-ray phase contrast micro computed tomography (micro-CT) can non-destructively provide the internal structure information of soft tissues and low atomic number materials. It has become an invaluable analysis tool for biomedical specimens. Here an in-line phase contrast micro-CT reconstruction technique is reported, which consists of a projection extraction method and the conventional filter back-projection (FBP) reconstruction algorithm. The projection extraction is implemented by applying the Fourier transform to the forward projections of in-line phase contrast micro-CT. This work comprises a numerical study of the method and its experimental verification using a biomedical specimen dataset measured at an X-ray tube source micro-CT setup. The numerical and experimental results demonstrate that the presented technique can improve the imaging contrast of biomedical specimens. It will be of interest for a wide range of in-line phase contrast micro-CT applications in medicine and biology.

Implicitly solving phase appearance and disappearance problems using two-fluid six-equation model

DOE PAGES

Zou, Ling; Zhao, Haihua; Zhang, Hongbin

2016-01-25

Phase appearance and disappearance issue presents serious numerical challenges in two-phase flow simulations using the two-fluid six-equation model. Numerical challenges arise from the singular equation system when one phase is absent, as well as from the discontinuity in the solution space when one phase appears or disappears. In this work, a high-resolution spatial discretization scheme on staggered grids and fully implicit methods were applied for the simulation of two-phase flow problems using the two-fluid six-equation model. A Jacobian-free Newton-Krylov (JFNK) method was used to solve the discretized nonlinear problem. An improved numerical treatment was proposed and proved to be effectivemore » to handle the numerical challenges. The treatment scheme is conceptually simple, easy to implement, and does not require explicit truncations on solutions, which is essential to conserve mass and energy. Various types of phase appearance and disappearance problems relevant to thermal-hydraulics analysis have been investigated, including a sedimentation problem, an oscillating manometer problem, a non-condensable gas injection problem, a single-phase flow with heat addition problem and a subcooled flow boiling problem. Successful simulations of these problems demonstrate the capability and robustness of the proposed numerical methods and numerical treatments. As a result, volume fraction of the absent phase can be calculated effectively as zero.« less

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

PubMed

Ye, Diru; Wu, Susu; Xu, Jianqiao; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

2016-02-01

Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Simplified method to solve sound transmission through structures lined with elastic porous material.

PubMed

Lee, J H; Kim, J

2001-11-01

An approximate analysis method is developed to calculate sound transmission through structures lined with porous material. Because the porous material has both the solid phase and fluid phase, three wave components exist in the material, which makes the related analysis very complicated. The main idea in developing the approximate method is very simple: modeling the porous material using only the strongest of the three waves, which in effect idealizes the material as an equivalent fluid. The analysis procedure has to be conducted in two steps. In the first step, sound transmission through a flat double panel with a porous liner of infinite extents, which has the same cross sectional construction as the actual structure, is solved based on the full theory and the strongest wave component is identified. In the second step sound transmission through the actual structure is solved modeling the porous material as an equivalent fluid while using the actual geometry of the structure. The development and validation of the method are discussed in detail. As an application example, the transmission loss through double walled cylindrical shells with a porous core is calculated utilizing the simplified method.

Critical Thinking and the Use of Nontraditional Instructional Methodologies.

PubMed

Orique, Sabrina B; McCarthy, Mary Ann

2015-08-01

The purpose of this study was to examine the relationship between critical thinking and the use of concept mapping (CM) and problem-based learning (PBL) during care plan development. A quasi-experimental study with a pretest-posttest design was conducted using a convenience sample (n = 49) of first-semester undergraduate baccalaureate nursing students. Critical thinking was measured using the Holistic Critical Thinking Scoring Rubric. Data analysis consisted of a repeated measures analysis of variance with post hoc mean comparison tests using the Bonferroni method. Findings indicated that mean critical thinking at phase 4 (CM and PBL) was significantly higher, compared with phase 1 (baseline), phase 2 (PBL), and phase 3 (CM [p < 0.001]). The results support the utilization of nontraditional instructional (CM and PBL) methodologies in undergraduate nursing curricula. Copyright 2015, SLACK Incorporated.

A complex systems analysis of stick-slip dynamics of a laboratory fault

DOE Office of Scientific and Technical Information (OSTI.GOV)

Walker, David M.; Tordesillas, Antoinette, E-mail: atordesi@unimelb.edu.au; Small, Michael

2014-03-15

We study the stick-slip behavior of a granular bed of photoelastic disks sheared by a rough slider pulled along the surface. Time series of a proxy for granular friction are examined using complex systems methods to characterize the observed stick-slip dynamics of this laboratory fault. Nonlinear surrogate time series methods show that the stick-slip behavior appears more complex than a periodic dynamics description. Phase space embedding methods show that the dynamics can be locally captured within a four to six dimensional subspace. These slider time series also provide an experimental test for recent complex network methods. Phase space networks, constructedmore » by connecting nearby phase space points, proved useful in capturing the key features of the dynamics. In particular, network communities could be associated to slip events and the ranking of small network subgraphs exhibited a heretofore unreported ordering.« less

Spread spectrum phase modulation for coherent X-ray diffraction imaging.

PubMed

Zhang, Xuesong; Jiang, Jing; Xiangli, Bin; Arce, Gonzalo R

2015-09-21

High dynamic range, phase ambiguity and radiation limited resolution are three challenging issues in coherent X-ray diffraction imaging (CXDI), which limit the achievable imaging resolution. This paper proposes a spread spectrum phase modulation (SSPM) method to address the aforementioned problems in a single strobe. The requirements on phase modulator parameters are presented, and a practical implementation of SSPM is discussed via ray optics analysis. Numerical experiments demonstrate the performance of SSPM under the constraint of available X-ray optics fabrication accuracy, showing its potential to real CXDI applications.

Network structure of multivariate time series.

PubMed

Lacasa, Lucas; Nicosia, Vincenzo; Latora, Vito

2015-10-21

Our understanding of a variety of phenomena in physics, biology and economics crucially depends on the analysis of multivariate time series. While a wide range tools and techniques for time series analysis already exist, the increasing availability of massive data structures calls for new approaches for multidimensional signal processing. We present here a non-parametric method to analyse multivariate time series, based on the mapping of a multidimensional time series into a multilayer network, which allows to extract information on a high dimensional dynamical system through the analysis of the structure of the associated multiplex network. The method is simple to implement, general, scalable, does not require ad hoc phase space partitioning, and is thus suitable for the analysis of large, heterogeneous and non-stationary time series. We show that simple structural descriptors of the associated multiplex networks allow to extract and quantify nontrivial properties of coupled chaotic maps, including the transition between different dynamical phases and the onset of various types of synchronization. As a concrete example we then study financial time series, showing that a multiplex network analysis can efficiently discriminate crises from periods of financial stability, where standard methods based on time-series symbolization often fail.

A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium.

PubMed

Nakao, Ryuji; Halldin, Christer

2013-07-01

A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for (11)C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma. Copyright © 2013 Elsevier Inc. All rights reserved.

Analysis of catecholamines in urine by unique LC/MS suitable ion-pairing chromatography.

PubMed

Bergmann, Marianne L; Sadjadi, Seyed; Schmedes, Anne

2017-07-01

The catecholamines, epinephrine (E) and norepinephrine (NE) are small polar, hydrophilic molecules, posing significant challenges to liquid chromatography - tandem mass spectrometry (LC-MS/MS) method development. Specifically, these compounds show little retention on conventional reversed-phase liquid chromatography columns. This work presents development and validation of an LC-MS/MS method for determining catecholamines in urine, based on a new approach to ion-pairing chromatography (IPC), in which the ion-pairing reagent (IPR), 1-Heptane Sulfonic Acid (HSA), is added to the extracted samples instead of the mobile phases. A Hamilton STARlet workstation carried out the solid phase extraction of urine samples. The extracted samples were diluted with 60mmol/L HSA and injected on a Kinetex core-shell biphenyl column with conventional LC-MS/MS suitable mobile phases. Chromatographic separation of E and NE was achieved successfully with very stable retention times (RT). In 484 injections, the RTs were steady with a CV of less than ±4%. Furthermore, HSA was separated from E and NE, allowing HSA to be diverted to waste instead of entering the mass spectrometer ion chamber. The method was validated with good analytical performance, and even though the analysis for urinary catecholamines is increasingly being replaced by plasma free metanephrines in diagnosing pheochromocytomas, this work represents the application of a new analytical technique that can be transferred to other small polar molecules, that are difficult to chromatograph on traditional reversed phase columns. Copyright © 2017 Elsevier B.V. All rights reserved.

METHOD DEVELOPMENT FOR THE ANALYSIS OF N-NITROSODIMETHYLAMINE AND OTHER N-NITROSAMINES IN DRINKING WATER AT LOW NANOGRAM/LITER CONCENTRATIONS USING SOLID PHASE EXTRACTION AND GAS CHROMATOGRAPHY WITH CHEMICAL IONIZATION TANDEM MASS SPECTROMETRY

EPA Science Inventory

N-Nitrosodimethylamine (NDMA) is a probable human carcinogen that has been identified as a drinking water contaminant of concern. United States Environmental Protection Agency (USEPA) Method 521 has been developed for the analysis of NDMA and six additional N-nitrosamines in dri...

Microscopic optical path length difference and polarization measurement system for cell analysis

NASA Astrophysics Data System (ADS)

Satake, H.; Ikeda, K.; Kowa, H.; Hoshiba, T.; Watanabe, E.

2018-03-01

In recent years, noninvasive, nonstaining, and nondestructive quantitative cell measurement techniques have become increasingly important in the medical field. These cell measurement techniques enable the quantitative analysis of living cells, and are therefore applied to various cell identification processes, such as those determining the passage number limit during cell culturing in regenerative medicine. To enable cell measurement, we developed a quantitative microscopic phase imaging system based on a Mach-Zehnder interferometer that measures the optical path length difference distribution without phase unwrapping using optical phase locking. The applicability of our phase imaging system was demonstrated by successful identification of breast cancer cells amongst normal cells. However, the cell identification method using this phase imaging system exhibited a false identification rate of approximately 7%. In this study, we implemented a polarimetric imaging system by introducing a polarimetric module to one arm of the Mach-Zehnder interferometer of our conventional phase imaging system. This module was comprised of a quarter wave plate and a rotational polarizer on the illumination side of the sample, and a linear polarizer on the optical detector side. In addition, we developed correction methods for the measurement errors of the optical path length and birefringence phase differences that arose through the influence of elements other than cells, such as the Petri dish. As the Petri dish holding the fluid specimens was transparent, it did not affect the amplitude information; however, the optical path length and birefringence phase differences were affected. Therefore, we proposed correction of the optical path length and birefringence phase for the influence of elements other than cells, as a prerequisite for obtaining highly precise phase and polarimetric images.

Fifty years of solid-phase extraction in water analysis--historical development and overview.

PubMed

Liska, I

2000-07-14

The use of an appropriate sample handling technique is a must in an analysis of organic micropollutants in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior to their detection have a long history. Since the first experimental trials using activated carbon filters that were performed 50 years ago, solid-phase extraction (SPE) has become an established sample preparation technique. The initial experimental applications of SPE resulted in widespread use of this technique in current water analysis and also to adoption of SPE into standardized analytical methods. During the decades of its evolution, chromatographers became aware of the advantages of SPE and, despite many innovations that appeared in the last decade, new SPE developments are still expected in the future. A brief overview of 50 years of the history of the use of SPE in organic trace analysis of water is given in presented paper.

A novel approach to detect respiratory phases from pulmonary acoustic signals using normalised power spectral density and fuzzy inference system.

PubMed

Palaniappan, Rajkumar; Sundaraj, Kenneth; Sundaraj, Sebastian; Huliraj, N; Revadi, S S

2016-07-01

Monitoring respiration is important in several medical applications. One such application is respiratory rate monitoring in patients with sleep apnoea. The respiratory rate in patients with sleep apnoea disorder is irregular compared with the controls. Respiratory phase detection is required for a proper monitoring of respiration in patients with sleep apnoea. To develop a model to detect the respiratory phases present in the pulmonary acoustic signals and to evaluate the performance of the model in detecting the respiratory phases. Normalised averaged power spectral density for each frame and change in normalised averaged power spectral density between the adjacent frames were fuzzified and fuzzy rules were formulated. The fuzzy inference system (FIS) was developed with both Mamdani and Sugeno methods. To evaluate the performance of both Mamdani and Sugeno methods, correlation coefficient and root mean square error (RMSE) were calculated. In the correlation coefficient analysis in evaluating the fuzzy model using Mamdani and Sugeno method, the strength of the correlation was found to be r = 0.9892 and r = 0.9964, respectively. The RMSE for Mamdani and Sugeno methods are RMSE = 0.0853 and RMSE = 0.0817, respectively. The correlation coefficient and the RMSE of the proposed fuzzy models in detecting the respiratory phases reveals that Sugeno method performs better compared with the Mamdani method. © 2014 John Wiley & Sons Ltd.

Application of a Short Intracellular pH Method to Flow Cytometry for Determining Saccharomyces cerevisiae Vitality ▿

PubMed Central

Weigert, Claudia; Steffler, Fabian; Kurz, Tomas; Shellhammer, Thomas H.; Methner, Frank-Jürgen

2009-01-01

The measurement of yeast's intracellular pH (ICP) is a proven method for determining yeast vitality. Vitality describes the condition or health of viable cells as opposed to viability, which defines living versus dead cells. In contrast to fluorescence photometric measurements, which show only average ICP values of a population, flow cytometry allows the presentation of an ICP distribution. By examining six repeated propagations with three separate growth phases (lag, exponential, and stationary), the ICP method previously established for photometry was transferred successfully to flow cytometry by using the pH-dependent fluorescent probe 5,6-carboxyfluorescein. The correlation between the two methods was good (r2 = 0.898, n = 18). With both methods it is possible to track the course of growth phases. Although photometry did not yield significant differences between exponentially and stationary phases (P = 0.433), ICP via flow cytometry did (P = 0.012). Yeast in an exponential phase has a unimodal ICP distribution, reflective of a homogeneous population; however, yeast in a stationary phase displays a broader ICP distribution, and subpopulations could be defined by using the flow cytometry method. In conclusion, flow cytometry yielded specific evidence of the heterogeneity in vitality of a yeast population as measured via ICP. In contrast to photometry, flow cytometry increases information about the yeast population's vitality via a short measurement, which is suitable for routine analysis. PMID:19581482

Regio-Selective Intramolecular Hydrogen/Deuterium Exchange in Gas-Phase Electron Transfer Dissociation

NASA Astrophysics Data System (ADS)

Hamuro, Yoshitomo

2017-05-01

Protein backbone amide hydrogen/deuterium exchange mass spectrometry (HDX-MS) typically utilizes enzymatic digestion after the exchange reaction and before MS analysis to improve data resolution. Gas-phase fragmentation of a peptic fragment prior to MS analysis is a promising technique to further increase the resolution. The biggest technical challenge for this method is elimination of intramolecular hydrogen/deuterium exchange (scrambling) in the gas phase. The scrambling obscures the location of deuterium. Jørgensen's group pioneered a method to minimize the scrambling in gas-phase electron capture/transfer dissociation. Despite active investigation, the mechanism of hydrogen scrambling is not well-understood. The difficulty stems from the fact that the degree of hydrogen scrambling depends on instruments, various parameters of mass analysis, and peptide analyzed. In most hydrogen scrambling investigations, the hydrogen scrambling is measured by the percentage of scrambling in a whole molecule. This paper demonstrates that the degree of intramolecular hydrogen/deuterium exchange depends on the nature of exchangeable hydrogen sites. The deuterium on Tyr amide of neurotensin (9-13), Arg-Pro-Tyr-Ile-Leu, migrated significantly faster than that on Ile or Leu amides, indicating the loss of deuterium from the original sites is not mere randomization of hydrogen and deuterium but more site-specific phenomena. This more precise approach may help understand the mechanism of intramolecular hydrogen exchange and provide higher confidence for the parameter optimization to eliminate intramolecular hydrogen/deuterium exchange during gas-phase fragmentation.

Regio-Selective Intramolecular Hydrogen/Deuterium Exchange in Gas-Phase Electron Transfer Dissociation.

PubMed

Hamuro, Yoshitomo

2017-05-01

Protein backbone amide hydrogen/deuterium exchange mass spectrometry (HDX-MS) typically utilizes enzymatic digestion after the exchange reaction and before MS analysis to improve data resolution. Gas-phase fragmentation of a peptic fragment prior to MS analysis is a promising technique to further increase the resolution. The biggest technical challenge for this method is elimination of intramolecular hydrogen/deuterium exchange (scrambling) in the gas phase. The scrambling obscures the location of deuterium. Jørgensen's group pioneered a method to minimize the scrambling in gas-phase electron capture/transfer dissociation. Despite active investigation, the mechanism of hydrogen scrambling is not well-understood. The difficulty stems from the fact that the degree of hydrogen scrambling depends on instruments, various parameters of mass analysis, and peptide analyzed. In most hydrogen scrambling investigations, the hydrogen scrambling is measured by the percentage of scrambling in a whole molecule. This paper demonstrates that the degree of intramolecular hydrogen/deuterium exchange depends on the nature of exchangeable hydrogen sites. The deuterium on Tyr amide of neurotensin (9-13), Arg-Pro-Tyr-Ile-Leu, migrated significantly faster than that on Ile or Leu amides, indicating the loss of deuterium from the original sites is not mere randomization of hydrogen and deuterium but more site-specific phenomena. This more precise approach may help understand the mechanism of intramolecular hydrogen exchange and provide higher confidence for the parameter optimization to eliminate intramolecular hydrogen/deuterium exchange during gas-phase fragmentation. Graphical Abstract ᅟ.

An Examination of the Phase Transition Thermodynamics of (S)- and (RS)-Naproxen as a Basis for the Design of Enantioselective Crystallization Processes.

PubMed

Buchholz, Hannes; Emel'yanenko, Vladimir N; Lorenz, Heike; Verevkin, Sergey P

2016-05-01

A detailed experimental analysis of the phase transition thermodynamics of (S)-naproxen and (RS)-naproxen is reported. Vapor pressures were determined experimentally via the transpiration method. Sublimation enthalpies were obtained from the vapor pressures and from independent TGA measurements. Thermodynamics of fusion which have been well-studied in the literature were systematically remeasured by DSC. Both sublimation and fusion enthalpies were adjusted to one reference temperature, T = 298 K, using measured heat capacities of the solid and the melt phase by DSC. Average values from the measurements and from literature data were suggested for the sublimation and fusion enthalpies. In order to prove consistency of the proposed values the vaporization enthalpies obtained by combination of both were compared to vaporization enthalpies obtained by the group-additivity method and the correlation-gas chromatography method. The importance of reliable and precise phase transition data for thermochemical calculations such as the prediction of solid/liquid phase behaviour of chiral compounds is highlighted. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

A pilot study of river flow prediction in urban area based on phase space reconstruction

NASA Astrophysics Data System (ADS)

Adenan, Nur Hamiza; Hamid, Nor Zila Abd; Mohamed, Zulkifley; Noorani, Mohd Salmi Md

2017-08-01

River flow prediction is significantly related to urban hydrology impact which can provide information to solve any problems such as flood in urban area. The daily river flow of Klang River, Malaysia was chosen to be forecasted in this pilot study which based on phase space reconstruction. The reconstruction of phase space involves a single variable of river flow data to m-dimensional phase space in which the dimension (m) is based on the optimal values of Cao method. The results from the reconstruction of phase space have been used in the forecasting process using local linear approximation method. From our investigation, river flow at Klang River is chaotic based on the analysis from Cao method. The overall results provide good value of correlation coefficient. The value of correlation coefficient is acceptable since the area of the case study is influence by a lot of factors. Therefore, this pilot study may be proposed to forecast daily river flow data with the purpose of providing information about the flow of the river system in urban area.

Microscale reconstruction of biogeochemical substrates using multimode X-ray tomography and scanning electron microscopy

NASA Astrophysics Data System (ADS)

Miller, M.; Miller, E.; Liu, J.; Lund, R. M.; McKinley, J. P.

2012-12-01

X-ray computed tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, CT images will be collected using both x-ray absorption and differential phase contrast modes. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume) as well as the images' mutual information. Elemental and solid-phase distributions on the exposed surfaces, co-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from the CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray differential phase contrast tomography, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine CT images are resolved at 10-20 μm, while SEM images are resolved at 10-20 nm; grayscale values vary according to collection time and instrument sensitivity; and compositional sensitivities via EMP vary in interrogation volume and scale. We have so far successfully registered SEM imagery within a multimode tomographic volume and have used standard methods to isolate pore space within the volume. We are developing a three-dimensional solid-phase identification and registration method that is constrained by bulk-sample X-ray diffraction Rietveld refinements. The results of this project will prove useful in fields that require the fine-scale definition of solid-phase distributions and relationships, and could replace more inefficient methods for making these estimations.

Development and Validation of HPLC-DAD and UHPLC-DAD Methods for the Simultaneous Determination of Guanylhydrazone Derivatives Employing a Factorial Design.

PubMed

Azevedo de Brito, Wanessa; Gomes Dantas, Monique; Andrade Nogueira, Fernando Henrique; Ferreira da Silva-Júnior, Edeildo; Xavier de Araújo-Júnior, João; Aquino, Thiago Mendonça de; Adélia Nogueira Ribeiro, Êurica; da Silva Solon, Lilian Grace; Soares Aragão, Cícero Flávio; Barreto Gomes, Ana Paula

2017-08-30

Guanylhydrazones are molecules with great pharmacological potential in various therapeutic areas, including antitumoral activity. Factorial design is an excellent tool in the optimization of a chromatographic method, because it is possible quickly change factors such as temperature, mobile phase composition, mobile phase pH, column length, among others to establish the optimal conditions of analysis. The aim of the present work was to develop and validate a HPLC and UHPLC methods for the simultaneous determination of guanylhydrazones with anticancer activity employing experimental design. Precise, exact, linear and robust HPLC and UHPLC methods were developed and validated for the simultaneous quantification of the guanylhydrazones LQM10, LQM14, and LQM17. The UHPLC method was more economic, with a four times less solvent consumption, and 20 times less injection volume, what allowed better column performance. Comparing the empirical approach employed in the HPLC method development to the DoE approach employed in the UHPLC method development, we can conclude that the factorial design made the method development faster, more practical and rational. This resulted in methods that can be employed in the analysis, evaluation and quality control of these new synthetic guanylhydrazones.

Improved quality-by-design compliant methodology for method development in reversed-phase liquid chromatography.

PubMed

Debrus, Benjamin; Guillarme, Davy; Rudaz, Serge

2013-10-01

A complete strategy dedicated to quality-by-design (QbD) compliant method development using design of experiments (DOE), multiple linear regressions responses modelling and Monte Carlo simulations for error propagation was evaluated for liquid chromatography (LC). The proposed approach includes four main steps: (i) the initial screening of column chemistry, mobile phase pH and organic modifier, (ii) the selectivity optimization through changes in gradient time and mobile phase temperature, (iii) the adaptation of column geometry to reach sufficient resolution, and (iv) the robust resolution optimization and identification of the method design space. This procedure was employed to obtain a complex chromatographic separation of 15 antipsychotic basic drugs, widely prescribed. To fully automate and expedite the QbD method development procedure, short columns packed with sub-2 μm particles were employed, together with a UHPLC system possessing columns and solvents selection valves. Through this example, the possibilities of the proposed QbD method development workflow were exposed and the different steps of the automated strategy were critically discussed. A baseline separation of the mixture of antipsychotic drugs was achieved with an analysis time of less than 15 min and the robustness of the method was demonstrated simultaneously with the method development phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Massively parallel haplotyping on microscopic beads for the high-throughput phase analysis of single molecules.

PubMed

Boulanger, Jérôme; Muresan, Leila; Tiemann-Boege, Irene

2012-01-01

In spite of the many advances in haplotyping methods, it is still very difficult to characterize rare haplotypes in tissues and different environmental samples or to accurately assess the haplotype diversity in large mixtures. This would require a haplotyping method capable of analyzing the phase of single molecules with an unprecedented throughput. Here we describe such a haplotyping method capable of analyzing in parallel hundreds of thousands single molecules in one experiment. In this method, multiple PCR reactions amplify different polymorphic regions of a single DNA molecule on a magnetic bead compartmentalized in an emulsion drop. The allelic states of the amplified polymorphisms are identified with fluorescently labeled probes that are then decoded from images taken of the arrayed beads by a microscope. This method can evaluate the phase of up to 3 polymorphisms separated by up to 5 kilobases in hundreds of thousands single molecules. We tested the sensitivity of the method by measuring the number of mutant haplotypes synthesized by four different commercially available enzymes: Phusion, Platinum Taq, Titanium Taq, and Phire. The digital nature of the method makes it highly sensitive to detecting haplotype ratios of less than 1:10,000. We also accurately quantified chimera formation during the exponential phase of PCR by different DNA polymerases.

SU-G-BRA-07: An Innovative Fiducial-Less Tracking Method for Radiation Treatment of Abdominal Tumors by Diaphragm Disparity Analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dick, D; Zhao, W; Wu, X

2016-06-15

Purpose: To investigate the feasibility of tracking abdominal tumors without the use of gold fiducial markers Methods: In this simulation study, an abdominal 4DCT dataset, acquired previously and containing 8 phases of the breathing cycle, was used as the testing data. Two sets of DRR images (45 and 135 degrees) were generated for each phase. Three anatomical points along the lung-diaphragm interface on each of the Digital Reconstructed Radiograph(DRR) images were identified by cross-correlation. The gallbladder, which simulates the tumor, was contoured for each phase of the breathing cycle and the corresponding centroid values serve as the measured center ofmore » the tumor. A linear model was created to correlate the diaphragm’s disparity of the three identified anatomical points with the center of the tumor. To verify the established linear model, we sequentially removed one phase of the data (i.e., 3 anatomical points and the corresponding tumor center) and created new linear models with the remaining 7 phases. Then we substituted the eliminated phase data (disparities of the 3 anatomical points) into the corresponding model to compare model-generated tumor center and the measured tumor center. Results: The maximum difference between the modeled and the measured centroid values across the 8 phases were 0.72, 0.29 and 0.30 pixels in the x, y and z directions respectively, which yielded a maximum mean-squared-error value of 0.75 pixels. The outcomes of the verification process, by eliminating each phase, produced mean-squared-errors ranging from 0.41 to 1.28 pixels. Conclusion: Gold fiducial markers, requiring surgical procedures to be implanted, are conventionally used in radiation therapy. The present work shows the feasibility of a fiducial-less tracking method for localizing abdominal tumors. Through developed diaphragm disparity analysis, the established linear model was verified with clinically accepted errors. The tracking method in real time under different radiation therapy platforms will be further investigated.« less

Observing Tin-Lead Alloys by Scanning Electron Microscopy: A Physical Chemistry Experiment Investigating Macro-Level Behaviors and Micro-Level Structures

ERIC Educational Resources Information Center

Wang, Yue; Xu, Xinhua; Wu, Meifen; Hu, Huikang; Wang, Xiaogang

2015-01-01

Scanning electron microscopy (SEM) was introduced into undergraduate physical chemistry laboratory curriculum to help students observe the phase composition and morphology characteristics of tin-lead alloys and thus further their understanding of binary alloy phase diagrams. The students were captivated by this visual analysis method, which…

Separation and structural analysis of saponins in a bark extract from Quillaja saponaria Molina.

PubMed

Nord, L I; Kenne, L

1999-07-20

Six major saponins were isolated from a bark extract from Quillaja saponaria Molina. Solid-phase extraction, followed by a two-step reversed-phase HPLC separation procedure with phosphate and ammonium acetate buffers of different pH values, was used. The compounds were characterised using NMR spectroscopy, mass spectrometry and chemical methods.

Dynamical Analysis in the Mathematical Modelling of Human Blood Glucose

ERIC Educational Resources Information Center

Bae, Saebyok; Kang, Byungmin

2012-01-01

We want to apply the geometrical method to a dynamical system of human blood glucose. Due to the educational importance of model building, we show a relatively general modelling process using observational facts. Next, two models of some concrete forms are analysed in the phase plane by means of linear stability, phase portrait and vector…

Patterns of Teacher's Instructional Moves: What Makes Mathematical Instructional Practices Unique?

ERIC Educational Resources Information Center

Pinter, Holly Henderson

2013-01-01

The purpose of this study was to examine patterns in fourth-grade teachers' use of instructional moves in the implementation of standards-based mathematical teaching practices. Using a mixed methods sequential explanatory design, the study consisted of two phases: quantitative selection and qualitative analysis. The first phase of the study…

Testing sequential extraction methods for the analysis of multiple stable isotope systems from a bone sample

NASA Astrophysics Data System (ADS)

Sahlstedt, Elina; Arppe, Laura

2017-04-01

Stable isotope composition of bones, analysed either from the mineral phase (hydroxyapatite) or from the organic phase (mainly collagen) carry important climatological and ecological information and are therefore widely used in paleontological and archaeological research. For the analysis of the stable isotope compositions, both of the phases, hydroxyapatite and collagen, have their more or less well established separation and analytical techniques. Recent development in IRMS and wet chemical extraction methods have facilitated the analysis of very small bone fractions (500 μg or less starting material) for PO43-O isotope composition. However, the uniqueness and (pre-) historical value of each archaeological and paleontological finding lead to preciously little material available for stable isotope analyses, encouraging further development of microanalytical methods for the use of stable isotope analyses. Here we present the first results in developing extraction methods for combining collagen C- and N-isotope analyses to PO43-O-isotope analyses from a single bone sample fraction. We tested sequential extraction starting with dilute acid demineralization and collection of both collagen and PO43-fractions, followed by further purification step by H2O2 (PO43-fraction). First results show that bone sample separates as small as 2 mg may be analysed for their δ15N, δ13C and δ18OPO4 values. The method may be incorporated in detailed investigation of sequentially developing skeletal material such as teeth, potentially allowing for the investigation of interannual variability in climatological/environmental signals or investigation of the early life history of an individual.

Development and validation of LC methods for the separation of misoprostol related substances and diastereoisomers.

PubMed

Kahsay, Getu; Song, Huiying; Eerdekens, Fran; Tie, Yaxin; Hendriks, Danny; Van Schepdael, Ann; Cabooter, Deirdre; Adams, Erwin

2015-01-01

Misoprostol is a synthetic prostaglandin E1 analogue which is mainly used for prevention and treatment of gastric ulcers, but also for abortion due to its labour inducing effect. Misoprostol exists as a mixture of diastereoisomers (1:1) and has several related impurities owing to its instability at higher temperatures and moisture. A simple and robust reversed phase liquid chromatographic (RPLC) method is described for the separation of the related substances and a normal phase (NP) LC method for the separation of misoprostol diastereoisomers. The RPLC method was performed using an Ascentis Express C18 (150 mm × 4.6 mm, 5 μm) column kept at 35 °C. The mobile phase was a gradient mixture of mobile phase A (ACN-H2O-MeOH, 28:69:3 v/v/v) and mobile phase B (ACN-H2O-MeOH, 47:50:3 v/v/v) eluted at a flow rate of 1.5 mL/min. UV detection was performed at 200 nm. The NPLC method was undertaken by using an XBridge bare silica (150 mm × 2.1 mm, 3.5 μm) column at 35 °C. The mobile phase contained 1-propanol-heptane-TFA (4:96:0.1%, v/v/v), pumped at a flow rate of 0.5 mL/min. UV detection was performed at 205 nm. This LC method can properly separate the two diastereoisomers (Rs > 2) within an analysis time of less than 20 min. Both methods were validated according to the ICH guidelines. Furthermore, these new LC methods have been successfully applied for purity control and diastereoisomers ratio determination of misoprostol bulk drug, tablets and dispersion. Copyright © 2015 Elsevier B.V. All rights reserved.

Dynamical inference: where phase synchronization and generalized synchronization meet.

PubMed

Stankovski, Tomislav; McClintock, Peter V E; Stefanovska, Aneta

2014-06-01

Synchronization is a widespread phenomenon that occurs among interacting oscillatory systems. It facilitates their temporal coordination and can lead to the emergence of spontaneous order. The detection of synchronization from the time series of such systems is of great importance for the understanding and prediction of their dynamics, and several methods for doing so have been introduced. However, the common case where the interacting systems have time-variable characteristic frequencies and coupling parameters, and may also be subject to continuous external perturbation and noise, still presents a major challenge. Here we apply recent developments in dynamical Bayesian inference to tackle these problems. In particular, we discuss how to detect phase slips and the existence of deterministic coupling from measured data, and we unify the concepts of phase synchronization and general synchronization. Starting from phase or state observables, we present methods for the detection of both phase and generalized synchronization. The consistency and equivalence of phase and generalized synchronization are further demonstrated, by the analysis of time series from analog electronic simulations of coupled nonautonomous van der Pol oscillators. We demonstrate that the detection methods work equally well on numerically simulated chaotic systems. In all the cases considered, we show that dynamical Bayesian inference can clearly identify noise-induced phase slips and distinguish coherence from intrinsic coupling-induced synchronization.

Phase-based motion magnification video for monitoring of vital signals using the Hermite transform

NASA Astrophysics Data System (ADS)

Brieva, Jorge; Moya-Albor, Ernesto

2017-11-01

In this paper we present a new Eulerian phase-based motion magnification technique using the Hermite Transform (HT) decomposition that is inspired in the Human Vision System (HVS). We test our method in one sequence of the breathing of a newborn baby and on a video sequence that shows the heartbeat on the wrist. We detect and magnify the heart pulse applying our technique. Our motion magnification approach is compared to the Laplacian phase based approach by means of quantitative metrics (based on the RMS error and the Fourier transform) to measure the quality of both reconstruction and magnification. In addition a noise robustness analysis is performed for the two methods.

Method for assessing motor insulation on operating motors

DOEpatents

Kueck, John D.; Otaduy, Pedro J.

1997-01-01

A method for monitoring the condition of electrical-motor-driven devices. The method is achieved by monitoring electrical variables associated with the functioning of an operating motor, applying these electrical variables to a three phase equivalent circuit and determining non-symmetrical faults in the operating motor based upon symmetrical components analysis techniques.

Synchronized mammalian cell culture: part I--a physical strategy for synchronized cultivation under physiological conditions.

PubMed

Barradas, Oscar Platas; Jandt, Uwe; Becker, Max; Bahnemann, Janina; Pörtner, Ralf; Zeng, An-Ping

2015-01-01

Conventional analysis and optimization procedures of mammalian cell culture processes mostly treat the culture as a homogeneous population. Hence, the focus is on cell physiology and metabolism, cell line development, and process control strategy. Impact on cultivations caused by potential variations in cellular properties between different subpopulations, however, has not yet been evaluated systematically. One main cause for the formation of such subpopulations is the progress of all cells through the cell cycle. The interaction of potential cell cycle specific variations in the cell behavior with large-scale process conditions can be optimally determined by means of (partially) synchronized cultivations, with subsequent population resolved model analysis. Therefore, it is desirable to synchronize a culture with minimal perturbation, which is possible with different yield and quality using physical selection methods, but not with frequently used chemical or whole-culture methods. Conventional nonsynchronizing methods with subsequent cell-specific, for example, flow cytometric analysis, can only resolve cell-limited effects of the cell cycle. In this work, we demonstrate countercurrent-flow centrifugal elutriation as a useful physical method to enrich mammalian cell populations within different phases of a cell cycle, which can be further cultivated for synchronized growth in bioreactors under physiological conditions. The presented combined approach contrasts with other physical selection methods especially with respect to the achievable yield, which makes it suitable for bioreactor scale cultivations. As shown with two industrial cell lines (CHO-K1 and human AGE1.HN), synchronous inocula can be obtained with overall synchrony degrees of up to 82% in the G1 phase, 53% in the S phase and 60% in the G2/M phase, with enrichment factors (Ysync) of 1.71, 1.79, and 4.24 respectively. Cells are able to grow with synchrony in bioreactors over several cell cycles. This strategy, combined with population-resolved model analysis and parameter extraction as described in the accompanying paper, offers new possibilities for studies of cell lines and processes at levels of cell cycle and population under physiological conditions. © 2014 American Institute of Chemical Engineers.

Testing for nonlinearity in non-stationary physiological time series.

PubMed

Guarín, Diego; Delgado, Edilson; Orozco, Álvaro

2011-01-01

Testing for nonlinearity is one of the most important preprocessing steps in nonlinear time series analysis. Typically, this is done by means of the linear surrogate data methods. But it is a known fact that the validity of the results heavily depends on the stationarity of the time series. Since most physiological signals are non-stationary, it is easy to falsely detect nonlinearity using the linear surrogate data methods. In this document, we propose a methodology to extend the procedure for generating constrained surrogate time series in order to assess nonlinearity in non-stationary data. The method is based on the band-phase-randomized surrogates, which consists (contrary to the linear surrogate data methods) in randomizing only a portion of the Fourier phases in the high frequency domain. Analysis of simulated time series showed that in comparison to the linear surrogate data method, our method is able to discriminate between linear stationarity, linear non-stationary and nonlinear time series. Applying our methodology to heart rate variability (HRV) records of five healthy patients, we encountered that nonlinear correlations are present in this non-stationary physiological signals.

Human Systems Integration (HSI) Associated Development Activities in Japan

DTIC Science & Technology

2008-06-12

machine learning and data mining methods. The continuous effort ( KAIZEN ) to improve the analysis phases are illustrated in Figure 14. Although there...model Extraction of a workflow Extraction of a control rule Variation analysis and improvement Plant operation KAIZEN Fig. 14

Development of a novel ultrasound-assisted headspace liquid-phase microextraction and its application to the analysis of chlorophenols in real aqueous samples.

PubMed

Xu, Hui; Liao, Ying; Yao, Jinrong

2007-10-05

A new sample pretreatment technique, ultrasound-assisted headspace liquid-phase microextraction was developed as mentioned in this paper. In the technique, the volatile analytes were headspace extracted into a small drop of solvent, which suspended on the bottom of a cone-shaped PCR tube instead of the needle tip of a microsyringe. More solvent could be suspended in the PCR tube than microsyringe due to the larger interfacial tension, thus the analysis sensitivity was significantly improved with the increase of the extractant volume. Moreover, ultrasound-assisted extraction and independent controlling temperature of the extractant and the sample were performed to enhance the extraction efficiency. Following the extraction, the solvent-loaded sample was analyzed by high-performance liquid chromatography. Chlorophenols (2-chlorophenol, 2,4-dichlorophenol and 2,6-dichlorophenol) were chosen as model analytes to investigate the feasibility of the method. The experimental conditions related to the extraction efficiency were systematically studied. Under the optimum experimental conditions, the detection limit (S/N=3), intra- and inter-day RSD were 6 ng mL(-1), 4.6%, 3.9% for 2-chlorophenol, 12 ng mL(-1), 2.4%, 8.8% for 2,4-dichlorophenol and 23 ng mL(-1), 3.3%, 5.3% for 2,6-dichlorophenol, respectively. The proposed method was successfully applied to determine chlorophenols in real aqueous samples. Good recoveries ranging from 84.6% to 100.7% were obtained. In addition, the extraction efficiency of our method and the conventional headspace liquid-phase microextraction were compared; the extraction efficiency of the former was about 21 times higher than that of the latter. The results demonstrated that the proposed method is a promising sample pretreatment approach, its advantages over the conventional headspace liquid-phase microextraction include simple setup, ease of operation, rapidness, sensitivity, precision and no cross-contamination. The method is very suitable for the analysis of trace volatile and semivolatile pollutants in real aqueous sample.

A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

PubMed

Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2017-07-01

Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

Modelling and Analysis of the Excavation Phase by the Theory of Blocks Method of Tunnel 4 Kherrata Gorge, Algeria

NASA Astrophysics Data System (ADS)

Boukarm, Riadh; Houam, Abdelkader; Fredj, Mohammed; Boucif, Rima

2017-12-01

The aim of our work is to check the stability during excavation tunnel work in the rock mass of Kherrata, connecting the cities of Bejaia to Setif. The characterization methods through the Q system (method of Barton), RMR (Bieniawski classification) allowed us to conclude that the quality of rock mass is average in limestone, and poor in fractured limestone. Then modelling of excavation phase using the theory of blocks method (Software UNWEDGE) with the parameters from the recommendations of classification allowed us to check stability and to finally conclude that the use of geomechanical classification and the theory of blocks can be considered reliable in preliminary design.

An imaging method of wavefront coding system based on phase plate rotation

NASA Astrophysics Data System (ADS)

Yi, Rigui; Chen, Xi; Dong, Liquan; Liu, Ming; Zhao, Yuejin; Liu, Xiaohua

2018-01-01

Wave-front coding has a great prospect in extending the depth of the optical imaging system and reducing optical aberrations, but the image quality and noise performance are inevitably reduced. According to the theoretical analysis of the wave-front coding system and the phase function expression of the cubic phase plate, this paper analyzed and utilized the feature that the phase function expression would be invariant in the new coordinate system when the phase plate rotates at different angles around the z-axis, and we proposed a method based on the rotation of the phase plate and image fusion. First, let the phase plate rotated at a certain angle around the z-axis, the shape and distribution of the PSF obtained on the image surface remain unchanged, the rotation angle and direction are consistent with the rotation angle of the phase plate. Then, the middle blurred image is filtered by the point spread function of the rotation adjustment. Finally, the reconstruction images were fused by the method of the Laplacian pyramid image fusion and the Fourier transform spectrum fusion method, and the results were evaluated subjectively and objectively. In this paper, we used Matlab to simulate the images. By using the Laplacian pyramid image fusion method, the signal-to-noise ratio of the image is increased by 19% 27%, the clarity is increased by 11% 15% , and the average gradient is increased by 4% 9% . By using the Fourier transform spectrum fusion method, the signal-to-noise ratio of the image is increased by 14% 23%, the clarity is increased by 6% 11% , and the average gradient is improved by 2% 6%. The experimental results show that the image processing by the above method can improve the quality of the restored image, improving the image clarity, and can effectively preserve the image information.

A system for analysis and classification of voice communications

NASA Technical Reports Server (NTRS)

Older, H. J.; Jenney, L. L.; Garland, L.

1973-01-01

A method for analysis and classification of verbal communications typically associated with manned space missions or simulations was developed. The study was carried out in two phases. Phase 1 was devoted to identification of crew tasks and activities which require voice communication for accomplishment or reporting. Phase 2 entailed development of a message classification system and a preliminary test of its feasibility. The classification system permits voice communications to be analyzed to three progressively more specific levels of detail and to be described in terms of message content, purpose, and the participants in the information exchange. A coding technique was devised to allow messages to be recorded by an eight-digit number.

Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.

PubMed

Bie, Zhenying; Lu, Wei; Zhu, You; Chen, Yusong; Ren, Hubo; Ji, Lishun

2017-01-27

A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of Transformation Plasticity in Steel Using a Finite Element Method Coupled with a Phase Field Model

PubMed Central

Cho, Yi-Gil; Kim, Jin-You; Cho, Hoon-Hwe; Cha, Pil-Ryung; Suh, Dong-Woo; Lee, Jae Kon; Han, Heung Nam

2012-01-01

An implicit finite element model was developed to analyze the deformation behavior of low carbon steel during phase transformation. The finite element model was coupled hierarchically with a phase field model that could simulate the kinetics and micro-structural evolution during the austenite-to-ferrite transformation of low carbon steel. Thermo-elastic-plastic constitutive equations for each phase were adopted to confirm the transformation plasticity due to the weaker phase yielding that was proposed by Greenwood and Johnson. From the simulations under various possible plastic properties of each phase, a more quantitative understanding of the origin of transformation plasticity was attempted by a comparison with the experimental observation. PMID:22558295