Extending the solvent-free MALDI sample preparation method.

PubMed

Hanton, Scott D; Parees, David M

2005-01-01

Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important technique to characterize many different materials, including synthetic polymers. MALDI mass spectral data can be used to determine the polymer average molecular weights, repeat units, and end groups. One of the key issues in traditional MALDI sample preparation is making good solutions of the analyte and the matrix. Solvent-free sample preparation methods have been developed to address these issues. Previous results of solvent-free or dry prepared samples show some advantages over traditional wet sample preparation methods. Although the results of the published solvent-free sample preparation methods produced excellent mass spectra, we found the method to be very time-consuming, with significant tool cleaning, which presents a significant possibility of cross contamination. To address these issues, we developed an extension of the solvent-free method that replaces the mortar and pestle grinding with ball milling the sample in a glass vial with two small steel balls. This new method generates mass spectra with equal quality of the previous methods, but has significant advantages in productivity, eliminates cross contamination, and is applicable to liquid and soft or waxy analytes.

Analytical solution for vacuum preloading considering the nonlinear distribution of horizontal permeability within the smear zone.

PubMed

Peng, Jie; He, Xiang; Ye, Hanming

2015-01-01

The vacuum preloading is an effective method which is widely used in ground treatment. In consolidation analysis, the soil around prefabricated vertical drain (PVD) is traditionally divided into smear zone and undisturbed zone, both with constant permeability. In reality, the permeability of soil changes continuously within the smear zone. In this study, the horizontal permeability coefficient of soil within the smear zone is described by an exponential function of radial distance. A solution for vacuum preloading consolidation considers the nonlinear distribution of horizontal permeability within the smear zone is presented and compared with previous analytical results as well as a numerical solution, the results show that the presented solution correlates well with the numerical solution, and is more precise than previous analytical solution.

Analytical solution for vacuum preloading considering the nonlinear distribution of horizontal permeability within the smear zone

PubMed Central

Peng, Jie; He, Xiang; Ye, Hanming

2015-01-01

The vacuum preloading is an effective method which is widely used in ground treatment. In consolidation analysis, the soil around prefabricated vertical drain (PVD) is traditionally divided into smear zone and undisturbed zone, both with constant permeability. In reality, the permeability of soil changes continuously within the smear zone. In this study, the horizontal permeability coefficient of soil within the smear zone is described by an exponential function of radial distance. A solution for vacuum preloading consolidation considers the nonlinear distribution of horizontal permeability within the smear zone is presented and compared with previous analytical results as well as a numerical solution, the results show that the presented solution correlates well with the numerical solution, and is more precise than previous analytical solution. PMID:26447973

Correlation of ground tests and analyses of a dynamically scaled Space Station model configuration

NASA Technical Reports Server (NTRS)

Javeed, Mehzad; Edighoffer, Harold H.; Mcgowan, Paul E.

1993-01-01

Verification of analytical models through correlation with ground test results of a complex space truss structure is demonstrated. A multi-component, dynamically scaled space station model configuration is the focus structure for this work. Previously established test/analysis correlation procedures are used to develop improved component analytical models. Integrated system analytical models, consisting of updated component analytical models, are compared with modal test results to establish the accuracy of system-level dynamic predictions. Design sensitivity model updating methods are shown to be effective for providing improved component analytical models. Also, the effects of component model accuracy and interface modeling fidelity on the accuracy of integrated model predictions is examined.

Analysis of modal behavior at frequency cross-over

NASA Astrophysics Data System (ADS)

Costa, Robert N., Jr.

1994-11-01

The existence of the mode crossing condition is detected and analyzed in the Active Control of Space Structures Model 4 (ACOSS4). The condition is studied for its contribution to the inability of previous algorithms to successfully optimize the structure and converge to a feasible solution. A new algorithm is developed to detect and correct for mode crossings. The existence of the mode crossing condition is verified in ACOSS4 and found not to have appreciably affected the solution. The structure is then successfully optimized using new analytic methods based on modal expansion. An unrelated error in the optimization algorithm previously used is verified and corrected, thereby equipping the optimization algorithm with a second analytic method for eigenvector differentiation based on Nelson's Method. The second structure is the Control of Flexible Structures (COFS). The COFS structure is successfully reproduced and an initial eigenanalysis completed.

Improved full analytical polygon-based method using Fourier analysis of the three-dimensional affine transformation.

PubMed

Pan, Yijie; Wang, Yongtian; Liu, Juan; Li, Xin; Jia, Jia

2014-03-01

Previous research [Appl. Opt.52, A290 (2013)] has revealed that Fourier analysis of three-dimensional affine transformation theory can be used to improve the computation speed of the traditional polygon-based method. In this paper, we continue our research and propose an improved full analytical polygon-based method developed upon this theory. Vertex vectors of primitive and arbitrary triangles and the pseudo-inverse matrix were used to obtain an affine transformation matrix representing the spatial relationship between the two triangles. With this relationship and the primitive spectrum, we analytically obtained the spectrum of the arbitrary triangle. This algorithm discards low-level angular dependent computations. In order to add diffusive reflection to each arbitrary surface, we also propose a whole matrix computation approach that takes advantage of the affine transformation matrix and uses matrix multiplication to calculate shifting parameters of similar sub-polygons. The proposed method improves hologram computation speed for the conventional full analytical approach. Optical experimental results are demonstrated which prove that the proposed method can effectively reconstruct three-dimensional scenes.

On-line solid-phase microextraction of triclosan, bisphenol A, chlorophenols, and selected pharmaceuticals in environmental water samples by high-performance liquid chromatography-ultraviolet detection.

PubMed

Kim, Dalho; Han, Jungho; Choi, Yongwook

2013-01-01

A method using on-line solid-phase microextraction (SPME) on a carbowax-templated fiber followed by liquid chromatography (LC) with ultraviolet (UV) detection was developed for the determination of triclosan in environmental water samples. Along with triclosan, other selected phenolic compounds, bisphenol A, and acidic pharmaceuticals were studied. Previous SPME/LC or stir-bar sorptive extraction/LC-UV for polar analytes showed lack of sensitivity. In this study, the calculated octanol-water distribution coefficient (log D) values of the target analytes at different pH values were used to estimate polarity of the analytes. The lack of sensitivity observed in earlier studies is identified as a lack of desorption by strong polar-polar interactions between analyte and solid-phase. Calculated log D values were useful to understand or predict the interaction between analyte and solid phase. Under the optimized conditions, the method detection limit of selected analytes by using on-line SPME-LC-UV method ranged from 5 to 33 ng L(-1), except for very polar 3-chlorophenol and 2,4-dichlorophenol which was obscured in wastewater samples by an interfering substance. This level of detection represented a remarkable improvement over the conventional existing methods. The on-line SPME-LC-UV method, which did not require derivatization of analytes, was applied to the determination of TCS including phenolic compounds and acidic pharmaceuticals in tap water and river water and municipal wastewater samples.

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.

Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods

DOE PAGES

Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.; ...

2016-07-05

Here, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. In this paper, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 °C), 31P NMR for determination ofmore » hydroxyl groups, and a quantitative gas chromatography–mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to -determine metrics for bio-oil quality. Lastly, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.« less

Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods

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

Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.

Here, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. In this paper, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 °C), 31P NMR for determination ofmore » hydroxyl groups, and a quantitative gas chromatography–mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to -determine metrics for bio-oil quality. Lastly, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.« less

RCRA Facility investigation report for Waste Area Grouping 6 at Oak Ridge National Laboratory, Oak Ridge, Tennessee. Volume 5, Technical Memorandums 06-09A, 06-10A, and 06-12A

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

None

This report provides a detailed summary of the activities carried out to sample groundwater at Waste Area Grouping (WAG) 6. The analytical results for samples collected during Phase 1, Activity 2 of the WAG 6 Resource Conservation and Recovery Act Facility Investigation (RFI) are also presented. In addition, analytical results for Phase 1, activity sampling events for which data were not previously reported are included in this TM. A summary of the groundwater sampling activities of WAG 6, to date, are given in the Introduction. The Methodology section describes the sampling procedures and analytical parameters. Six attachments are included. Attachmentsmore » 1 and 2 provide analytical results for selected RFI groundwater samples and ORNL sampling event. Attachment 3 provides a summary of the contaminants detected in each well sampled for all sampling events conducted at WAG 6. Bechtel National Inc. (BNI)/IT Corporation Contract Laboratory (IT) RFI analytical methods and detection limits are given in Attachment 4. Attachment 5 provides the Oak Ridge National Laboratory (ORNL)/Analytical Chemistry Division (ACD) analytical methods and detection limits and Resource Conservation and Recovery Act (RCRA) quarterly compliance monitoring (1988--1989). Attachment 6 provides ORNL/ACD groundwater analytical methods and detection limits (for the 1990 RCRA semi-annual compliance monitoring).« less

A simplified analytic form for generation of axisymmetric plasma boundaries

DOE PAGES

Luce, Timothy C.

2017-02-23

An improved method has been formulated for generating analytic boundary shapes as input for axisymmetric MHD equilibria. This method uses the family of superellipses as the basis function, as previously introduced. The improvements are a simplified notation, reduction of the number of simultaneous nonlinear equations to be solved, and the realization that not all combinations of input parameters admit a solution to the nonlinear constraint equations. The method tests for the existence of a self-consistent solution and, when no solution exists, it uses a deterministic method to find a nearby solution. As a result, examples of generation of boundaries, includingmore » tests with an equilibrium solver, are given.« less

A simplified analytic form for generation of axisymmetric plasma boundaries

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

Luce, Timothy C.

An improved method has been formulated for generating analytic boundary shapes as input for axisymmetric MHD equilibria. This method uses the family of superellipses as the basis function, as previously introduced. The improvements are a simplified notation, reduction of the number of simultaneous nonlinear equations to be solved, and the realization that not all combinations of input parameters admit a solution to the nonlinear constraint equations. The method tests for the existence of a self-consistent solution and, when no solution exists, it uses a deterministic method to find a nearby solution. As a result, examples of generation of boundaries, includingmore » tests with an equilibrium solver, are given.« less

Genetics-based methods for detection of Salmonella spp. in foods.

PubMed

Mozola, Mark A

2006-01-01

Genetic methods are now at the forefront of foodborne pathogen testing. The sensitivity, specificity, and inclusivity advantages offered by deoxyribonucleic acid (DNA) probe technology have driven an intense effort in methods development over the past 20 years. DNA probe-based methods for Salmonella spp. and other pathogens have progressed from time-consuming procedures involving the use of radioisotopes to simple, high throughput, automated assays. The analytical sensitivity of nucleic acid amplification technology has facilitated a reduction in analysis time by allowing enriched samples to be tested for previously undetectable quantities of analyte. This article will trace the evolution of the development of genetic methods for detection of Salmonella in foods, review the basic assay formats and their advantages and limitations, and discuss method performance characteristics and considerations for selection of methods.

Analytical solutions for solute transport in groundwater and riverine flow using Green's Function Method and pertinent coordinate transformation method

NASA Astrophysics Data System (ADS)

Sanskrityayn, Abhishek; Suk, Heejun; Kumar, Naveen

2017-04-01

In this study, analytical solutions of one-dimensional pollutant transport originating from instantaneous and continuous point sources were developed in groundwater and riverine flow using both Green's Function Method (GFM) and pertinent coordinate transformation method. Dispersion coefficient and flow velocity are considered spatially and temporally dependent. The spatial dependence of the velocity is linear, non-homogeneous and that of dispersion coefficient is square of that of velocity, while the temporal dependence is considered linear, exponentially and asymptotically decelerating and accelerating. Our proposed analytical solutions are derived for three different situations depending on variations of dispersion coefficient and velocity, respectively which can represent real physical processes occurring in groundwater and riverine systems. First case refers to steady solute transport situation in steady flow in which dispersion coefficient and velocity are only spatially dependent. The second case represents transient solute transport in steady flow in which dispersion coefficient is spatially and temporally dependent while the velocity is spatially dependent. Finally, the third case indicates transient solute transport in unsteady flow in which both dispersion coefficient and velocity are spatially and temporally dependent. The present paper demonstrates the concentration distribution behavior from a point source in realistically occurring flow domains of hydrological systems including groundwater and riverine water in which the dispersivity of pollutant's mass is affected by heterogeneity of the medium as well as by other factors like velocity fluctuations, while velocity is influenced by water table slope and recharge rate. Such capabilities give the proposed method's superiority about application of various hydrological problems to be solved over other previously existing analytical solutions. Especially, to author's knowledge, any other solution doesn't exist for both spatially and temporally variations of dispersion coefficient and velocity. In this study, the existing analytical solutions from previous widely known studies are used for comparison as validation tools to verify the proposed analytical solution as well as the numerical code of the Two-Dimensional Subsurface Flow, Fate and Transport of Microbes and Chemicals (2DFATMIC) code and the developed 1D finite difference code (FDM). All such solutions show perfect match with the respective proposed solutions.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and alpha-spectrometry.

PubMed

Goldstein, S J; Hensley, C A; Armenta, C E; Peters, R J

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for alpha-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of "real" environmental and bioassay samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of approximately 2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously.

A comparison of several techniques for imputing tree level data

Treesearch

David Gartner

2002-01-01

As Forest Inventory and Analysis (FIA) changes from periodic surveys to the multipanel annual survey, new analytical methods become available. The current official statistic is the moving average. One alternative is an updated moving average. Several methods of updating plot per acre volume have been discussed previously. However, these methods may not be appropriate...

Simultaneous determination of gabapentin, pregabalin, vigabatrin, and topiramate in plasma by HPLC with fluorescence detection.

PubMed

Martinc, Boštjan; Roškar, Robert; Grabnar, Iztok; Vovk, Tomaž

2014-07-01

Therapeutic drug monitoring (TDM) of antiepileptic drugs (AEDs) has been recognized as a useful tool in management of epilepsy. We developed a simple analytical method for simultaneous determination of four second generation AEDs, including gabapentin (GBP), pregabalin (PGB), vigabatrin (VGB), and topiramate (TOP). Analytes were extracted from human plasma using universal solid phase extraction, derivatized with 4-chloro-7-nitrobenzofurazan (NBD-Cl) and analyzed by HPLC with fluorescence detection. Using mass spectrometry we confirmed that NBD-Cl reacts with sulfamate group of TOP similarly as with amine group of the other three analytes. The method is linear (r(2)>0.998) across investigated analytical ranges (0.375-30.0μg/mL for GBP, PGB, and VGB; 0.50-20.0μg/mL for TOP). Intraday and interday precision do not exceed 9.40%. The accuracy is from 95.6% to 106%. The recovery is higher than 80.6%, and the lower limit of quantification is at least 0.5μg/mL. The method is selective and robust. For TOP determination the method was compared to a previously published method and the results obtained by the two methods were in good agreement. The developed method is suitable for routine TDM. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Song, Ehwang; Gao, Yuqian; Wu, Chaochao

Here, mass spectrometry (MS) based targeted proteomic methods such as selected reaction monitoring (SRM) are becoming the method of choice for preclinical verification of candidate protein biomarkers. The Clinical Proteomic Tumor Analysis Consortium (CPTAC) of the National Cancer Institute has investigated the standardization and analytical validation of the SRM assays and demonstrated robust analytical performance on different instruments across different laboratories. An Assay Portal has also been established by CPTAC to provide the research community a resource consisting of large set of targeted MS-based assays, and a depository to share assays publicly, providing that assays meet the guidelines proposed bymore » CPTAC. Herein, we report 98 SRM assays covering 70 candidate protein biomarkers previously reported as associated with ovarian cancer that have been thoroughly characterized according to the CPTAC Assay Characterization Guidance Document. The experiments, methods and results for characterizing these SRM assays for their MS response, repeatability, selectivity, stability, and reproducible detection of endogenous analytes are described in detail.« less

Blade loss transient dynamics analysis, volume 2. Task 2: Theoretical and analytical development. Task 3: Experimental verification

NASA Technical Reports Server (NTRS)

Gallardo, V. C.; Storace, A. S.; Gaffney, E. F.; Bach, L. J.; Stallone, M. J.

1981-01-01

The component element method was used to develop a transient dynamic analysis computer program which is essentially based on modal synthesis combined with a central, finite difference, numerical integration scheme. The methodology leads to a modular or building-block technique that is amenable to computer programming. To verify the analytical method, turbine engine transient response analysis (TETRA), was applied to two blade-out test vehicles that had been previously instrumented and tested. Comparison of the time dependent test data with those predicted by TETRA led to recommendations for refinement or extension of the analytical method to improve its accuracy and overcome its shortcomings. The development of working equations, their discretization, numerical solution scheme, the modular concept of engine modelling, the program logical structure and some illustrated results are discussed. The blade-loss test vehicles (rig full engine), the type of measured data, and the engine structural model are described.

Examining the Efficacy of Self-Regulated Strategy Development for Students with Emotional or Behavioral Disorders: A Meta-Analysis

ERIC Educational Resources Information Center

Losinski, Mickey; Cuenca-Carlino, Yojanna; Zablocki, Mark; Teagarden, James

2014-01-01

Two previous reviews have indicated that self-regulated strategy instruction (SRSD) is an evidence-based practice that can improve the writing skills of students with emotional and behavioral disorders. The purpose of this meta-analysis is to extend the findings and analytic methods of previous reviews by examining published studies regarding…

Projected 1981 exposure estimates using iterative proportional fitting

DOT National Transportation Integrated Search

1985-10-01

1981 VMT estimates categorized by eight driver, vehicle, and environmental : variables are produced. These 1981 estimates are produced using analytical : methods developed in a previous report. The estimates are based on 1977 : NPTS data (the latest ...

Reader's Block: A Systematic Review of Barriers to Adoption, Access and Use in E-Book User Studies

ERIC Educational Resources Information Center

Girard, Adam

2014-01-01

Introduction: This review of barriers to e-book use systematically identifies obstacles to engaging reading experiences. Through the use of an analytical framework, the users being studied, study setting, and methods used in previous work are described in order to identify promising areas for future research. Method: The method used is a…

Quantifying construction and demolition waste: an analytical review.

PubMed

Wu, Zezhou; Yu, Ann T W; Shen, Liyin; Liu, Guiwen

2014-09-01

Quantifying construction and demolition (C&D) waste generation is regarded as a prerequisite for the implementation of successful waste management. In literature, various methods have been employed to quantify the C&D waste generation at both regional and project levels. However, an integrated review that systemically describes and analyses all the existing methods has yet to be conducted. To bridge this research gap, an analytical review is conducted. Fifty-seven papers are retrieved based on a set of rigorous procedures. The characteristics of the selected papers are classified according to the following criteria - waste generation activity, estimation level and quantification methodology. Six categories of existing C&D waste quantification methodologies are identified, including site visit method, waste generation rate method, lifetime analysis method, classification system accumulation method, variables modelling method and other particular methods. A critical comparison of the identified methods is given according to their characteristics and implementation constraints. Moreover, a decision tree is proposed for aiding the selection of the most appropriate quantification method in different scenarios. Based on the analytical review, limitations of previous studies and recommendations of potential future research directions are further suggested. Copyright © 2014 Elsevier Ltd. All rights reserved.

A Requirements-Driven Optimization Method for Acoustic Liners Using Analytic Derivatives

NASA Technical Reports Server (NTRS)

Berton, Jeffrey J.; Lopes, Leonard V.

2017-01-01

More than ever, there is flexibility and freedom in acoustic liner design. Subject to practical considerations, liner design variables may be manipulated to achieve a target attenuation spectrum. But characteristics of the ideal attenuation spectrum can be difficult to know. Many multidisciplinary system effects govern how engine noise sources contribute to community noise. Given a hardwall fan noise source to be suppressed, and using an analytical certification noise model to compute a community noise measure of merit, the optimal attenuation spectrum can be derived using multidisciplinary systems analysis methods. In a previous paper on this subject, a method deriving the ideal target attenuation spectrum that minimizes noise perceived by observers on the ground was described. A simple code-wrapping approach was used to evaluate a community noise objective function for an external optimizer. Gradients were evaluated using a finite difference formula. The subject of this paper is an application of analytic derivatives that supply precise gradients to an optimization process. Analytic derivatives improve the efficiency and accuracy of gradient-based optimization methods and allow consideration of more design variables. In addition, the benefit of variable impedance liners is explored using a multi-objective optimization.

A theoretical analysis of the free vibrations of ring- and/or stringer-stiffened elliptical cylinders with arbitrary end conditions. Volume 1: Analytical derivation and applications

NASA Technical Reports Server (NTRS)

Boyd, D. E.; Rao, C. K. P.

1973-01-01

The derivation and application of a Rayleigh-Ritz modal vibration analysis are presented for ring and/or stringer stiffened noncircular cylindrical shells with arbitrary end conditions. Comparisons with previous results from experimental and analytical studies showed this method of analysis to be accurate for a variety of end conditions. Results indicate a greater effect of rings on natural frequencies than of stringers.

Analytic theory of photoacoustic wave generation from a spheroidal droplet.

PubMed

Li, Yong; Fang, Hui; Min, Changjun; Yuan, Xiaocong

2014-08-25

In this paper, we develop an analytic theory for describing the photoacoustic wave generation from a spheroidal droplet and derive the first complete analytic solution. Our derivation is based on solving the photoacoustic Helmholtz equation in spheroidal coordinates with the separation-of-variables method. As the verification, besides carrying out the asymptotic analyses which recover the standard solutions for a sphere, an infinite cylinder and an infinite layer, we also confirm that the partial transmission and reflection model previously demonstrated for these three geometries still stands. We expect that this analytic solution will find broad practical uses in interpreting experiment results, considering that its building blocks, the spheroidal wave functions (SWFs), can be numerically calculated by the existing computer programs.

Simultaneous determination of thirteen different steroid hormones using micro UHPLC-MS/MS with on-line SPE system.

PubMed

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tímea; Mészáros, Katalin Viola; Bálint, Mária; Szabó, Pál Tamás

2018-02-20

Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LOQ). Micro UHPLC coupled to sensitive tandem mass spectrometry provides state of the art solution for such analytical problems. Using on-line SPE with column switching on a micro UHPLC-MS/MS system allowed to decrease LOQ without any complex sample preparation protocol. The presented method is capable of reaching satisfactory low LOQ values for analysis of thirteen different steroid molecules from human plasma without the most commonly used off-line SPE or compound derivatization. Steroids were determined by using two simple sample preparation methods, based on lower and higher plasma steroid concentrations. In the first method, higher analyte concentrations were directly determined after protein precipitation with methanol. The organic phase obtained from the precipitation was diluted with water and directly injected into the LC-MS system. In the second method, low steroid levels were determined by concentrating the organic phase after steroid extraction. In this case, analytes were extracted with ethyl acetate and reconstituted in 90/10 water/acetonitrile following evaporation to dryness. This step provided much lower LOQs, outperforming previously published values. The method has been validated and subsequently applied to clinical laboratory measurement. Copyright © 2017 Elsevier B.V. All rights reserved.

Fourier Transform Infrared Absorption Spectroscopy for Quantitative Analysis of Gas Mixtures at Low Temperatures for Homeland Security Applications.

PubMed

Meier, D C; Benkstein, K D; Hurst, W S; Chu, P M

2017-05-01

Performance standard specifications for point chemical vapor detectors are established in ASTM E 2885-13 and ASTM E 2933-13. The performance evaluation of the detectors requires the accurate delivery of known concentrations of the chemical target to the system under test. Referee methods enable the analyte test concentration and associated uncertainties in the analyte test concentration to be validated by independent analysis, which is especially important for reactive analytes. This work extends the capability of a previously demonstrated method for using Fourier transform infrared (FT-IR) absorption spectroscopy for quantitatively evaluating the composition of vapor streams containing hazardous materials at Acute Exposure Guideline Levels (AEGL) to include test conditions colder than laboratory ambient temperatures. The described method covers the use of primary reference spectra to establish analyte concentrations, the generation of secondary reference spectra suitable for measuring analyte concentrations under specified testing environments, and the use of additional reference spectra and spectral profile strategies to mitigate the uncertainties due to impurities and water condensation within the low-temperature (7 °C, -5 °C) test cell. Important benefits of this approach include verification of the test analyte concentration with characterized uncertainties by in situ measurements co-located with the detector under test, near-real-time feedback, and broad applicability to toxic industrial chemicals.

Fourier Transform Infrared Absorption Spectroscopy for Quantitative Analysis of Gas Mixtures at Low Temperatures for Homeland Security Applications

PubMed Central

Meier, D.C.; Benkstein, K.D.; Hurst, W.S.; Chu, P.M.

2016-01-01

Performance standard specifications for point chemical vapor detectors are established in ASTM E 2885-13 and ASTM E 2933-13. The performance evaluation of the detectors requires the accurate delivery of known concentrations of the chemical target to the system under test. Referee methods enable the analyte test concentration and associated uncertainties in the analyte test concentration to be validated by independent analysis, which is especially important for reactive analytes. This work extends the capability of a previously demonstrated method for using Fourier transform infrared (FT-IR) absorption spectroscopy for quantitatively evaluating the composition of vapor streams containing hazardous materials at Acute Exposure Guideline Levels (AEGL) to include test conditions colder than laboratory ambient temperatures. The described method covers the use of primary reference spectra to establish analyte concentrations, the generation of secondary reference spectra suitable for measuring analyte concentrations under specified testing environments, and the use of additional reference spectra and spectral profile strategies to mitigate the uncertainties due to impurities and water condensation within the low-temperature (7 °C, −5 °C) test cell. Important benefits of this approach include verification of the test analyte concentration with characterized uncertainties by in situ measurements co-located with the detector under test, near-real-time feedback, and broad applicability to toxic industrial chemicals. PMID:28090126

Semi-automated solid phase extraction method for the mass spectrometric quantification of 12 specific metabolites of organophosphorus pesticides, synthetic pyrethroids, and select herbicides in human urine.

PubMed

Davis, Mark D; Wade, Erin L; Restrepo, Paula R; Roman-Esteva, William; Bravo, Roberto; Kuklenyik, Peter; Calafat, Antonia M

2013-06-15

Organophosphate and pyrethroid insecticides and phenoxyacetic acid herbicides represent important classes of pesticides applied in commercial and residential settings. Interest in assessing the extent of human exposure to these pesticides exists because of their widespread use and their potential adverse health effects. An analytical method for measuring 12 biomarkers of several of these pesticides in urine has been developed. The target analytes were extracted from one milliliter of urine by a semi-automated solid phase extraction technique, separated from each other and from other urinary biomolecules by reversed-phase high performance liquid chromatography, and detected using tandem mass spectrometry with isotope dilution quantitation. This method can be used to measure all the target analytes in one injection with similar repeatability and detection limits of previous methods which required more than one injection. Each step of the procedure was optimized to produce a robust, reproducible, accurate, precise and efficient method. The required selectivity and sensitivity for trace-level analysis (e.g., limits of detection below 0.5ng/mL) was achieved using a narrow diameter analytical column, higher than unit mass resolution for certain analytes, and stable isotope labeled internal standards. The method was applied to the analysis of 55 samples collected from adult anonymous donors with no known exposure to the target pesticides. This efficient and cost-effective method is adequate to handle the large number of samples required for national biomonitoring surveys. Published by Elsevier B.V.

Characterizing the uncertainty of classification methods and its impact on the performance of crowdsourcing

NASA Astrophysics Data System (ADS)

Ribera, Javier; Tahboub, Khalid; Delp, Edward J.

2015-03-01

Video surveillance systems are widely deployed for public safety. Real-time monitoring and alerting are some of the key requirements for building an intelligent video surveillance system. Real-life settings introduce many challenges that can impact the performance of real-time video analytics. Video analytics are desired to be resilient to adverse and changing scenarios. In this paper we present various approaches to characterize the uncertainty of a classifier and incorporate crowdsourcing at the times when the method is uncertain about making a particular decision. Incorporating crowdsourcing when a real-time video analytic method is uncertain about making a particular decision is known as online active learning from crowds. We evaluate our proposed approach by testing a method we developed previously for crowd flow estimation. We present three different approaches to characterize the uncertainty of the classifier in the automatic crowd flow estimation method and test them by introducing video quality degradations. Criteria to aggregate crowdsourcing results are also proposed and evaluated. An experimental evaluation is conducted using a publicly available dataset.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and {alpha}-Spectrometry

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

Goldstein, S.J.; Hensley, C.A.; Armenta, C.E.

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for {alpha}-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of `real` environmental and bioassaymore » samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of {approx}2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously. 24 refs., 2 figs., 2 tabs.« less

Airside HVAC BESTEST: HVAC Air-Distribution System Model Test Cases for ASHRAE Standard 140

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

Judkoff, Ronald; Neymark, Joel; Kennedy, Mike D.

This paper summarizes recent work to develop new airside HVAC equipment model analytical verification test cases for ANSI/ASHRAE Standard 140, Standard Method of Test for the Evaluation of Building Energy Analysis Computer Programs. The analytical verification test method allows comparison of simulation results from a wide variety of building energy simulation programs with quasi-analytical solutions, further described below. Standard 140 is widely cited for evaluating software for use with performance-path energy efficiency analysis, in conjunction with well-known energy-efficiency standards including ASHRAE Standard 90.1, the International Energy Conservation Code, and other international standards. Airside HVAC Equipment is a common area ofmore » modelling not previously explicitly tested by Standard 140. Integration of the completed test suite into Standard 140 is in progress.« less

The exact solution of the monoenergetic transport equation for critical cylinders

NASA Technical Reports Server (NTRS)

Westfall, R. M.; Metcalf, D. R.

1972-01-01

An analytic solution for the critical, monoenergetic, bare, infinite cylinder is presented. The solution is obtained by modifying a previous development based on a neutron density transform and Case's singular eigenfunction method. Numerical results for critical radii and the neutron density as a function of position are included and compared with the results of other methods.

Developments in mycotoxin analysis: an update for 2014-2015

USDA-ARS?s Scientific Manuscript database

This review summarizes developments in the determination of mycotoxins over a period between mid-2014 and mid-2015. In tradition with previous articles of this series, analytical methods to determine aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxins, patulin, trichothecenes, an...

Dynamic Looping of a Free-Draining Polymer

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

Ye, Felix X. -F.; Stinis, Panos; Qian, Hong

Here, we revisit the celebrated Wilemski--Fixman (WF) treatment for the looping time of a free-draining polymer. The WF theory introduces a sink term into the Fokker--Planck equation for themore » $3(N+1)$-dimensional Ornstein--Uhlenbeck process of polymer dynamics, which accounts for the appropriate boundary condition due to the formation of a loop. The assumption for WF theory is considerably relaxed. A perturbation method approach is developed that justifies and generalizes the previous results using either a delta sink or a Heaviside sink. For both types of sinks, we show that under the condition of a small dimensionless $$\\epsilon$$, the ratio of capture radius to the Kuhn length, we are able to systematically produce all known analytical and asymptotic results obtained by other methods. This includes most notably the transition regime between the $N^2$ scaling of Doi, and $$N\\sqrt{N}/\\epsilon$$ scaling of Szabo, Schulten, and Schulten. The mathematical issue at play is the nonuniform convergence of $$\\epsilon\\to 0$$ and $$N\\to\\infty$$, the latter being an inherent part of the theory of a Gaussian polymer. Our analysis yields a novel term in the analytical expression for the looping time with small $$\\epsilon$$, which was previously unknown. Monte Carlo numerical simulations corroborate the analytical findings. The systematic method developed here can be applied to other systems modeled by multidimensional Smoluchowski equations.« less

Single-Cell Detection of Secreted Aβ and sAPPα from Human IPSC-Derived Neurons and Astrocytes.

PubMed

Liao, Mei-Chen; Muratore, Christina R; Gierahn, Todd M; Sullivan, Sarah E; Srikanth, Priya; De Jager, Philip L; Love, J Christopher; Young-Pearse, Tracy L

2016-02-03

Secreted factors play a central role in normal and pathological processes in every tissue in the body. The brain is composed of a highly complex milieu of different cell types and few methods exist that can identify which individual cells in a complex mixture are secreting specific analytes. By identifying which cells are responsible, we can better understand neural physiology and pathophysiology, more readily identify the underlying pathways responsible for analyte production, and ultimately use this information to guide the development of novel therapeutic strategies that target the cell types of relevance. We present here a method for detecting analytes secreted from single human induced pluripotent stem cell (iPSC)-derived neural cells and have applied the method to measure amyloid β (Aβ) and soluble amyloid precursor protein-alpha (sAPPα), analytes central to Alzheimer's disease pathogenesis. Through these studies, we have uncovered the dynamic range of secretion profiles of these analytes from single iPSC-derived neuronal and glial cells and have molecularly characterized subpopulations of these cells through immunostaining and gene expression analyses. In examining Aβ and sAPPα secretion from single cells, we were able to identify previously unappreciated complexities in the biology of APP cleavage that could not otherwise have been found by studying averaged responses over pools of cells. This technique can be readily adapted to the detection of other analytes secreted by neural cells, which would have the potential to open new perspectives into human CNS development and dysfunction. We have established a technology that, for the first time, detects secreted analytes from single human neurons and astrocytes. We examine secretion of the Alzheimer's disease-relevant factors amyloid β (Aβ) and soluble amyloid precursor protein-alpha (sAPPα) and present novel findings that could not have been observed without a single-cell analytical platform. First, we identify a previously unappreciated subpopulation that secretes high levels of Aβ in the absence of detectable sAPPα. Further, we show that multiple cell types secrete high levels of Aβ and sAPPα, but cells expressing GABAergic neuronal markers are overrepresented. Finally, we show that astrocytes are competent to secrete high levels of Aβ and therefore may be a significant contributor to Aβ accumulation in the brain. Copyright © 2016 the authors 0270-6474/16/361730-17$15.00/0.

Analysis of polyphosphates in fish and shrimps tissues by two different ion chromatography methods: implications on false-negative and -positive findings.

PubMed

Kaufmann, A; Maden, K; Leisser, W; Matera, M; Gude, T

2005-11-01

Inorganic polyphosphates (di-, tri- and higher polyphosphates) can be used to treat fish, fish fillets and shrimps in order to improve their water-binding capacity. The practical relevance of this treatment is a significant gain of weight caused by the retention/uptake of water and natural juice into the fish tissues. This practice is legal; however, the use of phosphates has to be declared. The routine control testing of fish for the presence of polyphosphates, produced some results that were difficult to explain. One of the two analytical methods used determined low diphosphate concentrations in a number of untreated samples, while the other ion chromatography (IC) method did not detect them. This initiated a number of investigations: results showed that polyphosphates in fish and shrimps tissue undergo a rapid enzymatic degradation, producing the ubiquitous orthophosphate. This led to the conclusion that sensitive analytical methods are required in order to detect previous polyphosphate treatment of a sample. The polyphosphate concentrations detected by one of the analytical methods could not be explained by the degradation of endogenous high-energy nucleotides like ATP into diphosphate, but by a coeluting compound. Further investigations by LC-MS-MS proved that the substance responsible for the observed peak was inosine monophsosphate (IMP) and not as thought the inorganic diphosphate. The method producing the false-positive result was modified and both methods were ultimately able to detect polyphosphates well separated from natural nucleotides. Polyphosphates could no longer be detected (<0.5 mg kg-1) after modification of the analytical methodology. The relevance of these findings lies in the fact that similar analytical methods are employed in various control laboratories, which might lead to false interpretation of measurements.

Liquid chromatography method to determine polyamines in thermosetting polymers.

PubMed

Dopico-García, M S; López-Vilariño, J M; Fernández-Martínez, G; González-Rodríguez, M V

2010-05-14

A simple, robust and sensitive analytical method to determine three polyamines commonly used as hardeners in epoxy resin systems and in the manufacture of polyurethane is reported. The studied polyamines are: one tetramine, TETA (triethylenetetramine), and two diamines, IPDA (Isophorone diamine) and TCD-diamine (4,7-methano-1H-indene-5,?-dimethanamine, octahydro-). The latter has an incompletely defined structure, and, as far as we know, has not been previously determined by other methods. All three polyamines contain primary amines; TETA also contains secondary amines. The analytical method involves derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, used for the first time for these compounds, followed by high performance liquid chromatography (HPLC) analysis with a fluorescence (FL) detector (lambda excitation 248nm, lambda emision 395nm). The HPLC-DAD-LTQ Orbitrap MS was used in order to provide structural information about the obtained derivatized compounds. The hybrid linear ion trap LTQ Orbitrap mass spectrometer has been introduced in recent years and provides a high mass accuracy. The structures of the derivatized analytes were identified from the protonated molecular ions [M+H](+) and corresponded to the fully labelled analytes. The following analytical parameters were determined for the method using the HPLC-FL: linearity, precision (2.5-10%), instrumental precision intraday (0.8-1.5%) and interday (2.9-6.3%), and detection limits (0.02-0.14mgL(-1)). The stability of stock solutions and derivatized compounds was also investigated. The method was applied to determine the amine free content in epoxy resin dust collected in workplaces. Copyright 2010 Elsevier B.V. All rights reserved.

Targeted proteomic assays for quantitation of proteins identified by proteogenomic analysis of ovarian cancer

DOE PAGES

Song, Ehwang; Gao, Yuqian; Wu, Chaochao; ...

2017-07-19

Here, mass spectrometry (MS) based targeted proteomic methods such as selected reaction monitoring (SRM) are becoming the method of choice for preclinical verification of candidate protein biomarkers. The Clinical Proteomic Tumor Analysis Consortium (CPTAC) of the National Cancer Institute has investigated the standardization and analytical validation of the SRM assays and demonstrated robust analytical performance on different instruments across different laboratories. An Assay Portal has also been established by CPTAC to provide the research community a resource consisting of large set of targeted MS-based assays, and a depository to share assays publicly, providing that assays meet the guidelines proposed bymore » CPTAC. Herein, we report 98 SRM assays covering 70 candidate protein biomarkers previously reported as associated with ovarian cancer that have been thoroughly characterized according to the CPTAC Assay Characterization Guidance Document. The experiments, methods and results for characterizing these SRM assays for their MS response, repeatability, selectivity, stability, and reproducible detection of endogenous analytes are described in detail.« less

A method of extracting speed-dependent vector correlations from 2 + 1 REMPI ion images.

PubMed

Wei, Wei; Wallace, Colin J; Grubb, Michael P; North, Simon W

2017-07-07

We present analytical expressions for extracting Dixon's bipolar moments in the semi-classical limit from experimental anisotropy parameters of sliced or reconstructed non-sliced images. The current method focuses on images generated by 2 + 1 REMPI (Resonance Enhanced Multi-photon Ionization) and is a necessary extension of our previously published 1 + 1 REMPI equations. Two approaches for applying the new equations, direct inversion and forward convolution, are presented. As demonstration of the new method, bipolar moments were extracted from images of carbonyl sulfide (OCS) photodissociation at 230 nm and NO 2 photodissociation at 355 nm, and the results are consistent with previous publications.

Improving LC-MS sensitivity through increases in chromatographic performance: comparisons of UPLC-ES/MS/MS to HPLC-ES/MS/MS.

PubMed

Churchwell, Mona I; Twaddle, Nathan C; Meeker, Larry R; Doerge, Daniel R

2005-10-25

Recent technological advances have made available reverse phase chromatographic media with a 1.7 microm particle size along with a liquid handling system that can operate such columns at much higher pressures. This technology, termed ultra performance liquid chromatography (UPLC), offers significant theoretical advantages in resolution, speed, and sensitivity for analytical determinations, particularly when coupled with mass spectrometers capable of high-speed acquisitions. This paper explores the differences in LC-MS performance by conducting a side-by-side comparison of UPLC for several methods previously optimized for HPLC-based separation and quantification of multiple analytes with maximum throughput. In general, UPLC produced significant improvements in method sensitivity, speed, and resolution. Sensitivity increases with UPLC, which were found to be analyte-dependent, were as large as 10-fold and improvements in method speed were as large as 5-fold under conditions of comparable peak separations. Improvements in chromatographic resolution with UPLC were apparent from generally narrower peak widths and from a separation of diastereomers not possible using HPLC. Overall, the improvements in LC-MS method sensitivity, speed, and resolution provided by UPLC show that further advances can be made in analytical methodology to add significant value to hypothesis-driven research.

Bioanalytical Applications of Fluorescence Line-Narrowing and Non-Line-Narrowing Spectroscopy Interfaced with Capillary Electrophoresis and High-Performance Liquid Chromatography

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

Roberts, Kenneth Paul

Capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC) are widely used analytical separation techniques with many applications in chemical, biochemical, and biomedical sciences. Conventional analyte identification in these techniques is based on retention/migration times of standards; requiring a high degree of reproducibility, availability of reliable standards, and absence of coelution. From this, several new information-rich detection methods (also known as hyphenated techniques) are being explored that would be capable of providing unambiguous on-line identification of separating analytes in CE and HPLC. As further discussed, a number of such on-line detection methods have shown considerable success, including Raman, nuclear magnetic resonancemore » (NMR), mass spectrometry (MS), and fluorescence line-narrowing spectroscopy (FLNS). In this thesis, the feasibility and potential of combining the highly sensitive and selective laser-based detection method of FLNS with analytical separation techniques are discussed and presented. A summary of previously demonstrated FLNS detection interfaced with chromatography and electrophoresis is given, and recent results from on-line FLNS detection in CE (CE-FLNS), and the new combination of HPLC-FLNS, are shown.« less

Drift-Free Position Estimation of Periodic or Quasi-Periodic Motion Using Inertial Sensors

PubMed Central

Latt, Win Tun; Veluvolu, Kalyana Chakravarthy; Ang, Wei Tech

2011-01-01

Position sensing with inertial sensors such as accelerometers and gyroscopes usually requires other aided sensors or prior knowledge of motion characteristics to remove position drift resulting from integration of acceleration or velocity so as to obtain accurate position estimation. A method based on analytical integration has previously been developed to obtain accurate position estimate of periodic or quasi-periodic motion from inertial sensors using prior knowledge of the motion but without using aided sensors. In this paper, a new method is proposed which employs linear filtering stage coupled with adaptive filtering stage to remove drift and attenuation. The prior knowledge of the motion the proposed method requires is only approximate band of frequencies of the motion. Existing adaptive filtering methods based on Fourier series such as weighted-frequency Fourier linear combiner (WFLC), and band-limited multiple Fourier linear combiner (BMFLC) are modified to combine with the proposed method. To validate and compare the performance of the proposed method with the method based on analytical integration, simulation study is performed using periodic signals as well as real physiological tremor data, and real-time experiments are conducted using an ADXL-203 accelerometer. Results demonstrate that the performance of the proposed method outperforms the existing analytical integration method. PMID:22163935

Verification of spatial and temporal pressure distributions in segmented solid rocket motors

NASA Technical Reports Server (NTRS)

Salita, Mark

1989-01-01

A wide variety of analytical tools are in use today to predict the history and spatial distributions of pressure in the combustion chambers of solid rocket motors (SRMs). Experimental and analytical methods are presented here that allow the verification of many of these predictions. These methods are applied to the redesigned space shuttle booster (RSRM). Girth strain-gage data is compared to the predictions of various one-dimensional quasisteady analyses in order to verify the axial drop in motor static pressure during ignition transients as well as quasisteady motor operation. The results of previous modeling of radial flows in the bore, slots, and around grain overhangs are supported by approximate analytical and empirical techniques presented here. The predictions of circumferential flows induced by inhibitor asymmetries, nozzle vectoring, and propellant slump are compared to each other and to subscale cold air and water tunnel measurements to ascertain their validity.

Developments in mycotoxin analysis: an update for 2013 – 2014

USDA-ARS?s Scientific Manuscript database

This review highlights developments in the determination of mycotoxins over a period between mid-2013 and mid-2014. It continues in the format of the previous articles of this series, emphasising on analytical methods to determine aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxi...

Reagentless, Structure-Switching, Electrochemical Aptamer-Based Sensors

NASA Astrophysics Data System (ADS)

Schoukroun-Barnes, Lauren R.; Macazo, Florika C.; Gutierrez, Brenda; Lottermoser, Justine; Liu, Juan; White, Ryan J.

2016-06-01

The development of structure-switching, electrochemical, aptamer-based sensors over the past ˜10 years has led to a variety of reagentless sensors capable of analytical detection in a range of sample matrices. The crux of this methodology is the coupling of target-induced conformation changes of a redox-labeled aptamer with electrochemical detection of the resulting altered charge transfer rate between the redox molecule and electrode surface. Using aptamer recognition expands the highly sensitive detection ability of electrochemistry to a range of previously inaccessible analytes. In this review, we focus on the methods of sensor fabrication and how sensor signaling is affected by fabrication parameters. We then discuss recent studies addressing the fundamentals of sensor signaling as well as quantitative characterization of the analytical performance of electrochemical aptamer-based sensors. Although the limits of detection of reported electrochemical aptamer-based sensors do not often reach that of gold-standard methods such as enzyme-linked immunosorbent assays, the operational convenience of the sensor platform enables exciting analytical applications that we address. Using illustrative examples, we highlight recent advances in the field that impact important areas of analytical chemistry. Finally, we discuss the challenges and prospects for this class of sensors.

Evaluation of generalized degrees of freedom for sparse estimation by replica method

NASA Astrophysics Data System (ADS)

Sakata, A.

2016-12-01

We develop a method to evaluate the generalized degrees of freedom (GDF) for linear regression with sparse regularization. The GDF is a key factor in model selection, and thus its evaluation is useful in many modelling applications. An analytical expression for the GDF is derived using the replica method in the large-system-size limit with random Gaussian predictors. The resulting formula has a universal form that is independent of the type of regularization, providing us with a simple interpretation. Within the framework of replica symmetric (RS) analysis, GDF has a physical meaning as the effective fraction of non-zero components. The validity of our method in the RS phase is supported by the consistency of our results with previous mathematical results. The analytical results in the RS phase are calculated numerically using the belief propagation algorithm.

Modeling and Analysis of Large Amplitude Flight Maneuvers

NASA Technical Reports Server (NTRS)

Anderson, Mark R.

2004-01-01

Analytical methods for stability analysis of large amplitude aircraft motion have been slow to develop because many nonlinear system stability assessment methods are restricted to a state-space dimension of less than three. The proffered approach is to create regional cell-to-cell maps for strategically located two-dimensional subspaces within the higher-dimensional model statespace. These regional solutions capture nonlinear behavior better than linearized point solutions. They also avoid the computational difficulties that emerge when attempting to create a cell map for the entire state-space. Example stability results are presented for a general aviation aircraft and a micro-aerial vehicle configuration. The analytical results are consistent with characteristics that were discovered during previous flight-testing.

A study of cell electrophoresis as a means of purifying growth hormone secreting cells

NASA Technical Reports Server (NTRS)

Plank, Lindsay D.; Hymer, W. C.; Kunze, M. Elaine; Marks, Gary M.; Lanham, J. Wayne

1983-01-01

Growth hormone secreting cells of the rat anterior pituitary are heavily laden with granules of growth hormone and can be partialy purified on the basis of their resulting high density. Two methods of preparative cell electrophoresis were investigated as methods of enhancing the purification of growth hormone producing cells: density gradient electrophoresis and continuous flow electrophoresis. Both methods provided a two- to four-fold enrichment in growth hormone production per cell relative to that achieved by previous methods. Measurements of electrophoretic mobilities by two analytical methods, microscopic electrophoresis and laser-tracking electrophoresis, revealed very little distinction between unpurified anterior pituitary cell suspensions and somatotroph-enriched cell suspensions. Predictions calculated on the basis of analytical electrophoretic data are consistent with the hypothesis that sedimentation plays a significant role in both types of preparative electrophoresis and the electrophoretic mobility of the growth hormone secreting subpopulation of cells remains unknown.

The Rack-Gear Tool Generation Modelling. Non-Analytical Method Developed in CATIA, Using the Relative Generating Trajectories Method

NASA Astrophysics Data System (ADS)

Teodor, V. G.; Baroiu, N.; Susac, F.; Oancea, N.

2016-11-01

The modelling of a curl of surfaces associated with a pair of rolling centrodes, when it is known the profile of the rack-gear's teeth profile, by direct measuring, as a coordinate matrix, has as goal the determining of the generating quality for an imposed kinematics of the relative motion of tool regarding the blank. In this way, it is possible to determine the generating geometrical error, as a base of the total error. The generation modelling allows highlighting the potential errors of the generating tool, in order to correct its profile, previously to use the tool in machining process. A method developed in CATIA is proposed, based on a new method, namely the method of “relative generating trajectories”. They are presented the analytical foundation, as so as some application for knows models of rack-gear type tools used on Maag teething machines.

Hybrid perturbation methods based on statistical time series models

NASA Astrophysics Data System (ADS)

San-Juan, Juan Félix; San-Martín, Montserrat; Pérez, Iván; López, Rosario

2016-04-01

In this work we present a new methodology for orbit propagation, the hybrid perturbation theory, based on the combination of an integration method and a prediction technique. The former, which can be a numerical, analytical or semianalytical theory, generates an initial approximation that contains some inaccuracies derived from the fact that, in order to simplify the expressions and subsequent computations, not all the involved forces are taken into account and only low-order terms are considered, not to mention the fact that mathematical models of perturbations not always reproduce physical phenomena with absolute precision. The prediction technique, which can be based on either statistical time series models or computational intelligence methods, is aimed at modelling and reproducing missing dynamics in the previously integrated approximation. This combination results in the precision improvement of conventional numerical, analytical and semianalytical theories for determining the position and velocity of any artificial satellite or space debris object. In order to validate this methodology, we present a family of three hybrid orbit propagators formed by the combination of three different orders of approximation of an analytical theory and a statistical time series model, and analyse their capability to process the effect produced by the flattening of the Earth. The three considered analytical components are the integration of the Kepler problem, a first-order and a second-order analytical theories, whereas the prediction technique is the same in the three cases, namely an additive Holt-Winters method.

Complex formation of vanadium(V) with resorcylalhydrazides of carboxylic acids

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

Dudarev, V.I.; Dolgorev, V.A.; Volkov, A.N.

1986-08-01

In this work, a previous investigation of hydrazine derivatives as analytical reagents for vanadium(V) was continued. The authors studied arylalhydrazones -- derivatives of resorcylalhydrazides of anisic (RHASA), anthranilic (RHANA), and benzoic (RHBA) acids. The reagents presented differ from those studied previously by the presence of a second hydroxy group in the para-position of the benzene ring -the resorcinol fragment -- and substituents in the benzoin fragment. Such changes made it possible to increase the solubility of the reagents in aqueous medium and to estimate the change in the main spectrophotometric parameters of the analytical reaction. A rapid method was developedmore » for the determination of vanadium in steels with the resorcylalhydrazide of anthranilic acid. The minimum determinable vanadium content is 0.18 micrograms/ml.« less

A SIMPLE, EFFICIENT SOLUTION OF FLUX-PROFILE RELATIONSHIPS IN THE ATMOSPHERIC SURFACE LAYER

EPA Science Inventory

This note describes a simple scheme for analytical estimation of the surface layer similarity functions from state variables. What distinguishes this note from the many previous papers on this topic is that this method is specifically targeted for numerical models where simplici...

Sonic horizon formation for oscillating Bose-Einstein condensates in isotropic harmonic potential

PubMed Central

Wang, Ying; Zhou, Yu; Zhou, Shuyu

2016-01-01

We study the sonic horizon phenomena of the oscillating Bose-Einstein condensates in isotropic harmonic potential. Based on the Gross-Pitaevskii equation model and variational method, we derive the original analytical formula for the criteria and lifetime of the formation of the sonic horizon, demonstrating pictorially the interaction parameter dependence for the occur- rence of the sonic horizon and damping effect of the system distribution width. Our analytical results corroborate quantitatively the particular features of the sonic horizon reported in previous numerical study. PMID:27922129

High Rayleigh number convection in rectangular enclosures with differentially heated vertical walls and aspect ratios between zero and unity

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

Kassemi, S.A.

1988-04-01

High Rayleigh number convection in a rectangular cavity with insulated horizontal surfaces and differentially heated vertical walls was analyzed for an arbitrary aspect ratio smaller than or equal to unity. Unlike previous analytical studies, a systematic method of solution based on linearization technique and analytical iteration procedure was developed to obtain approximate closed-form solutions for a wide range of aspect ratios. The predicted velocity and temperature fields are shown to be in excellent agreement with available experimental and numerical data.

High Rayleigh number convection in rectangular enclosures with differentially heated vertical walls and aspect ratios between zero and unity

NASA Technical Reports Server (NTRS)

Kassemi, Siavash A.

1988-01-01

High Rayleigh number convection in a rectangular cavity with insulated horizontal surfaces and differentially heated vertical walls was analyzed for an arbitrary aspect ratio smaller than or equal to unity. Unlike previous analytical studies, a systematic method of solution based on linearization technique and analytical iteration procedure was developed to obtain approximate closed-form solutions for a wide range of aspect ratios. The predicted velocity and temperature fields are shown to be in excellent agreement with available experimental and numerical data.

Space vehicle engine and heat shield environment review. Volume 1: Engineering analysis

NASA Technical Reports Server (NTRS)

Mcanelly, W. B.; Young, C. T. K.

1973-01-01

Methods for predicting the base heating characteristics of a multiple rocket engine installation are discussed. The environmental data is applied to the design of adequate protection system for the engine components. The methods for predicting the base region thermal environment are categorized as: (1) scale model testing, (2) extrapolation of previous and related flight test results, and (3) semiempirical analytical techniques.

A rapid miniaturized residue analytical method for the determination of zoxamide and its two acid metabolites in ginseng roots using UPLC-MS/MS.

PubMed

Podhorniak, Lynda V

2014-04-30

A miniaturized residue method was developed for the analysis of the fungicide zoxamide and its metabolites in dried ginseng root. The zoxamide metabolites, 3,5-dichloro-1,4-benzenedicarboxylic acid (DCBC) and 3,5-dichloro-4-hydroxymethylbenzoic acid (DCHB), are small acid molecules that have not been previously extracted from the ginseng matrix with common multiresidue methods. The presented extraction method effectively and rapidly recovers both the zoxamide parent compound and its acid metabolites from fortified ginseng root. The metabolites are extracted with an alkaline glycine buffer and the aqueous ginseng mixture is partitioned with ethyl acetate. In addition, this method avoids the use of derivatization of the small acid molecules by using UPLC-MS/MS instrumental analysis. In a quantitative validation of the analytical method at three levels for zoxamide (0.007 (LOD), 0.02 (LOQ), and 0.2 mg/kg) and four levels (0.07 (LOD), 0.2 (LOQ), and 0.6 and 6 mg/kg) for both metabolites, acceptable method performances were achieved with recoveries ranging from 86 to 107% (at levels of LOQ and 3×, 10×, and 30× the LOQ) with <20% RSD for the three analytes in accordance with international guidelines.1.

Identification of Balanced Chromosomal Rearrangements Previously Unknown Among Participants in the 1000 Genomes Project: Implications for Interpretation of Structural Variation in Genomes and the Future of Clinical Cytogenetics

PubMed Central

Dong, Zirui; Wang, Huilin; Chen, Haixiao; Jiang, Hui; Yuan, Jianying; Yang, Zhenjun; Wang, Wen-Jing; Xu, Fengping; Guo, Xiaosen; Cao, Ye; Zhu, Zhenzhen; Geng, Chunyu; Cheung, Wan Chee; Kwok, Yvonne K; Yang, Huangming; Leung, Tak Yeung; Morton, Cynthia C.; Cheung, Sau Wai; Choy, Kwong Wai

2017-01-01

Purpose Recent studies demonstrate that whole-genome sequencing (WGS) enables detection of cryptic rearrangements in apparently balanced chromosomal rearrangements (also known as balanced chromosomal abnormalities, BCAs) previously identified by conventional cytogenetic methods. We aimed to assess our analytical tool for detecting BCAs in The 1000 Genomes Project without knowing affected bands. Methods The 1000 Genomes Project provides an unprecedented integrated map of structural variants in phenotypically normal subjects, but there is no information on potential inclusion of subjects with apparently BCAs akin to those traditionally detected in diagnostic cytogenetics laboratories. We applied our analytical tool to 1,166 genomes from the 1000 Genomes Project with sufficient physical coverage (8.25-fold). Results Our approach detected four reciprocal balanced translocations and four inversions ranging in size from 57.9 kb to 13.3 Mb, all of which were confirmed by cytogenetic methods and PCR studies. One of DNAs has a subtle translocation that is not readily identified by chromosome analysis due to similar banding patterns and size of exchanged segments, and another results in disruption of all transcripts of an OMIM gene. Conclusions Our study demonstrates the extension of utilizing low-coverage WGS for unbiased detection of BCAs including translocations and inversions previously unknown in the 1000 Genomes Project. PMID:29095815

Laboratory Investigations Of Mechanisms For 1,4-Dioxane Destruction By Ozone In Water (Presentation)

EPA Science Inventory

Advances in analytical detection methods have made it possible to quantify 1,4-dioxane contamination in groundwater, even a well-characterized sites where it had not been previously detected. Although 1,4-dioxane is difficult to treat because of its chemical and physical propert...

Classical Civilization (Greece-Hellenistic-Rome). Teacher's Manual. 1968 Edition.

ERIC Educational Resources Information Center

Leppert, Ella C.; Smith, Rozella B.

This secondary teachers guide builds upon a previous sequential course described in SO 003 173, and consists of three sections on the classical civilizations--Greek, Hellenistic, and Rome. Major emphasis is upon students gaining an understanding of cultural development and transmission. Using an analytic method, students learn to examine primary…

Laboratory Investigation Of Mechanisms For 1,4-Dioxane Destruction By Ozone In Water

EPA Science Inventory

Advances in analytical detection methods have made it possible to quantify 1,4-dioxane contamination in groundwater, even at well-characterized sites where it had not been previously detected. Although 1,4-dioxane is difficult to treat because of its chemical and physical proper...

Extending existing structural identifiability analysis methods to mixed-effects models.

PubMed

Janzén, David L I; Jirstrand, Mats; Chappell, Michael J; Evans, Neil D

2018-01-01

The concept of structural identifiability for state-space models is expanded to cover mixed-effects state-space models. Two methods applicable for the analytical study of the structural identifiability of mixed-effects models are presented. The two methods are based on previously established techniques for non-mixed-effects models; namely the Taylor series expansion and the input-output form approach. By generating an exhaustive summary, and by assuming an infinite number of subjects, functions of random variables can be derived which in turn determine the distribution of the system's observation function(s). By considering the uniqueness of the analytical statistical moments of the derived functions of the random variables, the structural identifiability of the corresponding mixed-effects model can be determined. The two methods are applied to a set of examples of mixed-effects models to illustrate how they work in practice. Copyright © 2017 Elsevier Inc. All rights reserved.

Quantitative 1H NMR: Development and Potential of an Analytical Method – an Update

PubMed Central

Pauli, Guido F.; Gödecke, Tanja; Jaki, Birgit U.; Lankin, David C.

2012-01-01

Covering the literature from mid-2004 until the end of 2011, this review continues a previous literature overview on quantitative 1H NMR (qHNMR) methodology and its applications in the analysis of natural products (NPs). Among the foremost advantages of qHNMR is its accurate function with external calibration, the lack of any requirement for identical reference materials, a high precision and accuracy when properly validated, and an ability to quantitate multiple analytes simultaneously. As a result of the inclusion of over 170 new references, this updated review summarizes a wealth of detailed experiential evidence and newly developed methodology that supports qHNMR as a valuable and unbiased analytical tool for natural product and other areas of research. PMID:22482996

Analytical difficulties facing today's regulatory laboratories: issues in method validation.

PubMed

MacNeil, James D

2012-08-01

The challenges facing analytical laboratories today are not unlike those faced in the past, although both the degree of complexity and the rate of change have increased. Challenges such as development and maintenance of expertise, maintenance and up-dating of equipment, and the introduction of new test methods have always been familiar themes for analytical laboratories, but international guidelines for laboratories involved in the import and export testing of food require management of such changes in a context which includes quality assurance, accreditation, and method validation considerations. Decisions as to when a change in a method requires re-validation of the method or on the design of a validation scheme for a complex multi-residue method require a well-considered strategy, based on a current knowledge of international guidance documents and regulatory requirements, as well the laboratory's quality system requirements. Validation demonstrates that a method is 'fit for purpose', so the requirement for validation should be assessed in terms of the intended use of a method and, in the case of change or modification of a method, whether that change or modification may affect a previously validated performance characteristic. In general, method validation involves method scope, calibration-related parameters, method precision, and recovery. Any method change which may affect method scope or any performance parameters will require re-validation. Some typical situations involving change in methods are discussed and a decision process proposed for selection of appropriate validation measures. © 2012 John Wiley & Sons, Ltd.

Not All Biofluids Are Created Equal: Chewing Over Salivary Diagnostics and the Epigenome

PubMed Central

Wren, M.E.; Shirtcliff, E.A.; Drury, Stacy S.

2015-01-01

Purpose This article describes progress to date in the characterization of the salivary epigenome and considers the importance of previous work in the salivary microbiome, proteome, endocrine analytes, genome, and transcriptome. Methods PubMed and Web of Science were used to extensively search the existing literature (original research and reviews) related to salivary diagnostics and bio-marker development, of which 125 studies were examined. This article was derived from the most relevant 73 sources highlighting the recent state of the evolving field of salivary epigenomics and contributing significantly to the foundational work in saliva-based research. Findings Validation of any new saliva-based diagnostic or analyte will require comparison to previously accepted standards established in blood. Careful attention to the collection, processing, and analysis of salivary analytes is critical for the development and implementation of newer applications that include genomic, transcriptomic, and epigenomic markers. All these factors must be integrated into initial study design. Implications This commentary highlights the appeal of the salivary epigenome for translational applications and its utility in future studies of development and the interface among environment, disease, and health. PMID:25778408

A microfluidic paper-based analytical device for the assay of albumin-corrected fructosamine values from whole blood samples.

PubMed

Boonyasit, Yuwadee; Laiwattanapaisal, Wanida

2015-01-01

A method for acquiring albumin-corrected fructosamine values from whole blood using a microfluidic paper-based analytical system that offers substantial improvement over previous methods is proposed. The time required to quantify both serum albumin and fructosamine is shortened to 10 min with detection limits of 0.50 g dl(-1) and 0.58 mM, respectively (S/N = 3). The proposed system also exhibited good within-run and run-to-run reproducibility. The results of the interference study revealed that the acceptable recoveries ranged from 95.1 to 106.2%. The system was compared with currently used large-scale methods (n = 15), and the results demonstrated good agreement among the techniques. The microfluidic paper-based system has the potential to continuously monitor glycemic levels in low resource settings.

Spectrophotometric determination of sulphate in automotive fuel ethanol by sequential injection analysis using dimethylsulphonazo(III) reaction.

PubMed

de Oliveira, Fabio Santos; Korn, Mauro

2006-01-15

A sensitive SIA method was developed for sulphate determination in automotive fuel ethanol. This method was based on the reaction of sulphate with barium-dimethylsulphonazo(III) leading to a decrease on the magnitude of analytical signal monitored at 665 nm. Alcohol fuel samples were previously burned up to avoid matrix effects for sulphate determinations. Binary sampling and stop-flow strategies were used to increase the sensitivity of the method. The optimization of analytical parameter was performed by response surface method using Box-Behnker and central composite designs. The proposed sequential flow procedure permits to determine up to 10.0mg SO(4)(2-)l(-1) with R.S.D. <2.5% and limit of detection of 0.27 mg l(-1). The method has been successfully applied for sulphate determination in automotive fuel alcohol and the results agreed with the reference volumetric method. In the optimized condition the SIA system carried out 27 samples per hour.

Structural response synthesis

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

Ozisik, H.; Keltie, R.F.

The open loop control technique of predicting a conditioned input signal based on a specified output response for a second order system has been analyzed both analytically and numerically to gain a firm understanding of the method. Differences between this method of control and digital closed loop control using pole cancellation were investigated as a follow up to previous experimental work. Application of the technique to diamond turning using a fast tool is also discussed.

Numerical evaluation of electromagnetic fields due to dipole antennas in the presence of stratified media

NASA Technical Reports Server (NTRS)

Tsang, L.; Brown, R.; Kong, J. A.; Simmons, G.

1974-01-01

Two numerical methods are used to evaluate the integrals that express the em fields due to dipole antennas radiating in the presence of a stratified medium. The first method is a direct integration by means of Simpson's rule. The second method is indirect and approximates the kernel of the integral by means of the fast Fourier transform. In contrast to previous analytical methods that applied only to two-layer cases the numerical methods can be used for any arbitrary number of layers with general properties.

Validation of a method to detect cocaine and its metabolites in nails by gas chromatography-mass spectrometry.

PubMed

Valente-Campos, Simone; Yonamine, Mauricio; de Moraes Moreau, Regina Lucia; Silva, Ovandir Alves

2006-06-02

The objective of the present work was to compare previously published methods and provide validation data to detect simultaneously cocaine (COC), benzoylecgonine (BE) and norcocaine (NCOC) in nail. Finger and toenail samples (5mg) were cut in very small pieces and submitted to an initial procedure for external decontamination. Methanol (3 ml) was used to release analytes from the matrix. A cleanup step was performed simultaneously by solid-phase extraction (SPE) and the residue was derivatized with pentafluoropropionic anhydride/pentafluoropropanol (PFPA/PFP). Gas chromatography-mass spectrometry (GC-MS) was used to detect the analytes in selected ion monitoring mode (SIM). Confidence parameters of validation of the method were: recovery, intra- and inter-assay precision, as well as limit of detection (LOD) of the analytes. The limits of detection were: 3.5 ng/mg for NCOC and 3.0 ng/mg for COC and BE. Good intra-assay precision was observed for all detected substances (coefficient of variation (CV)<11%). The inter-assay precision for norcocaine and benzoylecgonine were <4%. For intra- and inter-assay precision deuterated internal standards were used. Toenail and fingernail samples from eight declared cocaine users were submitted to the validated method.

Structure Shapes Dynamics and Directionality in Diverse Brain Networks: Mathematical Principles and Empirical Confirmation in Three Species

NASA Astrophysics Data System (ADS)

Moon, Joon-Young; Kim, Junhyeok; Ko, Tae-Wook; Kim, Minkyung; Iturria-Medina, Yasser; Choi, Jee-Hyun; Lee, Joseph; Mashour, George A.; Lee, Uncheol

2017-04-01

Identifying how spatially distributed information becomes integrated in the brain is essential to understanding higher cognitive functions. Previous computational and empirical studies suggest a significant influence of brain network structure on brain network function. However, there have been few analytical approaches to explain the role of network structure in shaping regional activities and directionality patterns. In this study, analytical methods are applied to a coupled oscillator model implemented in inhomogeneous networks. We first derive a mathematical principle that explains the emergence of directionality from the underlying brain network structure. We then apply the analytical methods to the anatomical brain networks of human, macaque, and mouse, successfully predicting simulation and empirical electroencephalographic data. The results demonstrate that the global directionality patterns in resting state brain networks can be predicted solely by their unique network structures. This study forms a foundation for a more comprehensive understanding of how neural information is directed and integrated in complex brain networks.

Detection of Pesticides and Pesticide Metabolites Using the Cross Reactivity of Enzyme Immunoassays

USGS Publications Warehouse

Thurman, E.M.; Aga, D.S.

2001-01-01

Enzyme immunoassay is an important environmental analysis method that may be used to identify many pesticide analytes in water samples. Because of similarities in chemical structure between various members of a pesticide class, there often may be an unwanted response that is characterized by a percentage of cross reactivity. Also, there may be cross reactivity caused by degradation products of the target analyte that may be present in the sample. In this paper, the concept of cross reactivity caused by degradation products or by nontarget analytes is explored as a tool for identification of metabolites or structurally similar compounds not previously known to be present in water samples. Two examples are examined in this paper from various water quality studies. They are alachlor and its metabolite, alachlor ethane sulfonic acid, and atrazine and its class members, prometryn and propazine. A method for using cross reactivity for the detection of these compounds is explained in this paper.

Ethinylestradiol and levonorgestrel preparations on the Belgian market: a comparative study.

PubMed

Vanheusden, V; De Braekeleer, K; Corthout, J

2012-03-01

Preparations formulated as coated or film-coated tablets, containing levonorgestrel and the combination ethinylestradiol/levonorgestrel, were evaluated in a comparative study. This study comprised in vitro dissolution, assay and content uniformity. The analytical methods were previously validated according to international guidelines. All examined products complied with the postulated requirements.

Analytical alternatives for an annual inventory system

Treesearch

Francis A. Roesch; Gregory A. Reams

1999-01-01

Methods for analyzing data from the Southern Annual Forest Inventory System (SAFIS) are discussed. Differences between the annual inventory approach and the more traditional periodic approach require that we revisit the previous assumption that there are no important spatial and temporal trends in the data. Over the next few years, the USDA Forest Service Southern...

Activity Theory in Information Systems Research and Practice: Theoretical Underpinnings for an Information Systems Development Model

ERIC Educational Resources Information Center

Mursu, Anja; Luukkonen, Irmeli; Toivanen, Marika; Korpela, Mikko

2007-01-01

Introduction: The purpose of information systems is to facilitate work activities: here we consider how Activity Theory can be applied in information systems development. Method. The requirements for an analytical model for emancipatory, work-oriented information systems research and practice are specified. Previous research work in Activity…

Development of an analytical method for the simultaneous analysis of MCPD esters and glycidyl esters in oil-based foodstuffs.

PubMed

Ermacora, Alessia; Hrnčiřík, Karel

2014-01-01

Substantial progress has been recently made in the development and optimisation of analytical methods for the quantification of 2-MCPD, 3-MCPD and glycidyl esters in oils and fats, and there are a few methods currently available that allow a reliable quantification of these contaminants in bulk oils and fats. On the other hand, no standard method for the analysis of foodstuffs has yet been established. The aim of this study was the development and validation of a new method for the simultaneous quantification of 2-MCPD, 3-MCPD and glycidyl esters in oil-based food products. The developed protocol includes a first step of liquid-liquid extraction and purification of the lipophilic substances of the sample, followed by the application of a previously developed procedure based on acid transesterification, for the indirect quantification of these contaminants in oils and fats. The method validation was carried out on food products (fat-based spreads, creams, margarine, mayonnaise) manufactured in-house, in order to control the manufacturing process and account for any food matrix-analyte interactions (the sample spiking was carried out on the single components used for the formulations rather than the final products). The method showed good accuracy (the recoveries ranged from 97% to 106% for bound 3-MCPD and 2-MCPD and from 88% to 115% for bound glycidol) and sensitivity (the LOD was 0.04 and 0.05 mg kg(-1) for bound MCPD and glycidol, respectively). Repeatability and reproducibility were satisfactory (RSD below 2% and 5%, respectively) for all analytes. The levels of salts and surface-active compounds in the formulation were found to have no impact on the accuracy and the other parameters of the method.

Development of a dynamic headspace gas chromatography-mass spectrometry method for on-site analysis of sulfur mustard degradation products in sediments.

PubMed

Magnusson, R; Nordlander, T; Östin, A

2016-01-15

Sampling teams performing work at sea in areas where chemical munitions may have been dumped require rapid and reliable analytical methods for verifying sulfur mustard leakage from suspected objects. Here we present such an on-site analysis method based on dynamic headspace GC-MS for analysis of five cyclic sulfur mustard degradation products that have previously been detected in sediments from chemical weapon dumping sites: 1,4-oxathiane, 1,3-dithiolane, 1,4-dithiane, 1,4,5-oxadithiephane, and 1,2,5-trithiephane. An experimental design involving authentic Baltic Sea sediments spiked with the target analytes was used to develop an optimized protocol for sample preparation, headspace extraction and analysis that afforded recoveries of up to 60-90%. The optimized method needs no organic solvents, uses only two grams of sediment on a dry weight basis and involves a unique sample presentation whereby sediment is spread uniformly as a thin layer inside the walls of a glass headspace vial. The method showed good linearity for analyte concentrations of 5-200 ng/g dw, good repeatability, and acceptable carry-over. The method's limits of detection for spiked sediment samples ranged from 2.5 to 11 μg/kg dw, with matrix interference being the main limiting factor. The instrumental detection limits were one to two orders of magnitude lower. Full-scan GC-MS analysis enabled the use of automated mass spectral deconvolution for rapid identification of target analytes. Using this approach, analytes could be identified in spiked sediment samples at concentrations down to 13-65 μg/kg dw. On-site validation experiments conducted aboard the research vessel R/V Oceania demonstrated the method's practical applicability, enabling the successful identification of four cyclic sulfur mustard degradation products at concentrations of 15-308μg/kg in sediments immediately after being collected near a wreck at the Bornholm Deep dumpsite in the Baltic Sea. Copyright © 2015 Elsevier B.V. All rights reserved.

Validation of mega composite sampling and nationwide mass inventories for 26 previously unmonitored contaminants in archived biosolids from the U.S National Biosolids Repository

PubMed Central

Chari, Bipin P.; Halden, Rolf U.

2012-01-01

In the present study, archived U.S biosolids from the 2001 Environmental Protection Agency (EPA) National Sewage Sludge Survey were analyzed with an expanded U.S EPA Method 1694, to determine the occurrence of 26 previously unmonitored pharmaceuticals and personal care products (PPCPs) among a total of 120 analytes. The study further served to examine the reproducibility of a mega-composite approach for creating chemical mass inventories in biosolids based on pooled samples from wastewater treatment plants (WWTPs) nationwide. Five mega-composites reflecting 94 WWTPs in 32 states and the District of Columbia were constructed from archived biosolids and analyzed by LC/ESI-MS/MS using a newly introduced analytical method expanding upon U.S EPA Method 1694. In addition, soil-biosolids mixtures from a mesocosm setup were analyzed to experimentally determine the half-lives of biosolids-borne compounds applied on U.S land. Among 59 analytes detected, 33 had been reported previously, whereas 26 are reported in biosolids for the first time, at levels ranging from 1.65 to 673 μg kg−1 dry weight. Newly recognized biosolids constituents were identified as Ca2+ channel blockers, antidepressants, diuretics, β-blockers and analgesics. Using a mass balance approach, the total loading of these 26 pharmaceuticals to U.S soils from biosolids land application was estimated at 5–15 tons year−1. Past and present datasets for 30 pharmaceuticals and personal care products (PPCPs) were determined to be statistically indistinguishable (paired t-test; p = 0.01). This study expands the list of PPCPs reported in U.S biosolids, provides the first estimates of nationwide release rates to and environmental half-lives in U.S agricultural soils, and confirms the utility of using mega-composite sampling for economical tracking of chemical inventories in biosolids on a national scale. PMID:22789759

Helios: Understanding Solar Evolution Through Text Analytics

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

Randazzese, Lucien

This proof-of-concept project focused on developing, testing, and validating a range of bibliometric, text analytic, and machine-learning based methods to explore the evolution of three photovoltaic (PV) technologies: Cadmium Telluride (CdTe), Dye-Sensitized solar cells (DSSC), and Multi-junction solar cells. The analytical approach to the work was inspired by previous work by the same team to measure and predict the scientific prominence of terms and entities within specific research domains. The goal was to create tools that could assist domain-knowledgeable analysts in investigating the history and path of technological developments in general, with a focus on analyzing step-function changes in performance,more » or “breakthroughs,” in particular. The text-analytics platform developed during this project was dubbed Helios. The project relied on computational methods for analyzing large corpora of technical documents. For this project we ingested technical documents from the following sources into Helios: Thomson Scientific Web of Science (papers), the U.S. Patent & Trademark Office (patents), the U.S. Department of Energy (technical documents), the U.S. National Science Foundation (project funding summaries), and a hand curated set of full-text documents from Thomson Scientific and other sources.« less

PROPOSED SIAM PROBLEM

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

BAILEY, DAVID H.; BORWEIN, JONATHAN M.

A recent paper by the present authors, together with mathematical physicists David Broadhurst and M. Larry Glasser, explored Bessel moment integrals, namely definite integrals of the general form {integral}{sub 0}{sup {infinity}} t{sup m}f{sup n}(t) dt, where the function f(t) is one of the classical Bessel functions. In that paper, numerous previously unknown analytic evaluations were obtained, using a combination of analytic methods together with some fairly high-powered numerical computations, often performed on highly parallel computers. In several instances, while we were able to numerically discover what appears to be a solid analytic identity, based on extremely high-precision numerical computations, wemore » were unable to find a rigorous proof. Thus we present here a brief list of some of these unproven but numerically confirmed identities.« less

Tire Changes, Fresh Air, and Yellow Flags: Challenges in Predictive Analytics for Professional Racing.

PubMed

Tulabandhula, Theja; Rudin, Cynthia

2014-06-01

Our goal is to design a prediction and decision system for real-time use during a professional car race. In designing a knowledge discovery process for racing, we faced several challenges that were overcome only when domain knowledge of racing was carefully infused within statistical modeling techniques. In this article, we describe how we leveraged expert knowledge of the domain to produce a real-time decision system for tire changes within a race. Our forecasts have the potential to impact how racing teams can optimize strategy by making tire-change decisions to benefit their rank position. Our work significantly expands previous research on sports analytics, as it is the only work on analytical methods for within-race prediction and decision making for professional car racing.

Development of the Ion Exchange-Gravimetric Method for Sodium in Serum as a Definitive Method

PubMed Central

Moody, John R.; Vetter, Thomas W.

1996-01-01

An ion exchange-gravimetric method, previously developed as a National Committee for Clinical Laboratory Standards (NCCLS) reference method for the determination of sodium in human serum, has been re-evaluated and improved. Sources of analytical error in this method have been examined more critically and the overall uncertainties decreased. Additionally, greater accuracy and repeatability have been achieved by the application of this definitive method to a sodium chloride reference material. In this method sodium in serum is ion-exchanged, selectively eluted and converted to a weighable precipitate as Na2SO4. Traces of sodium eluting before or after the main fraction, and precipitate contaminants are determined instrumentally. Co-precipitating contaminants contribute less than 0.1 % while the analyte lost to other eluted ion-exchange fractions contributes less than 0.02 % to the total precipitate mass. With improvements, the relative expanded uncertainty (k = 2) of the method, as applied to serum, is 0.3 % to 0.4 % and is less than 0.1 % when applied to a sodium chloride reference material. PMID:27805122

Quantifying construction and demolition waste: An analytical review

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

Wu, Zezhou; Yu, Ann T.W., E-mail: bsannyu@polyu.edu.hk; Shen, Liyin

2014-09-15

Highlights: • Prevailing C and D waste quantification methodologies are identified and compared. • One specific methodology cannot fulfill all waste quantification scenarios. • A relevance tree for appropriate quantification methodology selection is proposed. • More attentions should be paid to civil and infrastructural works. • Classified information is suggested for making an effective waste management plan. - Abstract: Quantifying construction and demolition (C and D) waste generation is regarded as a prerequisite for the implementation of successful waste management. In literature, various methods have been employed to quantify the C and D waste generation at both regional and projectmore » levels. However, an integrated review that systemically describes and analyses all the existing methods has yet to be conducted. To bridge this research gap, an analytical review is conducted. Fifty-seven papers are retrieved based on a set of rigorous procedures. The characteristics of the selected papers are classified according to the following criteria - waste generation activity, estimation level and quantification methodology. Six categories of existing C and D waste quantification methodologies are identified, including site visit method, waste generation rate method, lifetime analysis method, classification system accumulation method, variables modelling method and other particular methods. A critical comparison of the identified methods is given according to their characteristics and implementation constraints. Moreover, a decision tree is proposed for aiding the selection of the most appropriate quantification method in different scenarios. Based on the analytical review, limitations of previous studies and recommendations of potential future research directions are further suggested.« less

Data analysis considerations for pesticides determined by National Water Quality Laboratory schedule 2437

USGS Publications Warehouse

Shoda, Megan E.; Nowell, Lisa H.; Stone, Wesley W.; Sandstrom, Mark W.; Bexfield, Laura M.

2018-04-02

In 2013, the U.S. Geological Survey National Water Quality Laboratory (NWQL) made a new method available for the analysis of pesticides in filtered water samples: laboratory schedule 2437. Schedule 2437 is an improvement on previous analytical methods because it determines the concentrations of 225 fungicides, herbicides, insecticides, and associated degradates in one method at similar or lower concentrations than previously available methods. Additionally, the pesticides included in schedule 2437 were strategically identified in a prioritization analysis that assessed likelihood of occurrence, prevalence of use, and potential toxicity. When the NWQL reports pesticide concentrations for analytes in schedule 2437, the laboratory also provides supplemental information useful to data users for assessing method performance and understanding data quality. That supplemental information is discussed in this report, along with an initial analysis of analytical recovery of pesticides in water-quality samples analyzed by schedule 2437 during 2013–2015. A total of 523 field matrix spike samples and their paired environmental samples and 277 laboratory reagent spike samples were analyzed for this report (1,323 samples total). These samples were collected in the field as part of the U.S. Geological Survey National Water-Quality Assessment groundwater and surface-water studies and as part of the NWQL quality-control program. This report reviews how pesticide samples are processed by the NWQL, addresses how to obtain all the data necessary to interpret pesticide concentrations, explains the circumstances that result in a reporting level change or the occurrence of a raised reporting level, and describes the calculation and assessment of recovery. This report also discusses reasons why a data user might choose to exclude data in an interpretive analysis and outlines the approach used to identify the potential for decreased data quality in the assessment of method recovery. The information provided in this report is essential to understanding pesticide data determined by schedule 2437 and should be reviewed before interpretation of these data.

Boundary Electron and Beta Dosimetry-Quantification of the Effects of Dissimilar Media on Absorbed Dose

NASA Astrophysics Data System (ADS)

Nunes, Josane C.

1991-02-01

This work quantifies the changes effected in electron absorbed dose to a soft-tissue equivalent medium when part of this medium is replaced by a material that is not soft -tissue equivalent. That is, heterogeneous dosimetry is addressed. Radionuclides which emit beta particles are the electron sources of primary interest. They are used in brachytherapy and in nuclear medicine: for example, beta -ray applicators made with strontium-90 are employed in certain ophthalmic treatments and iodine-131 is used to test thyroid function. More recent medical procedures under development and which involve beta radionuclides include radioimmunotherapy and radiation synovectomy; the first is a cancer modality and the second deals with the treatment of rheumatoid arthritis. In addition, the possibility of skin surface contamination exists whenever there is handling of radioactive material. Determination of absorbed doses in the examples of the preceding paragraph requires considering boundaries of interfaces. Whilst the Monte Carlo method can be applied to boundary calculations, for routine work such as in clinical situations, or in other circumstances where doses need to be determined quickly, analytical dosimetry would be invaluable. Unfortunately, few analytical methods for boundary beta dosimetry exist. Furthermore, the accuracy of results from both Monte Carlo and analytical methods has to be assessed. Although restricted to one radionuclide, phosphorus -32, the experimental data obtained in this work serve several purposes, one of which is to provide standards against which calculated results can be tested. The experimental data also contribute to the relatively sparse set of published boundary dosimetry data. At the same time, they may be useful in developing analytical boundary dosimetry methodology. The first application of the experimental data is demonstrated. Results from two Monte Carlo codes and two analytical methods, which were developed elsewhere, are compared with experimental data. Monte Carlo results compare satisfactory with experimental results for the boundaries considered. The agreement with experimental results for air interfaces is of particular interest because of discrepancies reported previously by another investigator who used data obtained from a different experimental technique. Results from one of the analytical methods differ significantly from the experimental data obtained here. The second analytical method provided data which approximate experimental results to within 30%. This is encouraging but it remains to be determined whether this method performs equally well for other source energies.

High Sensitivity Analysis of Nanoliter Volumes of Volatile and Nonvolatile Compounds using Matrix Assisted Ionization (MAI) Mass Spectrometry

NASA Astrophysics Data System (ADS)

Hoang, Khoa; Pophristic, Milan; Horan, Andrew J.; Johnston, Murray V.; McEwen, Charles N.

2016-10-01

First results are reported using a simple, fast, and reproducible matrix-assisted ionization (MAI) sample introduction method that provides substantial improvements relative to previously published MAI methods. The sensitivity of the new MAI methods, which requires no laser, high voltage, or nebulizing gas, is comparable to those reported for MALDI-TOF and n-ESI. High resolution full acquisition mass spectra having low chemical background are acquired from low nanoliters of solution using only a few femtomoles of analyte. The limit-of-detection for angiotensin II is less than 50 amol on an Orbitrap Exactive mass spectrometer. Analysis of peptides, including a bovine serum albumin digest, and drugs, including drugs in urine without a purification step, are reported using a 1 μL zero dead volume syringe in which only the analyte solution wetting the walls of the syringe needle is used in the analysis.

A systematic and feasible method for computing nuclear contributions to electrical properties of polyatomic molecules

NASA Astrophysics Data System (ADS)

Luis, Josep M.; Duran, Miquel; Andrés, José L.

1997-08-01

An analytic method to evaluate nuclear contributions to electrical properties of polyatomic molecules is presented. Such contributions control changes induced by an electric field on equilibrium geometry (nuclear relaxation contribution) and vibrational motion (vibrational contribution) of a molecular system. Expressions to compute the nuclear contributions have been derived from a power series expansion of the potential energy. These contributions to the electrical properties are given in terms of energy derivatives with respect to normal coordinates, electric field intensity or both. Only one calculation of such derivatives at the field-free equilibrium geometry is required. To show the useful efficiency of the analytical evaluation of electrical properties (the so-called AEEP method), results for calculations on water and pyridine at the SCF/TZ2P and the MP2/TZ2P levels of theory are reported. The results obtained are compared with previous theoretical calculations and with experimental values.

On the vacuum Einstein equations along curves with a discrete local rotation and reflection symmetry

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

Korzyński, Mikołaj; Hinder, Ian; Bentivegna, Eloisa, E-mail: korzynski@cft.edu.pl, E-mail: ian.hinder@aei.mpg.de, E-mail: eloisa.bentivegna@ct.infn.it

We discuss the possibility of a dimensional reduction of the Einstein equations in S{sup 3} black-hole lattices. It was reported in previous literature that the evolution of spaces containing curves of local, discrete rotation and reflection symmetry (LDRRS) can be carried out via a system of ODEs along these curves. However, 3+1 Numerical Relativity computations demonstrate that this is not the case, and we show analytically that this is due to the presence of a tensorial quantity which is not suppressed by the symmetry. We calculate the term analytically, and verify numerically for an 8-black-hole lattice that it fully accountsmore » for the anomalous results, and thus quantify its magnitude in this specific case. The presence of this term prevents the exact evolution of these spaces via previously-reported methods which do not involve a full 3+1 integration of Einstein's equation.« less

Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

PubMed

Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

2011-11-01

This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in biological or environmental samples. Due to low consumption of eluent (usually 0.3-1mL/run) mainly composed of water-alcohol binary mixtures, this method can be considered as environmentally friendly and green chemistry focused analytical tool, supplementary to analytical protocols involving column chromatography or planar micro-fluidic devices. Copyright © 2011 Elsevier Ltd. All rights reserved.

THE IMPACT OF POINT-SOURCE SUBTRACTION RESIDUALS ON 21 cm EPOCH OF REIONIZATION ESTIMATION

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

Trott, Cathryn M.; Wayth, Randall B.; Tingay, Steven J., E-mail: cathryn.trott@curtin.edu.au

Precise subtraction of foreground sources is crucial for detecting and estimating 21 cm H I signals from the Epoch of Reionization (EoR). We quantify how imperfect point-source subtraction due to limitations of the measurement data set yields structured residual signal in the data set. We use the Cramer-Rao lower bound, as a metric for quantifying the precision with which a parameter may be measured, to estimate the residual signal in a visibility data set due to imperfect point-source subtraction. We then propagate these residuals into two metrics of interest for 21 cm EoR experiments-the angular power spectrum and two-dimensional powermore » spectrum-using a combination of full analytic covariant derivation, analytic variant derivation, and covariant Monte Carlo simulations. This methodology differs from previous work in two ways: (1) it uses information theory to set the point-source position error, rather than assuming a global rms error, and (2) it describes a method for propagating the errors analytically, thereby obtaining the full correlation structure of the power spectra. The methods are applied to two upcoming low-frequency instruments that are proposing to perform statistical EoR experiments: the Murchison Widefield Array and the Precision Array for Probing the Epoch of Reionization. In addition to the actual antenna configurations, we apply the methods to minimally redundant and maximally redundant configurations. We find that for peeling sources above 1 Jy, the amplitude of the residual signal, and its variance, will be smaller than the contribution from thermal noise for the observing parameters proposed for upcoming EoR experiments, and that optimal subtraction of bright point sources will not be a limiting factor for EoR parameter estimation. We then use the formalism to provide an ab initio analytic derivation motivating the 'wedge' feature in the two-dimensional power spectrum, complementing previous discussion in the literature.« less

Development of an analytical procedure to study linear alkylbenzenesulphonate (LAS) degradation in sewage sludge-amended soils.

PubMed

Comellas, L; Portillo, J L; Vaquero, M T

1993-12-24

A procedure for determining linear alkylbenzenesulphonates (LASs) in sewage sludge and amended soils has been developed. Extraction by sample treatment with 0.5 M potassium hydroxide in methanol and reflux was compared with a previously described extraction procedure in Soxhlet with methanol and solid sodium hydroxide in the sample. Repeatability results were similar with savings in extraction time, solvents and evaporation time. A clean-up method involving a C18 cartridge has been developed. Analytes were quantified by a reversed-phase HPLC method with UV and fluorescence detectors. Recoveries obtained were higher than 84%. The standing procedure was applied to high doses of sewage sludge-amended soils (15%) with increasing quantities of added LASs. Degradation data for a 116-day period are presented.

The detection of problem analytes in a single proficiency test challenge in the absence of the Health Care Financing Administration rule violations.

PubMed

Cembrowski, G S; Hackney, J R; Carey, N

1993-04-01

The Clinical Laboratory Improvement Act of 1988 (CLIA 88) has dramatically changed proficiency testing (PT) practices having mandated (1) satisfactory PT for certain analytes as a condition of laboratory operation, (2) fixed PT limits for many of these "regulated" analytes, and (3) an increased number of PT specimens (n = 5) for each testing cycle. For many of these analytes, the fixed limits are much broader than the previously employed Standard Deviation Index (SDI) criteria. Paradoxically, there may be less incentive to identify and evaluate analytically significant outliers to improve the analytical process. Previously described "control rules" to evaluate these PT results are unworkable as they consider only two or three results. We used Monte Carlo simulations of Kodak Ektachem analyzers participating in PT to determine optimal control rules for the identification of PT results that are inconsistent with those from other laboratories using the same methods. The analysis of three representative analytes, potassium, creatine kinase, and iron was simulated with varying intrainstrument and interinstrument standard deviations (si and sg, respectively) obtained from the College of American Pathologists (Northfield, Ill) Quality Assurance Services data and Proficiency Test data, respectively. Analytical errors were simulated in each of the analytes and evaluated in terms of multiples of the interlaboratory SDI. Simple control rules for detecting systematic and random error were evaluated with power function graphs, graphs of probability of error detected vs magnitude of error. Based on the simulation results, we recommend screening all analytes for the occurrence of two or more observations exceeding the same +/- 1 SDI limit. For any analyte satisfying this condition, the mean of the observations should be calculated. For analytes with sg/si ratios between 1.0 and 1.5, a significant systematic error is signaled by the mean exceeding 1.0 SDI. Significant random error is signaled by one observation exceeding the +/- 3-SDI limit or the range of the observations exceeding 4 SDIs. For analytes with higher sg/si, significant systematic or random error is signaled by violation of the screening rule (having at least two observations exceeding the same +/- 1 SDI limit). Random error can also be signaled by one observation exceeding the +/- 1.5-SDI limit or the range of the observations exceeding 3 SDIs. We present a practical approach to the workup of apparent PT errors.

Determination of glycols in air: development of sampling and analytical methodology and application to theatrical smokes.

PubMed

Pendergrass, S M

1999-01-01

Glycol-based fluids are used in the production of theatrical smokes in theaters, concerts, and other stage productions. The fluids are heated and dispersed in aerosol form to create the effect of a smoke, mist, or fog. There have been reports of adverse health effects such as respiratory irritation, chest tightness, shortness of breath, asthma, and skin rashes. Previous attempts to collect and quantify the aerosolized glycols used in fogging agents have been plagued by inconsistent results, both in the efficiency of collection and in the chromatographic analysis of the glycol components. The development of improved sampling and analytical methodology for aerosolized glycols was required to assess workplace exposures more effectively. An Occupational Safety and Health Administration versatile sampler tube was selected for the collection of ethylene glycol, propylene glycol, 1,3-butylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol aerosols. Analytical methodology for the separation, identification, and quantitation of the six glycols using gas chromatography/flame ionization detection is described. Limits of detection of the glycol analytes ranged from 7 to 16 micrograms/sample. Desorption efficiencies for all glycol compounds were determined over the range of study and averaged greater than 90%. Storage stability results were acceptable after 28 days for all analytes except ethylene glycol, which was stable at ambient temperature for 14 days. Based on the results of this study, the new glycol method was published in the NIOSH Manual of Analytical Methods.

Quantification of six herbicide metabolites in human urine.

PubMed

Norrgran, Jessica; Bravo, Roberto; Bishop, Amanda M; Restrepo, Paula; Whitehead, Ralph D; Needham, Larry L; Barr, Dana B

2006-01-18

We developed a sensitive, selective and precise method for measuring herbicide metabolites in human urine. Our method uses automated liquid delivery of internal standards and acetate buffer and a mixed polarity polymeric phase solid phase extraction of a 2 mL urine sample. The concentrated eluate is analyzed using high-performance liquid chromatography-tandem mass spectrometry. Isotope dilution calibration is used for quantification of all analytes. The limits of detection of our method range from 0.036 to 0.075 ng/mL. The within- and between-day variation in pooled quality control samples range from 2.5 to 9.0% and from 3.2 to 16%, respectively, for all analytes at concentrations ranging from 0.6 to 12 ng/mL. Precision was similar with samples fortified with 0.1 and 0.25 ng/mL that were analyzed in each run. We validated our selective method against a less selective method used previously in our laboratory by analyzing human specimens using both methods. The methods produced results that were in agreement, with no significant bias observed.

Direct measurement of carbon-14 in carbon dioxide by liquid scintillation counting

NASA Technical Reports Server (NTRS)

Horrocks, D. L.

1969-01-01

Liquid scintillation counting technique is applied to the direct measurement of carbon-14 in carbon dioxide. This method has high counting efficiency and eliminates many of the basic problems encountered with previous techniques. The technique can be used to achieve a percent substitution reaction and is of interest as an analytical technique.

Asymptotic Standard Errors for Item Response Theory True Score Equating of Polytomous Items

ERIC Educational Resources Information Center

Cher Wong, Cheow

2015-01-01

Building on previous works by Lord and Ogasawara for dichotomous items, this article proposes an approach to derive the asymptotic standard errors of item response theory true score equating involving polytomous items, for equivalent and nonequivalent groups of examinees. This analytical approach could be used in place of empirical methods like…

A Simplified Digestion Protocol for the Analysis of Hg in Fish by Cold Vapor Atomic Absorption Spectroscopy

ERIC Educational Resources Information Center

Kristian, Kathleen E.; Friedbauer, Scott; Kabashi, Donika; Ferencz, Kristen M.; Barajas, Jennifer C.; O'Brien, Kelly

2015-01-01

Analysis of mercury in fish is an interesting problem with the potential to motivate students in chemistry laboratory courses. The recommended method for mercury analysis in fish is cold vapor atomic absorption spectroscopy (CVAAS), which requires homogeneous analyte solutions, typically prepared by acid digestion. Previously published digestion…

Potential concerns with analytical methods used for the detection of Batrachochytrium salamandrivorans from archived DNA of amphibian swab samples, Oregon, USA

Treesearch

Deborah D. Iwanowicz; William B. Schill; Deanna H. Olson; Michael J. Adams; Christine Densmore; R. Scott Cornman; Cynthia Adams; Jr. Figiel; Chauncey W. Anderson; Andrew R. Blaustein; Tara Chestnut

2017-01-01

We report on the results of surveillance for the salamander chytrid fungus, Batrachochytrium salamandrivorans (Bsal). Two samples from archived DNA used in a previous chytrid study in Oregon were Bsal-positive, alerting us to the first potential finding of this pathogen in North America, infecting American...

Family Meals and Child Academic and Behavioral Outcomes

ERIC Educational Resources Information Center

Miller, Daniel P.; Waldfogel, Jane; Han, Wen-Jui

2012-01-01

This study investigates the link between the frequency of family breakfasts and dinners and child academic and behavioral outcomes in a panel sample of 21,400 children aged 5-15. It complements previous work by examining younger and older children separately and by using information on a large number of controls and rigorous analytic methods to…

Operator's manual on the visual-accumulation tube method for sedimentation analysis of sands

USGS Publications Warehouse

Colby, V.C.; Witzgman, F.W.

1958-01-01

The personnel who will be operating these units may have little or no previous knowledge of either the principles involved or the details of opera.ting procedure. This manual is intended as an aid to them in setting up the apparatus, learning the analytical procedure, interpreting the results, and understanding the primary principles encountered.

Global approach for the validation of an in-line Raman spectroscopic method to determine the API content in real-time during a hot-melt extrusion process.

PubMed

Netchacovitch, L; Thiry, J; De Bleye, C; Dumont, E; Cailletaud, J; Sacré, P-Y; Evrard, B; Hubert, Ph; Ziemons, E

2017-08-15

Since the Food and Drug Administration (FDA) published a guidance based on the Process Analytical Technology (PAT) approach, real-time analyses during manufacturing processes are in real expansion. In this study, in-line Raman spectroscopic analyses were performed during a Hot-Melt Extrusion (HME) process to determine the Active Pharmaceutical Ingredient (API) content in real-time. The method was validated based on a univariate and a multivariate approach and the analytical performances of the obtained models were compared. Moreover, on one hand, in-line data were correlated with the real API concentration present in the sample quantified by a previously validated off-line confocal Raman microspectroscopic method. On the other hand, in-line data were also treated in function of the concentration based on the weighing of the components in the prepared mixture. The importance of developing quantitative methods based on the use of a reference method was thus highlighted. The method was validated according to the total error approach fixing the acceptance limits at ±15% and the α risk at ±5%. This method reaches the requirements of the European Pharmacopeia norms for the uniformity of content of single-dose preparations. The validation proves that future results will be in the acceptance limits with a previously defined probability. Finally, the in-line validated method was compared with the off-line one to demonstrate its ability to be used in routine analyses. Copyright © 2017 Elsevier B.V. All rights reserved.

Differential Privacy Preserving in Big Data Analytics for Connected Health.

PubMed

Lin, Chi; Song, Zihao; Song, Houbing; Zhou, Yanhong; Wang, Yi; Wu, Guowei

2016-04-01

In Body Area Networks (BANs), big data collected by wearable sensors usually contain sensitive information, which is compulsory to be appropriately protected. Previous methods neglected privacy protection issue, leading to privacy exposure. In this paper, a differential privacy protection scheme for big data in body sensor network is developed. Compared with previous methods, this scheme will provide privacy protection with higher availability and reliability. We introduce the concept of dynamic noise thresholds, which makes our scheme more suitable to process big data. Experimental results demonstrate that, even when the attacker has full background knowledge, the proposed scheme can still provide enough interference to big sensitive data so as to preserve the privacy.

The impact of capillary backpressure on spontaneous counter-current imbibition in porous media

NASA Astrophysics Data System (ADS)

Foley, Amir Y.; Nooruddin, Hasan A.; Blunt, Martin J.

2017-09-01

We investigate the impact of capillary backpressure on spontaneous counter-current imbibition. For such displacements in strongly water-wet systems, the non-wetting phase is forced out through the inlet boundary as the wetting phase imbibes into the rock, creating a finite capillary backpressure. Under the assumption that capillary backpressure depends on the water saturation applied at the inlet boundary of the porous medium, its impact is determined using the continuum modelling approach by varying the imposed inlet saturation in the analytical solution. We present analytical solutions for the one-dimensional incompressible horizontal displacement of a non-wetting phase by a wetting phase in a porous medium. There exists an inlet saturation value above which any change in capillary backpressure has a negligible impact on the solutions. Above this threshold value, imbibition rates and front positions are largely invariant. A method for identifying this inlet saturation is proposed using an analytical procedure and we explore how varying multiphase flow properties affects the analytical solutions and this threshold saturation. We show the value of this analytical approach through the analysis of previously published experimental data.

An analytical solution for Dean flow in curved ducts with rectangular cross section

NASA Astrophysics Data System (ADS)

Norouzi, M.; Biglari, N.

2013-05-01

In this paper, a full analytical solution for incompressible flow inside the curved ducts with rectangular cross-section is presented for the first time. The perturbation method is applied to solve the governing equations and curvature ratio is considered as the perturbation parameter. The previous perturbation solutions are usually restricted to the flow in curved circular or annular pipes related to the overly complex form of solutions or singularity situation for flow in curved ducts with non-circular shapes of cross section. This issue specifies the importance of analytical studies in the field of Dean flow inside the non-circular ducts. In this study, the main flow velocity, stream function of lateral velocities (secondary flows), and flow resistance ratio in rectangular curved ducts are obtained analytically. The effect of duct curvature and aspect ratio on flow field is investigated as well. Moreover, it is important to mention that the current analytical solution is able to simulate the Taylor-Görtler and Dean vortices (vortices in stable and unstable situations) in curved channels.

Effect of analytical conditions in wavelength dispersive electron microprobe analysis on the measurement of strontium-to-calcium (Sr/Ca) ratios in otoliths of anadromous salmonids

USGS Publications Warehouse

Zimmerman, Christian E.; Nielsen, Roger L.

2003-01-01

The use of strontium-to-calcium (Sr/Ca) ratios in otoliths is becoming a standard method to describe life history type and the chronology of migrations between freshwater and seawater habitats in teleosts (e.g. Kalish, 1990; Radtke et al., 1990; Secor, 1992; Rieman et al., 1994; Radtke, 1995; Limburg, 1995; Tzeng et al. 1997; Volk et al., 2000; Zimmerman, 2000; Zimmerman and Reeves, 2000, 2002). This method provides critical information concerning the relationship and ecology of species exhibiting phenotypic variation in migratory behavior (Kalish, 1990; Secor, 1999). Methods and procedures, however, vary among laboratories because a standard method or protocol for measurement of Sr in otoliths does not exist. In this note, we examine the variations in analytical conditions in an effort to increase precision of Sr/Ca measurements. From these findings we argue that precision can be maximized with higher beam current (although there is specimen damage) than previously recommended by Gunn et al. (1992).

HPLC-Based Method to Evaluate Kinetics of Glucosinolate Hydrolysis by Sinapis alba Myrosinase1

PubMed Central

Vastenhout, Kayla J.; Tornberg, Ruthellen H.; Johnson, Amanda L.; Amolins, Michael W.; Mays, Jared R.

2014-01-01

Isothiocyanates (ITCs) are one of several hydrolysis products of glucosinolates, plant secondary metabolites which are substrates for the thioglucohydrolase myrosinase. Recent pursuits toward the development of synthetic, non-natural ITCs have consequently led to an exploration of generating these compounds from non-natural glucosinolate precursors. Evaluation of the myrosinase-dependent conversion of select non-natural glucosinolates to non-natural ITCs cannot be accomplished using established UV-Vis spectroscopic methods. To overcome this limitation, an alternative HPLC-based analytical approach was developed where initial reaction velocities were generated from non-linear reaction progress curves. Validation of this HPLC method was accomplished through parallel evaluation of three glucosinolates with UV-Vis methodology. The results of this study demonstrate that kinetic data is consistent between both analytical methods and that the tested glucosinolates respond similarly to both Michaelis–Menten and specific activity analyses. Consequently, this work resulted in the complete kinetic characterization of three glucosinolates with Sinapis alba myrosinase, with results that were consistent with previous reports. PMID:25068719

A Conceptual Analytics Model for an Outcome-Driven Quality Management Framework as Part of Professional Healthcare Education

PubMed Central

Loe, Alan; Barman, Linda; O'Donoghue, John; Zary, Nabil

2015-01-01

Background Preparing the future health care professional workforce in a changing world is a significant undertaking. Educators and other decision makers look to evidence-based knowledge to improve quality of education. Analytics, the use of data to generate insights and support decisions, have been applied successfully across numerous application domains. Health care professional education is one area where great potential is yet to be realized. Previous research of Academic and Learning analytics has mainly focused on technical issues. The focus of this study relates to its practical implementation in the setting of health care education. Objective The aim of this study is to create a conceptual model for a deeper understanding of the synthesizing process, and transforming data into information to support educators’ decision making. Methods A deductive case study approach was applied to develop the conceptual model. Results The analytics loop works both in theory and in practice. The conceptual model encompasses the underlying data, the quality indicators, and decision support for educators. Conclusions The model illustrates how a theory can be applied to a traditional data-driven analytics approach, and alongside the context- or need-driven analytics approach. PMID:27731840

Carbon nanotubes as adsorbent of solid-phase extraction and matrix for laser desorption/ionization mass spectrometry.

PubMed

Pan, Chensong; Xu, Songyun; Zou, Hanfa; Guo, Zhong; Zhang, Yu; Guo, Baochuan

2005-02-01

A method with carbon nanotubes functioning both as the adsorbent of solid-phase extraction (SPE) and the matrix for matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) to analyze small molecules in solution has been developed. In this method, 10 microL suspensions of carbon nanotubes in 50% (vol/vol) methanol were added to the sample solution to extract analytes onto surface of carbon nanotubes because of their dramatic hydrophobicity. Carbon nanotubes in solution are deposited onto the bottom of tube with centrifugation. After removing the supernatant fluid, carbon nanotubes are suspended again with dispersant and pipetted directly onto the sample target of the MALDI-MS to perform a mass spectrometric analysis. It was demonstrated by analysis of a variety of small molecules that the resolution of peaks and the efficiency of desorption/ionization on the carbon nanotubes are better than those on the activated carbon. It is found that with the addition of glycerol and sucrose to the dispersant, the intensity, the ratio of signal to noise (S/N), and the resolution of peaks for analytes by mass spectrometry increased greatly. Compared with the previously reported method by depositing sample solution onto thin layer of carbon nanotubes, it is observed that the detection limit for analytes can be enhanced about 10 to 100 times due to solid-phase extraction of analytes in solution by carbon nanotubes. An acceptable result of simultaneously quantitative analysis of three analytes in solution has been achieved. The application in determining drugs spiked into urine has also been realized.

Full velocity difference model for a car-following theory.

PubMed

Jiang, R; Wu, Q; Zhu, Z

2001-07-01

In this paper, we present a full velocity difference model for a car-following theory based on the previous models in the literature. To our knowledge, the model is an improvement over the previous ones theoretically, because it considers more aspects in car-following process than others. This point is verified by numerical simulation. Then we investigate the property of the model using both analytic and numerical methods, and find that the model can describe the phase transition of traffic flow and estimate the evolution of traffic congestion.

Brownian systems with spatially inhomogeneous activity

NASA Astrophysics Data System (ADS)

Sharma, A.; Brader, J. M.

2017-09-01

We generalize the Green-Kubo approach, previously applied to bulk systems of spherically symmetric active particles [J. Chem. Phys. 145, 161101 (2016), 10.1063/1.4966153], to include spatially inhomogeneous activity. The method is applied to predict the spatial dependence of the average orientation per particle and the density. The average orientation is given by an integral over the self part of the Van Hove function and a simple Gaussian approximation to this quantity yields an accurate analytical expression. Taking this analytical result as input to a dynamic density functional theory approximates the spatial dependence of the density in good agreement with simulation data. All theoretical predictions are validated using Brownian dynamics simulations.

Closed-form analytical solutions of high-temperature heat pipe startup and frozen startup limitation

NASA Technical Reports Server (NTRS)

Cao, Y.; Faghri, A.

1992-01-01

Previous numerical and experimental studies indicate that the high-temperature heat pipe startup process is characterized by a moving hot zone with relatively sharp fronts. Based on the above observation, a flat-front model for an approximate analytical solution is proposed. A closed-form solution related to the temperature distribution in the hot zone and the hot zone length as a function of time are obtained. The analytical results agree well with the corresponding experimental data, and provide a quick prediction method for the heat pipe startup performance. Finally, a heat pipe limitation related to the frozen startup process is identified, and an explicit criterion for the high-temperature heat pipe startup is derived. The frozen startup limit identified in this paper provides a fundamental guidance for high-temperature heat pipe design.

Risk analysis by FMEA as an element of analytical validation.

PubMed

van Leeuwen, J F; Nauta, M J; de Kaste, D; Odekerken-Rombouts, Y M C F; Oldenhof, M T; Vredenbregt, M J; Barends, D M

2009-12-05

We subjected a Near-Infrared (NIR) analytical procedure used for screening drugs on authenticity to a Failure Mode and Effects Analysis (FMEA), including technical risks as well as risks related to human failure. An FMEA team broke down the NIR analytical method into process steps and identified possible failure modes for each step. Each failure mode was ranked on estimated frequency of occurrence (O), probability that the failure would remain undetected later in the process (D) and severity (S), each on a scale of 1-10. Human errors turned out to be the most common cause of failure modes. Failure risks were calculated by Risk Priority Numbers (RPNs)=O x D x S. Failure modes with the highest RPN scores were subjected to corrective actions and the FMEA was repeated, showing reductions in RPN scores and resulting in improvement indices up to 5.0. We recommend risk analysis as an addition to the usual analytical validation, as the FMEA enabled us to detect previously unidentified risks.

An analytical method for free vibration analysis of functionally graded beams with edge cracks

NASA Astrophysics Data System (ADS)

Wei, Dong; Liu, Yinghua; Xiang, Zhihai

2012-03-01

In this paper, an analytical method is proposed for solving the free vibration of cracked functionally graded material (FGM) beams with axial loading, rotary inertia and shear deformation. The governing differential equations of motion for an FGM beam are established and the corresponding solutions are found first. The discontinuity of rotation caused by the cracks is simulated by means of the rotational spring model. Based on the transfer matrix method, then the recurrence formula is developed to get the eigenvalue equations of free vibration of FGM beams. The main advantage of the proposed method is that the eigenvalue equation for vibrating beams with an arbitrary number of cracks can be conveniently determined from a third-order determinant. Due to the decrease in the determinant order as compared with previous methods, the developed method is simpler and more convenient to analytically solve the free vibration problem of cracked FGM beams. Moreover, free vibration analyses of the Euler-Bernoulli and Timoshenko beams with any number of cracks can be conducted using the unified procedure based on the developed method. These advantages of the proposed procedure would be more remarkable as the increase of the number of cracks. A comprehensive analysis is conducted to investigate the influences of the location and total number of cracks, material properties, axial load, inertia and end supports on the natural frequencies and vibration mode shapes of FGM beams. The present work may be useful for the design and control of damaged structures.

Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

PubMed

Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

2017-01-20

A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

An efficient formulation and implementation of the analytic energy gradient method to the single and double excitation coupled-cluster wave function - Application to Cl2O2

NASA Technical Reports Server (NTRS)

Rendell, Alistair P.; Lee, Timothy J.

1991-01-01

The analytic energy gradient for the single and double excitation coupled-cluster (CCSD) wave function has been reformulated and implemented in a new set of programs. The reformulated set of gradient equations have a smaller computational cost than any previously published. The iterative solution of the linear equations and the construction of the effective density matrices are fully vectorized, being based on matrix multiplications. The new method has been used to investigate the Cl2O2 molecule, which has recently been postulated as an important intermediate in the destruction of ozone in the stratosphere. In addition to reporting computational timings, the CCSD equilibrium geometries, harmonic vibrational frequencies, infrared intensities, and relative energetics of three isomers of Cl2O2 are presented.

A finite element study of the EIDI system. [Electro-Impulse De-Icing System

NASA Technical Reports Server (NTRS)

Khatkhate, A. A.; Scavuzzo, R. J.; Chu, M. L.

1988-01-01

This paper presents a method for modeling the structural dynamics of an Electro-Impulse De-Icing System, using finite element analyses procedures. A guideline for building a representative finite element model is discussed. Modeling was done initially using four noded cubic elements, four noded isoparametric plate elements and eight noded isoparametric shell elements. Due to the size of the problem and due to the underestimation of shear stress results when compared to previous analytical work an approximate model was created to predict possible areas of shedding of ice. There appears to be good agreement with the test data provided by The Boeing Commercial Airplane Company. Thus these initial results of this method were found to be encouraging. Additional analytical work and comparison with experiment is needed in order to completely evaluate this approach.

Quantitative Method for Simultaneous Analysis of Acetaminophen and 6 Metabolites.

PubMed

Lammers, Laureen A; Achterbergh, Roos; Pistorius, Marcel C M; Romijn, Johannes A; Mathôt, Ron A A

2017-04-01

Hepatotoxicity after ingestion of high-dose acetaminophen [N-acetyl-para-aminophenol (APAP)] is caused by the metabolites of the drug. To gain more insight into factors influencing susceptibility to APAP hepatotoxicity, quantification of APAP and metabolites is important. A few methods have been developed to simultaneously quantify APAP and its most important metabolites. However, these methods require a comprehensive sample preparation and long run times. The aim of this study was to develop and validate a simplified, but sensitive method for the simultaneous quantification of acetaminophen, the main metabolites acetaminophen glucuronide and acetaminophen sulfate, and 4 Cytochrome P450-mediated metabolites by using liquid chromatography with mass spectrometric (LC-MS) detection. The method was developed and validated for the human plasma, and it entailed a single method for sample preparation, enabling quick processing of the samples followed by an LC-MS method with a chromatographic run time of 9 minutes. The method was validated for selectivity, linearity, accuracy, imprecision, dilution integrity, recovery, process efficiency, ionization efficiency, and carryover effect. The method showed good selectivity without matrix interferences. For all analytes, the mean process efficiency was >86%, and the mean ionization efficiency was >94%. Furthermore, the accuracy was between 90.3% and 112% for all analytes, and the within- and between-run imprecision were <20% for the lower limit of quantification and <14.3% for the middle level and upper limit of quantification. The method presented here enables the simultaneous quantification of APAP and 6 of its metabolites. It is less time consuming than previously reported methods because it requires only a single and simple method for the sample preparation followed by an LC-MS method with a short run time. Therefore, this analytical method provides a useful method for both clinical and research purposes.

Water equivalent thickness values of materials used in beams of protons, helium, carbon and iron ions.

PubMed

Zhang, Rui; Taddei, Phillip J; Fitzek, Markus M; Newhauser, Wayne D

2010-05-07

Heavy charged particle beam radiotherapy for cancer is of increasing interest because it delivers a highly conformal radiation dose to the target volume. Accurate knowledge of the range of a heavy charged particle beam after it penetrates a patient's body or other materials in the beam line is very important and is usually stated in terms of the water equivalent thickness (WET). However, methods of calculating WET for heavy charged particle beams are lacking. Our objective was to test several simple analytical formulas previously developed for proton beams for their ability to calculate WET values for materials exposed to beams of protons, helium, carbon and iron ions. Experimentally measured heavy charged particle beam ranges and WET values from an iterative numerical method were compared with the WET values calculated by the analytical formulas. In most cases, the deviations were within 1 mm. We conclude that the analytical formulas originally developed for proton beams can also be used to calculate WET values for helium, carbon and iron ion beams with good accuracy.

Water equivalent thickness values of materials used in beams of protons, helium, carbon and iron ions

PubMed Central

Zhang, Rui; Taddei, Phillip J; Fitzek, Markus M; Newhauser, Wayne D

2010-01-01

Heavy charged particle beam radiotherapy for cancer is of increasing interest because it delivers a highly conformal radiation dose to the target volume. Accurate knowledge of the range of a heavy charged particle beam after it penetrates a patient’s body or other materials in the beam line is very important and is usually stated in terms of the water equivalent thickness (WET). However, methods of calculating WET for heavy charged particle beams are lacking. Our objective was to test several simple analytical formulas previously developed for proton beams for their ability to calculate WET values for materials exposed to beams of protons, helium, carbon and iron ions. Experimentally measured heavy charged particle beam ranges and WET values from an iterative numerical method were compared with the WET values calculated by the analytical formulas. Inmost cases, the deviations were within 1 mm. We conclude that the analytical formulas originally developed for proton beams can also be used to calculate WET values for helium, carbon and iron ion beams with good accuracy. PMID:20371908

Nuclear magnetic resonance signal dynamics of liquids in the presence of distant dipolar fields, revisited

PubMed Central

Barros, Wilson; Gochberg, Daniel F.; Gore, John C.

2009-01-01

The description of the nuclear magnetic resonance magnetization dynamics in the presence of long-range dipolar interactions, which is based upon approximate solutions of Bloch–Torrey equations including the effect of a distant dipolar field, has been revisited. New experiments show that approximate analytic solutions have a broader regime of validity as well as dependencies on pulse-sequence parameters that seem to have been overlooked. In order to explain these experimental results, we developed a new method consisting of calculating the magnetization via an iterative formalism where both diffusion and distant dipolar field contributions are treated as integral operators incorporated into the Bloch–Torrey equations. The solution can be organized as a perturbative series, whereby access to higher order terms allows one to set better boundaries on validity regimes for analytic first-order approximations. Finally, the method legitimizes the use of simple analytic first-order approximations under less demanding experimental conditions, it predicts new pulse-sequence parameter dependencies for the range of validity, and clarifies weak points in previous calculations. PMID:19425789

Quantifying Protein Concentrations Using Smartphone Colorimetry: A New Method for an Established Test

ERIC Educational Resources Information Center

Gee, Clifford T.; Kehoe, Eric; Pomerantz, William C. K.; Penn, R. Lee

2017-01-01

Proteins are involved in nearly every biological process, which makes them of interest to a range of scientists. Previous work has shown that hand-held cameras can be used to determine the concentration of colored analytes in solution, and this paper extends the approach to reactions involving a color change in order to quantify protein…

Improvements to sample processing and measurement to enable more widespread environmental application of tritium

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

Moran, James; Alexander, Thomas; Aalseth, Craig

2017-08-01

Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. We present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120 mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. This enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps in our understanding of T behavior in the environment.

Identification of balanced chromosomal rearrangements previously unknown among participants in the 1000 Genomes Project: implications for interpretation of structural variation in genomes and the future of clinical cytogenetics.

PubMed

Dong, Zirui; Wang, Huilin; Chen, Haixiao; Jiang, Hui; Yuan, Jianying; Yang, Zhenjun; Wang, Wen-Jing; Xu, Fengping; Guo, Xiaosen; Cao, Ye; Zhu, Zhenzhen; Geng, Chunyu; Cheung, Wan Chee; Kwok, Yvonne K; Yang, Huanming; Leung, Tak Yeung; Morton, Cynthia C; Cheung, Sau Wai; Choy, Kwong Wai

2017-11-02

PurposeRecent studies demonstrate that whole-genome sequencing enables detection of cryptic rearrangements in apparently balanced chromosomal rearrangements (also known as balanced chromosomal abnormalities, BCAs) previously identified by conventional cytogenetic methods. We aimed to assess our analytical tool for detecting BCAs in the 1000 Genomes Project without knowing which bands were affected.MethodsThe 1000 Genomes Project provides an unprecedented integrated map of structural variants in phenotypically normal subjects, but there is no information on potential inclusion of subjects with apparent BCAs akin to those traditionally detected in diagnostic cytogenetics laboratories. We applied our analytical tool to 1,166 genomes from the 1000 Genomes Project with sufficient physical coverage (8.25-fold).ResultsWith this approach, we detected four reciprocal balanced translocations and four inversions, ranging in size from 57.9 kb to 13.3 Mb, all of which were confirmed by cytogenetic methods and polymerase chain reaction studies. One of these DNAs has a subtle translocation that is not readily identified by chromosome analysis because of the similarity of the banding patterns and size of exchanged segments, and another results in disruption of all transcripts of an OMIM gene.ConclusionOur study demonstrates the extension of utilizing low-pass whole-genome sequencing for unbiased detection of BCAs including translocations and inversions previously unknown in the 1000 Genomes Project.GENETICS in MEDICINE advance online publication, 2 November 2017; doi:10.1038/gim.2017.170.

Alkaloids Profiling of Fumaria capreolata by Analytical Platforms Based on the Hyphenation of Gas Chromatography and Liquid Chromatography with Quadrupole-Time-of-Flight Mass Spectrometry.

PubMed

Contreras, María Del Mar; Bribi, Noureddine; Gómez-Caravaca, Ana María; Gálvez, Julio; Segura-Carretero, Antonio

2017-01-01

Two analytical platforms, gas chromatography (GC) coupled to quadrupole-time-of-flight (QTOF) mass spectrometry (MS) and reversed-phase ultrahigh performance liquid chromatography (UHPLC) coupled to diode array (DAD) and QTOF detection, were applied in order to study the alkaloid profile of Fumaria capreolata . The use of these mass analyzers enabled tentatively identifying the alkaloids by matching their accurate mass signals and suggested molecular formulae with those previously reported in libraries and databases. Moreover, the proposed structures were corroborated by studying their fragmentation pattern obtained by both platforms. In this way, 8 and 26 isoquinoline alkaloids were characterized using GC-QTOF-MS and RP-UHPLC-DAD-QTOF-MS, respectively, and they belonged to the following subclasses: protoberberine, protopine, aporphine, benzophenanthridine, spirobenzylisoquinoline, morphinandienone, and benzylisoquinoline. Moreover, the latter analytical method was selected to determine at 280 nm the concentration of protopine (9.6 ± 0.7 mg/g), a potential active compound of the extract. In conclusion, although GC-MS has been commonly used for the analysis of this type of phytochemicals, RP-UHPLC-DAD-QTOF-MS provided essential complementary information. This analytical method can be applied for the quality control of phytopharmaceuticals containing Fumaria extracts currently found in the market.

Alkaloids Profiling of Fumaria capreolata by Analytical Platforms Based on the Hyphenation of Gas Chromatography and Liquid Chromatography with Quadrupole-Time-of-Flight Mass Spectrometry

PubMed Central

Bribi, Noureddine; Gómez-Caravaca, Ana María

2017-01-01

Two analytical platforms, gas chromatography (GC) coupled to quadrupole-time-of-flight (QTOF) mass spectrometry (MS) and reversed-phase ultrahigh performance liquid chromatography (UHPLC) coupled to diode array (DAD) and QTOF detection, were applied in order to study the alkaloid profile of Fumaria capreolata. The use of these mass analyzers enabled tentatively identifying the alkaloids by matching their accurate mass signals and suggested molecular formulae with those previously reported in libraries and databases. Moreover, the proposed structures were corroborated by studying their fragmentation pattern obtained by both platforms. In this way, 8 and 26 isoquinoline alkaloids were characterized using GC-QTOF-MS and RP-UHPLC-DAD-QTOF-MS, respectively, and they belonged to the following subclasses: protoberberine, protopine, aporphine, benzophenanthridine, spirobenzylisoquinoline, morphinandienone, and benzylisoquinoline. Moreover, the latter analytical method was selected to determine at 280 nm the concentration of protopine (9.6 ± 0.7 mg/g), a potential active compound of the extract. In conclusion, although GC-MS has been commonly used for the analysis of this type of phytochemicals, RP-UHPLC-DAD-QTOF-MS provided essential complementary information. This analytical method can be applied for the quality control of phytopharmaceuticals containing Fumaria extracts currently found in the market. PMID:29348751

An automated online turboflow cleanup LC/MS/MS method for the determination of 11 plasticizers in beverages and milk.

PubMed

Ates, Ebru; Mittendorf, Klaus; Senyuva, Hamide

2013-01-01

An automated sample preparation technique involving cleanup and analytical separation in a single operation using an online coupled TurboFlow (RP-LC system) is reported. This method eliminates time-consuming sample preparation steps that can be potential sources for cross-contamination in the analysis of plasticizers. Using TurboFlow chromatography, liquid samples were injected directly into the automated system without previous extraction or cleanup. Special cleanup columns enabled specific binding of target compounds; higher MW compounds, i.e., fats and proteins, and other matrix interferences with different chemical properties were removed to waste, prior to LC/MS/MS. Systematic stepwise method development using this new technology in the food safety area is described. Selection of optimum columns and mobile phases for loading onto the cleanup column followed by transfer onto the analytical column and MS detection are critical method parameters. The method was optimized for the assay of 10 phthalates (dimethyl, diethyl, dipropyl, butyl benzyl, diisobutyl, dicyclohexyl, dihexyl, diethylhexyl, diisononyl, and diisododecyl) and one adipate (diethylhexyl) in beverages and milk.

Enantioselective determination of representative profens in wastewater by a single-step sample treatment and chiral liquid chromatography-tandem mass spectrometry.

PubMed

Caballo, C; Sicilia, M D; Rubio, S

2015-03-01

This manuscript describes, for the first time, the simultaneous enantioselective determination of ibuprofen, naproxen and ketoprofen in wastewater based on liquid chromatography tandem mass spectrometry (LC-MS/MS). The method uses a single-step sample treatment based on microextraction with a supramolecular solvent made up of hexagonal inverted aggregates of decanoic acid, formed in situ in the wastewater sample through a spontaneous self-assembly process. Microextraction of profens was optimized and the analytical method validated. Isotopically labeled internal standards were used to compensate for both matrix interferences and recoveries. Apparent recoveries for the six enantiomers in influent and effluent wastewater samples were in the interval 97-103%. Low method detection limits (MDLs) were obtained (0.5-1.2 ng L(-1)) as a result of the high concentration factors achieved in the microextraction process (i.e. actual concentration factors 469-736). No analyte derivatization or evaporation of extracts, as it is required with GC-MS, was necessary. Relative standard deviations for enantiomers in wastewater were always below 8%. The method was applied to the determination of the concentrations and enantiomeric fractions of the targeted analytes in influents and effluents from three wastewater treatment plants. All the values found for profen enantiomers were consistent with those previously reported and confirmed again the suitability of using the enantiomeric fraction of ibuprofen as an indicator of the discharge of untreated or poorly treated wastewaters. Both the analytical and operational features of this method make it applicable to the assessment of the enantiomeric fate of profens in the environment. Copyright © 2014 Elsevier B.V. All rights reserved.

Reliably Discriminating Stock Structure with Genetic Markers:Mixture Models with Robust and Fast Computation.

PubMed

Foster, Scott D; Feutry, Pierre; Grewe, Peter M; Berry, Oliver; Hui, Francis K C; Davies, Campbell R

2018-06-26

Delineating naturally occurring and self-sustaining sub-populations (stocks) of a species is an important task, especially for species harvested from the wild. Despite its central importance to natural resource management, analytical methods used to delineate stocks are often, and increasingly, borrowed from superficially similar analytical tasks in human genetics even though models specifically for stock identification have been previously developed. Unfortunately, the analytical tasks in resource management and human genetics are not identical { questions about humans are typically aimed at inferring ancestry (often referred to as 'admixture') rather than breeding stocks. In this article, we argue, and show through simulation experiments and an analysis of yellowfin tuna data, that ancestral analysis methods are not always appropriate for stock delineation. In this work, we advocate a variant of a previouslyintroduced and simpler model that identifies stocks directly. We also highlight that the computational aspects of the analysis, irrespective of the model, are difficult. We introduce some alternative computational methods and quantitatively compare these methods to each other and to established methods. We also present a method for quantifying uncertainty in model parameters and in assignment probabilities. In doing so, we demonstrate that point estimates can be misleading. One of the computational strategies presented here, based on an expectation-maximisation algorithm with judiciously chosen starting values, is robust and has a modest computational cost. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Validating a faster method for reconstitution of Crotalidae Polyvalent Immune Fab (ovine).

PubMed

Gerring, David; King, Thomas R; Branton, Richard

2013-07-01

Reconstitution of CroFab(®) (Crotalidae Polyvalent Immune Fab [ovine]) lyophilized drug product was previously performed using 10 mL sterile water for injection followed by up to 36 min of gentle swirling of the vial. CroFab has been clinically demonstrated to be most effective when administered within 6 h of snake envenomation, and improved clinical outcomes are correlated with quicker timing of administration. An alternate reconstitution method was devised, using 18 mL 0.9% saline with manual inversion, with the goal of shortening reconstitution time while maintaining a high quality, efficacious product. An analytical study was designed to compare the physicochemical properties of 3 separate batches of CroFab when reconstituted using the standard procedure (10 mL WFI with gentle swirling) and a modified rapid procedure using 18 mL 0.9% saline and manual inversion. The physical and chemical characteristics of the same 3 batches were assessed using various analytic methodologies associated with routine quality control release testing. In addition further analytical methodologies were applied in order to elucidate possible structural changes that may be induced by the changed reconstitution procedure. Batches A, B, and C required mean reconstitution times of 25 min 51 s using the label method and 3 min 07 s (a 88.0% mean decrease) using the modified method. Physicochemical characteristics (color and clarity, pH, purity, protein content, potency) were found to be highly comparable. Characterization assays (dynamic light scattering, analytical ultracentrifugation, LC-MS, SDS-PAGE and circular dichroism spectroscopy were also all found to be comparable between methods. When comparing CroFab batches that were reconstituted using the labeled and modified methods, the physicochemical and biological (potency) characteristics of CroFab were not significantly changed when challenged by the various standard analytical methodologies applied in routine quality control analysis. Additionally, no changes in the CroFab molecule regarding degradation, aggregation, purity, structure, or mass were observed. The analyses performed validated the use of the more rapid reconstitution method using 18 mL 0.9% saline in order to allow a significantly reduced time to administration of CroFab to patients in need. Copyright © 2013 Elsevier Ltd. All rights reserved.

Integration of gas chromatography mass spectrometry methods for differentiating ricin preparation methods.

PubMed

Wunschel, David S; Melville, Angela M; Ehrhardt, Christopher J; Colburn, Heather A; Victry, Kristin D; Antolick, Kathryn C; Wahl, Jon H; Wahl, Karen L

2012-05-07

The investigation of crimes involving chemical or biological agents is infrequent, but presents unique analytical challenges. The protein toxin ricin is encountered more frequently than other agents and is found in the seeds of Ricinus communis, commonly known as the castor plant. Typically, the toxin is extracted from castor seeds utilizing a variety of different recipes that result in varying purity of the toxin. Moreover, these various purification steps can also leave or differentially remove a variety of exogenous and endogenous residual components with the toxin that may indicate the type and number of purification steps involved. We have applied three gas chromatography-mass spectrometry (GC-MS) based analytical methods to measure the variation in seed carbohydrates and castor oil ricinoleic acid, as well as the presence of solvents used for purification. These methods were applied to the same samples prepared using four previously identified toxin preparation methods, starting from four varieties of castor seeds. The individual data sets for seed carbohydrate profiles, ricinoleic acid, or acetone amount each provided information capable of differentiating different types of toxin preparations across seed types. However, the integration of the data sets using multivariate factor analysis provided a clear distinction of all samples based on the preparation method, independent of the seed source. In particular, the abundance of mannose, arabinose, fucose, ricinoleic acid, and acetone were shown to be important differentiating factors. These complementary tools provide a more confident determination of the method of toxin preparation than would be possible using a single analytical method.

Determination of the aerosol size distribution by analytic inversion of the extinction spectrum in the complex anomalous diffraction approximation.

PubMed

Franssens, G; De Maziére, M; Fonteyn, D

2000-08-20

A new derivation is presented for the analytical inversion of aerosol spectral extinction data to size distributions. It is based on the complex analytic extension of the anomalous diffraction approximation (ADA). We derive inverse formulas that are applicable to homogeneous nonabsorbing and absorbing spherical particles. Our method simplifies, generalizes, and unifies a number of results obtained previously in the literature. In particular, we clarify the connection between the ADA transform and the Fourier and Laplace transforms. Also, the effect of the particle refractive-index dispersion on the inversion is examined. It is shown that, when Lorentz's model is used for this dispersion, the continuous ADA inverse transform is mathematically well posed, whereas with a constant refractive index it is ill posed. Further, a condition is given, in terms of Lorentz parameters, for which the continuous inverse operator does not amplify the error.

Validation of a BOTDR-based system for the detection of smuggling tunnels

NASA Astrophysics Data System (ADS)

Elkayam, Itai; Klar, Assaf; Linker, Raphael; Marshall, Alec M.

2010-04-01

Cross-border smuggling tunnels enable unmonitored movement of people, drugs and weapons and pose a very serious threat to homeland security. Recently, Klar and Linker (2009) [SPIE paper No. 731603] presented an analytical study of the feasibility of a Brillouin Optical Time Domain Reflectometry (BOTDR) based system for the detection of small sized smuggling tunnels. The current study extends this work by validating the analytical models against real strain measurements in soil obtained from small scale experiments in a geotechnical centrifuge. The soil strains were obtained using an image analysis method that tracked the displacement of discrete patches of soil through a sequence of digital images of the soil around the tunnel during the centrifuge test. The results of the present study are in agreement with those of a previous study which was based on synthetic signals generated using empirical and analytical models from the literature.

Molecular properties of excited electronic state: Formalism, implementation, and applications of analytical second energy derivatives within the framework of the time-dependent density functional theory/molecular mechanics

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

Zeng, Qiao; Liang, WanZhen, E-mail: liangwz@xmu.edu.cn; Liu, Jie

2014-05-14

This work extends our previous works [J. Liu and W. Z. Liang, J. Chem. Phys. 135, 014113 (2011); J. Liu and W. Z. Liang, J. Chem. Phys. 135, 184111 (2011)] on analytical excited-state energy Hessian within the framework of time-dependent density functional theory (TDDFT) to couple with molecular mechanics (MM). The formalism, implementation, and applications of analytical first and second energy derivatives of TDDFT/MM excited state with respect to the nuclear and electric perturbations are presented. Their performances are demonstrated by the calculations of adiabatic excitation energies, and excited-state geometries, harmonic vibrational frequencies, and infrared intensities for a number ofmore » benchmark systems. The consistent results with the full quantum mechanical method and other hybrid theoretical methods indicate the reliability of the current numerical implementation of developed algorithms. The computational accuracy and efficiency of the current analytical approach are also checked and the computational efficient strategies are suggested to speed up the calculations of complex systems with many MM degrees of freedom. Finally, we apply the current analytical approach in TDDFT/MM to a realistic system, a red fluorescent protein chromophore together with part of its nearby protein matrix. The calculated results indicate that the rearrangement of the hydrogen bond interactions between the chromophore and the protein matrix is responsible for the large Stokes shift.« less

Extrapolation of scattering data to the negative-energy region. II. Applicability of effective range functions within an exactly solvable model

DOE PAGES

Blokhintsev, L. D.; Kadyrov, A. S.; Mukhamedzhanov, A. M.; ...

2018-02-05

A problem of analytical continuation of scattering data to the negative-energy region to obtain information about bound states is discussed within an exactly solvable potential model. This work is continuation of the previous one by the same authors [L. D. Blokhintsev et al., Phys. Rev. C 95, 044618 (2017)]. The goal of this paper is to determine the most effective way of analytic continuation for different systems. The d + α and α + 12C systems are considered and, for comparison, an effective-range function approach and a recently suggested Δ method [O. L. Ramírez Suárez and J.-M. Sparenberg, Phys. Rev.more » C 96, 034601 (2017).] are applied. We conclude that the method is more effective for heavier systems with large values of the Coulomb parameter, whereas for light systems with small values of the Coulomb parameter the effective-range function method might be preferable.« less

Extrapolation of scattering data to the negative-energy region. II. Applicability of effective range functions within an exactly solvable model

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

Blokhintsev, L. D.; Kadyrov, A. S.; Mukhamedzhanov, A. M.

A problem of analytical continuation of scattering data to the negative-energy region to obtain information about bound states is discussed within an exactly solvable potential model. This work is continuation of the previous one by the same authors [L. D. Blokhintsev et al., Phys. Rev. C 95, 044618 (2017)]. The goal of this paper is to determine the most effective way of analytic continuation for different systems. The d + α and α + 12C systems are considered and, for comparison, an effective-range function approach and a recently suggested Δ method [O. L. Ramírez Suárez and J.-M. Sparenberg, Phys. Rev.more » C 96, 034601 (2017).] are applied. We conclude that the method is more effective for heavier systems with large values of the Coulomb parameter, whereas for light systems with small values of the Coulomb parameter the effective-range function method might be preferable.« less

Development of a Novel Method for in vivo Determination of Activation Energy of Glucose Transport Across S. cerevisiae Cellular Membranes. A Biosensor-like Approach.

PubMed

Kormes, Diego J; Cortón, Eduardo

2009-01-01

Whereas biosensors have been usually proposed as analytical tools, used to investigate the surrounding media pursuing an analytical answer, we have used a biosensor-like device to characterize the microbial cells immobilized on it. We have studied the kinetics of transport and degradation of glucose at different concentrations and temperatures. When glucose concentrations of 15 and 1.5 mM were assayed, calculated activation energies were 25.2 and 18.4 kcal mol(-1), respectively, in good agreement with previously published data. The opportunity and convenience of using Arrhenius plots to estimate the activation energy in metabolic-related processes is also discussed.

Prediction of light aircraft interior noise

NASA Technical Reports Server (NTRS)

Howlett, J. T.; Morales, D. A.

1976-01-01

At the present time, predictions of aircraft interior noise depend heavily on empirical correction factors derived from previous flight measurements. However, to design for acceptable interior noise levels and to optimize acoustic treatments, analytical techniques which do not depend on empirical data are needed. This paper describes a computerized interior noise prediction method for light aircraft. An existing analytical program (developed for commercial jets by Cockburn and Jolly in 1968) forms the basis of some modal analysis work which is described. The accuracy of this modal analysis technique for predicting low-frequency coupled acoustic-structural natural frequencies is discussed along with trends indicating the effects of varying parameters such as fuselage length and diameter, structural stiffness, and interior acoustic absorption.

Determination of Global Stability of the Slosh Motion in a Spacecraft via Num Erical Experiment

NASA Astrophysics Data System (ADS)

Kang, Ja-Young

2003-12-01

The global stability of the attitude motion of a spin-stabilized space vehicle is investigated by performing numerical experiment. In the previous study, a stationary solution and a particular resonant condition for a given model were found by using analytical method but failed to represent the system stability over parameter values near and off the stationary points. Accordingly, as an extension of the previous work, this study performs numerical experiment to investigate the stability of the system across the parameter space and determines stable and unstable regions of the design parameters of the system.

The motions and wave fields produced by an ellipse moving through a stratified fluid

NASA Astrophysics Data System (ADS)

Hurlen, Erik Curtis

Solid-fluid interactions are ubiquitous in nature, from leaves falling from trees to fish swimming in the ocean. This dissertation examines a certain class of these interactions, namely asymmetric objects moving through stratified fluids. In the first part, the equations of motion are derived and subsequently solved for a displaced neutrally buoyant ellipse of varying aspect ratio. This is accomplished by using a spectral numerical algorithm, although in certain specific cases the equations can also be solved analytically using Laplace transform techniques. Experiments are conducted to which these analytical and numerical results are compared. General quantitative agreement is observed between the two sets of data. The discrepancies which are observed are consistent with both previous research and expectation. In the second part, the focus is shifted from the solid to the fluid, as the primary concern is now the wave field produced by these moving bodies. The spectral method developed in the first part is easily adapted to this second situation, in which the drag forces on the solid are also easily extracted. The results from this section are compared to previous results, and match very well. The results are then expanded to cases which have not been previously studied.

An analytical method to predict efficiency of aircraft gearboxes

NASA Technical Reports Server (NTRS)

Anderson, N. E.; Loewenthal, S. H.; Black, J. D.

1984-01-01

A spur gear efficiency prediction method previously developed by the authors was extended to include power loss of planetary gearsets. A friction coefficient model was developed for MIL-L-7808 oil based on disc machine data. This combined with the recent capability of predicting losses in spur gears of nonstandard proportions allows the calculation of power loss for complete aircraft gearboxes that utilize spur gears. The method was applied to the T56/501 turboprop gearbox and compared with measured test data. Bearing losses were calculated with large scale computer programs. Breakdowns of the gearbox losses point out areas for possible improvement.

Reply to Comment by Roques et al. on "Base Flow Recession from Unsaturated-Saturated Porous Media considering Lateral Unsaturated Discharge and Aquifer Compressibility"

NASA Astrophysics Data System (ADS)

Liang, Xiuyu; Zhan, Hongbin; Zhang, You-Kuan; Schilling, Keith

2018-04-01

Roques et al. (https://doi.org/10.1002/2017WR022085) claims that they have proposed an exponential time step (ETS) method to improve the computing method of Liang et al. (https://doi.org/10.1002/2017WR020938) which used a constant time step (CTS) method on the derivative for dQ/dt in field data, where Q is the base flow discharge and t is the time since the start of base flow recession. This reply emphasizes that the main objective of Liang et al. (https://doi.org/10.1002/2017WR020938) was to develop an analytical model to investigate the effects of the unsaturated flow on base flow recession, not on the data interpretation methods. The analytical model indicates that the base flow recession hydrograph behaves as dQ/dt ˜aQb with the exponent b close to 1 at late times, which is consistent with previous theoretical models. The model of Liang et al. (https://doi.org/10.1002/2017WR020938) was applied to field data where the derivative of dQ/dt was computed using the CTS method, a method that has been widely adopted in previous studies. The ETS method proposed by Roques et al. (https://doi.org/10.1016/j.advwatres.2017.07.013) appears to be a good alternative but its accuracy needs further validation. Using slopes to fit field data as proposed by Roques et al. (https://doi.org/10.1002/2017WR022085) appears to match data satisfactorily at early times whereas it performs less satisfactorily at late times and leads to the exponent b being obviously larger than 1.

Tensor scale: An analytic approach with efficient computation and applications☆

PubMed Central

Xu, Ziyue; Saha, Punam K.; Dasgupta, Soura

2015-01-01

Scale is a widely used notion in computer vision and image understanding that evolved in the form of scale-space theory where the key idea is to represent and analyze an image at various resolutions. Recently, we introduced a notion of local morphometric scale referred to as “tensor scale” using an ellipsoidal model that yields a unified representation of structure size, orientation and anisotropy. In the previous work, tensor scale was described using a 2-D algorithmic approach and a precise analytic definition was missing. Also, the application of tensor scale in 3-D using the previous framework is not practical due to high computational complexity. In this paper, an analytic definition of tensor scale is formulated for n-dimensional (n-D) images that captures local structure size, orientation and anisotropy. Also, an efficient computational solution in 2- and 3-D using several novel differential geometric approaches is presented and the accuracy of results is experimentally examined. Also, a matrix representation of tensor scale is derived facilitating several operations including tensor field smoothing to capture larger contextual knowledge. Finally, the applications of tensor scale in image filtering and n-linear interpolation are presented and the performance of their results is examined in comparison with respective state-of-art methods. Specifically, the performance of tensor scale based image filtering is compared with gradient and Weickert’s structure tensor based diffusive filtering algorithms. Also, the performance of tensor scale based n-linear interpolation is evaluated in comparison with standard n-linear and windowed-sinc interpolation methods. PMID:26236148

Liquid Metering Centrifuge Sticks (LMCS): A Centrifugal Approach to Metering Known Sample Volumes for Colorimetric Solid Phase Extraction (C-SPE)

NASA Technical Reports Server (NTRS)

Gazda, Daniel B.; Schultz, John R.; Clarke, Mark S.

2007-01-01

Phase separation is one of the most significant obstacles encountered during the development of analytical methods for water quality monitoring in spacecraft environments. Removing air bubbles from water samples prior to analysis is a routine task on earth; however, in the absence of gravity, this routine task becomes extremely difficult. This paper details the development and initial ground testing of liquid metering centrifuge sticks (LMCS), devices designed to collect and meter a known volume of bubble-free water in microgravity. The LMCS uses centrifugal force to eliminate entrapped air and reproducibly meter liquid sample volumes for analysis with Colorimetric Solid Phase Extraction (C-SPE). C-SPE is a sorption-spectrophotometric platform that is being developed as a potential spacecraft water quality monitoring system. C-SPE utilizes solid phase extraction membranes impregnated with analyte-specific colorimetric reagents to concentrate and complex target analytes in spacecraft water samples. The mass of analyte extracted from the water sample is determined using diffuse reflectance (DR) data collected from the membrane surface and an analyte-specific calibration curve. The analyte concentration can then be calculated from the mass of extracted analyte and the volume of the sample analyzed. Previous flight experiments conducted in microgravity conditions aboard the NASA KC-135 aircraft demonstrated that the inability to collect and meter a known volume of water using a syringe was a limiting factor in the accuracy of C-SPE measurements. Herein, results obtained from ground based C-SPE experiments using ionic silver as a test analyte and either the LMCS or syringes for sample metering are compared to evaluate the performance of the LMCS. These results indicate very good agreement between the two sample metering methods and clearly illustrate the potential of utilizing centrifugal forces to achieve phase separation and metering of water samples in microgravity.

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory

NASA Astrophysics Data System (ADS)

Bozkaya, Uǧur

2013-09-01

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory (OMP3) [U. Bozkaya, J. Chem. Phys. 135, 224103 (2011)], 10.1063/1.3665134 are presented. The OMP3 method is applied to problematic chemical systems with challenging electronic structures. The performance of the OMP3 method is compared with those of canonical second-order Møller-Plesset perturbation theory (MP2), third-order Møller-Plesset perturbation theory (MP3), coupled-cluster singles and doubles (CCSD), and coupled-cluster singles and doubles with perturbative triples [CCSD(T)] for investigating equilibrium geometries, vibrational frequencies, and open-shell reaction energies. For bond lengths, the performance of OMP3 is in between those of MP3 and CCSD. For harmonic vibrational frequencies, the OMP3 method significantly eliminates the singularities arising from the abnormal response contributions observed for MP3 in case of symmetry-breaking problems, and provides noticeably improved vibrational frequencies for open-shell molecules. For open-shell reaction energies, OMP3 exhibits a better performance than MP3 and CCSD as in case of barrier heights and radical stabilization energies. As discussed in previous studies, the OMP3 method is several times faster than CCSD in energy computations. Further, in analytic gradient computations for the CCSD method one needs to solve λ-amplitude equations, however for OMP3 one does not since λ _{ab}^{ij(1)} = t_{ij}^{ab(1)} and λ _{ab}^{ij(2)} = t_{ij}^{ab(2)}. Additionally, one needs to solve orbital Z-vector equations for CCSD, but for OMP3 orbital response contributions are zero owing to the stationary property of OMP3. Overall, for analytic gradient computations the OMP3 method is several times less expensive than CCSD (roughly ˜4-6 times). Considering the balance of computational cost and accuracy we conclude that the OMP3 method emerges as a very useful tool for the study of electronically challenging chemical systems.

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory.

PubMed

Bozkaya, Uğur

2013-09-14

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory (OMP3) [U. Bozkaya, J. Chem. Phys. 135, 224103 (2011)] are presented. The OMP3 method is applied to problematic chemical systems with challenging electronic structures. The performance of the OMP3 method is compared with those of canonical second-order Møller-Plesset perturbation theory (MP2), third-order Møller-Plesset perturbation theory (MP3), coupled-cluster singles and doubles (CCSD), and coupled-cluster singles and doubles with perturbative triples [CCSD(T)] for investigating equilibrium geometries, vibrational frequencies, and open-shell reaction energies. For bond lengths, the performance of OMP3 is in between those of MP3 and CCSD. For harmonic vibrational frequencies, the OMP3 method significantly eliminates the singularities arising from the abnormal response contributions observed for MP3 in case of symmetry-breaking problems, and provides noticeably improved vibrational frequencies for open-shell molecules. For open-shell reaction energies, OMP3 exhibits a better performance than MP3 and CCSD as in case of barrier heights and radical stabilization energies. As discussed in previous studies, the OMP3 method is several times faster than CCSD in energy computations. Further, in analytic gradient computations for the CCSD method one needs to solve λ-amplitude equations, however for OMP3 one does not since λ(ab)(ij(1))=t(ij)(ab(1)) and λ(ab)(ij(2))=t(ij)(ab(2)). Additionally, one needs to solve orbital Z-vector equations for CCSD, but for OMP3 orbital response contributions are zero owing to the stationary property of OMP3. Overall, for analytic gradient computations the OMP3 method is several times less expensive than CCSD (roughly ~4-6 times). Considering the balance of computational cost and accuracy we conclude that the OMP3 method emerges as a very useful tool for the study of electronically challenging chemical systems.

Calculation of Thermal Conductivity Coefficients of Electrons in Magnetized Dense Matter

NASA Astrophysics Data System (ADS)

Bisnovatyi-Kogan, G. S.; Glushikhina, M. V.

2018-04-01

The solution of Boltzmann equation for plasma in magnetic field with arbitrarily degenerate electrons and nondegenerate nuclei is obtained by Chapman-Enskog method. Functions generalizing Sonine polynomials are used for obtaining an approximate solution. Fully ionized plasma is considered. The tensor of the heat conductivity coefficients in nonquantized magnetic field is calculated. For nondegenerate and strongly degenerate plasma the asymptotic analytic formulas are obtained and compared with results of previous authors. The Lorentz approximation with neglecting of electron-electron encounters is asymptotically exact for strongly degenerate plasma. For the first time, analytical expressions for the heat conductivity tensor for nondegenerate electrons in the presence of a magnetic field are obtained in the three-polynomial approximation with account of electron-electron collisions. Account of the third polynomial improved substantially the precision of results. In the two-polynomial approximation, the obtained solution coincides with the published results. For strongly degenerate electrons, an asymptotically exact analytical solution for the heat conductivity tensor in the presence of a magnetic field is obtained for the first time. This solution has a considerably more complicated dependence on the magnetic field than those in previous publications and gives a several times smaller relative value of the thermal conductivity across the magnetic field at ωτ * 0.8.

Targeted analyte deconvolution and identification by four-way parallel factor analysis using three-dimensional gas chromatography with mass spectrometry data.

PubMed

Watson, Nathanial E; Prebihalo, Sarah E; Synovec, Robert E

2017-08-29

Comprehensive three-dimensional gas chromatography with time-of-flight mass spectrometry (GC 3 -TOFMS) creates an opportunity to explore a new paradigm in chemometric analysis. Using this newly described instrument and the well understood Parallel Factor Analysis (PARAFAC) model we present one option for utilization of the novel GC 3 -TOFMS data structure. We present a method which builds upon previous work in both GC 3 and targeted analysis using PARAFAC to simplify some of the implementation challenges previously discovered. Conceptualizing the GC 3 -TOFMS instead as a one-dimensional gas chromatograph with GC × GC-TOFMS detection we allow the instrument to create the PARAFAC target window natively. Each first dimension modulation thus creates a full GC × GC-TOFMS chromatogram fully amenable to PARAFAC. A simple mixture of 115 compounds and a diesel sample are interrogated through this methodology. All test analyte targets are successfully identified in both mixtures. In addition, mass spectral matching of the PARAFAC loadings to library spectra yielded results greater than 900 in 40 of 42 test analyte cases. Twenty-nine of these cases produced match values greater than 950. Copyright © 2017 Elsevier B.V. All rights reserved.

Systems-Level Annotation of a Metabolomics Data Set Reduces 25 000 Features to Fewer than 1000 Unique Metabolites.

PubMed

Mahieu, Nathaniel G; Patti, Gary J

2017-10-03

When using liquid chromatography/mass spectrometry (LC/MS) to perform untargeted metabolomics, it is now routine to detect tens of thousands of features from biological samples. Poor understanding of the data, however, has complicated interpretation and masked the number of unique metabolites actually being measured in an experiment. Here we place an upper bound on the number of unique metabolites detected in Escherichia coli samples analyzed with one untargeted metabolomics method. We first group multiple features arising from the same analyte, which we call "degenerate features", using a context-driven annotation approach. Surprisingly, this analysis revealed thousands of previously unreported degeneracies that reduced the number of unique analytes to ∼2961. We then applied an orthogonal approach to remove nonbiological features from the data using the 13 C-based credentialing technology. This further reduced the number of unique analytes to less than 1000. Our 90% reduction in data is 5-fold greater than previously published studies. On the basis of the results, we propose an alternative approach to untargeted metabolomics that relies on thoroughly annotated reference data sets. To this end, we introduce the creDBle database ( http://creDBle.wustl.edu ), which contains accurate mass, retention time, and MS/MS fragmentation data as well as annotations of all credentialed features.

Comparative artificial neural network and partial least squares models for analysis of Metronidazole, Diloxanide, Spiramycin and Cliquinol in pharmaceutical preparations.

PubMed

Elkhoudary, Mahmoud M; Abdel Salam, Randa A; Hadad, Ghada M

2014-09-15

Metronidazole (MNZ) is a widely used antibacterial and amoebicide drug. Therefore, it is important to develop a rapid and specific analytical method for the determination of MNZ in mixture with Spiramycin (SPY), Diloxanide (DIX) and Cliquinol (CLQ) in pharmaceutical preparations. This work describes simple, sensitive and reliable six multivariate calibration methods, namely linear and nonlinear artificial neural networks preceded by genetic algorithm (GA-ANN) and principle component analysis (PCA-ANN) as well as partial least squares (PLS) either alone or preceded by genetic algorithm (GA-PLS) for UV spectrophotometric determination of MNZ, SPY, DIX and CLQ in pharmaceutical preparations with no interference of pharmaceutical additives. The results manifest the problem of nonlinearity and how models like ANN can handle it. Analytical performance of these methods was statistically validated with respect to linearity, accuracy, precision and specificity. The developed methods indicate the ability of the previously mentioned multivariate calibration models to handle and solve UV spectra of the four components' mixtures using easy and widely used UV spectrophotometer. Copyright © 2014 Elsevier B.V. All rights reserved.

Computing the Evans function via solving a linear boundary value ODE

NASA Astrophysics Data System (ADS)

Wahl, Colin; Nguyen, Rose; Ventura, Nathaniel; Barker, Blake; Sandstede, Bjorn

2015-11-01

Determining the stability of traveling wave solutions to partial differential equations can oftentimes be computationally intensive but of great importance to understanding the effects of perturbations on the physical systems (chemical reactions, hydrodynamics, etc.) they model. For waves in one spatial dimension, one may linearize around the wave and form an Evans function - an analytic Wronskian-like function which has zeros that correspond in multiplicity to the eigenvalues of the linearized system. If eigenvalues with a positive real part do not exist, the traveling wave will be stable. Two methods exist for calculating the Evans function numerically: the exterior-product method and the method of continuous orthogonalization. The first is numerically expensive, and the second reformulates the originally linear system as a nonlinear system. We develop a new algorithm for computing the Evans function through appropriate linear boundary-value problems. This algorithm is cheaper than the previous methods, and we prove that it preserves analyticity of the Evans function. We also provide error estimates and implement it on some classical one- and two-dimensional systems, one being the Swift-Hohenberg equation in a channel, to show the advantages.

Analytical methods for determination of mycotoxins: An update (2009-2014).

PubMed

Turner, Nicholas W; Bramhmbhatt, Heli; Szabo-Vezse, Monika; Poma, Alessandro; Coker, Raymond; Piletsky, Sergey A

2015-12-11

Mycotoxins are a problematic and toxic group of small organic molecules that are produced as secondary metabolites by several fungal species that colonise crops. They lead to contamination at both the field and postharvest stages of food production with a considerable range of foodstuffs affected, from coffee and cereals, to dried fruit and spices. With wide ranging structural diversity of mycotoxins, severe toxic effects caused by these molecules and their high chemical stability the requirement for robust and effective detection methods is clear. This paper builds on our previous review and summarises the most recent advances in this field, in the years 2009-2014 inclusive. This review summarises traditional methods such as chromatographic and immunochemical techniques, as well as newer approaches such as biosensors, and optical techniques which are becoming more prevalent. A section on sampling and sample treatment has been prepared to highlight the importance of this step in the analytical methods. We close with a look at emerging technologies that will bring effective and rapid analysis out of the laboratory and into the field. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparative artificial neural network and partial least squares models for analysis of Metronidazole, Diloxanide, Spiramycin and Cliquinol in pharmaceutical preparations

NASA Astrophysics Data System (ADS)

Elkhoudary, Mahmoud M.; Abdel Salam, Randa A.; Hadad, Ghada M.

2014-09-01

Metronidazole (MNZ) is a widely used antibacterial and amoebicide drug. Therefore, it is important to develop a rapid and specific analytical method for the determination of MNZ in mixture with Spiramycin (SPY), Diloxanide (DIX) and Cliquinol (CLQ) in pharmaceutical preparations. This work describes simple, sensitive and reliable six multivariate calibration methods, namely linear and nonlinear artificial neural networks preceded by genetic algorithm (GA-ANN) and principle component analysis (PCA-ANN) as well as partial least squares (PLS) either alone or preceded by genetic algorithm (GA-PLS) for UV spectrophotometric determination of MNZ, SPY, DIX and CLQ in pharmaceutical preparations with no interference of pharmaceutical additives. The results manifest the problem of nonlinearity and how models like ANN can handle it. Analytical performance of these methods was statistically validated with respect to linearity, accuracy, precision and specificity. The developed methods indicate the ability of the previously mentioned multivariate calibration models to handle and solve UV spectra of the four components’ mixtures using easy and widely used UV spectrophotometer.

Detecting a wide range of environmental contaminants in human blood samples--combining QuEChERS with LC-MS and GC-MS methods.

PubMed

Plassmann, Merle M; Schmidt, Magdalena; Brack, Werner; Krauss, Martin

2015-09-01

Exposure to environmental pollution and consumer products may result in an uptake of chemicals into human tissues. Several studies have reported the presence of diverse environmental contaminants in human blood samples. However, previously developed multi-target methods for the analysis of human blood include a fairly limited amount of compounds stemming from one or two related compound groups. Thus, the sample preparation method QuEChERS (quick easy cheap effective rugged and safe) was tested for the extraction of 64 analytes covering a broad compound domain followed by detection using liquid and gas chromatography coupled to mass spectrometry (LC- and GC-MS). Forty-seven analytes showed absolute recoveries above 70% in the first QuEChERS step, being a simple liquid-liquid extraction (LLE) using acetonitrile and salt. The second QuEChERS step, being a dispersive solid phase extraction, did not result in an overall improvement of recoveries or removal of background signals. Using solely the LLE step, eight analytes could subsequently be detected in human blood samples from the German Environmental Specimen Bank. Using a LC-multiple reaction monitoring (MRM) method with a triple quadrupole instrument, better recoveries were achieved than with an older LC-high-resolution (HR) MS full scan orbitrap instrument, which required a higher concentration factor of the extracts. However, the application of HRMS full scan methods could be used for the detection of additional compounds retrospectively.

Improvement of ion chromatography with ultraviolet photometric detection and comparison with conductivity detection for the determination of serum cations.

PubMed

Shintani, H

1985-05-31

Studies were made of the analytical conditions required for indirect photometric ion chromatography using ultraviolet photometric detection (UV method) for the determination of serum cations following a previously developed serum pre-treatment. The sensitivities of the conductivity detection (CD) and UV methods and the amounts of serum cations determined by both methods were compared. Attempts to improve the sensitivity of the conventional UV method are reported. It was found that the mobile phase previously reported by Small and Miller showed no quantitative response when more than 4 mM copper(II) sulphate pentahydrate was used. As a result, there was no significant difference in the amounts of serum cations shown by the CD and UV methods. However, by adding 0.5-5 mM cobalt(II) sulphate heptahydrate, nickel(II) sulphate hexahydrate, zinc(II) sulphate heptahydrate or cobalt(II) diammonium sulphate hexahydrate to 0.5-1.5 mM copper(II) sulphate pentahydrate, higher sensitivity and a quantitative response were attained.

Surface-Enhanced Raman Scattering (SERS) for Detection in Immunoassays. Applications, fundamentals, and optimization

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

Driskell, Jeremy Daniel

2006-08-09

Immunoassays have been utilized for the detection of biological analytes for several decades. Many formats and detection strategies have been explored, each having unique advantages and disadvantages. More recently, surface-enhanced Raman scattering (SERS) has been introduced as a readout method for immunoassays, and has shown great potential to meet many key analytical figures of merit. This technology is in its infancy and this dissertation explores the diversity of this method as well as the mechanism responsible for surface enhancement. Approaches to reduce assay times are also investigated. Implementing the knowledge gained from these studies will lead to a more sensitivemore » immunoassay requiring less time than its predecessors. This dissertation is organized into six sections. The first section includes a literature review of the previous work that led to this dissertation. A general overview of the different approaches to immunoassays is given, outlining the strengths and weaknesses of each. Included is a detailed review of binding kinetics, which is central for decreasing assay times. Next, the theoretical underpinnings of SERS is reviewed at its current level of understanding. Past work has argued that surface plasmon resonance (SPR) of the enhancing substrate influences the SERS signal; therefore, the SPR of the extrinsic Raman labels (ERLs) utilized in our SERS-based immunoassay is discussed. Four original research chapters follow the Introduction, each presented as separate manuscripts. Chapter 2 modifies a SERS-based immunoassay previously developed in our group, extending it to the low-level detection of viral pathogens and demonstrating its versatility in terms of analyte type, Chapter 3 investigates the influence of ERL size, material composition, and separation distance between the ERLs and capture substrate on the SERS signal. This chapter links SPR with SERS enhancement factors and is consistent with many of the results from theoretical treatments of SPR and SERS. Chapter 4 introduces a novel method of reducing sample incubation time via capture substrate rotation. Moreover, this work led to a method of virus quantification without the use of standards. Chapter 5 extends the methodology developed in Chapter 4 to both the antigen and ERL labeling step to perform assays with improved analytical performance in less time than can be accomplished in diffusion controlled assays. This dissertation concludes with a general summary and speculates on the future of this exciting approach to carrying out immunoassays.« less

On Bayesian Testing of Additive Conjoint Measurement Axioms Using Synthetic Likelihood.

PubMed

Karabatsos, George

2018-06-01

This article introduces a Bayesian method for testing the axioms of additive conjoint measurement. The method is based on an importance sampling algorithm that performs likelihood-free, approximate Bayesian inference using a synthetic likelihood to overcome the analytical intractability of this testing problem. This new method improves upon previous methods because it provides an omnibus test of the entire hierarchy of cancellation axioms, beyond double cancellation. It does so while accounting for the posterior uncertainty that is inherent in the empirical orderings that are implied by these axioms, together. The new method is illustrated through a test of the cancellation axioms on a classic survey data set, and through the analysis of simulated data.

Determining the Depth of Infinite Horizontal Cylindrical Sources from Spontaneous Polarization Data

NASA Astrophysics Data System (ADS)

Cooper, G. R. J.; Stettler, E. H.

2017-03-01

Previously published semi-automatic interpretation methods that use ratios of analytic signal amplitudes of orders that differ by one to determine the distance to potential field sources are shown also to apply to self-potential (S.P.) data when the source is a horizontal cylinder. Local minima of the distance (when it becomes closest to zero) give the source depth. The method was applied to an S.P. anomaly from the Bourkes Luck potholes district in Mpumalanga Province, South Africa, and gave results that were confirmed by drilling.

Thermal desorption of metals from tungsten single crystal surfaces

NASA Technical Reports Server (NTRS)

Bauer, E.; Bonczek, F.; Poppa, H.; Todd, G.

1975-01-01

After a short review of experimental methods used to determine desorption energies and frequencies the assumptions underlying the theoretical analysis of experimental data are discussed. Recent experimental results on the flash desorption of Cu, Ag, and Au from clean, well characterized W (110) and (100) surfaces are presented and analyzed in detail with respect to the coverage dependence. The results obtained clearly reveal the limitations of previous analytical methods and of the experimental technique per se (such as structure and phase changes below and in the temperature region in which desorption occurs).

On the Local Convergence of Pattern Search

NASA Technical Reports Server (NTRS)

Dolan, Elizabeth D.; Lewis, Robert Michael; Torczon, Virginia; Bushnell, Dennis M. (Technical Monitor)

2000-01-01

We examine the local convergence properties of pattern search methods, complementing the previously established global convergence properties for this class of algorithms. We show that the step-length control parameter which appears in the definition of pattern search algorithms provides a reliable asymptotic measure of first-order stationarity. This gives an analytical justification for a traditional stopping criterion for pattern search methods. Using this measure of first-order stationarity, we analyze the behavior of pattern search in the neighborhood of an isolated local minimizer. We show that a recognizable subsequence converges r-linearly to the minimizer.

Electronic response to nuclear breathing mode

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

Ludwig, Hendrik; Ruffini, Remo; ICRANet, University of Nice-Sophia Antipolis, 28 Av. de Valrose, 06103 Nice Cedex 2

2015-12-17

Based on our previous work on stationary oscillation modes of electrons around giant nuclei, we show how to treat a general driving force on the electron gas, such as the one generated by the breathing mode of the nucleus, by means of the spectral method. As an example we demonstrate this method for a system with Z = 10{sup 4} in β-equilibrium with the electrons compressed up to the nuclear radius. In this case the stationary modes can be obtained analytically, which allows for a very speedy numerical calculation of the final result.

General Relativistic Precession in Small Solar System Bodies

NASA Astrophysics Data System (ADS)

Sekhar, Aswin; Werner, Stephanie; Hoffmann, Volker; Asher, David; Vaubaillon, Jeremie; Hajdukova, Maria; Li, Gongjie

2016-10-01

Introduction: One of the greatest successes of the Einstein's General Theory of Relativity (GR) was the correct prediction of the precession of perihelion of Mercury. The closed form expression to compute this precession tells us that substantial GR precession would occur only if the bodies have a combination of both moderately small perihelion distance and semi-major axis. Minimum Orbit Intersection Distance (MOID) is a quantity which helps us to understand the closest proximity of two orbits in space. Hence evaluating MOID is crucial to understand close encounters and collision scenarios better. In this work, we look at the possible scenarios where a small GR precession in argument of pericentre (ω) can create substantial changes in MOID for small bodies ranging from meteoroids to comets and asteroids.Analytical Approach and Numerical Integrations: Previous works have looked into neat analytical techniques to understand different collision scenarios and we use those standard expressions to compute MOID analytically. We find the nature of this mathematical function is such that a relatively small GR precession can lead to drastic changes in MOID values depending on the initial value of ω. Numerical integrations were done with package MERCURY incorporating the GR code to test the same effects. Numerical approach showed the same interesting relationship (as shown by analytical theory) between values of ω and the peaks/dips in MOID values. Previous works have shown that GR precession suppresses Kozai oscillations and this aspect was verified using our integrations. There is an overall agreement between both analytical and numerical methods.Summary and Discussion: We find that GR precession could play an important role in the calculations pertaining to MOID and close encounter scenarios in the case of certain small solar system bodies (depending on their initial orbital elements). Previous works have looked into impact probabilities and collision scenarios on planets from different small body populations. This work aims to find certain sub-sets of orbits where GR could play an interesting role. Certain parallels are drawn between the cases of asteroids, comets and small perihelion distance meteoroid streams.

Robust electroencephalogram phase estimation with applications in brain-computer interface systems.

PubMed

Seraj, Esmaeil; Sameni, Reza

2017-03-01

In this study, a robust method is developed for frequency-specific electroencephalogram (EEG) phase extraction using the analytic representation of the EEG. Based on recent theoretical findings in this area, it is shown that some of the phase variations-previously associated to the brain response-are systematic side-effects of the methods used for EEG phase calculation, especially during low analytical amplitude segments of the EEG. With this insight, the proposed method generates randomized ensembles of the EEG phase using minor perturbations in the zero-pole loci of narrow-band filters, followed by phase estimation using the signal's analytical form and ensemble averaging over the randomized ensembles to obtain a robust EEG phase and frequency. This Monte Carlo estimation method is shown to be very robust to noise and minor changes of the filter parameters and reduces the effect of fake EEG phase jumps, which do not have a cerebral origin. As proof of concept, the proposed method is used for extracting EEG phase features for a brain computer interface (BCI) application. The results show significant improvement in classification rates using rather simple phase-related features and a standard K-nearest neighbors and random forest classifiers, over a standard BCI dataset. The average performance was improved between 4-7% (in absence of additive noise) and 8-12% (in presence of additive noise). The significance of these improvements was statistically confirmed by a paired sample t-test, with 0.01 and 0.03 p-values, respectively. The proposed method for EEG phase calculation is very generic and may be applied to other EEG phase-based studies.

Gradient retention prediction of acid-base analytes in reversed phase liquid chromatography: a simplified approach for acetonitrile-water mobile phases.

PubMed

Andrés, Axel; Rosés, Martí; Bosch, Elisabeth

2014-11-28

In previous work, a two-parameter model to predict chromatographic retention of ionizable analytes in gradient mode was proposed. However, the procedure required some previous experimental work to get a suitable description of the pKa change with the mobile phase composition. In the present study this previous experimental work has been simplified. The analyte pKa values have been calculated through equations whose coefficients vary depending on their functional group. Forced by this new approach, other simplifications regarding the retention of the totally neutral and totally ionized species also had to be performed. After the simplifications were applied, new prediction values were obtained and compared with the previously acquired experimental data. The simplified model gave pretty good predictions while saving a significant amount of time and resources. Copyright © 2014 Elsevier B.V. All rights reserved.

Sample-independent approach to normalize two-dimensional data for orthogonality evaluation using whole separation space scaling.

PubMed

Jáčová, Jaroslava; Gardlo, Alžběta; Friedecký, David; Adam, Tomáš; Dimandja, Jean-Marie D

2017-08-18

Orthogonality is a key parameter that is used to evaluate the separation power of chromatography-based two-dimensional systems. It is necessary to scale the separation data before the assessment of the orthogonality. Current scaling approaches are sample-dependent, and the extent of the retention space that is converted into a normalized retention space is set according to the retention times of the first and last analytes contained in a unique sample to elute. The presence or absence of a highly retained analyte in a sample can thus significantly influence the amount of information (in terms of the total amount of separation space) contained in the normalized retention space considered for the calculation of the orthogonality. We propose a Whole Separation Space Scaling (WOSEL) approach that accounts for the whole separation space delineated by the analytical method, and not the sample. This approach enables an orthogonality-based evaluation of the efficiency of the analytical system that is independent of the sample selected. The WOSEL method was compared to two currently used orthogonality approaches through the evaluation of in silico-generated chromatograms and real separations of human biofluids and petroleum samples. WOSEL exhibits sample-to-sample stability values of 3.8% on real samples, compared to 7.0% and 10.1% for the two other methods, respectively. Using real analyses, we also demonstrate that some previously developed approaches can provide misleading conclusions on the overall orthogonality of a two-dimensional chromatographic system. Copyright © 2017 Elsevier B.V. All rights reserved.

Nano-flow vs standard-flow: Which is the more suitable LC/MS method for quantifying hepcidin-25 in human serum in routine clinical settings?

PubMed

Vialaret, Jérôme; Picas, Alexia; Delaby, Constance; Bros, Pauline; Lehmann, Sylvain; Hirtz, Christophe

2018-06-01

Hepcidin-25 peptide is a biomarker which is known to have considerable clinical potential for diagnosing iron-related diseases. Developing analytical methods for the absolute quantification of hepcidin is still a real challenge, however, due to the sensitivity, specificity and reproducibility issues involved. In this study, we compare and discuss two MS-based assays for quantifying hepcidin, which differ only in terms of the type of liquid chromatography (nano LC/MS versus standard LC/MS) involved. The same sample preparation, the same internal standards and the same MS analyzer were used with both approaches. In the field of proteomics, nano LC chromatography is generally known to be more sensitive and less robust than standard LC methods. In this study, we established that the performances of the standard LC method are equivalent to those of our previously developed nano LC method. Although the analytical performances were very similar in both cases. The standard-flow platform therefore provides the more suitable alternative for accurately determining hepcidin in clinical settings. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous stable carbon isotopic analysis of wine glycerol and ethanol by liquid chromatography coupled to isotope ratio mass spectrometry.

PubMed

Cabañero, Ana I; Recio, Jose L; Rupérez, Mercedes

2010-01-27

A novel procedure was established for the simultaneous characterization of wine glycerol and ethanol (13)C/(12)C isotope ratio, using liquid chromatography/isotope ratio mass spectrometry (LC-IRMS). Several parameters influencing separation of glycerol and ethanol from wine matrix were optimized. Results obtained for 35 Spanish samples exposed no significant differences and very strong correlations (r = 0.99) between the glycerol (13)C/(12)C ratios obtained by an alternative method (gas chromatography/isotope ratio mass spectrometry) and the proposed new methodology, and between the ethanol (13)C/(12)C ratios obtained by the official method (elemental analyzer/isotope ratio mass spectrometry) and the proposed new methodology. The accuracy of the proposed method varied from 0.01 to 0.19 per thousand, and the analytical precision was better than 0.25 per thousand. The new developed LC-IRMS method it is the first isotopic method that allows (13)C/(12)C determination of both analytes in the same run directly from a liquid sample with no previous glycerol or ethanol isolation, overcoming technical difficulties associated with complex sample treatment and improving in terms of simplicity and speed.

Nonlinear modelling of high-speed catenary based on analytical expressions of cable and truss elements

NASA Astrophysics Data System (ADS)

Song, Yang; Liu, Zhigang; Wang, Hongrui; Lu, Xiaobing; Zhang, Jing

2015-10-01

Due to the intrinsic nonlinear characteristics and complex structure of the high-speed catenary system, a modelling method is proposed based on the analytical expressions of nonlinear cable and truss elements. The calculation procedure for solving the initial equilibrium state is proposed based on the Newton-Raphson iteration method. The deformed configuration of the catenary system as well as the initial length of each wire can be calculated. Its accuracy and validity of computing the initial equilibrium state are verified by comparison with the separate model method, absolute nodal coordinate formulation and other methods in the previous literatures. Then, the proposed model is combined with a lumped pantograph model and a dynamic simulation procedure is proposed. The accuracy is guaranteed by the multiple iterative calculations in each time step. The dynamic performance of the proposed model is validated by comparison with EN 50318, the results of the finite element method software and SIEMENS simulation report, respectively. At last, the influence of the catenary design parameters (such as the reserved sag and pre-tension) on the dynamic performance is preliminarily analysed by using the proposed model.

Analytical quality by design: a tool for regulatory flexibility and robust analytics.

PubMed

Peraman, Ramalingam; Bhadraya, Kalva; Padmanabha Reddy, Yiragamreddy

2015-01-01

Very recently, Food and Drug Administration (FDA) has approved a few new drug applications (NDA) with regulatory flexibility for quality by design (QbD) based analytical approach. The concept of QbD applied to analytical method development is known now as AQbD (analytical quality by design). It allows the analytical method for movement within method operable design region (MODR). Unlike current methods, analytical method developed using analytical quality by design (AQbD) approach reduces the number of out-of-trend (OOT) results and out-of-specification (OOS) results due to the robustness of the method within the region. It is a current trend among pharmaceutical industry to implement analytical quality by design (AQbD) in method development process as a part of risk management, pharmaceutical development, and pharmaceutical quality system (ICH Q10). Owing to the lack explanatory reviews, this paper has been communicated to discuss different views of analytical scientists about implementation of AQbD in pharmaceutical quality system and also to correlate with product quality by design and pharmaceutical analytical technology (PAT).

Analytical Quality by Design: A Tool for Regulatory Flexibility and Robust Analytics

PubMed Central

Bhadraya, Kalva; Padmanabha Reddy, Yiragamreddy

2015-01-01

Very recently, Food and Drug Administration (FDA) has approved a few new drug applications (NDA) with regulatory flexibility for quality by design (QbD) based analytical approach. The concept of QbD applied to analytical method development is known now as AQbD (analytical quality by design). It allows the analytical method for movement within method operable design region (MODR). Unlike current methods, analytical method developed using analytical quality by design (AQbD) approach reduces the number of out-of-trend (OOT) results and out-of-specification (OOS) results due to the robustness of the method within the region. It is a current trend among pharmaceutical industry to implement analytical quality by design (AQbD) in method development process as a part of risk management, pharmaceutical development, and pharmaceutical quality system (ICH Q10). Owing to the lack explanatory reviews, this paper has been communicated to discuss different views of analytical scientists about implementation of AQbD in pharmaceutical quality system and also to correlate with product quality by design and pharmaceutical analytical technology (PAT). PMID:25722723

Development of a Novel Method for in vivo Determination of Activation Energy of Glucose Transport Across S. cerevisiae Cellular Membranes. A Biosensor-like Approach

PubMed Central

Kormes, Diego J.; Cortón, Eduardo

2009-01-01

Whereas biosensors have been usually proposed as analytical tools, used to investigate the surrounding media pursuing an analytical answer, we have used a biosensor-like device to characterize the microbial cells immobilized on it. We have studied the kinetics of transport and degradation of glucose at different concentrations and temperatures. When glucose concentrations of 15 and 1.5 mM were assayed, calculated activation energies were 25.2 and 18.4 kcal mol−1, respectively, in good agreement with previously published data. The opportunity and convenience of using Arrhenius plots to estimate the activation energy in metabolic-related processes is also discussed. PMID:22573975

Control of flexible beams using a free-free active truss

NASA Technical Reports Server (NTRS)

Clark, W. W.; Kimiavi, B.; Robertshaw, H. H.

1989-01-01

An analytical and experimental study involving controlling flexible beams using a free-free active truss is presented. This work extends previous work in controlling flexible continua with active trusses which were configured with fixed-free boundary conditions. The following describes the Lagrangian approach used to derive the equations of motion for the active truss and the beams attached to it. A partial-state feedback control law is derived for this system based on a full-state feedback Linear Quadratic Regulator method. The analytical model is examined via numerical simulations and the results are compared to a similar experimental apparatus described herein. The results show that control of a flexible continua is possible with a free-free active truss.

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

SAM Radiochemical Methods Query

EPA Pesticide Factsheets

Laboratories measuring target radiochemical analytes in environmental samples can use this online query tool to identify analytical methods in EPA's Selected Analytical Methods for Environmental Remediation and Recovery for select radiochemical analytes.

Determination of free sulphydryl groups in wheat gluten under the influence of different time and temperature of incubation: method validation.

PubMed

Rakita, Slađana; Pojić, Milica; Tomić, Jelena; Torbica, Aleksandra

2014-05-01

The aim of the present study was to determine the characteristics of an analytical method for determination of free sulphydryl (SH) groups of wheat gluten performed with previous gluten incubation for variable times (45, 90 and 135min) at variable temperatures (30 and 37°C), in order to determine its fitness-for-purpose. It was observed that the increase in temperature and gluten incubation time caused the increase in the amount of free SH groups, with more dynamic changes at 37°C. The method characteristics identified as relevant were: linearity, limit of detection, limit of quantification, precision (repeatability and reproducibility) and measurement uncertainty, which were checked within the validation protocol, while the method performance was monitored by X- and R-control charts. Identified method characteristics demonstrated its acceptable fitness-for-purpose, when assay included previous gluten incubation at 30°C. Although the method repeatability at 37°C was acceptable, the corresponding reproducibility did not meet the performance criterion on the basis of HORRAT value (HORRAT<2). Copyright © 2013 Elsevier Ltd. All rights reserved.

High precision analytical description of the allowed β spectrum shape

NASA Astrophysics Data System (ADS)

Hayen, Leendert; Severijns, Nathal; Bodek, Kazimierz; Rozpedzik, Dagmara; Mougeot, Xavier

2018-01-01

A fully analytical description of the allowed β spectrum shape is given in view of ongoing and planned measurements. Its study forms an invaluable tool in the search for physics beyond the standard electroweak model and the weak magnetism recoil term. Contributions stemming from finite size corrections, mass effects, and radiative corrections are reviewed. Particular focus is placed on atomic and chemical effects, where the existing description is extended and analytically provided. The effects of QCD-induced recoil terms are discussed, and cross-checks were performed for different theoretical formalisms. Special attention was given to a comparison of the treatment of nuclear structure effects in different formalisms. Corrections were derived for both Fermi and Gamow-Teller transitions, and methods of analytical evaluation thoroughly discussed. In its integrated form, calculated f values were in agreement with the most precise numerical results within the aimed for precision. The need for an accurate evaluation of weak magnetism contributions was stressed, and the possible significance of the oft-neglected induced pseudoscalar interaction was noted. Together with improved atomic corrections, an analytical description was presented of the allowed β spectrum shape accurate to a few parts in 10-4 down to 1 keV for low to medium Z nuclei, thereby extending the work by previous authors by nearly an order of magnitude.

A microarray immunoassay for simultaneous detection of proteins and bacteria

NASA Technical Reports Server (NTRS)

Delehanty, James B.; Ligler, Frances S.

2002-01-01

We report the development and characterization of an antibody microarray biosensor for the rapid detection of both protein and bacterial analytes under flow conditions. Using a noncontact microarray printer, biotinylated capture antibodies were immobilized at discrete locations on the surface of an avidin-coated glass microscope slide. Preservation of capture antibody function during the deposition process was accomplished with the use of a low-salt buffer containing sucrose and bovine serum albumin. The slide was fitted with a six-channel flow module that conducted analyte-containing solutions over the array of capture antibody microspots. Detection of bound analyte was subsequently achieved using fluorescent tracer antibodies. The pattern of fluorescent complexes was interrogated using a scanning confocal microscope equipped with a 635-nm laser. This microarray system was employed to detect protein and bacterial analytes both individually and in samples containing mixtures of analytes. Assays were completed in 15 min, and detection of cholera toxin, staphylococcal enterotoxin B, ricin, and Bacillus globigii was demonstrated at levels as low as 8 ng/mL, 4 ng/mL, 10 ng/mL, and 6.2 x 10(4) cfu/mL, respectively. The assays presented here are very fast, as compared to previously published methods for measuring antibody-antigen interactions using microarrays (minutes versus hours).

A multi-analyte serum test for the detection of non-small cell lung cancer

PubMed Central

Farlow, E C; Vercillo, M S; Coon, J S; Basu, S; Kim, A W; Faber, L P; Warren, W H; Bonomi, P; Liptay, M J; Borgia, J A

2010-01-01

Background: In this study, we appraised a wide assortment of biomarkers previously shown to have diagnostic or prognostic value for non-small cell lung cancer (NSCLC) with the intent of establishing a multi-analyte serum test capable of identifying patients with lung cancer. Methods: Circulating levels of 47 biomarkers were evaluated against patient cohorts consisting of 90 NSCLC and 43 non-cancer controls using commercial immunoassays. Multivariate statistical methods were used on all biomarkers achieving statistical relevance to define an optimised panel of diagnostic biomarkers for NSCLC. The resulting biomarkers were fashioned into a classification algorithm and validated against serum from a second patient cohort. Results: A total of 14 analytes achieved statistical relevance upon evaluation. Multivariate statistical methods then identified a panel of six biomarkers (tumour necrosis factor-α, CYFRA 21-1, interleukin-1ra, matrix metalloproteinase-2, monocyte chemotactic protein-1 and sE-selectin) as being the most efficacious for diagnosing early stage NSCLC. When tested against a second patient cohort, the panel successfully classified 75 of 88 patients. Conclusions: Here, we report the development of a serum algorithm with high specificity for classifying patients with NSCLC against cohorts of various ‘high-risk' individuals. A high rate of false positives was observed within the cohort in which patients had non-neoplastic lung nodules, possibly as a consequence of the inflammatory nature of these conditions. PMID:20859284

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture... Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MREs are listed as follows: (1) Official Methods of Analysis of AOAC...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

Gradient-based multiconfiguration Shepard interpolation for generating potential energy surfaces for polyatomic reactions.

PubMed

Tishchenko, Oksana; Truhlar, Donald G

2010-02-28

This paper describes and illustrates a way to construct multidimensional representations of reactive potential energy surfaces (PESs) by a multiconfiguration Shepard interpolation (MCSI) method based only on gradient information, that is, without using any Hessian information from electronic structure calculations. MCSI, which is called multiconfiguration molecular mechanics (MCMM) in previous articles, is a semiautomated method designed for constructing full-dimensional PESs for subsequent dynamics calculations (classical trajectories, full quantum dynamics, or variational transition state theory with multidimensional tunneling). The MCSI method is based on Shepard interpolation of Taylor series expansions of the coupling term of a 2 x 2 electronically diabatic Hamiltonian matrix with the diagonal elements representing nonreactive analytical PESs for reactants and products. In contrast to the previously developed method, these expansions are truncated in the present version at the first order, and, therefore, no input of electronic structure Hessians is required. The accuracy of the interpolated energies is evaluated for two test reactions, namely, the reaction OH+H(2)-->H(2)O+H and the hydrogen atom abstraction from a model of alpha-tocopherol by methyl radical. The latter reaction involves 38 atoms and a 108-dimensional PES. The mean unsigned errors averaged over a wide range of representative nuclear configurations (corresponding to an energy range of 19.5 kcal/mol in the former case and 32 kcal/mol in the latter) are found to be within 1 kcal/mol for both reactions, based on 13 gradients in one case and 11 in the other. The gradient-based MCMM method can be applied for efficient representations of multidimensional PESs in cases where analytical electronic structure Hessians are too expensive or unavailable, and it provides new opportunities to employ high-level electronic structure calculations for dynamics at an affordable cost.

Generalized analytical solutions to sequentially coupled multi-species advective-dispersive transport equations in a finite domain subject to an arbitrary time-dependent source boundary condition

NASA Astrophysics Data System (ADS)

Chen, Jui-Sheng; Liu, Chen-Wuing; Liang, Ching-Ping; Lai, Keng-Hsin

2012-08-01

SummaryMulti-species advective-dispersive transport equations sequentially coupled with first-order decay reactions are widely used to describe the transport and fate of the decay chain contaminants such as radionuclide, chlorinated solvents, and nitrogen. Although researchers attempted to present various types of methods for analytically solving this transport equation system, the currently available solutions are mostly limited to an infinite or a semi-infinite domain. A generalized analytical solution for the coupled multi-species transport problem in a finite domain associated with an arbitrary time-dependent source boundary is not available in the published literature. In this study, we first derive generalized analytical solutions for this transport problem in a finite domain involving arbitrary number of species subject to an arbitrary time-dependent source boundary. Subsequently, we adopt these derived generalized analytical solutions to obtain explicit analytical solutions for a special-case transport scenario involving an exponentially decaying Bateman type time-dependent source boundary. We test the derived special-case solutions against the previously published coupled 4-species transport solution and the corresponding numerical solution with coupled 10-species transport to conduct the solution verification. Finally, we compare the new analytical solutions derived for a finite domain against the published analytical solutions derived for a semi-infinite domain to illustrate the effect of the exit boundary condition on coupled multi-species transport with an exponential decaying source boundary. The results show noticeable discrepancies between the breakthrough curves of all the species in the immediate vicinity of the exit boundary obtained from the analytical solutions for a finite domain and a semi-infinite domain for the dispersion-dominated condition.

Design Criteria for Low Profile Flange Calculations

NASA Technical Reports Server (NTRS)

Leimbach, K. R.

1973-01-01

An analytical method and a design procedure to develop flanged separable pipe connectors are discussed. A previously established algorithm is the basis for calculating low profile flanges. The characteristics and advantages of the low profile flange are analyzed. The use of aluminum, titanium, and plastics for flange materials is described. Mathematical models are developed to show the mechanical properties of various flange configurations. A computer program for determining the structural stability of the flanges is described.

A dynamical-systems approach for computing ice-affected streamflow

USGS Publications Warehouse

Holtschlag, David J.

1996-01-01

A dynamical-systems approach was developed and evaluated for computing ice-affected streamflow. The approach provides for dynamic simulation and parameter estimation of site-specific equations relating ice effects to routinely measured environmental variables. Comparison indicates that results from the dynamical-systems approach ranked higher than results from 11 analytical methods previously investigated on the basis of accuracy and feasibility criteria. Additional research will likely lead to further improvements in the approach.

UPLC-MS/MS determination of ptaquiloside and pterosin B in preserved natural water.

PubMed

Clauson-Kaas, Frederik; Hansen, Hans Christian Bruun; Strobel, Bjarne W

2016-11-01

The naturally occurring carcinogen ptaquiloside and its degradation product pterosin B are found in water leaching from bracken stands. The objective of this work is to present a new sample preservation method and a fast UPLC-MS/MS method for quantification of ptaquiloside and pterosin B in environmental water samples, employing a novel internal standard. A faster, reliable, and efficient method was developed for isolation of high purity ptaquiloside and pterosin B from plant material for use as analytical standards, with purity verified by 1 H-NMR. The chemical analysis was performed by cleanup and preconcentration of samples with solid phase extraction, before analyte quantification with UPLC-MS/MS. By including gradient elution and optimizing the liquid chromatography mobile phase buffer system, a total run cycle of 5 min was achieved, with method detection limits, including preconcentration, of 8 and 4 ng/L for ptaquiloside and pterosin B, respectively. The use of loganin as internal standard improved repeatability of the determination of both analytes, though it could not be employed for sample preparation. Buffering raw water samples in situ with ammonium acetate to pH ∼5.5 decisively increased sample integrity at realistic transportation and storing conditions prior to extraction. Groundwater samples collected in November 2015 at the shallow water table below a Danish bracken stand were preserved and analyzed using the above methods, and PTA concentrations of 3.8 ± 0.24 μg/L (±sd, n = 3) were found, much higher than previously reported. Graphical abstract Workflow overview of ptaquiloside determination.

Development of a defect stream function, law of the wall/wake method for compressible turbulent boundary layers. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Wahls, Richard A.

1990-01-01

The method presented is designed to improve the accuracy and computational efficiency of existing numerical methods for the solution of flows with compressible turbulent boundary layers. A compressible defect stream function formulation of the governing equations assuming an arbitrary turbulence model is derived. This formulation is advantageous because it has a constrained zero-order approximation with respect to the wall shear stress and the tangential momentum equation has a first integral. Previous problems with this type of formulation near the wall are eliminated by using empirically based analytic expressions to define the flow near the wall. The van Driest law of the wall for velocity and the modified Crocco temperature-velocity relationship are used. The associated compressible law of the wake is determined and it extends the valid range of the analytical expressions beyond the logarithmic region of the boundary layer. The need for an inner-region eddy viscosity model is completely avoided. The near-wall analytic expressions are patched to numerically computed outer region solutions at a point determined during the computation. A new boundary condition on the normal derivative of the tangential velocity at the surface is presented; this condition replaces the no-slip condition and enables numerical integration to the surface with a relatively coarse grid using only an outer region turbulence model. The method was evaluated for incompressible and compressible equilibrium flows and was implemented into an existing Navier-Stokes code using the assumption of local equilibrium flow with respect to the patching. The method has proven to be accurate and efficient.

40 CFR 161.180 - Enforcement analytical method.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 25 2012-07-01 2012-07-01 false Enforcement analytical method. 161.180... DATA REQUIREMENTS FOR REGISTRATION OF ANTIMICROBIAL PESTICIDES Product Chemistry Data Requirements § 161.180 Enforcement analytical method. An analytical method suitable for enforcement purposes must be...

Characterization of supersonic radiation diffusion waves

DOE PAGES

Moore, Alastair S.; Guymer, Thomas M.; Morton, John; ...

2015-02-27

Supersonic and diffusive radiation flow is an important test problem for the radiative transfer models used in radiation-hydrodynamics computer codes owing to solutions being accessible via analytic and numeric methods. We present experimental results with which we compare these solutions by studying supersonic and diffusive flow in the laboratory. Here, we present results of higher-accuracy experiments than previously possible studying radiation flow through up to 7 high-temperature mean free paths of low-density, chlorine-doped polystyrene foam and silicon dioxide aerogel contained by an Au tube. Measurements of the heat front position and absolute measurements of the x-ray emission arrival at themore » end of the tube are used to test numerical and analytical models. We find excellent absolute agreement with simulations provided that the opacity and the equation of state are adjusted within expected uncertainties; analytical models provide a good phenomenological match to measurements but are not in quantitative agreement due to their limited scope.« less

Activating analytic thinking enhances the value given to individualizing moral foundations.

PubMed

Yilmaz, Onurcan; Saribay, S Adil

2017-08-01

Two central debates within Moral Foundations Theory concern (1) which moral foundations are core and (2) how conflict between ideological camps stemming from valuing different moral foundations can be resolved. Previous studies have attempted to answer the first question by imposing cognitive load on participants to direct them toward intuitive and automatic thought. However, this method has limitations and has produced mixed findings. In the present research, in two experiments, instead of directing participants toward intuitive thought, we tested the effects of activating high-effort, analytic thought on participants' moral foundations. In both experiments, analytic thought activation caused participants to value individualizing foundations greater than the control condition. This effect was not qualified by participants' political orientation. No effect was observed on binding foundations. The results are consistent with the idea that upholding individualizing foundations requires mental effort and may provide the basis for reconciliation between different ideological camps. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical balance-based Faraday magnetometer

NASA Astrophysics Data System (ADS)

Riminucci, Alberto; Uhlarz, Marc; De Santis, Roberto; Herrmannsdörfer, Thomas

2017-03-01

We introduce a Faraday magnetometer based on an analytical balance in which we were able to apply magnetic fields up to 0.14 T. We calibrated it with a 1 mm Ni sphere previously characterized in a superconducting quantum interference device (SQUID) magnetometer. The proposed magnetometer reached a theoretical sensitivity of 3 × 10-8 A m2. We demonstrated its operation on magnetic composite scaffolds made of poly(ɛ-caprolactone)/iron-doped hydroxyapatite. To confirm the validity of the method, we measured the same scaffold properties in a SQUID magnetometer. The agreement between the two measurements was within 5% at 0.127 T and 12% at 24 mT. With the addition, for a small cost, of a permanent magnet and computer controlled linear translators, we were thus able to assemble a Faraday magnetometer based on an analytical balance, which is a virtually ubiquitous instrument. This will make simple but effective magnetometry easily accessible to most laboratories, in particular, to life sciences ones, which are increasingly interested in magnetic materials.

Characterization of supersonic radiation diffusion waves

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

Moore, Alastair S.; Guymer, Thomas M.; Morton, John

Supersonic and diffusive radiation flow is an important test problem for the radiative transfer models used in radiation-hydrodynamics computer codes owing to solutions being accessible via analytic and numeric methods. We present experimental results with which we compare these solutions by studying supersonic and diffusive flow in the laboratory. Here, we present results of higher-accuracy experiments than previously possible studying radiation flow through up to 7 high-temperature mean free paths of low-density, chlorine-doped polystyrene foam and silicon dioxide aerogel contained by an Au tube. Measurements of the heat front position and absolute measurements of the x-ray emission arrival at themore » end of the tube are used to test numerical and analytical models. We find excellent absolute agreement with simulations provided that the opacity and the equation of state are adjusted within expected uncertainties; analytical models provide a good phenomenological match to measurements but are not in quantitative agreement due to their limited scope.« less

A stochastic Markov chain approach for tennis: Monte Carlo simulation and modeling

NASA Astrophysics Data System (ADS)

Aslam, Kamran

This dissertation describes the computational formulation of probability density functions (pdfs) that facilitate head-to-head match simulations in tennis along with ranking systems developed from their use. A background on the statistical method used to develop the pdfs , the Monte Carlo method, and the resulting rankings are included along with a discussion on ranking methods currently being used both in professional sports and in other applications. Using an analytical theory developed by Newton and Keller in [34] that defines a tennis player's probability of winning a game, set, match and single elimination tournament, a computational simulation has been developed in Matlab that allows further modeling not previously possible with the analytical theory alone. Such experimentation consists of the exploration of non-iid effects, considers the concept the varying importance of points in a match and allows an unlimited number of matches to be simulated between unlikely opponents. The results of these studies have provided pdfs that accurately model an individual tennis player's ability along with a realistic, fair and mathematically sound platform for ranking them.

Projected regression method for solving Fredholm integral equations arising in the analytic continuation problem of quantum physics

NASA Astrophysics Data System (ADS)

Arsenault, Louis-François; Neuberg, Richard; Hannah, Lauren A.; Millis, Andrew J.

2017-11-01

We present a supervised machine learning approach to the inversion of Fredholm integrals of the first kind as they arise, for example, in the analytic continuation problem of quantum many-body physics. The approach provides a natural regularization for the ill-conditioned inverse of the Fredholm kernel, as well as an efficient and stable treatment of constraints. The key observation is that the stability of the forward problem permits the construction of a large database of outputs for physically meaningful inputs. Applying machine learning to this database generates a regression function of controlled complexity, which returns approximate solutions for previously unseen inputs; the approximate solutions are then projected onto the subspace of functions satisfying relevant constraints. Under standard error metrics the method performs as well or better than the Maximum Entropy method for low input noise and is substantially more robust to increased input noise. We suggest that the methodology will be similarly effective for other problems involving a formally ill-conditioned inversion of an integral operator, provided that the forward problem can be efficiently solved.

Solvent-free MALDI-MS for the analysis of a membrane protein via the mini ball mill approach: case study of bacteriorhodopsin.

PubMed

Trimpin, Sarah; Deinzer, Max L

2007-01-01

A mini ball mill (MBM) solvent-free matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) method allows for the analysis of bacteriorhodopsin (BR), an integral membrane protein that previously presented special analytical problems. For well-defined signals in the molecular ion region of the analytes, a desalting procedure of the MBM sample directly on the MALDI target plate was used to reduce adduction by sodium and other cations that are normally attendant with hydrophobic peptides and proteins as a result of the sample preparation procedure. Mass analysis of the intact hydrophobic protein and the few hydrophobic and hydrophilic tryptic peptides available in the digest is demonstrated with this robust new approach. MS and MS/MS spectra of BR tryptic peptides and intact protein were generally superior to the traditional solvent-based method using the desalted "dry" MALDI preparation procedure. The solvent-free method expands the range of peptides that can be effectively analyzed by MALDI-MS to those that are hydrophobic and solubility-limited.

The analytic structure of conformal blocks and the generalized Wilson-Fisher fixed points

DOE PAGES

Gliozzi, Ferdinando; Guerrieri, Andrea L.; Petkou, Anastasios C.; ...

2017-04-11

Here, we describe in detail the method used in our previous work arXiv:1611.10344 to study the Wilson-Fisher critical points nearby generalized free CFTs, exploiting the analytic structure of conformal blocks as functions of the conformal dimension of the exchanged operator. Our method is equivalent to the mechanism of conformal multiplet recombination set up by null states. We also compute, to the first non-trivial order in the ε-expansion, the anomalous dimensions and the OPE coefficients of infinite classes of scalar local operators using just CFT data. We study single-scalar and O(N)-invariant theories, as well as theories with multiple deformations. When availablemore » we agree with older results, but we also produce a wealth of new ones. Furthermore, unitarity and crossing symmetry are not used in our approach and we are able to apply our method to non-unitary theories as well. Some implications of our results for the study of the non-unitary theories containing partially conserved higher-spin currents are briefly mentioned.« less

Advanced Research and Data Methods in Women's Health: Big Data Analytics, Adaptive Studies, and the Road Ahead.

PubMed

Macedonia, Christian R; Johnson, Clark T; Rajapakse, Indika

2017-02-01

Technical advances in science have had broad implications in reproductive and women's health care. Recent innovations in population-level data collection and storage have made available an unprecedented amount of data for analysis while computational technology has evolved to permit processing of data previously thought too dense to study. "Big data" is a term used to describe data that are a combination of dramatically greater volume, complexity, and scale. The number of variables in typical big data research can readily be in the thousands, challenging the limits of traditional research methodologies. Regardless of what it is called, advanced data methods, predictive analytics, or big data, this unprecedented revolution in scientific exploration has the potential to dramatically assist research in obstetrics and gynecology broadly across subject matter. Before implementation of big data research methodologies, however, potential researchers and reviewers should be aware of strengths, strategies, study design methods, and potential pitfalls. Examination of big data research examples contained in this article provides insight into the potential and the limitations of this data science revolution and practical pathways for its useful implementation.

Experimental Design for a Macrofoam Swab Study Relating the Recovery Efficiency and False Negative Rate to Low Concentrations of Two Bacillus anthracis Surrogates on Four Surface Materials

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

Piepel, Gregory F.; Hutchison, Janine R.

2014-04-16

This report describes the experimental design for a laboratory study to quantify the recovery efficiencies and false negative rates of a validated, macrofoam swab sampling method for low concentrations of Bacillus anthracis Sterne (BAS) and Bacillus atrophaeus (BG) spores on four surface materials (stainless steel, glass, vinyl tile, plastic light cover panel). Two analytical methods (plating/counting and polymerase chain reaction) will be used. Only one previous study has investigated false negative as a function of affecting test factors. The surrogates BAS and BG have not been tested together in the same study previously. Hence, this study will provide for completingmore » gaps in the available information on the performance of macrofoam swab sampling at low concentrations.« less

Experimental Design for a Macrofoam-Swab Study Relating the Recovery Efficiency and False Negative Rate to Low Concentrations of Two Bacillus anthracis Surrogates on Four Surface Materials

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

Piepel, Gregory F.; Hutchison, Janine R.

This report describes the experimental design for a laboratory study to quantify the recovery efficiencies and false negative rates of a validated, macrofoam-swab sampling method for low concentrations of Bacillus anthracis Sterne (BAS) and Bacillus atrophaeus (BG) spores on four surface materials (stainless steel, glass, vinyl tile, plastic light cover panel). Two analytical methods (culture and polymerase chain reaction) will be used. Only one previous study has investigated how the false negative rate depends on test factors. The surrogates BAS and BG have not been tested together in the same study previously. Hence, this study will provide for completing gapsmore » in the available information on the performance of macrofoam-swab sampling at low concentrations.« less

40 CFR 158.355 - Enforcement analytical method.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 24 2014-07-01 2014-07-01 false Enforcement analytical method. 158.355... DATA REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.355 Enforcement analytical method. An analytical method suitable for enforcement purposes must be provided for each active ingredient in the...

40 CFR 141.23 - Inorganic chemical sampling and analytical requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... highest analytical result. (e) All public water systems (community; non-transient, non-community; and... each subsequent sample during the quarter(s) which previously resulted in the highest analytical result...). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www...

A deterministic particle method for one-dimensional reaction-diffusion equations

NASA Technical Reports Server (NTRS)

Mascagni, Michael

1995-01-01

We derive a deterministic particle method for the solution of nonlinear reaction-diffusion equations in one spatial dimension. This deterministic method is an analog of a Monte Carlo method for the solution of these problems that has been previously investigated by the author. The deterministic method leads to the consideration of a system of ordinary differential equations for the positions of suitably defined particles. We then consider the time explicit and implicit methods for this system of ordinary differential equations and we study a Picard and Newton iteration for the solution of the implicit system. Next we solve numerically this system and study the discretization error both analytically and numerically. Numerical computation shows that this deterministic method is automatically adaptive to large gradients in the solution.

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.

Virus removal retention challenge tests performed at lab scale and pilot scale during operation of membrane units.

PubMed

Humbert, H; Machinal, C; Labaye, Ivan; Schrotter, J C

2011-01-01

The determination of the virus retention capabilities of UF units during operation is essential for the operators of drinking water treatment facilities in order to guarantee an efficient and stable removal of viruses through time. In previous studies, an effective method (MS2-phage challenge tests) was developed by the Water Research Center of Veolia Environnement for the measurement of the virus retention rates (Log Removal Rate, LRV) of commercially available hollow fiber membranes at lab scale. In the present work, the protocol for monitoring membrane performance was transferred from lab scale to pilot scale. Membrane performances were evaluated during pilot trial and compared to the results obtained at lab scale with fibers taken from the pilot plant modules. PFU culture method was compared to RT-PCR method for the calculation of LRV in both cases. Preliminary tests at lab scale showed that both methods can be used interchangeably. For tests conducted on virgin membrane, a good consistency was observed between lab and pilot scale results with the two analytical methods used. This work intends to show that a reliable determination of the membranes performances based on RT-PCR analytical method can be achieved during the operation of the UF units.

A new analytical method for characterizing nonlinear visual processes with stimuli of arbitrary distribution: Theory and applications.

PubMed

Hayashi, Ryusuke; Watanabe, Osamu; Yokoyama, Hiroki; Nishida, Shin'ya

2017-06-01

Characterization of the functional relationship between sensory inputs and neuronal or observers' perceptual responses is one of the fundamental goals of systems neuroscience and psychophysics. Conventional methods, such as reverse correlation and spike-triggered data analyses are limited in their ability to resolve complex and inherently nonlinear neuronal/perceptual processes because these methods require input stimuli to be Gaussian with a zero mean. Recent studies have shown that analyses based on a generalized linear model (GLM) do not require such specific input characteristics and have advantages over conventional methods. GLM, however, relies on iterative optimization algorithms and its calculation costs become very expensive when estimating the nonlinear parameters of a large-scale system using large volumes of data. In this paper, we introduce a new analytical method for identifying a nonlinear system without relying on iterative calculations and yet also not requiring any specific stimulus distribution. We demonstrate the results of numerical simulations, showing that our noniterative method is as accurate as GLM in estimating nonlinear parameters in many cases and outperforms conventional, spike-triggered data analyses. As an example of the application of our method to actual psychophysical data, we investigated how different spatiotemporal frequency channels interact in assessments of motion direction. The nonlinear interaction estimated by our method was consistent with findings from previous vision studies and supports the validity of our method for nonlinear system identification.

A simple, rapid and validated high-performance liquid chromatography method suitable for clinical measurements of human mercaptalbumin and non-mercaptalbumin.

PubMed

Yasukawa, Keiko; Shimosawa, Tatsuo; Okubo, Shigeo; Yatomi, Yutaka

2018-01-01

Background Human mercaptalbumin and human non-mercaptalbumin have been reported as markers for various pathological conditions, such as kidney and liver diseases. These markers play important roles in redox regulations throughout the body. Despite the recognition of these markers in various pathophysiologic conditions, the measurements of human mercaptalbumin and non-mercaptalbumin have not been popular because of the technical complexity and long measurement time of conventional methods. Methods Based on previous reports, we explored the optimal analytical conditions for a high-performance liquid chromatography method using an anion-exchange column packed with a hydrophilic polyvinyl alcohol gel. The method was then validated using performance tests as well as measurements of various patients' serum samples. Results We successfully established a reliable high-performance liquid chromatography method with an analytical time of only 12 min per test. The repeatability (within-day variability) and reproducibility (day-to-day variability) were 0.30% and 0.27% (CV), respectively. A very good correlation was obtained with the results of the conventional method. Conclusions A practical method for the clinical measurement of human mercaptalbumin and non-mercaptalbumin was established. This high-performance liquid chromatography method is expected to be a powerful tool enabling the expansion of clinical usefulness and ensuring the elucidation of the roles of albumin in redox reactions throughout the human body.

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

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.

Analytical research on impacting load of aircraft crashing upon moveable concrete target

NASA Astrophysics Data System (ADS)

Zhu, Tong; Ou, Zhuocheng; Duan, Zhuoping; Huang, Fenglei

2018-03-01

The impact load of an aircraft impact upon moveable concrete target was analyzed in this paper by both theoretical and numerical methods. The aircraft was simplified as a one dimensional pole and stress-wave theory was used to deduce the new formula. Furthermore, aiming to compare with previous experimental data, a numerical calculation based on the new formula had been carried out which showed good agreement with the experimental data. The approach, a new formula with particular numerical method, can predict not only the impact load but also the deviation between moveable and static concrete target.

Electromagnetic Pulse Excitation of Finite-Long Dissipative Conductors over a Conducting Ground Plane in the Time Domain

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

Campione, Salvatore; Warne, Larry K.; Schiek, Richard

2017-09-01

This report details the modeling results for the response of a finite-length dissipative conductor interacting with a conducting ground to a hypothetical nuclear device with the same output energy spectrum as the Fat Man device. We use a time-domain method based on transmission line theory that allows accounting for time-varying air conductivities. We implemented such method in a code we call ATLOG - Analytic Transmission Line Over Ground. Results are compared the frequency-domain version of ATLOG previously developed and to the circuit simulator Xyce in some instances. Intentionally Left Blank

Stress analysis of ribbon parachutes

NASA Technical Reports Server (NTRS)

Reynolds, D. T.; Mullins, W. M.

1975-01-01

An analytical method has been developed for determining the internal load distribution for ribbon parachutes subjected to known riser and aerodynamic forces. Finite elements with non-linear elastic properties represent the parachute structure. This method is an extension of the analysis previously developed by the authors and implemented in the digital computer program CANO. The present analysis accounts for the effect of vertical ribbons in the solution for canopy shape and stress distribution. Parametric results are presented which relate the canopy stress distribution to such factors as vertical ribbon strength, number of gores, and gore shape in a ribbon parachute.

Diagnostics for insufficiencies of posterior calculations in Bayesian signal inference.

PubMed

Dorn, Sebastian; Oppermann, Niels; Ensslin, Torsten A

2013-11-01

We present an error-diagnostic validation method for posterior distributions in Bayesian signal inference, an advancement of a previous work. It transfers deviations from the correct posterior into characteristic deviations from a uniform distribution of a quantity constructed for this purpose. We show that this method is able to reveal and discriminate several kinds of numerical and approximation errors, as well as their impact on the posterior distribution. For this we present four typical analytical examples of posteriors with incorrect variance, skewness, position of the maximum, or normalization. We show further how this test can be applied to multidimensional signals.

[Raman spectroscopy applied to analytical quality control of injectable drugs: analytical evaluation and comparative economic versus HPLC and UV / visible-FTIR].

PubMed

Bourget, P; Amin, A; Vidal, F; Merlette, C; Troude, P; Corriol, O

2013-09-01

In France, central IV admixture of chemotherapy (CT) treatments at the hospital is now required by law. We have previously shown that the shaping of Therapeutic Objects (TOs) could profit from an Analytical Quality Assurance (AQA), closely linked to the batch release, for the three key parameters: identity, purity, and initial concentration of the compound of interest. In the course of recent and diversified works, we showed the technical superiority of non-intrusive Raman Spectroscopy (RS) vs. any other analytical option and, especially for both HPLC and vibrational method using a UV/visible-FTIR coupling. An interconnected qualitative and economic assessment strongly helps to enrich these relevant works. The study compares in operational situation, the performance of three analytical methods used for the AQC of TOs. We used: a) a set of evaluation criteria, b) the depreciation tables of the machinery, c) the cost of disposables, d) the weight of equipment and technical installations, e) the basic accounting unit (unit of work) and its composite costs (Euros), which vary according to the technical options, the weight of both human resources and disposables; finally, different combinations are described. So, the unit of work can take 12 different values between 1 and 5.5 Euros, and we provide various recommendations. A qualitative evaluation grid constantly places the SR technology as superior or equal to the 2 other techniques currently available. Our results demonstrated: a) the major interest of the non-intrusive AQC performed by RS, especially when it is not possible to analyze a TO with existing methods e.g. elastomeric portable pumps, and b) the high potential for this technique to be a strong contributor to the security of the medication circuit, and to fight the iatrogenic effects of drugs especially in the hospital. It also contributes to the protection of all actors in healthcare and of their working environment.

Development of a pressurized liquid extraction-solid-phase extraction followed by liquid chromatography-electrospray ionization tandem mass spectrometry method for the quantitative determination of benzoxazolinones and their degradation products in agricultural soil.

PubMed

Villagrasa, M; Guillamón, M; Navarro, A; Eljarrat, E; Barceló, D

2008-02-01

A new analytical method for the quantitative determination of benzoxazolinones and their degradation products in agricultural soils based on the use of pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) and then instrumental determination using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS) is described. Using this method, the characterization, separation and quantitative detection of a mixture of two benzoxazolinones, benzoxazolin-2-one (BOA) and 6-methoxybenzoxazolin-2-one (MBOA) and their degradation products, 2-aminophenol (APH), N-(2-hydroxyphenyl)malonamic acid (HMPMA), 2-amino-3-H-phenoxazin-3-one (APO), 9-methoxy-2-amino-3-H-phenoxazin-3-one (AMPO), 2-acetylamino-3-H-phenoxazin-3-one (AAPO) and 2-acetylamino-9-methoxy-2-amino-3-H-phenoxazin-3-one (AAMPO) was achieved. The complete LC-ESI-MS-MS precursor-product ion fragmentation pathways for the degradation products of benzoxazolinones are described for the first time. Quantitative analysis was done in the multiple reaction mode using two specific combinations of precursor-product ion transitions for each compound. The optimized method was quality assessed by the measure of parameter as recovery, linearity, sensitivity, repeatability and reproducibility. Recoveries of the analytes ranged from 53 to 123%. The developed method offered improvements to the sensitivity as compared with our previously LC-MS method, with detection limits down to 2.4-21 ng/g of dry weight. This achievement allows us to identify and quantify for the first time degradation products of benzoxazolinones in real agricultural soil samples. Analytes were found in the range of 20.6-149 ng/g dry weight.

Wavefront aberrations: analytical method to convert Zernike coefficients from a pupil to a scaled arbitrarily decentered one

NASA Astrophysics Data System (ADS)

Comastri, S. A.; Perez, Liliana I.; Pérez, Gervasio D.; Bastida, K.; Martin, G.

2008-04-01

The wavefront aberration of any image forming system and, in particular, of a human eye, is often expanded in Zernike modes each mode being weighed by a coefficient that depends both on the image forming components of the system and on the contour, size and centering of the pupil. In the present article, expanding up to 7th order the wavefront aberration, an analytical method to compute a new set of Zernike coefficients corresponding to a pupil in terms of an original set evaluated via ray tracing for a dilated and transversally arbitrarily displaced pupil is developed. A transformation matrix of dimension 36×36 is attained multiplying the scaling-horizontal traslation matrix previously derived by appropriate rotation matrices. Multiplying the original coefficients by this transformation matrix, analytical formulas for each new coefficient are attained and supplied and, for the information concerning the wavefront aberration to be available, these formulas must be employed in cases in which the new pupil is contained in the original one. The use of these analytical formulas is exemplified applying them to study the effect of pupil contraction and/or decentering in 3 situations: calculation of corneal aberrations of a keratoconic subject for the natural photopic pupil size and various decenterings; coma compensation by means of pupil shift in a fictitious system solely having primary aberrations and evaluation of the amount of astigmatism and coma of a hypothetical system originally having spherical aberration alone.

Preliminary Upper Estimate of Peak Currents in Transcranial Magnetic Stimulation at Distant Locations from a TMS Coil

PubMed Central

Makarov, Sergey N.; Yanamadala, Janakinadh; Piazza, Matthew W.; Helderman, Alex M.; Thang, Niang S.; Burnham, Edward H.; Pascual-Leone, Alvaro

2016-01-01

Goals Transcranial magnetic stimulation (TMS) is increasingly used as a diagnostic and therapeutic tool for numerous neuropsychiatric disorders. The use of TMS might cause whole-body exposure to undesired induced currents in patients and TMS operators. The aim of the present study is to test and justify a simple analytical model known previously, which may be helpful as an upper estimate of eddy current density at a particular distant observation point for any body composition and any coil setup. Methods We compare the analytical solution with comprehensive adaptive mesh refinement-based FEM simulations of a detailed full-body human model, two coil types, five coil positions, about 100,000 observation points, and two distinct pulse rise times, thus providing a representative number of different data sets for comparison, while also using other numerical data. Results Our simulations reveal that, after a certain modification, the analytical model provides an upper estimate for the eddy current density at any location within the body. In particular, it overestimates the peak eddy currents at distant locations from a TMS coil by a factor of 10 on average. Conclusion The simple analytical model tested in the present study may be valuable as a rapid method to safely estimate levels of TMS currents at different locations within a human body. Significance At present, safe limits of general exposure to TMS electric and magnetic fields are an open subject, including fetal exposure for pregnant women. PMID:26685221

Prioritizing pesticide compounds for analytical methods development

USGS Publications Warehouse

Norman, Julia E.; Kuivila, Kathryn; Nowell, Lisa H.

2012-01-01

The U.S. Geological Survey (USGS) has a periodic need to re-evaluate pesticide compounds in terms of priorities for inclusion in monitoring and studies and, thus, must also assess the current analytical capabilities for pesticide detection. To meet this need, a strategy has been developed to prioritize pesticides and degradates for analytical methods development. Screening procedures were developed to separately prioritize pesticide compounds in water and sediment. The procedures evaluate pesticide compounds in existing USGS analytical methods for water and sediment and compounds for which recent agricultural-use information was available. Measured occurrence (detection frequency and concentrations) in water and sediment, predicted concentrations in water and predicted likelihood of occurrence in sediment, potential toxicity to aquatic life or humans, and priorities of other agencies or organizations, regulatory or otherwise, were considered. Several existing strategies for prioritizing chemicals for various purposes were reviewed, including those that identify and prioritize persistent, bioaccumulative, and toxic compounds, and those that determine candidates for future regulation of drinking-water contaminants. The systematic procedures developed and used in this study rely on concepts common to many previously established strategies. The evaluation of pesticide compounds resulted in the classification of compounds into three groups: Tier 1 for high priority compounds, Tier 2 for moderate priority compounds, and Tier 3 for low priority compounds. For water, a total of 247 pesticide compounds were classified as Tier 1 and, thus, are high priority for inclusion in analytical methods for monitoring and studies. Of these, about three-quarters are included in some USGS analytical method; however, many of these compounds are included on research methods that are expensive and for which there are few data on environmental samples. The remaining quarter of Tier 1 compounds are high priority as new analytes. The objective for analytical methods development is to design an integrated analytical strategy that includes as many of the Tier 1 pesticide compounds as possible in a relatively few, cost-effective methods. More than 60 percent of the Tier 1 compounds are high priority because they are anticipated to be present at concentrations approaching levels that could be of concern to human health or aquatic life in surface water or groundwater. An additional 17 percent of Tier 1 compounds were frequently detected in monitoring studies, but either were not measured at levels potentially relevant to humans or aquatic organisms, or do not have benchmarks available with which to compare concentrations. The remaining 21 percent are pesticide degradates that were included because their parent pesticides were in Tier 1. Tier 1 pesticide compounds for water span all major pesticide use groups and a diverse range of chemical classes, with herbicides and their degradates composing half of compounds. Many of the high priority pesticide compounds also are in several national regulatory programs for water, including those that are regulated in drinking water by the U.S. Environmental Protection Agency under the Safe Drinking Water Act and those that are on the latest Contaminant Candidate List. For sediment, a total of 175 pesticide compounds were classified as Tier 1 and, thus, are high priority for inclusion in analytical methods available for monitoring and studies. More than 60 percent of these compounds are included in some USGS analytical method; however, some are spread across several research methods that are expensive to perform, and monitoring data are not extensive for many compounds. The remaining Tier 1 compounds for sediment are high priority as new analytes. The objective for analytical methods development for sediment is to enhance an existing analytical method that currently includes nearly half of the pesticide compounds in Tier 1 by adding as many additional Tier 1 compounds as are analytically compatible. About 35 percent of the Tier 1 compounds for sediment are high priority on the basis of measured occurrence. A total of 74 compounds, or 42 percent, are high priority on the basis of predicted likelihood of occurrence according to physical-chemical properties, and either have potential toxicity to aquatic life, high pesticide useage, or both. The remaining 22 percent of Tier 1 pesticide compounds were either degradates of Tier 1 parent compounds or included for other reasons. As with water, the Tier 1 pesticide compounds for sediment are distributed across the major pesticide-use groups; insecticides and their degradates are the largest fraction, making up 45 percent of Tier 1. In contrast to water, organochlorines, at 17 percent, are the largest chemical class for Tier 1 in sediment, which is to be expected because there is continued widespread detection in sediments of persistent organochlorine pesticides and their degradates at concentrations high enough for potential effects on aquatic life. Compared to water, there are fewer available benchmarks with which to compare contaminant concentrations in sediment, but a total of 19 Tier 1 compounds have at least one sediment benchmark or screening value for aquatic organisms. Of the 175 compounds in Tier 1, 77 percent have high aquatic-life toxicity, as defined for this process. This evaluation of pesticides and degradates resulted in two lists of compounds that are priorities for USGS analytical methods development, one for water and one for sediment. These lists will be used as the basis for redesigning and enhancing USGS analytical capabilities for pesticides in order to capture as many high-priority pesticide compounds as possible using an economically feasible approach.

Exact density-potential pairs from complex-shifted axisymmetric systems

NASA Astrophysics Data System (ADS)

Ciotti, Luca; Marinacci, Federico

2008-07-01

In a previous paper, the complex-shift method has been applied to self-gravitating spherical systems, producing new analytical axisymmetric density-potential pairs. We now extend the treatment to the Miyamoto-Nagai disc and the Binney logarithmic halo, and we study the resulting axisymmetric and triaxial analytical density-potential pairs; we also show how to obtain the surface density of shifted systems from the complex shift of the surface density of the parent model. In particular, the systems obtained from Miyamoto-Nagai discs can be used to describe disc galaxies with a peanut-shaped bulge or with a central triaxial bar, depending on the direction of the shift vector. By using a constructive method that can be applied to generic axisymmetric systems, we finally show that the Miyamoto-Nagai and the Satoh discs, and the Binney logarithmic halo cannot be obtained from the complex shift of any spherical parent distribution. As a by-product of this study, we also found two new generating functions in closed form for even and odd Legendre polynomials, respectively.

Heat transfer to and from vegetated surfaces - An analytical method for the bulk exchange coefficients

NASA Technical Reports Server (NTRS)

Massman, William J.

1987-01-01

The semianalytical model outlined in a previous study (Massman, 1987) to describe momentum exchange between the atmosphere and vegetated surfaces is extended to include the exchange of heat. The methods employed are based on one-dimensional turbulent diffusivities, and use analytical solutions to the steady-state diffusion equation. The model is used to assess the influence that the canopy foliage structure and density, the wind profile structure within the canopy, and the shelter factor can have upon the inverse surface Stanton number (kB exp -1), as well as to explore the consequences of introducing a scalar displacement height which can be different from the momentum displacement height. In general, the triangular foliage area density function gives results which agree more closely with observations than that for constant foliage area density. The intended application of this work is for parameterizing the bulk aerodynamic resistances for heat and momentum exchange for use within large-scale models of plant-atmosphere exchanges.

Determination of Curcuminoids in Curcuma longa Linn. by UPLC/Q-TOF-MS: An Application in Turmeric Cultivation.

PubMed

Ashraf, Kamran; Mujeeb, Mohd; Ahmad, Altaf; Ahmad, Niyaz; Amir, Mohd

2015-09-01

Cucuma longa Linn. (Fam-Zingiberaceae) is a valued medicinal plant contains curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) as major bioactive constituents. Previously reported analytical methods for analysis of curcuminoids were found to suffer from low resolution, lower sensitivity and longer analytical times. In this study, a rapid, sensitive, selective high-throughput ultra high performance liquid chromatography-tandem mass spectrometry (UPLC/Q-TOF-MS) method was developed and validated for the quantification of curcuminoids with an aim to reduce analysis time and enhance efficiency. UPLC/Q-TOF-MS analysis showed large variation (1.408-5.027% w/w) of curcuminoids among different samples with respect to their occurrence of metabolite and their concentration. The results showed that Erode (south province) contains highest quantity of curcuminoids and concluded to be the superior varieties. The results obtained here could be valuable for devising strategies for cultivating this medicinal plant. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Ultrafast quantitation of six quinolones in water samples by second-order capillary electrophoresis data modeling with multivariate curve resolution-alternating least squares.

PubMed

Alcaráz, Mirta R; Vera-Candioti, Luciana; Culzoni, María J; Goicoechea, Héctor C

2014-04-01

This paper presents the development of a capillary electrophoresis method with diode array detector coupled to multivariate curve resolution-alternating least squares (MCR-ALS) to conduct the resolution and quantitation of a mixture of six quinolones in the presence of several unexpected components. Overlapping of time profiles between analytes and water matrix interferences were mathematically solved by data modeling with the well-known MCR-ALS algorithm. With the aim of overcoming the drawback originated by two compounds with similar spectra, a special strategy was implemented to model the complete electropherogram instead of dividing the data in the region as usually performed in previous works. The method was first applied to quantitate analytes in standard mixtures which were randomly prepared in ultrapure water. Then, tap water samples spiked with several interferences were analyzed. Recoveries between 76.7 and 125 % and limits of detection between 5 and 18 μg L(-1) were achieved.

7 CFR 94.4 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 94.4 Section 94.4 Agriculture... POULTRY AND EGG PRODUCTS Mandatory Analyses of Egg Products § 94.4 Analytical methods. The majority of analytical methods used by the USDA laboratories to perform mandatory analyses for egg products are listed as...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2011 CFR

2011-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this Part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

Considerations regarding the validation of chromatographic mass spectrometric methods for the quantification of endogenous substances in forensics.

PubMed

Hess, Cornelius; Sydow, Konrad; Kueting, Theresa; Kraemer, Michael; Maas, Alexandra

2018-02-01

The requirement for correct evaluation of forensic toxicological results in daily routine work and scientific studies is reliable analytical data based on validated methods. Validation of a method gives the analyst tools to estimate the efficacy and reliability of the analytical method. Without validation, data might be contested in court and lead to unjustified legal consequences for a defendant. Therefore, new analytical methods to be used in forensic toxicology require careful method development and validation of the final method. Until now, there are no publications on the validation of chromatographic mass spectrometric methods for the detection of endogenous substances although endogenous analytes can be important in Forensic Toxicology (alcohol consumption marker, congener alcohols, gamma hydroxy butyric acid, human insulin and C-peptide, creatinine, postmortal clinical parameters). For these analytes, conventional validation instructions cannot be followed completely. In this paper, important practical considerations in analytical method validation for endogenous substances will be discussed which may be used as guidance for scientists wishing to develop and validate analytical methods for analytes produced naturally in the human body. Especially the validation parameters calibration model, analytical limits, accuracy (bias and precision) and matrix effects and recovery have to be approached differently. Highest attention should be paid to selectivity experiments. Copyright © 2017 Elsevier B.V. All rights reserved.

Simultaneous quantification of four metabolites of sulfur mustard in urine samples by ultra-high performance liquid chromatography-tandem mass spectrometry after solid phase extraction.

PubMed

Liu, Chang-Cai; Liu, Shi-Lei; Xi, Hai-Ling; Yu, Hui-Lan; Zhou, Shi-Kun; Huang, Gui-Lan; Liang, Long-Hui; Liu, Jing-Quan

2017-04-07

Four HD urinary metabolites including hydrolysis metabolite thiodiglycol (TDG), glutathione-derived metabolite 1,1'-sulfonylbis[2-S-(N-acetylcysteinyl)ethane] (SBSNAE), as well as the β-lyase metabolites 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] (SBMSE) and 1-methylsulfinyl-2-[2-(methylthio) ethylsulfonyl]ethane (MSMTESE) are considered as important biomarkers for short-term retrospective detection of HD exposure. In this study, a single method for simultaneous quantification of the four HD metabolites in urine samples was developed using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The four urinary metabolites were simultaneously extracted from urinary samples using a solid phase extraction (SPE) method with high extraction recoveries for all four metabolites varied in the range of 71.1-103% followed by UHPLC-MS/MS analysis. The SPE is simple and high effective only requiring 0.1mL of urinary samples and 0.5h time consuming. The problem of previous co-elution of TDG and SBSNAE in UHPLC was well solved, and complete separation of TDG, SBSNAE, SBMSE and MSMTESE from SPE-processed urine matrix was obtained to increase specificity and sensitivity. A full method validation was performed for each analyte in urine matrix. The linear range of calibration curves for the four analytes were respectively from 0.50-500ngmL -1 for TDG and SBSNAE, 0.05-500ngmL -1 for SBMSE and MSMTESE with coefficient of determination value (R 2 ) ≥0.990. The limit of detection was 0.25ngmL -1 for TDG and SBSNAE, 0.01ngmL -1 for SBMSE and MSMTESE spiked in normal urine. The intra/inter-day precision for each analyte at three QC levels had relative standard deviation (%RSD) of ≤10.3%, and the intra/inter-day accuracy ranged between 88.0-108%. This developed method allows for simultaneous and trace measurement of four HD urinary metabolites within one single determination with the lowest usage amount of urine samples over all previous methods This study provides a useful tool for early diagnosis and monitoring of HD poisoning for medical treatment with high confidence, avoiding the need for application of several analysis methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Template based rotation: A method for functional connectivity analysis with a priori templates☆

PubMed Central

Schultz, Aaron P.; Chhatwal, Jasmeer P.; Huijbers, Willem; Hedden, Trey; van Dijk, Koene R.A.; McLaren, Donald G.; Ward, Andrew M.; Wigman, Sarah; Sperling, Reisa A.

2014-01-01

Functional connectivity magnetic resonance imaging (fcMRI) is a powerful tool for understanding the network level organization of the brain in research settings and is increasingly being used to study large-scale neuronal network degeneration in clinical trial settings. Presently, a variety of techniques, including seed-based correlation analysis and group independent components analysis (with either dual regression or back projection) are commonly employed to compute functional connectivity metrics. In the present report, we introduce template based rotation,1 a novel analytic approach optimized for use with a priori network parcellations, which may be particularly useful in clinical trial settings. Template based rotation was designed to leverage the stable spatial patterns of intrinsic connectivity derived from out-of-sample datasets by mapping data from novel sessions onto the previously defined a priori templates. We first demonstrate the feasibility of using previously defined a priori templates in connectivity analyses, and then compare the performance of template based rotation to seed based and dual regression methods by applying these analytic approaches to an fMRI dataset of normal young and elderly subjects. We observed that template based rotation and dual regression are approximately equivalent in detecting fcMRI differences between young and old subjects, demonstrating similar effect sizes for group differences and similar reliability metrics across 12 cortical networks. Both template based rotation and dual-regression demonstrated larger effect sizes and comparable reliabilities as compared to seed based correlation analysis, though all three methods yielded similar patterns of network differences. When performing inter-network and sub-network connectivity analyses, we observed that template based rotation offered greater flexibility, larger group differences, and more stable connectivity estimates as compared to dual regression and seed based analyses. This flexibility owes to the reduced spatial and temporal orthogonality constraints of template based rotation as compared to dual regression. These results suggest that template based rotation can provide a useful alternative to existing fcMRI analytic methods, particularly in clinical trial settings where predefined outcome measures and conserved network descriptions across groups are at a premium. PMID:25150630

Solution of magnetic field and eddy current problem induced by rotating magnetic poles (abstract)

NASA Astrophysics Data System (ADS)

Liu, Z. J.; Low, T. S.

1996-04-01

The magnetic field and eddy current problems induced by rotating permanent magnet poles occur in electromagnetic dampers, magnetic couplings, and many other devices. Whereas numerical techniques, for example, finite element methods can be exploited to study various features of these problems, such as heat generation and drag torque development, etc., the analytical solution is always of interest to the designers since it helps them to gain the insight into the interdependence of the parameters involved and provides an efficient tool for designing. Some of the previous work showed that the solution of the eddy current problem due to the linearly moving magnet poles can give satisfactory approximation for the eddy current problem due to rotating fields. However, in many practical cases, especially when the number of magnet poles is small, there is significant effect of flux focusing due to the geometry. The above approximation can therefore lead to marked errors in the theoretical predictions of the device performance. Bernot et al. recently described an analytical solution in a polar coordinate system where the radial field is excited by a time-varying source. A discussion of an analytical solution of the magnetic field and eddy current problems induced by moving magnet poles in radial field machines will be given in this article. The theoretical predictions obtained from this method is compared with the results obtained from finite element calculations. The validity of the method is also checked by the comparison of the theoretical predictions and the measurements from a test machine. It is shown that the introduced solution leads to a significant improvement in the air gap field prediction as compared with the results obtained from the analytical solution that models the eddy current problems induced by linearly moving magnet poles.

Liquid chromatography-high resolution mass spectrometry (LC-HRMS) determination of stimulants, anorectic drugs and phosphodiesterase 5 inhibitors (PDE5I) in food supplements.

PubMed

Strano-Rossi, Sabina; Odoardi, Sara; Castrignanò, Erika; Serpelloni, Giovanni; Chiarotti, Marcello

2015-03-15

The paper describes a liquid chromatography/high resolution mass spectrometry LC/HRMS method for the simultaneous identification and quantification of stimulants (ephedrines, caffeine, anorectic drugs such as phentermine, phendimetrazine, phenmetrazine, fenfluramine, benfluorex, mephentermine, fencanfamine, sibutramine) and PDE5I (sildenafil, vardenafil and tadalafil) in food supplements using a benchtop Orbitrap mass spectrometer. The mass detector, with a nominal resolving power of 100,000 (FWHM at m/z 200), operated in full scan mode in ESI positive ionization mode. Analytes were identified by retention times, accurate masses and correspondence of experimental and calculated isotopic patterns. The limits of detection (LOD) obtained varied from 1 to 25 ng g(-1) and limits of quantification (LOQ) were 50 ng g(-1) for all compounds. The method was linear for all the analytes in the ranges from 50 to 2000 ng g(-1), giving correlation coefficients>0.99. Accuracy (intended as %E) and repeatability (% CV) were always lower than 15%. The method was applied to the analysis of 36 dietary supplements, revealing the presence of ephedrine and/or pseudoephedrine in four of them, caffeine in eight of them and sildenafil in four of them. In one case, ephedrine was not reported on the label of the dietary supplement, as well as for caffeine in other two cases. A further confirmation of the analytes identity in positive samples was obtained through in-source fragmentation and comparison of the obtained fragments and their relative abundances with those from certified standards. As the acquisition mode is full scan, it would be also possible to re-process a previously acquired datafile for the investigation of untargeted analytes. Copyright © 2014 Elsevier B.V. All rights reserved.

Protein molecular data from ancient (>1 million years old) fossil material: pitfalls, possibilities and grand challenges.

PubMed

Schweitzer, Mary Higby; Schroeter, Elena R; Goshe, Michael B

2014-07-15

Advances in resolution and sensitivity of analytical techniques have provided novel applications, including the analyses of fossil material. However, the recovery of original proteinaceous components from very old fossil samples (defined as >1 million years (1 Ma) from previously named limits in the literature) is far from trivial. Here, we discuss the challenges to recovery of proteinaceous components from fossils, and the need for new sample preparation techniques, analytical methods, and bioinformatics to optimize and fully utilize the great potential of information locked in the fossil record. We present evidence for survival of original components across geological time, and discuss the potential benefits of recovery, analyses, and interpretation of fossil materials older than 1 Ma, both within and outside of the fields of evolutionary biology.

Two types of modes in finite size one-dimensional coaxial photonic crystals: General rules and experimental evidence

NASA Astrophysics Data System (ADS)

El Boudouti, E. H.; El Hassouani, Y.; Djafari-Rouhani, B.; Aynaou, H.

2007-08-01

We demonstrate analytically and experimentally the existence and behavior of two types of modes in finite size one-dimensional coaxial photonic crystals made of N cells with vanishing magnetic field on both sides. We highlight the existence of N-1 confined modes in each band and one mode by gap associated to either one or the other of the two surfaces surrounding the structure. The latter modes are independent of N . These results generalize our previous findings on the existence of surface modes in two semi-infinite superlattices obtained from the cleavage of an infinite superlattice between two cells. The analytical results are obtained by means of the Green’s function method, whereas the experiments are carried out using coaxial cables in the radio-frequency regime.

Analytic algorithms for determining radiative transfer optical properties of ocean waters.

PubMed

Kaskas, Ayse; Güleçyüz, Mustafa C; Tezcan, Cevdet; McCormick, Norman J

2006-10-10

A synthetic model for the scattering phase function is used to develop simple algebraic equations, valid for any water type, for evaluating the ratio of the backscattering to absorption coefficients of spatially uniform, very deep waters with data from upward and downward planar irradiances and the remotely sensed reflectance. The phase function is a variable combination of a forward-directed Dirac delta function plus isotropic scattering, which is an elementary model for strongly forward scattering such as that encountered in oceanic optics applications. The incident illumination at the surface is taken to be diffuse plus a collimated beam. The algorithms are compared with other analytic correlations that were previously derived from extensive numerical simulations, and they are also numerically tested with forward problem results computed with a modified FN method.

Aerodynamic shape optimization of wing and wing-body configurations using control theory

NASA Technical Reports Server (NTRS)

Reuther, James; Jameson, Antony

1995-01-01

This paper describes the implementation of optimization techniques based on control theory for wing and wing-body design. In previous studies it was shown that control theory could be used to devise an effective optimization procedure for airfoils and wings in which the shape and the surrounding body-fitted mesh are both generated analytically, and the control is the mapping function. Recently, the method has been implemented for both potential flows and flows governed by the Euler equations using an alternative formulation which employs numerically generated grids, so that it can more easily be extended to treat general configurations. Here results are presented both for the optimization of a swept wing using an analytic mapping, and for the optimization of wing and wing-body configurations using a general mesh.

Rotor/Wing Interactions in Hover

NASA Technical Reports Server (NTRS)

Young, Larry A.; Derby, Michael R.

2002-01-01

Hover predictions of tiltrotor aircraft are hampered by the lack of accurate and computationally efficient models for rotor/wing interactional aerodynamics. This paper summarizes the development of an approximate, potential flow solution for the rotor-on-rotor and wing-on-rotor interactions. This analysis is based on actuator disk and vortex theory and the method of images. The analysis is applicable for out-of-ground-effect predictions. The analysis is particularly suited for aircraft preliminary design studies. Flow field predictions from this simple analytical model are validated against experimental data from previous studies. The paper concludes with an analytical assessment of the influence of rotor-on-rotor and wing-on-rotor interactions. This assessment examines the effect of rotor-to-wing offset distance, wing sweep, wing span, and flaperon incidence angle on tiltrotor inflow and performance.

An analytical strategy to investigate Semen Strychni nephrotoxicity based on simultaneous HILIC-ESI-MS/MS detection of Semen Strychni alkaloids, tyrosine and tyramine in HEK 293t cell lysates.

PubMed

Gu, Liqiang; Hou, Pengyi; Zhang, Ruowen; Liu, Ziying; Bi, Kaishun; Chen, Xiaohui

2016-10-15

A Previous metabolomics study has demonstrated that tyrosine metabolism might be disrupted by treating with Semen Strychni on the cell nephrotoxicity model. To investigate the relationship between Semen Strychni alkaloids (SAs) and endogenous tyrosine, tyramine under the nephrotoxicity condition, an HILIC-ESI-MS/MS based analytical strategy was applied in this study. Based on the established Semen Strychni nephrotoxicity cell model, strychnine and brucine were identified and screened as the main SAs by an HPLC-Q Exactive hybrid quadrupole Orbitrap mass system. Then, a sensitive HILIC-ESI-MS/MS method was developed to simultaneously monitor strychnine, brucine, tyrosine and tyramine in cell lysate. The analytes were separated by a Shiseido CAPCELL CORE PC (150mm×2.1mm, 2.7μm) HILIC column in an acetonitrile/0.1% formic acid gradient system. All the calibration curves were linear with regression coefficients above 0.9924. The absolute recoveries were more than 80.5% and the matrix effects were between 91.6%-107.0%. With the developed method, analytes were successfully determined in cell lysates. Decreased levels of tyrosine and tyramine were observed only in combination with increased levels of SAs, indicating that the disturbance of tyrosine metabolism might be induced by the accumulation of SAs in kidney cell after exposure of Semen Strychni. The HILIC-ESI-MS/MS based analytical strategy is a useful tool to reveal the relationships between the toxic herb components and the endogenous metabolite profiling in the toxicity investigation of herb medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

Review of Research on Student-Facing Learning Analytics Dashboards and Educational Recommender Systems

ERIC Educational Resources Information Center

Bodily, Robert; Verbert, Katrien

2017-01-01

This article is a comprehensive literature review of student-facing learning analytics reporting systems that track learning analytics data and report it directly to students. This literature review builds on four previously conducted literature reviews in similar domains. Out of the 945 articles retrieved from databases and journals, 93 articles…

A Progressive Approach to Teaching Analytics in the Marketing Curriculum

ERIC Educational Resources Information Center

Liu, Yiyuan; Levin, Michael A.

2018-01-01

With the emerging use of analytics tools and methodologies in marketing, marketing educators have provided students training and experiences beyond the soft skills associated with understanding consumer behavior. Previous studies have only discussed how to apply analytics in course designs, tools, and related practices. However, there is a lack of…

A simple method for the small scale synthesis and solid-phase extraction purification of steroid sulfates.

PubMed

Waller, Christopher C; McLeod, Malcolm D

2014-12-01

Steroid sulfates are a major class of steroid metabolite that are of growing importance in fields such as anti-doping analysis, the detection of residues in agricultural produce or medicine. Despite this, many steroid sulfate reference materials may have limited or no availability hampering the development of analytical methods. We report simple protocols for the rapid synthesis and purification of steroid sulfates that are suitable for adoption by analytical laboratories. Central to this approach is the use of solid-phase extraction (SPE) for purification, a technique routinely used for sample preparation in analytical laboratories around the world. The sulfate conjugates of sixteen steroid compounds encompassing a wide range of steroid substitution patterns and configurations are prepared, including the previously unreported sulfate conjugates of the designer steroids furazadrol (17β-hydroxyandrostan[2,3-d]isoxazole), isofurazadrol (17β-hydroxyandrostan[3,2-c]isoxazole) and trenazone (17β-hydroxyestra-4,9-dien-3-one). Structural characterization data, together with NMR and mass spectra are reported for all steroid sulfates, often for the first time. The scope of this approach for small scale synthesis is highlighted by the sulfation of 1μg of testosterone (17β-hydroxyandrost-4-en-3-one) as monitored by liquid chromatography-mass spectrometry (LCMS). Copyright © 2014 Elsevier Inc. All rights reserved.

Monitoring of Cr, Cu, Pb, V and Zn in polluted soils by laser induced breakdown spectroscopy (LIBS).

PubMed

Dell'Aglio, Marcella; Gaudiuso, Rosalba; Senesi, Giorgio S; De Giacomo, Alessandro; Zaccone, Claudio; Miano, Teodoro M; De Pascale, Olga

2011-05-01

Laser Induced Breakdown Spectroscopy (LIBS) is a fast and multi-elemental analytical technique particularly suitable for the qualitative and quantitative analysis of heavy metals in solid samples, including environmental ones. Although LIBS is often recognised in the literature as a well-established analytical technique, results about quantitative analysis of elements in chemically complex matrices such as soils are quite contrasting. In this work, soil samples of various origins have been analyzed by LIBS and data compared to those obtained by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). The emission intensities of one selected line for each of the five analytes (i.e., Cr, Cu, Pb, V, and Zn) were normalized to the background signal, and plotted as a function of the concentration values previously determined by ICP-OES. Data showed a good linearity for all calibration lines drawn, and the correlation between ICP-OES and LIBS was confirmed by the satisfactory agreement obtained between the corresponding values. Consequently, LIBS method can be used at least for metal monitoring in soils. In this respect, a simple method for the estimation of the soil pollution degree by heavy metals, based on the determination of an anthropogenic index, was proposed and determined for Cr and Zn.

Measured effects of coolant injection on the performance of a film cooled turbine

NASA Technical Reports Server (NTRS)

Mcdonel, J. D.; Eiswerth, J. E.

1977-01-01

Tests have been conducted on a 20-inch diameter single-stage air-cooled turbine designed to evaluate the effects of film cooling air on turbine aerodynamic performance. The present paper reports the results of five test configurations, including two different cooling designs and three combinations of cooled and solid airfoils. A comparison is made of the experimental results with a previously published analytical method of evaluating coolant injection effects on turbine performance.

New Methods for the Computational Fabrication of Appearance

DTIC Science & Technology

2015-06-01

disadvantage is that it does not model phenomena such as retro-reflection and grazing-angle e↵ects. We find that previously proposed BRDF metrics performed well...Figure 3.15-right shows the mean BRDF in blue and the corresponding error bars. In order to interpret our data, we fit a parametric model to slices of the...and Wojciech Matusik. Image-driven navigation of analytical brdf models . In Eurographics Symposium on Rendering, 2006. 107 [40] F. E. Nicodemus, J. C

FastChem: A computer program for efficient complex chemical equilibrium calculations in the neutral/ionized gas phase with applications to stellar and planetary atmospheres

NASA Astrophysics Data System (ADS)

Stock, Joachim W.; Kitzmann, Daniel; Patzer, A. Beate C.; Sedlmayr, Erwin

2018-06-01

For the calculation of complex neutral/ionized gas phase chemical equilibria, we present a semi-analytical versatile and efficient computer program, called FastChem. The applied method is based on the solution of a system of coupled nonlinear (and linear) algebraic equations, namely the law of mass action and the element conservation equations including charge balance, in many variables. Specifically, the system of equations is decomposed into a set of coupled nonlinear equations in one variable each, which are solved analytically whenever feasible to reduce computation time. Notably, the electron density is determined by using the method of Nelder and Mead at low temperatures. The program is written in object-oriented C++ which makes it easy to couple the code with other programs, although a stand-alone version is provided. FastChem can be used in parallel or sequentially and is available under the GNU General Public License version 3 at https://github.com/exoclime/FastChem together with several sample applications. The code has been successfully validated against previous studies and its convergence behavior has been tested even for extreme physical parameter ranges down to 100 K and up to 1000 bar. FastChem converges stable and robust in even most demanding chemical situations, which posed sometimes extreme challenges for previous algorithms.

Mechanisms of chemical vapor generation by aqueous tetrahydridoborate. Recent developments toward the definition of a more general reaction model

NASA Astrophysics Data System (ADS)

D'Ulivo, Alessandro

2016-05-01

A reaction model describing the reactivity of metal and semimetal species with aqueous tetrahydridoborate (THB) has been drawn taking into account the mechanism of chemical vapor generation (CVG) of hydrides, recent evidences on the mechanism of interference and formation of byproducts in arsane generation, and other evidences in the field of the synthesis of nanoparticles and catalytic hydrolysis of THB by metal nanoparticles. The new "non-analytical" reaction model is of more general validity than the previously described "analytical" reaction model for CVG. The non-analytical model is valid for reaction of a single analyte with THB and for conditions approaching those typically encountered in the synthesis of nanoparticles and macroprecipitates. It reduces to the previously proposed analytical model under conditions typically employed in CVG for trace analysis (analyte below the μM level, borane/analyte ≫ 103 mol/mol, no interference). The non-analytical reaction model is not able to explain all the interference effects observed in CVG, which can be achieved only by assuming the interaction among the species of reaction pathways of different analytical substrates. The reunification of CVG, the synthesis of nanoparticles by aqueous THB and the catalytic hydrolysis of THB inside a common frame contribute to rationalization of the complex reactivity of aqueous THB with metal and semimetal species.

Pesticides in near-surface aquifers: An assessment using highly sensitive analytical methods and tritium

USGS Publications Warehouse

Kolpin, D.W.; Goolsby, D.A.; Thurman, E.M.

1995-01-01

In 1992, the U.S. Geological Survey (USGS) determined the distribution of pesticides in near-surface aquifers of the midwestern USA to be much more widespread than originally determined during a 1991 USGS study. The frequency of pesticide detection increased from 28.4% during the 1991 study to 59.0% during the 1992 study. This increase in pesticide detection was primarily the result of a more sensitive analytical method that used reporting limits as much as 20 times lower than previously available and a threefold increase in the number of pesticide metabolites analyzed. No pesticide concentrations exceeded the U.S. Environmental Protection Agency's (USEPAs) maximum contaminant levels or health advisory levels for drinking water. However, five of the six most frequently detected compounds during 1992 were pesticide metabolites that currently do not have drinking water standards determined. The frequent presence of pesticide metabolites for this study documents the importance of obtaining information on these compounds to understand the fate and transport of pesticides in the hydrologic system. It appears that the 56 parent compounds analyzed follow similar pathways through the hydrologic system as atrazine. When atrazine was detected by routine or sensitive analytical methods, there was an increased likelihood of detecting additional parent compounds. As expected, the frequency of pesticide detection was highly dependent on the analytical reporting limit. The number of atrazine detections more than doubled as the reporting limit decreased from 0.10 to 0.01 µg/L. The 1992 data provided no indication that the frequency of pesticide detection would level off as improved analytical methods provide concentrations below 0.003 µg/L. A relation was determined between groundwater age and the frequency of pesticide detection, with 15.8% of the samples composed of pre-1953 water and 70.3% of the samples of post-1953 water having a detection of at least one pesticide or metabolite. Pre-1953 water is less likely to contain pesticides because it tends to predate the use of pesticides to increase crop production in the Midwest. Pre-1953 water was more likely to occur in the near-surface bedrock aquifers (50.0%) than in the near-surface unconsolidated aquifers (9.1%) sampled.

Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES.

PubMed

Matschat, Ralf; Hassler, Jürgen; Traub, Heike; Dette, Angelika

2005-12-01

The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and used to determine the repeatability and the reproducibility (expressed as standard deviations) of both methods. The calculation was carried out according to the related standard. The results are specified and discussed in this paper, as are the optimized analytical conditions determined and used by the authors of this paper. For both methods, the repeatability relative standard deviations were <25%, usually ~10%, and the reproducibility relative standard deviations were <35%, usually ~15%. These results were regarded as satifactory for both methods intended for rapid analysis of materials for which decomposition is difficult and time-consuming. Also described are some results from an interlaboratory comparison used to certify one of the materials that had been previously used for validation in both interlaboratory comparisons. Thirty laboratories (from eight countries) participated in this interlaboratory comparison for certification. As examples, accepted results are shown from laboratories that used ETV ICP OES or DC arc OES and had performed calibrations by using solutions or oxides, respectively. The certified mass fractions of the certified reference materials were also compared with the mass fractions determined in the interlaboratory comparisons performed within the framework of method standardization. Good agreement was found for most of the analytes.

Multipole moments in the effective fragment potential method

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

Bertoni, Colleen; Slipchenko, Lyudmila V.; Misquitta, Alston J.

In the effective fragment potential (EFP) method the Coulomb potential is represented using a set of multipole moments generated by the distributed multipole analysis (DMA) method. Misquitta, Stone, and Fazeli recently developed a basis space-iterated stockholder atom (BS-ISA) method to generate multipole moments. This study assesses the accuracy of the EFP interaction energies using sets of multipole moments generated from the BS-ISA method, and from several versions of the DMA method (such as analytic and numeric grid-based), with varying basis sets. Both methods lead to reasonable results, although using certain implementations of the DMA method can result in large errors.more » With respect to the CCSD(T)/CBS interaction energies, the mean unsigned error (MUE) of the EFP method for the S22 data set using BS-ISA–generated multipole moments and DMA-generated multipole moments (using a small basis set and the analytic DMA procedure) is 0.78 and 0.72 kcal/mol, respectively. Here, the MUE accuracy is on the same order as MP2 and SCS-MP2. The MUEs are lower than in a previous study benchmarking the EFP method without the EFP charge transfer term, demonstrating that the charge transfer term increases the accuracy of the EFP method. Regardless of the multipole moment method used, it is likely that much of the error is due to an insufficient short-range electrostatic term (i.e., charge penetration term), as shown by comparisons with symmetry-adapted perturbation theory.« less

Multipole moments in the effective fragment potential method

DOE PAGES

Bertoni, Colleen; Slipchenko, Lyudmila V.; Misquitta, Alston J.; ...

2017-02-17

In the effective fragment potential (EFP) method the Coulomb potential is represented using a set of multipole moments generated by the distributed multipole analysis (DMA) method. Misquitta, Stone, and Fazeli recently developed a basis space-iterated stockholder atom (BS-ISA) method to generate multipole moments. This study assesses the accuracy of the EFP interaction energies using sets of multipole moments generated from the BS-ISA method, and from several versions of the DMA method (such as analytic and numeric grid-based), with varying basis sets. Both methods lead to reasonable results, although using certain implementations of the DMA method can result in large errors.more » With respect to the CCSD(T)/CBS interaction energies, the mean unsigned error (MUE) of the EFP method for the S22 data set using BS-ISA–generated multipole moments and DMA-generated multipole moments (using a small basis set and the analytic DMA procedure) is 0.78 and 0.72 kcal/mol, respectively. Here, the MUE accuracy is on the same order as MP2 and SCS-MP2. The MUEs are lower than in a previous study benchmarking the EFP method without the EFP charge transfer term, demonstrating that the charge transfer term increases the accuracy of the EFP method. Regardless of the multipole moment method used, it is likely that much of the error is due to an insufficient short-range electrostatic term (i.e., charge penetration term), as shown by comparisons with symmetry-adapted perturbation theory.« less

Are LOD and LOQ Reliable Parameters for Sensitivity Evaluation of Spectroscopic Methods?

PubMed

Ershadi, Saba; Shayanfar, Ali

2018-03-22

The limit of detection (LOD) and the limit of quantification (LOQ) are common parameters to assess the sensitivity of analytical methods. In this study, the LOD and LOQ of previously reported terbium sensitized analysis methods were calculated by different methods, and the results were compared with sensitivity parameters [lower limit of quantification (LLOQ)] of U.S. Food and Drug Administration guidelines. The details of the calibration curve and standard deviation of blank samples of three different terbium-sensitized luminescence methods for the quantification of mycophenolic acid, enrofloxacin, and silibinin were used for the calculation of LOD and LOQ. A comparison of LOD and LOQ values calculated by various methods and LLOQ shows a considerable difference. The significant difference of the calculated LOD and LOQ with various methods and LLOQ should be considered in the sensitivity evaluation of spectroscopic methods.

Dissociable meta-analytic brain networks contribute to coordinated emotional processing.

PubMed

Riedel, Michael C; Yanes, Julio A; Ray, Kimberly L; Eickhoff, Simon B; Fox, Peter T; Sutherland, Matthew T; Laird, Angela R

2018-06-01

Meta-analytic techniques for mining the neuroimaging literature continue to exert an impact on our conceptualization of functional brain networks contributing to human emotion and cognition. Traditional theories regarding the neurobiological substrates contributing to affective processing are shifting from regional- towards more network-based heuristic frameworks. To elucidate differential brain network involvement linked to distinct aspects of emotion processing, we applied an emergent meta-analytic clustering approach to the extensive body of affective neuroimaging results archived in the BrainMap database. Specifically, we performed hierarchical clustering on the modeled activation maps from 1,747 experiments in the affective processing domain, resulting in five meta-analytic groupings of experiments demonstrating whole-brain recruitment. Behavioral inference analyses conducted for each of these groupings suggested dissociable networks supporting: (1) visual perception within primary and associative visual cortices, (2) auditory perception within primary auditory cortices, (3) attention to emotionally salient information within insular, anterior cingulate, and subcortical regions, (4) appraisal and prediction of emotional events within medial prefrontal and posterior cingulate cortices, and (5) induction of emotional responses within amygdala and fusiform gyri. These meta-analytic outcomes are consistent with a contemporary psychological model of affective processing in which emotionally salient information from perceived stimuli are integrated with previous experiences to engender a subjective affective response. This study highlights the utility of using emergent meta-analytic methods to inform and extend psychological theories and suggests that emotions are manifest as the eventual consequence of interactions between large-scale brain networks. © 2018 Wiley Periodicals, Inc.

Perioperative and ICU Healthcare Analytics within a Veterans Integrated System Network: a Qualitative Gap Analysis.

PubMed

Mudumbai, Seshadri; Ayer, Ferenc; Stefanko, Jerry

2017-08-01

Health care facilities are implementing analytics platforms as a way to document quality of care. However, few gap analyses exist on platforms specifically designed for patients treated in the Operating Room, Post-Anesthesia Care Unit, and Intensive Care Unit (ICU). As part of a quality improvement effort, we undertook a gap analysis of an existing analytics platform within the Veterans Healthcare Administration. The objectives were to identify themes associated with 1) current clinical use cases and stakeholder needs; 2) information flow and pain points; and 3) recommendations for future analytics development. Methods consisted of semi-structured interviews in 2 phases with a diverse set (n = 9) of support personnel and end users from five facilities across a Veterans Integrated Service Network. Phase 1 identified underlying needs and previous experiences with the analytics platform across various roles and operational responsibilities. Phase 2 validated preliminary feedback, lessons learned, and recommendations for improvement. Emerging themes suggested that the existing system met a small pool of national reporting requirements. However, pain points were identified with accessing data in several information system silos and performing multiple manual validation steps of data content. Notable recommendations included enhancing systems integration to create "one-stop shopping" for data, and developing a capability to perform trends analysis. Our gap analysis suggests that analytics platforms designed for surgical and ICU patients should employ approaches similar to those being used for primary care patients.

A multi-band semi-analytical algorithm for estimating chlorophyll-a concentration in the Yellow River Estuary, China.

PubMed

Chen, Jun; Quan, Wenting; Cui, Tingwei

2015-01-01

In this study, two sample semi-analytical algorithms and one new unified multi-band semi-analytical algorithm (UMSA) for estimating chlorophyll-a (Chla) concentration were constructed by specifying optimal wavelengths. The three sample semi-analytical algorithms, including the three-band semi-analytical algorithm (TSA), four-band semi-analytical algorithm (FSA), and UMSA algorithm, were calibrated and validated by the dataset collected in the Yellow River Estuary between September 1 and 10, 2009. By comparing of the accuracy of assessment of TSA, FSA, and UMSA algorithms, it was found that the UMSA algorithm had a superior performance in comparison with the two other algorithms, TSA and FSA. Using the UMSA algorithm in retrieving Chla concentration in the Yellow River Estuary decreased by 25.54% NRMSE (normalized root mean square error) when compared with the FSA algorithm, and 29.66% NRMSE in comparison with the TSA algorithm. These are very significant improvements upon previous methods. Additionally, the study revealed that the TSA and FSA algorithms are merely more specific forms of the UMSA algorithm. Owing to the special form of the UMSA algorithm, if the same bands were used for both the TSA and UMSA algorithms or FSA and UMSA algorithms, the UMSA algorithm would theoretically produce superior results in comparison with the TSA and FSA algorithms. Thus, good results may also be produced if the UMSA algorithm were to be applied for predicting Chla concentration for datasets of Gitelson et al. (2008) and Le et al. (2009).

Development of a CZE method for the quantification of pseudoephedrine and cetirizine.

PubMed

Alnajjar, Ahmed O; Idris, Abubakr M

2014-10-01

Pseudoephedrine and cetirizine have been combined in dosage forms with more therapeutic benefits when compared with single-drug treatment. The current manuscript reports the development of the first capillary zone electrophoresis (CZE) assay method for that combination. The effects of pH and buffer concentration on resolution, noise, migration time and peak area were examined employing experimental design approach. The analytes were electropherographed into a 50.2 cm-long and 50 µm i.d. fused-silica capillary column using 10 mmol/L borate at pH 8.3 with a potential of 25 kV at 25°C and UV detection at 214 nm. The method was successfully validated in order to verify its suitability for pharmaceutical analysis for the purposes of quality control. Over previous high-performance liquid chromatographic methods, the current CZE method features the benefits of the use of cost-effective electrolyte, besides high sample throughput (11 samples/h). Furthermore, other analytical results including linear dynamic ranges, recovery (96.9-98.1%), intra- and interday precision (relative standard deviation ≤ 1.70%) as well as the limits of detection and quantification (≤2.65 µg/mL) were all satisfactory for the intended purpose. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

21 CFR 530.22 - Safe levels and analytical methods for food-producing animals.

Code of Federal Regulations, 2011 CFR

2011-04-01

... analytical method; or (3) Establish a safe level based on other appropriate scientific, technical, or... 21 Food and Drugs 6 2011-04-01 2011-04-01 false Safe levels and analytical methods for food... § 530.22 Safe levels and analytical methods for food-producing animals. (a) FDA may establish a safe...

21 CFR 530.22 - Safe levels and analytical methods for food-producing animals.

Code of Federal Regulations, 2014 CFR

2014-04-01

... analytical method; or (3) Establish a safe level based on other appropriate scientific, technical, or... 21 Food and Drugs 6 2014-04-01 2014-04-01 false Safe levels and analytical methods for food... § 530.22 Safe levels and analytical methods for food-producing animals. (a) FDA may establish a safe...

21 CFR 530.22 - Safe levels and analytical methods for food-producing animals.

Code of Federal Regulations, 2012 CFR

2012-04-01

... analytical method; or (3) Establish a safe level based on other appropriate scientific, technical, or... 21 Food and Drugs 6 2012-04-01 2012-04-01 false Safe levels and analytical methods for food... § 530.22 Safe levels and analytical methods for food-producing animals. (a) FDA may establish a safe...

21 CFR 530.22 - Safe levels and analytical methods for food-producing animals.

Code of Federal Regulations, 2013 CFR

2013-04-01

... analytical method; or (3) Establish a safe level based on other appropriate scientific, technical, or... 21 Food and Drugs 6 2013-04-01 2013-04-01 false Safe levels and analytical methods for food... § 530.22 Safe levels and analytical methods for food-producing animals. (a) FDA may establish a safe...

Development and validation of a turbulent flow chromatography and tandem mass spectrometry method for the quantitation of methotrexate and its metabolites 7-hydroxy methotrexate and DAMPA in serum

PubMed Central

Schofield, Ryan C.; Ramanathan, Lakshmi V.; Murata, Kazunori; Grace, Marie; Fleisher, Martin; Pessin, Melissa S.; Carlow, Dean C.

2016-01-01

A rapid and simple turbulent flow liquid chromatography (TFC–LC) method implementing positive heated electrospray ionization (HESI) for the accurate and precise determination of methotrexate (MTX), 7-hydroxy methotrexate (7-OH MTX), and 4-amino-4-deoxy-N10-methylpteroic acid (DAMPA) concentrations in serum was developed. MTX was isolated from serum samples (100 μL) after protein precipitation with methanol containing formic acid and internal standard (MTX-D3) followed by centrifugation. The supernatant was injected into the turbulent flow liquid chromatography which is followed by electrospray positive ionization tandem mass spectrometry (TFC–LC–MS/MS) and quantified using a six-point calibration curve. For MTX and DAMPA the assays were linear from 10 to 1000 nmol/L and for 7-OH MTX from 20 to 2000 nmol/L. Dilutions of 10, 100 and 1000-fold were validated giving a clinically reportable range of 10 nmol/L to 5 × 105 nmol/L. Within-day and between-day precisions at concentrations spanning the analytical measurement ranges were less than 10% for all three analytes. MTX, DAMPA and 7-OH MTX were sufficiently stable under all relevant analytical conditions. No significant matrix effect was observed during the method validation. The TFC–LC-MS/MS MTX method was also compared with three other clinically validated MTX assays: a dihydrofolate reductase (DHFR) inhibition assay, an immunoassay based on fluorescence polarization and a previously developed LC–MS/MS assay. PMID:26322588

Documentation of spreadsheets for the analysis of aquifer-test and slug-test data

USGS Publications Warehouse

Halford, Keith J.; Kuniansky, Eve L.

2002-01-01

Several spreadsheets have been developed for the analysis of aquifer-test and slug-test data. Each spreadsheet incorporates analytical solution(s) of the partial differential equation for ground-water flow to a well for a specific type of condition or aquifer. The derivations of the analytical solutions were previously published. Thus, this report abbreviates the theoretical discussion, but includes practical information about each method and the important assumptions for the applications of each method. These spreadsheets were written in Microsoft Excel 9.0 (use of trade names does not constitute endorsement by the USGS). Storage properties should not be estimated with many of the spreadsheets because most are for analyzing single-well tests. Estimation of storage properties from single-well tests is generally discouraged because single-well tests are affected by wellbore storage and by well construction. These non-ideal effects frequently cause estimates of storage to be erroneous by orders of magnitude. Additionally, single-well tests are not sensitive to aquifer-storage properties. Single-well tests include all slug tests (Bouwer and Rice Method, Cooper, Bredehoeft, Papadopulos Method, and van der Kamp Method), the Cooper-Jacob straight-line Method, Theis recovery-data analysis, Jacob-Lohman method for flowing wells in a confined aquifer, and the step-drawdown test. Multi-well test spreadsheets included in this report are; Hantush-Jacob Leaky Aquifer Method and Distance-Drawdown Methods. The distance-drawdown method is an equilibrium or steady-state method, thus storage cannot be estimated.

An improvement of convergence of a dispersion-relation preserving method for the classical Boussinesq equation

NASA Astrophysics Data System (ADS)

Jang, T. S.

2018-03-01

A dispersion-relation preserving (DRP) method, as a semi-analytic iterative procedure, has been proposed by Jang (2017) for integrating the classical Boussinesq equation. It has been shown to be a powerful numerical procedure for simulating a nonlinear dispersive wave system because it preserves the dispersion-relation, however, there still exists a potential flaw, e.g., a restriction on nonlinear wave amplitude and a small region of convergence (ROC) and so on. To remedy the flaw, a new DRP method is proposed in this paper, aimed at improving convergence performance. The improved method is proved to have convergence properties and dispersion-relation preserving nature for small waves; of course, unique existence of the solutions is also proved. In addition, by a numerical experiment, the method is confirmed to be good at observing nonlinear wave phenomena such as moving solitary waves and their binary collision with different wave amplitudes. Especially, it presents a ROC (much) wider than that of the previous method by Jang (2017). Moreover, it gives the numerical simulation of a high (or large-amplitude) nonlinear dispersive wave. In fact, it is demonstrated to simulate a large-amplitude solitary wave and the collision of two solitary waves with large-amplitudes that we have failed to simulate with the previous method. Conclusively, it is worth noting that better convergence results are achieved compared to Jang (2017); i.e., they represent a major improvement in practice over the previous method.

Novel two-step laser ablation and ionization mass spectrometry (2S-LAIMS) of actor-spectator ice layers: Probing chemical composition of D{sub 2}O ice beneath a H{sub 2}O ice layer

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

Yang, Rui, E-mail: ryang73@ustc.edu; Gudipati, Murthy S., E-mail: gudipati@jpl.nasa.gov

2014-03-14

In this work, we report for the first time successful analysis of organic aromatic analytes imbedded in D{sub 2}O ices by novel infrared (IR) laser ablation of a layered non-absorbing D{sub 2}O ice (spectator) containing the analytes and an ablation-active IR-absorbing H{sub 2}O ice layer (actor) without the analyte. With these studies we have opened up a new method for the in situ analysis of solids containing analytes when covered with an IR laser-absorbing layer that can be resonantly ablated. This soft ejection method takes advantage of the tenability of two-step infrared laser ablation and ultraviolet laser ionization mass spectrometry,more » previously demonstrated in this lab to study chemical reactions of polycyclic aromatic hydrocarbons (PAHs) in cryogenic ices. The IR laser pulse tuned to resonantly excite only the upper H{sub 2}O ice layer (actor) generates a shockwave upon impact. This shockwave penetrates the lower analyte-containing D{sub 2}O ice layer (spectator, a non-absorbing ice that cannot be ablated directly with the wavelength of the IR laser employed) and is reflected back, ejecting the contents of the D{sub 2}O layer into the vacuum where they are intersected by a UV laser for ionization and detection by a time-of-flight mass spectrometer. Thus, energy is transmitted from the laser-absorbing actor layer into the non-absorbing spectator layer resulting its ablation. We found that isotope cross-contamination between layers was negligible. We also did not see any evidence for thermal or collisional chemistry of PAH molecules with H{sub 2}O molecules in the shockwave. We call this “shockwave mediated surface resonance enhanced subsurface ablation” technique as “two-step laser ablation and ionization mass spectrometry of actor-spectator ice layers.” This method has its roots in the well-established MALDI (matrix assisted laser desorption and ionization) method. Our method offers more flexibility to optimize both the processes—ablation and ionization. This new technique can thus be potentially employed to undertake in situ analysis of materials imbedded in diverse media, such as cryogenic ices, biological samples, tissues, minerals, etc., by covered with an IR-absorbing laser ablation medium and study the chemical composition and reaction pathways of the analyte in its natural surroundings.« less

SAM Methods Query

EPA Pesticide Factsheets

Laboratories measuring target chemical, radiochemical, pathogens, and biotoxin analytes in environmental samples can use this online query tool to identify analytical methods included in EPA's Selected Analytical Methods for Environmental Remediation

Simultaneous determination of flurbiprofen and its hydroxy metabolite in human plasma by liquid chromatography-tandem mass spectrometry for clinical application.

PubMed

Lee, Hye-In; Choi, Chang-Ik; Byeon, Ji-Yeong; Lee, Jung-Eun; Park, So-Young; Kim, Young-Hoon; Kim, Se-Hyung; Lee, Yun-Jeong; Jang, Choon-Gon; Lee, Seok-Yong

2014-11-15

Flurbiprofen (FLB) is one of the phenylalkanoic acid derivatives of non-steroidal anti-inflammatory drugs used for the management of pain and inflammation in patients with arthritis. We developed and validated a rapid and sensitive high-performance liquid chromatography analytical method utilizing tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of FLB and its major metabolite, 4'-hydroxyflurbiprofen (4'-OH-FLB), in human plasma. Probenecid was used as an internal standard (IS). After liquid-liquid extraction with methyl t-butyl ether, chromatographic separation of the two analytes was achieved using a reversed-phase Luna C18 column (2.0mm×50mm, 5μm particles) with a mobile phase of 10mM ammonium formate buffer (pH 3.5)-methanol (15:85, v/v) and quantified by MS/MS detection in ESI negative ion mode. The flow rate of the mobile phase was 250μl/min and the retention times of FLB, 4'-OH-FLB, and IS were 1.1, 0.8, and 0.9min, respectively. The calibration curves were linear over a range of 0.01-10μg/ml for FLB and 0.01-1μg/ml for 4'-OH-FLB. The lower limit of quantifications using 100μl of human plasma was 0.01μg/ml for both analytes. The mean accuracy and precision for intra- and inter-run validation of FLB and 4'-OH-FLB were all within acceptable limits. The present HPLC-MS/MS method showed improved sensitivity for quantification of the FLB and its major metabolite in human plasma compared with previously described analytical methods. The validated method was successfully applied to a pharmacokinetic study in humans. Copyright © 2014 Elsevier B.V. All rights reserved.

Sources and preparation of data for assessing trends in concentrations of pesticides in streams of the United States, 1992–2010

USGS Publications Warehouse

Martin, Jeffrey D.; Eberle, Michael; Nakagaki, Naomi

2011-01-01

This report updates a previously published water-quality dataset of 44 commonly used pesticides and 8 pesticide degradates suitable for a national assessment of trends in pesticide concentrations in streams of the United States. Water-quality samples collected from January 1992 through September 2010 at stream-water sites of the U.S. Geological Survey (USGS) National Water-Quality Assessment (NAWQA) Program and the National Stream Quality Accounting Network (NASQAN) were compiled, reviewed, selected, and prepared for trend analysis. The principal steps in data review for trend analysis were to (1) identify analytical schedule, (2) verify sample-level coding, (3) exclude inappropriate samples or results, (4) review pesticide detections per sample, (5) review high pesticide concentrations, and (6) review the spatial and temporal extent of NAWQA pesticide data and selection of analytical methods for trend analysis. The principal steps in data preparation for trend analysis were to (1) select stream-water sites for trend analysis, (2) round concentrations to a consistent level of precision for the concentration range, (3) identify routine reporting levels used to report nondetections unaffected by matrix interference, (4) reassign the concentration value for routine nondetections to the maximum value of the long-term method detection level (maxLT-MDL), (5) adjust concentrations to compensate for temporal changes in bias of recovery of the gas chromatography/mass spectrometry (GCMS) analytical method, and (6) identify samples considered inappropriate for trend analysis. Samples analyzed at the USGS National Water Quality Laboratory (NWQL) by the GCMS analytical method were the most extensive in time and space and, consequently, were selected for trend analysis. Stream-water sites with 3 or more water years of data with six or more samples per year were selected for pesticide trend analysis. The selection criteria described in the report produced a dataset of 21,988 pesticide samples at 212 stream-water sites. Only 21,144 pesticide samples, however, are considered appropriate for trend analysis.

Extracting laboratory test information from biomedical text

PubMed Central

Kang, Yanna Shen; Kayaalp, Mehmet

2013-01-01

Background: No previous study reported the efficacy of current natural language processing (NLP) methods for extracting laboratory test information from narrative documents. This study investigates the pathology informatics question of how accurately such information can be extracted from text with the current tools and techniques, especially machine learning and symbolic NLP methods. The study data came from a text corpus maintained by the U.S. Food and Drug Administration, containing a rich set of information on laboratory tests and test devices. Methods: The authors developed a symbolic information extraction (SIE) system to extract device and test specific information about four types of laboratory test entities: Specimens, analytes, units of measures and detection limits. They compared the performance of SIE and three prominent machine learning based NLP systems, LingPipe, GATE and BANNER, each implementing a distinct supervised machine learning method, hidden Markov models, support vector machines and conditional random fields, respectively. Results: Machine learning systems recognized laboratory test entities with moderately high recall, but low precision rates. Their recall rates were relatively higher when the number of distinct entity values (e.g., the spectrum of specimens) was very limited or when lexical morphology of the entity was distinctive (as in units of measures), yet SIE outperformed them with statistically significant margins on extracting specimen, analyte and detection limit information in both precision and F-measure. Its high recall performance was statistically significant on analyte information extraction. Conclusions: Despite its shortcomings against machine learning methods, a well-tailored symbolic system may better discern relevancy among a pile of information of the same type and may outperform a machine learning system by tapping into lexically non-local contextual information such as the document structure. PMID:24083058

Analytical Description of Ascending Motion of Rockets in the Atmosphere

ERIC Educational Resources Information Center

Rodrigues, H.; de Pinho, M. O.; Portes, D., Jr.; Santiago, A.

2009-01-01

In continuation of a previous work, we present an analytic study of ascending vertical motion of a rocket subjected to a quadratic drag for the case where the mass-variation law is a linear function of time. We discuss the detailed analytical solution of the model differential equations in closed form. Examples of application are presented and…

Assessing the utility of transcriptome data for inferring phylogenetic relationships among coleoid cephalopods.

PubMed

Lindgren, Annie R; Anderson, Frank E

2018-01-01

Historically, deep-level relationships within the molluscan class Cephalopoda (squids, cuttlefishes, octopods and their relatives) have remained elusive due in part to the considerable morphological diversity of extant taxa, a limited fossil record for species that lack a calcareous shell and difficulties in sampling open ocean taxa. Many conflicts identified by morphologists in the early 1900s remain unresolved today in spite of advances in morphological, molecular and analytical methods. In this study we assess the utility of transcriptome data for resolving cephalopod phylogeny, with special focus on the orders of Decapodiformes (open-eye squids, bobtail squids, cuttlefishes and relatives). To do so, we took new and previously published transcriptome data and used a unique cephalopod core ortholog set to generate a dataset that was subjected to an array of filtering and analytical methods to assess the impacts of: taxon sampling, ortholog number, compositional and rate heterogeneity and incongruence across loci. Analyses indicated that datasets that maximized taxonomic coverage but included fewer orthologs were less stable than datasets that sacrificed taxon sampling to increase the number of orthologs. Clades recovered irrespective of dataset, filtering or analytical method included Octopodiformes (Vampyroteuthis infernalis + octopods), Decapodiformes (squids, cuttlefishes and their relatives), and orders Oegopsida (open-eyed squids) and Myopsida (e.g., loliginid squids). Ordinal-level relationships within Decapodiformes were the most susceptible to dataset perturbation, further emphasizing the challenges associated with uncovering relationships at deep nodes in the cephalopod tree of life. Copyright © 2017 Elsevier Inc. All rights reserved.

An overview of gamma-hydroxybutyric acid: pharmacodynamics, pharmacokinetics, toxic effects, addiction, analytical methods, and interpretation of results.

PubMed

Andresen, H; Aydin, B E; Mueller, A; Iwersen-Bergmann, S

2011-09-01

Abuse of gamma-hydroxybutyric acid (GHB) has been known since the early 1990's, but is not as widespread as the consumption of other illegal drugs. However, the number of severe intoxications with fatal outcomes is comparatively high; not the least of which is brought about by the consumption of the currently legal precursor substances gamma-butyrolactone (GBL) and 1,4-butanediol (1,4-BD). In regards to previous assumptions, addiction to GHB or its analogues can occur with severe symptoms of withdrawal. Moreover, GHB can be used for drug-facilitated sexual assaults. Its pharmacological effects are generated mainly by interaction with both GABA(B) and GHB receptors, as well as its influence on other transmitter systems in the human brain. Numerous analytical methods for determining GHB using chromatographic techniques were published in recent years, and an enzymatic screening method was established. However, the short window of GHB detection in blood or urine due to its rapid metabolism is a challenge. Furthermore, despite several studies addressing this problem, evaluation of analytical results can be difficult: GHB is a metabolite of GABA (gamma-aminobutyric acid); a differentiation between endogenous and exogenous concentrations has to be made. Apart from this, in samples with a longer storage interval and especially in postmortem specimens, higher levels can be measured due to GHB generation during this postmortem interval or storage time. Copyright © 2011 John Wiley & Sons, Ltd.

Thermal transport in dimerized harmonic lattices: Exact solution, crossover behavior, and extended reservoirs

NASA Astrophysics Data System (ADS)

Chien, Chih-Chun; Kouachi, Said; Velizhanin, Kirill A.; Dubi, Yonatan; Zwolak, Michael

2017-01-01

We present a method for calculating analytically the thermal conductance of a classical harmonic lattice with both alternating masses and nearest-neighbor couplings when placed between individual Langevin reservoirs at different temperatures. The method utilizes recent advances in analytic diagonalization techniques for certain classes of tridiagonal matrices. It recovers the results from a previous method that was applicable for alternating on-site parameters only, and extends the applicability to realistic systems in which masses and couplings alternate simultaneously. With this analytic result in hand, we show that the thermal conductance is highly sensitive to the modulation of the couplings. This is due to the existence of topologically induced edge modes at the lattice-reservoir interface and is also a reflection of the symmetries of the lattice. We make a connection to a recent work that demonstrates thermal transport is analogous to chemical reaction rates in solution given by Kramers' theory [Velizhanin et al., Sci. Rep. 5, 17506 (2015)], 10.1038/srep17506. In particular, we show that the turnover behavior in the presence of edge modes prevents calculations based on single-site reservoirs from coming close to the natural—or intrinsic—conductance of the lattice. Obtaining the correct value of the intrinsic conductance through simulation of even a small lattice where ballistic effects are important requires quite large extended reservoir regions. Our results thus offer a route for both the design and proper simulation of thermal conductance of nanoscale devices.

New Method for calculating dynamical friction on a star moving through gas using Cartesian Simulations

NASA Astrophysics Data System (ADS)

Peng, Bo; Blackman, Eric

2018-01-01

Closely interacting binary stars can incur Common Envelope Evolution (CEE) when at least one of the stars enters a giant phase. The extent to which CEE leads to envelope ejection and how tight the binaries become after CEE as a function of the mass and type of the companion stars has a broad range of phenomenological implications for both low mass and high mass binary stellar systems. Global simulations of CEE are emerging, but to understand the underlying physics of CEE and make connections with analytic formalisms, it helpful to employ reduced numerical models. Here we present results and analyses from simulations of gravitational drag using a Cartesian approach. Using AstroBEAR, a parallelized hydrodynamic/MHD simulation code, we simulate a system in which a 0.1 MSun main sequence secondary star is embedded in gas characteristic of the Envelope of a 3 MSun AGB star. The relative motion of the secondary star against the stationary envelope is represented by a supersonic wind that immerses a point particle, which is initially at rest, yet gradually dragged by the wind. Our approach differs from previous related wind-tunnel work by MacLeod et al. (2015,2017) in that we allow the particle to be displaced, offering a direct measurement of the drag force from its motion. We verify the validity of our method, extract the accretion rate of material in the wake via numerical integration, and compare the results between our method and previous work. We also use the results to help constrain the efficiency parameter in widely used analytic parameterizations of CEE.

SAM Pathogen Methods Query

EPA Pesticide Factsheets

Laboratories measuring target pathogen analytes in environmental samples can use this online query tool to identify analytical methods in EPA's Selected Analytical Methods for Environmental Remediation and Recovery for select pathogens.

Dynamic one-dimensional modeling of secondary settling tanks and system robustness evaluation.

PubMed

Li, Ben; Stenstrom, M K

2014-01-01

One-dimensional secondary settling tank models are widely used in current engineering practice for design and optimization, and usually can be expressed as a nonlinear hyperbolic or nonlinear strongly degenerate parabolic partial differential equation (PDE). Reliable numerical methods are needed to produce approximate solutions that converge to the exact analytical solutions. In this study, we introduced a reliable numerical technique, the Yee-Roe-Davis (YRD) method as the governing PDE solver, and compared its reliability with the prevalent Stenstrom-Vitasovic-Takács (SVT) method by assessing their simulation results at various operating conditions. The YRD method also produced a similar solution to the previously developed Method G and Enquist-Osher method. The YRD and SVT methods were also used for a time-to-failure evaluation, and the results show that the choice of numerical method can greatly impact the solution. Reliable numerical methods, such as the YRD method, are strongly recommended.

Direct application of Padé approximant for solving nonlinear differential equations.

PubMed

Vazquez-Leal, Hector; Benhammouda, Brahim; Filobello-Nino, Uriel; Sarmiento-Reyes, Arturo; Jimenez-Fernandez, Victor Manuel; Garcia-Gervacio, Jose Luis; Huerta-Chua, Jesus; Morales-Mendoza, Luis Javier; Gonzalez-Lee, Mario

2014-01-01

This work presents a direct procedure to apply Padé method to find approximate solutions for nonlinear differential equations. Moreover, we present some cases study showing the strength of the method to generate highly accurate rational approximate solutions compared to other semi-analytical methods. The type of tested nonlinear equations are: a highly nonlinear boundary value problem, a differential-algebraic oscillator problem, and an asymptotic problem. The high accurate handy approximations obtained by the direct application of Padé method shows the high potential if the proposed scheme to approximate a wide variety of problems. What is more, the direct application of the Padé approximant aids to avoid the previous application of an approximative method like Taylor series method, homotopy perturbation method, Adomian Decomposition method, homotopy analysis method, variational iteration method, among others, as tools to obtain a power series solutions to post-treat with the Padé approximant. 34L30.

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... person or laboratory using a test procedure (analytical method) in this Part. (2) Chemistry of the method... (analytical method) provided that the chemistry of the method or the determinative technique is not changed... prevent efficient recovery of organic pollutants and prevent the method from meeting QC requirements, the...

SAM Biotoxin Methods Query

EPA Pesticide Factsheets

Laboratories measuring target biotoxin analytes in environmental samples can use this online query tool to identify analytical methods included in EPA's Selected Analytical Methods for Environmental Remediation and Recovery for select biotoxins.

SAM Chemical Methods Query

EPA Pesticide Factsheets

Laboratories measuring target chemical, radiochemical, pathogens, and biotoxin analytes in environmental samples can use this online query tool to identify analytical methods in EPA's Selected Analytical Methods for Environmental Remediation and Recovery

Schinus terebinthifolius countercurrent chromatography (Part III): Method transfer from small countercurrent chromatography column to preparative centrifugal partition chromatography ones as a part of method development.

PubMed

das Neves Costa, Fernanda; Hubert, Jane; Borie, Nicolas; Kotland, Alexis; Hewitson, Peter; Ignatova, Svetlana; Renault, Jean-Hugues

2017-03-03

Countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC) are support free liquid-liquid chromatography techniques sharing the same basic principles and features. Method transfer has previously been demonstrated for both techniques but never from one to another. This study aimed to show such a feasibility using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. Heptane - ethyl acetate - methanol -water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds. The optimized separation methodology previously described in Part I and II, was scaled up from an analytical hydrodynamic CCC column (17.4mL) to preparative hydrostatic CPC instruments (250mL and 303mL) as a part of method development. Flow-rate and sample loading were further optimized on CPC. Mobile phase linear velocity is suggested as a transfer invariant parameter if the CPC column contains sufficient number of partition cells. Copyright © 2017 Elsevier B.V. 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.

7 CFR 91.23 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 91.23 Section 91.23 Agriculture... SERVICES AND GENERAL INFORMATION Method Manuals § 91.23 Analytical methods. Most analyses are performed according to approved procedures described in manuals of standardized methodology. These standard methods...

7 CFR 91.23 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 91.23 Section 91.23 Agriculture... SERVICES AND GENERAL INFORMATION Method Manuals § 91.23 Analytical methods. Most analyses are performed according to approved procedures described in manuals of standardized methodology. These standard methods...

7 CFR 91.23 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 91.23 Section 91.23 Agriculture... SERVICES AND GENERAL INFORMATION Method Manuals § 91.23 Analytical methods. Most analyses are performed according to approved procedures described in manuals of standardized methodology. These standard methods...

Net analyte signal standard addition method (NASSAM) as a novel spectrofluorimetric and spectrophotometric technique for simultaneous determination, application to assay of melatonin and pyridoxine

NASA Astrophysics Data System (ADS)

Asadpour-Zeynali, Karim; Bastami, Mohammad

2010-02-01

In this work a new modification of the standard addition method called "net analyte signal standard addition method (NASSAM)" is presented for the simultaneous spectrofluorimetric and spectrophotometric analysis. The proposed method combines the advantages of standard addition method with those of net analyte signal concept. The method can be applied for the determination of analyte in the presence of known interferents. The accuracy of the predictions against H-point standard addition method is not dependent on the shape of the analyte and interferent spectra. The method was successfully applied to simultaneous spectrofluorimetric and spectrophotometric determination of pyridoxine (PY) and melatonin (MT) in synthetic mixtures and in a pharmaceutical formulation.

Nucleic acid hybridization with RNA immobilized on filter paper.

NASA Technical Reports Server (NTRS)

Saxinger, W. C.; Ponnamperuma, C.; Gillespie, D.

1972-01-01

RNA has been immobilized in a manner suitable for use in molecular hybridization experiments with dissolved RNA or DNA by a nonaqueous solid-phase reaction with carbonyldiimidazole and RNA 'dry coated' on cellulose or, preferably, on previously activated phosphocellulose filters. Immobilization of RNA does not appear to alter its chemical character or cause it to acquire affinity for unspecific RNA or DNA. The versatility and efficiency of this method make it potentially attractive for use in routine analytical or preparative hybridization experiments, among other applications.

Smart Phase Tuning in Microwave Photonic Integrated Circuits Toward Automated Frequency Multiplication by Design

NASA Astrophysics Data System (ADS)

Nabavi, N.

2018-07-01

The author investigates the monitoring methods for fine adjustment of the previously proposed on-chip architecture for frequency multiplication and translation of harmonics by design. Digital signal processing (DSP) algorithms are utilized to create an optimized microwave photonic integrated circuit functionality toward automated frequency multiplication. The implemented DSP algorithms are formed on discrete Fourier transform and optimization-based algorithms (Greedy and gradient-based algorithms), which are analytically derived and numerically compared based on the accuracy and speed of convergence criteria.

The Simpson's paradox unraveled

PubMed Central

Hernán, Miguel A; Clayton, David; Keiding, Niels

2011-01-01

Background In a famous article, Simpson described a hypothetical data example that led to apparently paradoxical results. Methods We make the causal structure of Simpson's example explicit. Results We show how the paradox disappears when the statistical analysis is appropriately guided by subject-matter knowledge. We also review previous explanations of Simpson's paradox that attributed it to two distinct phenomena: confounding and non-collapsibility. Conclusion Analytical errors may occur when the problem is stripped of its causal context and analyzed merely in statistical terms. PMID:21454324

An analytical model of leakage neutron equivalent dose for passively-scattered proton radiotherapy and validation with measurements.

PubMed

Schneider, Christopher; Newhauser, Wayne; Farah, Jad

2015-05-18

Exposure to stray neutrons increases the risk of second cancer development after proton therapy. Previously reported analytical models of this exposure were difficult to configure and had not been investigated below 100 MeV proton energy. The purposes of this study were to test an analytical model of neutron equivalent dose per therapeutic absorbed dose  at 75 MeV and to improve the model by reducing the number of configuration parameters and making it continuous in proton energy from 100 to 250 MeV. To develop the analytical model, we used previously published H/D values in water from Monte Carlo simulations of a general-purpose beamline for proton energies from 100 to 250 MeV. We also configured and tested the model on in-air neutron equivalent doses measured for a 75 MeV ocular beamline. Predicted H/D values from the analytical model and Monte Carlo agreed well from 100 to 250 MeV (10% average difference). Predicted H/D values from the analytical model also agreed well with measurements at 75 MeV (15% average difference). The results indicate that analytical models can give fast, reliable calculations of neutron exposure after proton therapy. This ability is absent in treatment planning systems but vital to second cancer risk estimation.

Teaching Analytical Method Transfer through Developing and Validating Then Transferring Dissolution Testing Methods for Pharmaceuticals

ERIC Educational Resources Information Center

Kimaru, Irene; Koether, Marina; Chichester, Kimberly; Eaton, Lafayette

2017-01-01

Analytical method transfer (AMT) and dissolution testing are important topics required in industry that should be taught in analytical chemistry courses. Undergraduate students in senior level analytical chemistry laboratory courses at Kennesaw State University (KSU) and St. John Fisher College (SJFC) participated in development, validation, and…

Revisiting the Relationship between Individual Differences in Analytic Thinking and Religious Belief: Evidence That Measurement Order Moderates Their Inverse Correlation.

PubMed

Finley, Anna J; Tang, David; Schmeichel, Brandon J

2015-01-01

Prior research has found that persons who favor more analytic modes of thought are less religious. We propose that individual differences in analytic thought are associated with reduced religious beliefs particularly when analytic thought is measured (hence, primed) first. The current study provides a direct replication of prior evidence that individual differences in analytic thinking are negatively related to religious beliefs when analytic thought is measured before religious beliefs. When religious belief is measured before analytic thinking, however, the negative relationship is reduced to non-significance, suggesting that the link between analytic thought and religious belief is more tenuous than previously reported. The current study suggests that whereas inducing analytic processing may reduce religious belief, more analytic thinkers are not necessarily less religious. The potential for measurement order to inflate the inverse correlation between analytic thinking and religious beliefs deserves additional consideration.

Revisiting the Relationship between Individual Differences in Analytic Thinking and Religious Belief: Evidence That Measurement Order Moderates Their Inverse Correlation

PubMed Central

Finley, Anna J.; Tang, David; Schmeichel, Brandon J.

2015-01-01

Prior research has found that persons who favor more analytic modes of thought are less religious. We propose that individual differences in analytic thought are associated with reduced religious beliefs particularly when analytic thought is measured (hence, primed) first. The current study provides a direct replication of prior evidence that individual differences in analytic thinking are negatively related to religious beliefs when analytic thought is measured before religious beliefs. When religious belief is measured before analytic thinking, however, the negative relationship is reduced to non-significance, suggesting that the link between analytic thought and religious belief is more tenuous than previously reported. The current study suggests that whereas inducing analytic processing may reduce religious belief, more analytic thinkers are not necessarily less religious. The potential for measurement order to inflate the inverse correlation between analytic thinking and religious beliefs deserves additional consideration. PMID:26402334

Optimal study design with identical power: an application of power equivalence to latent growth curve models.

PubMed

von Oertzen, Timo; Brandmaier, Andreas M

2013-06-01

Structural equation models have become a broadly applied data-analytic framework. Among them, latent growth curve models have become a standard method in longitudinal research. However, researchers often rely solely on rules of thumb about statistical power in their study designs. The theory of power equivalence provides an analytical answer to the question of how design factors, for example, the number of observed indicators and the number of time points assessed in repeated measures, trade off against each other while holding the power for likelihood-ratio tests on the latent structure constant. In this article, we present applications of power-equivalent transformations on a model with data from a previously published study on cognitive aging, and highlight consequences of participant attrition on power. PsycINFO Database Record (c) 2013 APA, all rights reserved.

Free iterative-complement-interaction calculations of the hydrogen molecule

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

Kurokawa, Yusaku; Nakashima, Hiroyuki; Nakatsuji, Hiroshi

2005-12-15

The free iterative-complement-interaction (ICI) method based on the scaled Schroedinger equation proposed previously has been applied to the calculations of very accurate wave functions of the hydrogen molecule in an analytical expansion form. All the variables were determined with the variational principle by calculating the necessary integrals analytically. The initial wave function and the scaling function were changes to see the effects on the convergence speed of the ICI calculations. The free ICI wave functions that were generated automatically were different from the existing wave functions, and this difference was shown to be physically important. The best wave function reportedmore » in this paper seems to be the best worldwide in the literature from the variational point of view. The quality of the wave function was examined by calculating the nuclear and electron cusps.« less

Multispectral scanner system parameter study and analysis software system description, volume 2

NASA Technical Reports Server (NTRS)

Landgrebe, D. A. (Principal Investigator); Mobasseri, B. G.; Wiersma, D. J.; Wiswell, E. R.; Mcgillem, C. D.; Anuta, P. E.

1978-01-01

The author has identified the following significant results. The integration of the available methods provided the analyst with the unified scanner analysis package (USAP), the flexibility and versatility of which was superior to many previous integrated techniques. The USAP consisted of three main subsystems; (1) a spatial path, (2) a spectral path, and (3) a set of analytic classification accuracy estimators which evaluated the system performance. The spatial path consisted of satellite and/or aircraft data, data correlation analyzer, scanner IFOV, and random noise model. The output of the spatial path was fed into the analytic classification and accuracy predictor. The spectral path consisted of laboratory and/or field spectral data, EXOSYS data retrieval, optimum spectral function calculation, data transformation, and statistics calculation. The output of the spectral path was fended into the stratified posterior performance estimator.

Resolved-particle simulation by the Physalis method: Enhancements and new capabilities

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

Sierakowski, Adam J., E-mail: sierakowski@jhu.edu; Prosperetti, Andrea; Faculty of Science and Technology and J.M. Burgers Centre for Fluid Dynamics, University of Twente, P.O. Box 217, 7500 AE Enschede

2016-03-15

We present enhancements and new capabilities of the Physalis method for simulating disperse multiphase flows using particle-resolved simulation. The current work enhances the previous method by incorporating a new type of pressure-Poisson solver that couples with a new Physalis particle pressure boundary condition scheme and a new particle interior treatment to significantly improve overall numerical efficiency. Further, we implement a more efficient method of calculating the Physalis scalar products and incorporate short-range particle interaction models. We provide validation and benchmarking for the Physalis method against experiments of a sedimenting particle and of normal wall collisions. We conclude with an illustrativemore » simulation of 2048 particles sedimenting in a duct. In the appendix, we present a complete and self-consistent description of the analytical development and numerical methods.« less

An analytical derivation of MC-SCF vibrational wave functions for the quantum dynamical simulation of multiple proton transfer reactions: Initial application to protonated water chains

NASA Astrophysics Data System (ADS)

Drukker, Karen; Hammes-Schiffer, Sharon

1997-07-01

This paper presents an analytical derivation of a multiconfigurational self-consistent-field (MC-SCF) solution of the time-independent Schrödinger equation for nuclear motion (i.e. vibrational modes). This variational MC-SCF method is designed for the mixed quantum/classical molecular dynamics simulation of multiple proton transfer reactions, where the transferring protons are treated quantum mechanically while the remaining degrees of freedom are treated classically. This paper presents a proof that the Hellmann-Feynman forces on the classical degrees of freedom are identical to the exact forces (i.e. the Pulay corrections vanish) when this MC-SCF method is used with an appropriate choice of basis functions. This new MC-SCF method is applied to multiple proton transfer in a protonated chain of three hydrogen-bonded water molecules. The ground state and the first three excited state energies and the ground state forces agree well with full configuration interaction calculations. Sample trajectories are obtained using adiabatic molecular dynamics methods, and nonadiabatic effects are found to be insignificant for these sample trajectories. The accuracy of the excited states will enable this MC-SCF method to be used in conjunction with nonadiabatic molecular dynamics methods. This application differs from previous work in that it is a real-time quantum dynamical nonequilibrium simulation of multiple proton transfer in a chain of water molecules.

Consistent Yokoya-Chen Approximation to Beamstrahlung(LCC-0010)

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

Peskin, M

2004-04-22

I reconsider the Yokoya-Chen approximate evolution equation for beamstrahlung and modify it slightly to generate simple, consistent analytical approximations for the electron and photon energy spectra. I compare these approximations to previous ones, and to simulation data.I reconsider the Yokoya-Chen approximate evolution equation for beamstrahlung and modify it slightly to generate simple, consistent analytical approximations for the electron and photon energy spectra. I compare these approximations to previous ones, and to simulation data.

Stiffness and Damping Coefficient Estimation of Compliant Surface Gas Bearings for Oil-Free Turbomachinery

NASA Technical Reports Server (NTRS)

Della-Corte, Christopher

2012-01-01

Foil gas bearings are a key technology in many commercial and emerging oilfree turbomachinery systems. These bearings are nonlinear and have been difficult to analytically model in terms of performance characteristics such as load capacity, power loss, stiffness, and damping. Previous investigations led to an empirically derived method to estimate load capacity. This method has been a valuable tool in system development. The current work extends this tool concept to include rules for stiffness and damping coefficient estimation. It is expected that these rules will further accelerate the development and deployment of advanced oil-free machines operating on foil gas bearings.

Digital Mapping Techniques '09-Workshop Proceedings, Morgantown, West Virginia, May 10-13, 2009

USGS Publications Warehouse

Soller, David R.

2011-01-01

As in the previous years' meetings, the objective was to foster informal discussion and exchange of technical information, principally in order to develop more efficient methods for digital mapping, cartography, GIS analysis, and information management. At this meeting, oral and poster presentations and special discussion sessions emphasized (1) methods for creating and publishing map products (here, "publishing" includes Web-based release); (2) field data capture software and techniques, including the use of LiDAR; (3) digital cartographic techniques; (4) migration of digital maps into ArcGIS Geodatabase format; (5) analytical GIS techniques; and (6) continued development of the National Geologic Map Database.

High-Fidelity Micromechanics Model Developed for the Response of Multiphase Materials

NASA Technical Reports Server (NTRS)

Aboudi, Jacob; Pindera, Marek-Jerzy; Arnold, Steven M.

2002-01-01

A new high-fidelity micromechanics model has been developed under funding from the NASA Glenn Research Center for predicting the response of multiphase materials with arbitrary periodic microstructures. The model's analytical framework is based on the homogenization technique, but the method of solution for the local displacement and stress fields borrows concepts previously employed in constructing the higher order theory for functionally graded materials. The resulting closed-form macroscopic and microscopic constitutive equations, valid for both uniaxial and multiaxial loading of periodic materials with elastic and inelastic constitutive phases, can be incorporated into a structural analysis computer code. Consequently, this model now provides an alternative, accurate method.

Analytical analysis and implementation of a low-speed high-torque permanent magnet vernier in-wheel motor for electric vehicle

NASA Astrophysics Data System (ADS)

Li, Jiangui; Wang, Junhua; Zhigang, Zhao; Yan, Weili

2012-04-01

In this paper, analytical analysis of the permanent magnet vernier (PMV) is presented. The key is to analytically solve the governing Laplacian/quasi-Poissonian field equations in the motor regions. By using the time-stepping finite element method, the analytical method is verified. Hence, the performances of the PMV machine are quantitatively compared with that of the analytical results. The analytical results agree well with the finite element method results. Finally, the experimental results are given to further show the validity of the analysis.

Community-Based Mental Health and Behavioral Programs for Low-Income Urban Youth: A Meta-Analytic Review

ERIC Educational Resources Information Center

Farahmand, Farahnaz K.; Duffy, Sophia N.; Tailor, Megha A.; Dubois, David L.; Lyon, Aaron L.; Grant, Kathryn E.; Zarlinski, Jennifer C.; Masini, Olivia; Zander, Keith J.; Nathanson, Alison M.

2012-01-01

A meta-analytic review of 33 studies and 41 independent samples was conducted of the effectiveness of community-based mental health and behavioral programs for low-income urban youth. Findings indicated positive effects, with an overall mean effect of 0.25 at post-test. While this is comparable to previous meta-analytic intervention research with…

One-year test-retest reliability of intrinsic connectivity network fMRI in older adults

PubMed Central

Guo, Cong C.; Kurth, Florian; Zhou, Juan; Mayer, Emeran A.; Eickhoff, Simon B; Kramer, Joel H.; Seeley, William W.

2014-01-01

“Resting-state” or task-free fMRI can assess intrinsic connectivity network (ICN) integrity in health and disease, suggesting a potential for use of these methods as disease-monitoring biomarkers. Numerous analytical options are available, including model-driven ROI-based correlation analysis and model-free, independent component analysis (ICA). High test-retest reliability will be a necessary feature of a successful ICN biomarker, yet available reliability data remains limited. Here, we examined ICN fMRI test-retest reliability in 24 healthy older subjects scanned roughly one year apart. We focused on the salience network, a disease-relevant ICN not previously subjected to reliability analysis. Most ICN analytical methods proved reliable (intraclass coefficients > 0.4) and could be further improved by wavelet analysis. Seed-based ROI correlation analysis showed high map-wise reliability, whereas graph theoretical measures and temporal concatenation group ICA produced the most reliable individual unit-wise outcomes. Including global signal regression in ROI-based correlation analyses reduced reliability. Our study provides a direct comparison between the most commonly used ICN fMRI methods and potential guidelines for measuring intrinsic connectivity in aging control and patient populations over time. PMID:22446491

The cloud radiation impact from optics simulation and airborne observation

NASA Astrophysics Data System (ADS)

Melnikova, Irina; Kuznetsov, Anatoly; Gatebe, Charles

2017-02-01

The analytical approach of inverse asymptotic formulas of the radiative transfer theory is used for solving inverse problems of cloud optics. The method has advantages because it does not impose strict constraints, but it is tied to the desired solution. Observations are accomplished in extended stratus cloudiness, above a homogeneous ocean surface. Data from NASA`s Cloud Absorption Radiometer (CAR) during two airborne experiments (SAFARI-2000 and ARCTAS-2008) were analyzed. The analytical method of inverse asymptotic formulas was used to retrieve cloud optical parameters (optical thickness, single scattering albedo and asymmetry parameter of the phase function) and ground albedo in all 8 spectral channels independently. The method is free from a priori restrictions and there is no links to parameters, and it has been applied to data set of different origin and geometry of observations. Results obtained from different airborne, satellite and ground radiative experiments appeared consistence and showed common features of values of cloud parameters and its spectral dependence (Vasiluev, Melnikova, 2004; Gatebe et al., 2014). Optical parameters, retrieved here, are used for calculation of radiative divergence, reflected and transmitted irradiance and heating rates in cloudy atmosphere, that agree with previous observational data.

A simple and green analytical method for determination of glyphosate in commercial formulations and water by diffuse reflectance spectroscopy

NASA Astrophysics Data System (ADS)

da Silva, Aline Santana; Fernandes, Flávio Cesar Bedatty; Tognolli, João Olímpio; Pezza, Leonardo; Pezza, Helena Redigolo

2011-09-01

This article describes a simple, inexpensive, and environmentally friendly method for the monitoring of glyphosate using diffuse reflectance spectroscopy. The proposed method is based on reflectance measurements of the colored compound produced from the spot test reaction between glyphosate and p-dimethylaminocinnamaldehyde ( p-DAC) in acid medium, using a filter paper as solid support. Experimental designs were used to optimize the analytical conditions. All reflectance measurements were carried out at 495 nm. Under optimal conditions, the glyphosate calibration graphs obtained by plotting the optical density of the reflectance signal (A R) against the concentration were linear in the range 50-500 μg mL -1, with a correlation coefficient of 0.9987. The limit of detection (LOD) for glyphosate was 7.28 μg mL -1. The technique was successfully applied to the direct determination of glyphosate in commercial formulations, as well as in water samples (river water, pure water and mineral drinking water) after a previous clean-up or pre-concentration step. Recoveries were in the ranges 93.2-102.6% and 91.3-102.9% for the commercial formulations and water samples, respectively.

A simple and green analytical method for determination of glyphosate in commercial formulations and water by diffuse reflectance spectroscopy.

PubMed

da Silva, Aline Santana; Fernandes, Flávio Cesar Bedatty; Tognolli, João Olímpio; Pezza, Leonardo; Pezza, Helena Redigolo

2011-09-01

This article describes a simple, inexpensive, and environmentally friendly method for the monitoring of glyphosate using diffuse reflectance spectroscopy. The proposed method is based on reflectance measurements of the colored compound produced from the spot test reaction between glyphosate and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, using a filter paper as solid support. Experimental designs were used to optimize the analytical conditions. All reflectance measurements were carried out at 495 nm. Under optimal conditions, the glyphosate calibration graphs obtained by plotting the optical density of the reflectance signal (AR) against the concentration were linear in the range 50-500 μg mL(-1), with a correlation coefficient of 0.9987. The limit of detection (LOD) for glyphosate was 7.28 μg mL(-1). The technique was successfully applied to the direct determination of glyphosate in commercial formulations, as well as in water samples (river water, pure water and mineral drinking water) after a previous clean-up or pre-concentration step. Recoveries were in the ranges 93.2-102.6% and 91.3-102.9% for the commercial formulations and water samples, respectively. Copyright © 2011 Elsevier B.V. All rights reserved.

Validation of pharmaceutical potency determinations by quantitative nuclear magnetic resonance spectrometry.

PubMed

Webster, Gregory K; Marsden, Ian; Pommerening, Cynthia A; Tyrakowski, Christina M

2010-05-01

With the changing development paradigms in the pharmaceutical industry, laboratories are challenged to release materials for clinical studies with rapid turnaround times. To minimize cost demands, many businesses are looking to develop ways of using early Good Manufacturing Practice (GMP) materials of active pharmaceutical ingredients (API) for Good Laboratory Practice (GLP) toxicology studies. To make this happen, the analytical laboratory releases the material by one of three scenarios: (1) holding the GLP release until full GMP testing is ready, (2) issuing a separate lot number for a portion of the GMP material and releasing the material for GLP use, or (3) releasing the lot of material for GLP using alternate (equivalent) method(s) not specified for GMP release testing. Many companies are finding the third scenario to be advantageous in terms of cost and efficiency through the use of quantitative nuclear magnetic resonance (q-NMR). The use of q-NMR has proved to be a single-point replacement for routine early development testing that previously combined elements of identity testing, chromatographic assay, moisture analysis, residual solvent analysis, and elemental analysis. This study highlights that q-NMR can be validated to meet current regulatory analytical method guidelines for routine pharmaceutical analysis.

Energy analysis in the elliptic restricted three-body problem

NASA Astrophysics Data System (ADS)

Qi, Yi; de Ruiter, Anton

2018-07-01

The gravity assist or flyby is investigated by analysing the inertial energy of a test particle in the elliptic restricted three-body problem (ERTBP), where two primary bodies are moving in elliptic orbits. First, the expression of the derivation of energy is obtained and discussed. Then, the approximate expressions of energy change in a circular neighbourhood of the smaller primary are derived. Numerical computation indicates that the obtained expressions can be applied to study the flyby problem of the nine planets and the Moon in the Solar system. Parameters related to the flyby are discussed analytically and numerically. The optimal conditions, including the position and time of the periapsis, for a flyby orbit are found to make a maximum energy gain or loss. Finally, the mechanical process of a flyby orbit is uncovered by an approximate expression in the ERTBP. Numerical computations testify that our analytical results well approximate the mechanical process of flyby orbits obtained by the numerical simulation in the ERTBP. Compared with the previous research established in the patched-conic method and numerical calculation, our analytical investigations based on a more elaborate derivation get more original results.

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

Chhiber, R; Usmanov, AV; Matthaeus, WH

Simple estimates of the number of Coulomb collisions experienced by the interplanetary plasma to the point of observation, i.e., the “collisional age”, can be usefully employed in the study of non-thermal features of the solar wind. Usually these estimates are based on local plasma properties at the point of observation. Here we improve the method of estimation of the collisional age by employing solutions obtained from global three-dimensional magnetohydrodynamics simulations. This enables evaluation of the complete analytical expression for the collisional age without using approximations. The improved estimation of the collisional timescale is compared with turbulence and expansion timescales tomore » assess the relative importance of collisions. The collisional age computed using the approximate formula employed in previous work is compared with the improved simulation-based calculations to examine the validity of the simplified formula. We also develop an analytical expression for the evaluation of the collisional age and we find good agreement between the numerical and analytical results. Finally, we briefly discuss the implications for an improved estimation of collisionality along spacecraft trajectories, including Solar Probe Plus.« less

Energy Analysis in the Elliptic Restricted Three-body Problem

NASA Astrophysics Data System (ADS)

Qi, Yi; de Ruiter, Anton

2018-05-01

The gravity assist or flyby is investigated by analyzing the inertial energy of a test particle in the elliptic restricted three-body problem (ERTBP), where two primary bodies are moving in elliptic orbits. Firstly, the expression of the derivation of energy is obtained and discussed. Then, the approximate expressions of energy change in a circular neighborhood of the smaller primary are derived. Numerical computation indicates that the obtained expressions can be applied to study the flyby problem of the nine planets and the Moon in the solar system. Parameters related to the flyby are discussed analytically and numerically. The optimal conditions, including the position and time of the periapsis, for a flyby orbit are found to make a maximum energy gain or loss. Finally, the mechanical process of a flyby orbit is uncovered by an approximate expression in the ERTBP. Numerical computations testify that our analytical results well approximate the mechanical process of flyby orbits obtained by the numerical simulation in the ERTBP. Compared with the previous research established in the patched-conic method and numerical calculation, our analytical investigations based on a more elaborate derivation get more original results.

Elucidation of several neglected reactions in the GC-MS identification of sialic acids as heptafluorobutyrates calls for an urgent reassessment of previous claims.

PubMed

Rota, Paola; Anastasia, Luigi; Allevi, Pietro

2015-05-07

The current analytical protocol used for the GC-MS determination of free or 1,7-lactonized natural sialic acids (Sias), as heptafluorobutyrates, overlooks several transformations. Using authentic reference standards and by combining GC-MS and NMR analyses, flaws in the analytical protocol were pinpointed and elucidated, thus establishing the scope and limitations of the method. It was demonstrated that (a) Sias 1,7-lactones, even if present in biological samples, decompose under the acidic hydrolysis conditions used for their release; (b) Sias 1,7-lactones are unpredicted artifacts, accidentally generated from their parent acids; (c) the N-acetyl group is quantitatively exchanged with that of the derivatizing perfluorinated anhydride; (d) the partial or complete failure of the Sias esterification-step with diazomethane leads to the incorrect quantification and structure attribution of all free Sias. While these findings prompt an urgent correction and improvement of the current analytical protocol, they could be instrumental for a critical revision of many incorrect claims reported in the literature.

Accurate expressions for solar cell fill factors including series and shunt resistances

NASA Astrophysics Data System (ADS)

Green, Martin A.

2016-02-01

Together with open-circuit voltage and short-circuit current, fill factor is a key solar cell parameter. In their classic paper on limiting efficiency, Shockley and Queisser first investigated this factor's analytical properties showing, for ideal cells, it could be expressed implicitly in terms of the maximum power point voltage. Subsequently, fill factors usually have been calculated iteratively from such implicit expressions or from analytical approximations. In the absence of detrimental series and shunt resistances, analytical fill factor expressions have recently been published in terms of the Lambert W function available in most mathematical computing software. Using a recently identified perturbative relationship, exact expressions in terms of this function are derived in technically interesting cases when both series and shunt resistances are present but have limited impact, allowing a better understanding of their effect individually and in combination. Approximate expressions for arbitrary shunt and series resistances are then deduced, which are significantly more accurate than any previously published. A method based on the insights developed is also reported for deducing one-diode fits to experimental data.

Three-Dimensional Flow Generated by a Partially Penetrating Well in a Two-Aquifer System

NASA Astrophysics Data System (ADS)

Sepulveda, N.

2007-12-01

An analytical solution is presented for three-dimensional (3D) flow in a confined aquifer and the overlying storative semiconfining layer and unconfined aquifer. The equation describing flow caused by a partially penetrating production well is solved analytically to provide a method to accurately determine the hydraulic parameters in the confined aquifer, semiconfining layer, and unconfined aquifer from aquifer-test data. Previous solutions for a partially penetrating well did not account for 3D flow or storativity in the semiconfining unit. The 3D and two- dimensional (2D) flow solutions in the semiconfining layer are compared for various hydraulic conductivity ratios between the aquifer and the semiconfining layer. Analysis of the drawdown data from an aquifer test in central Florida showed that the 3D solution in the semiconfining layer provides a more unique identification of the hydraulic parameters than the 2D solution. The analytical solution could be used to analyze, with higher accuracy, the effect that pumping water from the lower aquifer in a two-aquifer system has on wetlands.

A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS.

PubMed

Lou, Xianwen; de Waal, Bas F M; Milroy, Lech-Gustav; van Dongen, Joost L J

2015-05-01

In matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS), analyte signals can be substantially suppressed by other compounds in the sample. In this technical note, we describe a modified thin-layer sample preparation method that significantly reduces the analyte suppression effect (ASE). In our method, analytes are deposited on top of the surface of matrix preloaded on the MALDI plate. To prevent embedding of analyte into the matrix crystals, the sample solution were prepared without matrix and efforts were taken not to re-dissolve the preloaded matrix. The results with model mixtures of peptides, synthetic polymers and lipids show that detection of analyte ions, which were completely suppressed using the conventional dried-droplet method, could be effectively recovered by using our method. Our findings suggest that the incorporation of analytes in the matrix crystals has an important contributory effect on ASE. By reducing ASE, our method should be useful for the direct MALDI MS analysis of multicomponent mixtures. Copyright © 2015 John Wiley & Sons, Ltd.

Comprehensive Numerical Analysis of Finite Difference Time Domain Methods for Improving Optical Waveguide Sensor Accuracy

PubMed Central

Samak, M. Mosleh E. Abu; Bakar, A. Ashrif A.; Kashif, Muhammad; Zan, Mohd Saiful Dzulkifly

2016-01-01

This paper discusses numerical analysis methods for different geometrical features that have limited interval values for typically used sensor wavelengths. Compared with existing Finite Difference Time Domain (FDTD) methods, the alternating direction implicit (ADI)-FDTD method reduces the number of sub-steps by a factor of two to three, which represents a 33% time savings in each single run. The local one-dimensional (LOD)-FDTD method has similar numerical equation properties, which should be calculated as in the previous method. Generally, a small number of arithmetic processes, which result in a shorter simulation time, are desired. The alternating direction implicit technique can be considered a significant step forward for improving the efficiency of unconditionally stable FDTD schemes. This comparative study shows that the local one-dimensional method had minimum relative error ranges of less than 40% for analytical frequencies above 42.85 GHz, and the same accuracy was generated by both methods.

A new approximation for pore pressure accumulation in marine sediment due to water waves

NASA Astrophysics Data System (ADS)

Jeng, D.-S.; Seymour, B. R.; Li, J.

2007-01-01

The residual mechanism of wave-induced pore water pressure accumulation in marine sediments is re-examined. An analytical approximation is derived using a linear relation for pore pressure generation in cyclic loading, and mistakes in previous solutions (Int. J. Numer. Anal. Methods Geomech. 2001; 25:885-907; J. Offshore Mech. Arctic Eng. (ASME) 1989; 111(1):1-11) are corrected. A numerical scheme is then employed to solve the case with a non-linear relation for pore pressure generation. Both analytical and numerical solutions are verified with experimental data (Laboratory and field investigation of wave-sediment interaction. Joseph H. Defrees Hydraulics Laboratory, School of Civil and Environmental Engineering, Cornell University, Ithaca, NY, 1983), and provide a better prediction of pore pressure accumulation than the previous solution (J. Offshore Mech. Arctic Eng. (ASME) 1989; 111(1):1-11). The parametric study concludes that the pore pressure accumulation and use of full non-linear relation of pore pressure become more important under the following conditions: (1) large wave amplitude, (2) longer wave period, (3) shallow water, (4) shallow soil and (5) softer soils with a low consolidation coefficient. Copyright

Broadband infrared imaging spectroscopy for standoff detection of trace explosives

NASA Astrophysics Data System (ADS)

Kendziora, Christopher A.; Furstenberg, Robert; Papantonakis, Michael; Nguyen, Viet; McGill, R. Andrew

2016-05-01

This manuscript describes advancements toward a mobile platform for standoff detection of trace explosives on relevant substrates using broadband infrared spectroscopic imaging. In conjunction with this, we are developing a technology for detection based on photo-thermal infrared (IR) imaging spectroscopy (PT-IRIS). PT-IRIS leverages one or more IR quantum cascade lasers (QCL), tuned to strong absorption bands in the analytes and directed to illuminate an area on a surface of interest. An IR focal plane array is used to image the surface thermal emission upon laser illumination. The PT-IRIS signal is processed as a hyperspectral image cube comprised of spatial, spectral and temporal dimensions as vectors within a detection algorithm. Here we describe methods to increase both sensitivity to trace explosives and selectivity between different analyte types by exploiting a broader spectral range than in previous configurations. Previously we demonstrated PT-IRIS at several meters of standoff distance indoors and in field tests, while operating the lasers below the infrared eye-safe intensity limit (100 mW/cm2). Sensitivity to explosive traces as small as a single 10 μm diameter particle (~1 ng) has been demonstrated.

Optimization of detection conditions and single-laboratory validation of a multiresidue method for the determination of 135 pesticides and 25 organic pollutants in grapes and wine by gas chromatography time-of-flight mass spectrometry.

PubMed

Dasgupta, Soma; Banerjee, Kaushik; Dhumal, Kondiba N; Adsule, Pandurang G

2011-01-01

This paper describes single-laboratory validation of a multiresidue method for the determination of 135 pesticides, 12 dioxin-like polychlorinated biphenyls, 12 polyaromatic hydrocarbons, and bisphenol A in grapes and wine by GC/time-of-flight MS in a total run time of 48 min. The method is based on extraction with ethyl acetate in a sample-to-solvent ratio of 1:1, followed by selective dispersive SPE cleanup for grapes and wine. The GC/MS conditions were optimized for the chromatographic separation and to achieve highest S/N for all 160 target analytes, including the temperature-sensitive compounds, like captan and captafol, that are prone to degradation during analysis. An average recovery of 80-120% with RSD < 10% could be attained for all analytes except 17, for which the average recoveries were 70-80%. LOQ ranged within 10-50 ng/g, with < 25% expanded uncertainties, for 155 compounds in grapes and 151 in wine. In the incurred grape and wine samples, the residues of buprofezin, chlorpyriphos, metalaxyl, and myclobutanil were detected, with an RSD of < 5% (n = 6); the results were statistically similar to previously reported validated methods.

Proposal of Classification Method of Time Series Data in International Emissions Trading Market Using Agent-based Simulation

NASA Astrophysics Data System (ADS)

Nakada, Tomohiro; Takadama, Keiki; Watanabe, Shigeyoshi

This paper proposes the classification method using Bayesian analytical method to classify the time series data in the international emissions trading market depend on the agent-based simulation and compares the case with Discrete Fourier transform analytical method. The purpose demonstrates the analytical methods mapping time series data such as market price. These analytical methods have revealed the following results: (1) the classification methods indicate the distance of mapping from the time series data, it is easier the understanding and inference than time series data; (2) these methods can analyze the uncertain time series data using the distance via agent-based simulation including stationary process and non-stationary process; and (3) Bayesian analytical method can show the 1% difference description of the emission reduction targets of agent.

Analytical calculation of vibrations of electromagnetic origin in electrical machines

NASA Astrophysics Data System (ADS)

McCloskey, Alex; Arrasate, Xabier; Hernández, Xabier; Gómez, Iratxo; Almandoz, Gaizka

2018-01-01

Electrical motors are widely used and are often required to satisfy comfort specifications. Thus, vibration response estimations are necessary to reach optimum machine designs. This work presents an improved analytical model to calculate vibration response of an electrical machine. The stator and windings are modelled as a double circular cylindrical shell. As the stator is a laminated structure, orthotropic properties are applied to it. The values of those material properties are calculated according to the characteristics of the motor and the known material properties taken from previous works. Therefore, the model proposed takes into account the axial direction, so that length is considered, and also the contribution of windings, which differs from one machine to another. These aspects make the model valuable for a wide range of electrical motor types. In order to validate the analytical calculation, natural frequencies are calculated and compared to those obtained by Finite Element Method (FEM), giving relative errors below 10% for several circumferential and axial mode order combinations. It is also validated the analytical vibration calculation with acceleration measurements in a real machine. The comparison shows good agreement for the proposed model, being the most important frequency components in the same magnitude order. A simplified two dimensional model is also applied and the results obtained are not so satisfactory.

Application of kernel principal component analysis and computational machine learning to exploration of metabolites strongly associated with diet.

PubMed

Shiokawa, Yuka; Date, Yasuhiro; Kikuchi, Jun

2018-02-21

Computer-based technological innovation provides advancements in sophisticated and diverse analytical instruments, enabling massive amounts of data collection with relative ease. This is accompanied by a fast-growing demand for technological progress in data mining methods for analysis of big data derived from chemical and biological systems. From this perspective, use of a general "linear" multivariate analysis alone limits interpretations due to "non-linear" variations in metabolic data from living organisms. Here we describe a kernel principal component analysis (KPCA)-incorporated analytical approach for extracting useful information from metabolic profiling data. To overcome the limitation of important variable (metabolite) determinations, we incorporated a random forest conditional variable importance measure into our KPCA-based analytical approach to demonstrate the relative importance of metabolites. Using a market basket analysis, hippurate, the most important variable detected in the importance measure, was associated with high levels of some vitamins and minerals present in foods eaten the previous day, suggesting a relationship between increased hippurate and intake of a wide variety of vegetables and fruits. Therefore, the KPCA-incorporated analytical approach described herein enabled us to capture input-output responses, and should be useful not only for metabolic profiling but also for profiling in other areas of biological and environmental systems.

40 CFR 141.704 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Analytical methods. 141.704 Section... Monitoring Requirements § 141.704 Analytical methods. (a) Cryptosporidium. Systems must analyze for Cryptosporidium using Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA, 2005, United States...

40 CFR 141.704 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 23 2014-07-01 2014-07-01 false Analytical methods. 141.704 Section... Monitoring Requirements § 141.704 Analytical methods. (a) Cryptosporidium. Systems must analyze for Cryptosporidium using Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA, 2005, United States...

40 CFR 141.704 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 24 2013-07-01 2013-07-01 false Analytical methods. 141.704 Section... Monitoring Requirements § 141.704 Analytical methods. (a) Cryptosporidium. Systems must analyze for Cryptosporidium using Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA, 2005, United States...

77 FR 41336 - Analytical Methods Used in Periodic Reporting

Federal Register 2010, 2011, 2012, 2013, 2014

2012-07-13

... Methods Used in Periodic Reporting AGENCY: Postal Regulatory Commission. ACTION: Notice of filing. SUMMARY... proceeding to consider changes in analytical methods used in periodic reporting. This notice addresses... informal rulemaking proceeding to consider changes in the analytical methods approved for use in periodic...

40 CFR 141.704 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 23 2011-07-01 2011-07-01 false Analytical methods. 141.704 Section... Monitoring Requirements § 141.704 Analytical methods. (a) Cryptosporidium. Systems must analyze for Cryptosporidium using Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA, 2005, United States...

40 CFR 141.704 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 24 2012-07-01 2012-07-01 false Analytical methods. 141.704 Section... Monitoring Requirements § 141.704 Analytical methods. (a) Cryptosporidium. Systems must analyze for Cryptosporidium using Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA, 2005, United States...

Recently published analytical methods for determining alcohol in body materials : alcohol countermeasures literature review

DOT National Transportation Integrated Search

1974-10-01

The author has brought the review of published analytical methods for determining alcohol in body materials up-to- date. The review deals with analytical methods for alcohol in blood and other body fluids and tissues; breath alcohol methods; factors ...

Development and validation of an improved method for the determination of chloropropanols in paperboard food packaging by GC-MS.

PubMed

Mezouari, S; Liu, W Yun; Pace, G; Hartman, T G

2015-01-01

The objective of this study was to develop an improved analytical method for the determination of 3-chloro-1,2-propanediol (3-MCPD) and 1,3-dichloropropanol (1,3-DCP) in paper-type food packaging. The established method includes aqueous extraction, matrix spiking of a deuterated surrogate internal standard (3-MCPD-d₅), clean-up using Extrelut solid-phase extraction, derivatisation using a silylation reagent, and GC-MS analysis of the chloropropanols as their corresponding trimethyl silyl ethers. The new method is applicable to food-grade packaging samples using European Commission standard aqueous extraction and aqueous food stimulant migration tests. In this improved method, the derivatisation procedure was optimised; the cost and time of the analysis were reduced by using 10 times less sample, solvents and reagents than in previously described methods. Overall the validation data demonstrate that the method is precise and reliable. The limit of detection (LOD) of the aqueous extract was 0.010 mg kg(-1) (w/w) for both 3-MCPD and 1,3-DCP. Analytical precision had a relative standard deviation (RSD) of 3.36% for 3-MCPD and an RSD of 7.65% for 1,3-DCP. The new method was satisfactorily applied to the analysis of over 100 commercial paperboard packaging samples. The data are being used to guide the product development of a next generation of wet-strength resins with reduced chloropropanol content, and also for risk assessments to calculate the virtual safe dose (VSD).

Medio-lateral Knee Fluency in Anterior Cruciate Ligament-Injured Athletes During Dynamic Movement Trials

PubMed Central

Panos, Joseph A.; Hoffman, Joshua T.; Wordeman, Samuel C.; Hewett, Timothy E.

2016-01-01

Background Correction of neuromuscular impairments after anterior cruciate ligament injury is vital to successful return to sport. Frontal plane knee control during landing is a common measure of lower-extremity neuromuscular control and asymmetries in neuromuscular control of the knee can predispose injured athletes to additional injury and associated morbidities. Therefore, this study investigated the effects of anterior cruciate ligament injury on knee biomechanics during landing. Methods Two-dimensional frontal plane video of single leg drop, cross over drop, and drop vertical jump dynamic movement trials was analyzed for twenty injured and reconstructed athletes. The position of the knee joint center was tracked in ImageJ software for 500 milliseconds after landing to calculate medio-lateral knee motion velocities and determine normal fluency, the number of times per second knee velocity changed direction. The inverse of this calculation, analytical fluency, was used to associate larger numerical values with fluent movement. Findings Analytical fluency was decreased in involved limbs for single leg drop trials (P=0.0018). Importantly, analytical fluency for single leg drop differed compared to cross over drop trials for involved (P<0.001), but not uninvolved limbs (P=0.5029). For involved limbs, analytical fluency values exhibited a stepwise trend in relative magnitudes. Interpretation Decreased analytical fluency in involved limbs is consistent with previous studies. Fluency asymmetries observed during single leg drop tasks may be indicative of abhorrent landing strategies in the involved limb. Analytical fluency differences in unilateral tasks for injured limbs may represent neuromuscular impairment as a result of injury. PMID:26895446

Application of quality improvement analytic methodology in emergency medicine research: A comparative evaluation.

PubMed

Harries, Bruce; Filiatrault, Lyne; Abu-Laban, Riyad B

2018-05-30

Quality improvement (QI) analytic methodology is rarely encountered in the emergency medicine literature. We sought to comparatively apply QI design and analysis techniques to an existing data set, and discuss these techniques as an alternative to standard research methodology for evaluating a change in a process of care. We used data from a previously published randomized controlled trial on triage-nurse initiated radiography using the Ottawa ankle rules (OAR). QI analytic tools were applied to the data set from this study and evaluated comparatively against the original standard research methodology. The original study concluded that triage nurse-initiated radiographs led to a statistically significant decrease in mean emergency department length of stay. Using QI analytic methodology, we applied control charts and interpreted the results using established methods that preserved the time sequence of the data. This analysis found a compelling signal of a positive treatment effect that would have been identified after the enrolment of 58% of the original study sample, and in the 6th month of this 11-month study. Our comparative analysis demonstrates some of the potential benefits of QI analytic methodology. We found that had this approach been used in the original study, insights regarding the benefits of nurse-initiated radiography using the OAR would have been achieved earlier, and thus potentially at a lower cost. In situations where the overarching aim is to accelerate implementation of practice improvement to benefit future patients, we believe that increased consideration should be given to the use of QI analytic methodology.

How Much Can We Learn from a Single Chromatographic Experiment? A Bayesian Perspective.

PubMed

Wiczling, Paweł; Kaliszan, Roman

2016-01-05

In this work, we proposed and investigated a Bayesian inference procedure to find the desired chromatographic conditions based on known analyte properties (lipophilicity, pKa, and polar surface area) using one preliminary experiment. A previously developed nonlinear mixed effect model was used to specify the prior information about a new analyte with known physicochemical properties. Further, the prior (no preliminary data) and posterior predictive distribution (prior + one experiment) were determined sequentially to search towards the desired separation. The following isocratic high-performance reversed-phase liquid chromatographic conditions were sought: (1) retention time of a single analyte within the range of 4-6 min and (2) baseline separation of two analytes with retention times within the range of 4-10 min. The empirical posterior Bayesian distribution of parameters was estimated using the "slice sampling" Markov Chain Monte Carlo (MCMC) algorithm implemented in Matlab. The simulations with artificial analytes and experimental data of ketoprofen and papaverine were used to test the proposed methodology. The simulation experiment showed that for a single and two randomly selected analytes, there is 97% and 74% probability of obtaining a successful chromatogram using none or one preliminary experiment. The desired separation for ketoprofen and papaverine was established based on a single experiment. It was confirmed that the search for a desired separation rarely requires a large number of chromatographic analyses at least for a simple optimization problem. The proposed Bayesian-based optimization scheme is a powerful method of finding a desired chromatographic separation based on a small number of preliminary experiments.

ANALYTICAL CHEMISTRY IN NUCLEAR REACTOR TECHNOLOGY. Analysis of Reactor Fuels, Fission-Product Mixtures and Related Materials: Analytical Chemistry of Plutonium and the Transplutonic Elements. Third Conference, Gatlinburg, Tennessee, October 26-29, 1959

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

None

1960-01-01

Thirty-one papers and 10 summaries of papers presented at the Third Conference on Analytical Chemistry in Nuclear Reactor Technology held at Gatlinburg, Tennessee, October 26 to 29, 1959, are given. The papers are grouped into four sections: general, analytical chemistry of fuels, analytical chemistry of plutonium and the transplutonic elements, and the analysis of fission-product mixtures. Twenty-seven of the papers are covered by separate abstracts. Four were previously abstracted for NSA. (M.C.G.)

New method of extrapolation of the resistance of a model planing boat to full size

NASA Technical Reports Server (NTRS)

Sottorf, W

1942-01-01

The previously employed method of extrapolating the total resistance to full size with lambda(exp 3) (model scale) and thereby foregoing a separate appraisal of the frictional resistance, was permissible for large models and floats of normal size. But faced with the ever increasing size of aircraft a reexamination of the problem of extrapolation to full size is called for. A method is described by means of which, on the basis of an analysis of tests on planing surfaces, the variation of the wetted surface over the take-off range is analytically obtained. The friction coefficients are read from Prandtl's curve for turbulent boundary layer with laminar approach. With these two values a correction for friction is obtainable.

Optical information encryption based on incoherent superposition with the help of the QR code

NASA Astrophysics Data System (ADS)

Qin, Yi; Gong, Qiong

2014-01-01

In this paper, a novel optical information encryption approach is proposed with the help of QR code. This method is based on the concept of incoherent superposition which we introduce for the first time. The information to be encrypted is first transformed into the corresponding QR code, and thereafter the QR code is further encrypted into two phase only masks analytically by use of the intensity superposition of two diffraction wave fields. The proposed method has several advantages over the previous interference-based method, such as a higher security level, a better robustness against noise attack, a more relaxed work condition, and so on. Numerical simulation results and actual smartphone collected results are shown to validate our proposal.

7 CFR 93.13 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture... PROCESSED FRUITS AND VEGETABLES Peanuts, Tree Nuts, Corn and Other Oilseeds § 93.13 Analytical methods... manuals: (a) Approved Methods of the American Association of Cereal Chemists (AACC), American Association...

40 CFR 141.25 - Analytical methods for radioactivity.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 24 2012-07-01 2012-07-01 false Analytical methods for radioactivity... § 141.25 Analytical methods for radioactivity. (a) Analysis for the following contaminants shall be conducted to determine compliance with § 141.66 (radioactivity) in accordance with the methods in the...

7 CFR 93.13 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture... PROCESSED FRUITS AND VEGETABLES Peanuts, Tree Nuts, Corn and Other Oilseeds § 93.13 Analytical methods... manuals: (a) Approved Methods of the American Association of Cereal Chemists (AACC), American Association...

7 CFR 93.13 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture... PROCESSED FRUITS AND VEGETABLES Peanuts, Tree Nuts, Corn and Other Oilseeds § 93.13 Analytical methods... manuals: (a) Approved Methods of the American Association of Cereal Chemists (AACC), American Association...

7 CFR 93.13 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture... PROCESSED FRUITS AND VEGETABLES Peanuts, Tree Nuts, Corn and Other Oilseeds § 93.13 Analytical methods... manuals: (a) Approved Methods of the American Association of Cereal Chemists (AACC), American Association...

7 CFR 93.13 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture... PROCESSED FRUITS AND VEGETABLES Peanuts, Tree Nuts, Corn and Other Oilseeds § 93.13 Analytical methods... manuals: (a) Approved Methods of the American Association of Cereal Chemists (AACC), American Association...

Aspartame and Risk of Cancer: A Meta-analytic Review.

PubMed

Mallikarjun, Sreekanth; Sieburth, Rebecca McNeill

2015-01-01

Aspartame (APM) is the most commonly used artificial sweetener and flavor enhancer in the world. There is a rise in concern that APM is carcinogenic due to a variation in the findings of the previous APM carcinogenic bioassays. This article conducts a meta-analytic review of all previous APM carcinogenic bioassays on rodents that were conducted before 31 December 2012. The search yielded 10 original APM carcinogenic bioassays on rodents. The aggregate effect sizes suggest that APM consumption has no significant carcinogenic effect in rodents.

Generation of gas-phase ions from charged clusters: an important ionization step causing suppression of matrix and analyte ions in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Lou, Xianwen; van Dongen, Joost L J; Milroy, Lech-Gustav; Meijer, E W

2016-12-30

Ionization in matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a very complicated process. It has been reported that quaternary ammonium salts show extremely strong matrix and analyte suppression effects which cannot satisfactorily be explained by charge transfer reactions. Further investigation of the reasons causing these effects can be useful to improve our understanding of the MALDI process. The dried-droplet and modified thin-layer methods were used as sample preparation methods. In the dried-droplet method, analytes were co-crystallized with matrix, whereas in the modified thin-layer method analytes were deposited on the surface of matrix crystals. Model compounds, tetrabutylammonium iodide ([N(Bu) 4 ]I), cesium iodide (CsI), trihexylamine (THA) and polyethylene glycol 600 (PEG 600), were selected as the test analytes given their ability to generate exclusively pre-formed ions, protonated ions and metal ion adducts respectively in MALDI. The strong matrix suppression effect (MSE) observed using the dried-droplet method might disappear using the modified thin-layer method, which suggests that the incorporation of analytes in matrix crystals contributes to the MSE. By depositing analytes on the matrix surface instead of incorporating in the matrix crystals, the competition for evaporation/ionization from charged matrix/analyte clusters could be weakened resulting in reduced MSE. Further supporting evidence for this inference was found by studying the analyte suppression effect using the same two sample deposition methods. By comparing differences between the mass spectra obtained via the two sample preparation methods, we present evidence suggesting that the generation of gas-phase ions from charged matrix/analyte clusters may induce significant suppression of matrix and analyte ions. The results suggest that the generation of gas-phase ions from charged matrix/analyte clusters is an important ionization step in MALDI-MS. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Toward a universal carbonate clumped isotope calibration: Diverse synthesis and preparatory methods suggest a single temperature relationship

NASA Astrophysics Data System (ADS)

Kelson, Julia R.; Huntington, Katharine W.; Schauer, Andrew J.; Saenger, Casey; Lechler, Alex R.

2017-01-01

Carbonate clumped isotope (Δ47) thermometry has been applied to a wide range of problems in earth, ocean and biological sciences over the last decade, but is still plagued by discrepancies among empirical calibrations that show a range of Δ47-temperature sensitivities. The most commonly suggested causes of these discrepancies are the method of mineral precipitation and analytical differences, including the temperature of phosphoric acid used to digest carbonates. However, these mechanisms have yet to be tested in a consistent analytical setting, which makes it difficult to isolate the cause(s) of discrepancies and to evaluate which synthetic calibration is most appropriate for natural samples. Here, we systematically explore the impact of synthetic carbonate precipitation by replicating precipitation experiments of previous workers under a constant analytical setting. We (1) precipitate 56 synthetic carbonates at temperatures of 4-85 °C using different procedures to degas CO2, with and without the use of the enzyme carbonic anhydrase (CA) to promote rapid dissolved inorganic carbon (DIC) equilibration; (2) digest samples in phosphoric acid at both 90 °C and 25 °C; and (3) hold constant all analytical methods including acid preparation, CO2 purification, and mass spectrometry; and (4) reduce our data with 17O corrections that are appropriate for our samples. We find that the CO2 degassing method does not influence Δ47 values of these synthetic carbonates, and therefore probably only influences natural samples with very rapid degassing rates, like speleothems that precipitate out of drip solution with high pCO2. CA in solution does not influence Δ47 values in this work, suggesting that disequilibrium in the DIC pool is negligible. We also find the Δ47 values of samples reacted in 25 and 90 °C acid are within error of each other (once corrected with a constant acid fractionation factor). Taken together, our results show that the Δ47-temperature relationship does not measurably change with either the precipitation methods used in this study or acid digestion temperature. This leaves phosphoric acid preparation, CO2 gas purification, and/or data reduction methods as the possible sources of the discrepancy among published calibrations. In particular, the use of appropriate 17O corrections has the potential to reduce disagreement among calibrations. Our study nearly doubles the available synthetic carbonate calibration data for Δ47 thermometry (adding 56 samples to the 74 previously published samples). This large population size creates a robust calibration that enables us to examine the potential for calibration slope aliasing due to small sample size. The similarity of Δ47 values among carbonates precipitated under such diverse conditions suggests that many natural samples grown at 4-85 °C in moderate pH conditions (6-10) may also be described by our Δ47-temperature relationship.

Alternative Internal Standard Calibration of an Indirect Enzymatic Analytical Method for 2-MCPD Fatty Acid Esters.

PubMed

Koyama, Kazuo; Miyazaki, Kinuko; Abe, Kousuke; Egawa, Yoshitsugu; Fukazawa, Toru; Kitta, Tadashi; Miyashita, Takashi; Nezu, Toru; Nohara, Hidenori; Sano, Takashi; Takahashi, Yukinari; Taniguchi, Hideji; Yada, Hiroshi; Yamazaki, Kumiko; Watanabe, Yomi

2017-06-01

An indirect enzymatic analysis method for the quantification of fatty acid esters of 2-/3-monochloro-1,2-propanediol (2/3-MCPD) and glycidol was developed, using the deuterated internal standard of each free-form component. A statistical method for calibration and quantification of 2-MCPD-d 5 , which is difficult to obtain, is substituted by 3-MCPD-d 5 used for calculation of 3-MCPD. Using data from a previous collaborative study, the current method for the determination of 2-MCPD content using 2-MCPD-d 5 was compared to three alternative new methods using 3-MCPD-d 5 . The regression analysis showed that the alternative methods were unbiased compared to the current method. The relative standard deviation (RSD R ) among the testing laboratories was ≤ 15% and the Horwitz ratio was ≤ 1.0, a satisfactory value.

Finite-analytic numerical solution of heat transfer in two-dimensional cavity flow

NASA Technical Reports Server (NTRS)

Chen, C.-J.; Naseri-Neshat, H.; Ho, K.-S.

1981-01-01

Heat transfer in cavity flow is numerically analyzed by a new numerical method called the finite-analytic method. The basic idea of the finite-analytic method is the incorporation of local analytic solutions in the numerical solutions of linear or nonlinear partial differential equations. In the present investigation, the local analytic solutions for temperature, stream function, and vorticity distributions are derived. When the local analytic solution is evaluated at a given nodal point, it gives an algebraic relationship between a nodal value in a subregion and its neighboring nodal points. A system of algebraic equations is solved to provide the numerical solution of the problem. The finite-analytic method is used to solve heat transfer in the cavity flow at high Reynolds number (1000) for Prandtl numbers of 0.1, 1, and 10.

A sustainable on-line CapLC method for quantifying antifouling agents like irgarol-1051 and diuron in water samples: Estimation of the carbon footprint.

PubMed

Pla-Tolós, J; Serra-Mora, P; Hakobyan, L; Molins-Legua, C; Moliner-Martinez, Y; Campins-Falcó, P

2016-11-01

In this work, in-tube solid phase microextraction (in-tube SPME) coupled to capillary LC (CapLC) with diode array detection has been reported, for on-line extraction and enrichment of booster biocides (irgarol-1051 and diuron) included in Water Frame Directive 2013/39/UE (WFD). The analytical performance has been successfully demonstrated. Furthermore, in the present work, the environmental friendliness of the procedure has been quantified by means of the implementation of the carbon footprint calculation of the analytical procedure and the comparison with other methodologies previously reported. Under the optimum conditions, the method presents good linearity over the range assayed, 0.05-10μg/L for irgarol-1051 and 0.7-10μg/L for diuron. The LODs were 0.015μg/L and 0.2μg/L for irgarol-1051 and diuron, respectively. Precision was also satisfactory (relative standard deviation, RSD<3.5%). The proposed methodology was applied to monitor water samples, taking into account the EQS standards for these compounds. The carbon footprint values for the proposed procedure consolidate the operational efficiency (analytical and environmental performance) of in-tube SPME-CapLC-DAD, in general, and in particular for determining irgarol-1051 and diuron in water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Field portable low temperature porous layer open tubular cryoadsorption headspace sampling and analysis part II: Applications.

PubMed

Harries, Megan; Bukovsky-Reyes, Santiago; Bruno, Thomas J

2016-01-15

This paper details the sampling methods used with the field portable porous layer open tubular cryoadsorption (PLOT-cryo) approach, described in Part I of this two-part series, applied to several analytes of interest. We conducted tests with coumarin and 2,4,6-trinitrotoluene (two solutes that were used in initial development of PLOT-cryo technology), naphthalene, aviation turbine kerosene, and diesel fuel, on a variety of matrices and test beds. We demonstrated that these analytes can be easily detected and reliably identified using the portable unit for analyte collection. By leveraging efficiency-boosting temperature control and the high flow rate multiple capillary wafer, very short collection times (as low as 3s) yielded accurate detection. For diesel fuel spiked on glass beads, we determined a method detection limit below 1 ppm. We observed greater variability among separate samples analyzed with the portable unit than previously documented in work using the laboratory-based PLOT-cryo technology. We identify three likely sources that may help explain the additional variation: the use of a compressed air source to generate suction, matrix geometry, and variability in the local vapor concentration around the sampling probe as solute depletion occurs both locally around the probe and in the test bed as a whole. This field-portable adaptation of the PLOT-cryo approach has numerous and diverse potential applications. Published by Elsevier B.V.

Validation of surrogate endpoints in cancer clinical trials via principal stratification with an application to a prostate cancer trial.

PubMed

Tanaka, Shiro; Matsuyama, Yutaka; Ohashi, Yasuo

2017-08-30

Increasing attention has been focused on the use and validation of surrogate endpoints in cancer clinical trials. Previous literature on validation of surrogate endpoints are classified into four approaches: the proportion explained approach; the indirect effects approach; the meta-analytic approach; and the principal stratification approach. The mainstream in cancer research has seen the application of a meta-analytic approach. However, VanderWeele (2013) showed that all four of these approaches potentially suffer from the surrogate paradox. It was also shown that, if a principal surrogate satisfies additional criteria called one-sided average causal sufficiency, the surrogate cannot exhibit a surrogate paradox. Here, we propose a method for estimating principal effects under a monotonicity assumption. Specifically, we consider cancer clinical trials which compare a binary surrogate endpoint and a time-to-event clinical endpoint under two naturally ordered treatments (e.g. combined therapy vs. monotherapy). Estimation based on a mean score estimating equation will be implemented by the expectation-maximization algorithm. We will also apply the proposed method as well as other surrogacy criteria to evaluate the surrogacy of prostate-specific antigen using data from a phase III advanced prostate cancer trial, clarifying the complementary roles of both the principal stratification and meta-analytic approaches in the evaluation of surrogate endpoints in cancer. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Field Portable Low Temperature Porous Layer Open Tubular Cryoadsorption Headspace Sampling and Analysis Part II: Applications*

PubMed Central

Harries, Megan; Bukovsky-Reyes, Santiago; Bruno, Thomas J.

2016-01-01

This paper details the sampling methods used with the field portable porous layer open tubular cryoadsorption (PLOT-cryo) approach, described in Part I of this two-part series, applied to several analytes of interest. We conducted tests with coumarin and 2,4,6-trinitrotoluene (two solutes that were used in initial development of PLOT-cryo technology), naphthalene, aviation turbine kerosene, and diesel fuel, on a variety of matrices and test beds. We demonstrated that these analytes can be easily detected and reliably identified using the portable unit for analyte collection. By leveraging efficiency-boosting temperature control and the high flow rate multiple capillary wafer, very short collection times (as low as 3 s) yielded accurate detection. For diesel fuel spiked on glass beads, we determined a method detection limit below 1 ppm. We observed greater variability among separate samples analyzed with the portable unit than previously documented in work using the laboratory-based PLOT-cryo technology. We identify three likely sources that may help explain the additional variation: the use of a compressed air source to generate suction, matrix geometry, and variability in the local vapor concentration around the sampling probe as solute depletion occurs both locally around the probe and in the test bed as a whole. This field-portable adaptation of the PLOT-cryo approach has numerous and diverse potential applications. PMID:26726934

VALIDATION OF STANDARD ANALYTICAL PROTOCOL FOR ...

EPA Pesticide Factsheets

There is a growing concern with the potential for terrorist use of chemical weapons to cause civilian harm. In the event of an actual or suspected outdoor release of chemically hazardous material in a large area, the extent of contamination must be determined. This requires a system with the ability to prepare and quickly analyze a large number of contaminated samples for the traditional chemical agents, as well as numerous toxic industrial chemicals. Liquid samples (both aqueous and organic), solid samples (e.g., soil), vapor samples (e.g., air) and mixed state samples, all ranging from household items to deceased animals, may require some level of analyses. To meet this challenge, the U.S. Environmental Protection Agency (U.S. EPA) National Homeland Security Research Center, in collaboration with experts from across U.S. EPA and other Federal Agencies, initiated an effort to identify analytical methods for the chemical and biological agents that could be used to respond to a terrorist attack or a homeland security incident. U.S. EPA began development of standard analytical protocols (SAPs) for laboratory identification and measurement of target agents in case of a contamination threat. These methods will be used to help assist in the identification of existing contamination, the effectiveness of decontamination, as well as clearance for the affected population to reoccupy previously contaminated areas. One of the first SAPs developed was for the determin

Development of a fast capillary electrophoresis method for determination of carbohydrates in honey samples.

PubMed

Rizelio, Viviane Maria; Tenfen, Laura; da Silveira, Roberta; Gonzaga, Luciano Valdemiro; Costa, Ana Carolina Oliveira; Fett, Roseane

2012-05-15

In this study, the determination of fructose, glucose and sucrose by capillary electrophoresis (CE) was investigated. The tendency of the analyte to undergo electromigration dispersion and the buffer capacity were evaluated using the Peakmaster(®) software and considered in the optimization of the background electrolyte, which was composed of 20 mmol L(-1) sorbic acid, 0.2 mmol L(-1) CTAB and 40 mmol L(-1) NaOH at pH 12.2. Under optimal CE conditions, the separation of the substances investigated was achieved in less than 2 min. The detection limits for the three analytes were in the range of 0.022 and 0.029 g L(-1) and precision measurements within 0.62-4.69% were achieved. The proposed methodology was applied in the quantitative analysis by direct injection of in honey samples to determine the main sugars presents. The samples were previously dissolved in deionized water and filtered with no other sample treatment. The mean values for fructose, glucose and sucrose were in the ranges of 33.65-45.46 g 100g(-1), 24.63-35.06 g 100g(-1) and <0.22-1.32 g 100g(-1), respectively. The good analytical performance of the method makes it suitable for implementation in food laboratories for the routine analysis of honey samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Surface acoustic wave nebulization facilitating lipid mass spectrometric analysis.

PubMed

Yoon, Sung Hwan; Huang, Yue; Edgar, J Scott; Ting, Ying S; Heron, Scott R; Kao, Yuchieh; Li, Yanyan; Masselon, Christophe D; Ernst, Robert K; Goodlett, David R

2012-08-07

Surface acoustic wave nebulization (SAWN) is a novel method to transfer nonvolatile analytes directly from the aqueous phase to the gas phase for mass spectrometric analysis. The lower ion energetics of SAWN and its planar nature make it appealing for analytically challenging lipid samples. This challenge is a result of their amphipathic nature, labile nature, and tendency to form aggregates, which readily precipitate clogging capillaries used for electrospray ionization (ESI). Here, we report the use of SAWN to characterize the complex glycolipid, lipid A, which serves as the membrane anchor component of lipopolysaccharide (LPS) and has a pronounced tendency to clog nano-ESI capillaries. We also show that unlike ESI SAWN is capable of ionizing labile phospholipids without fragmentation. Lastly, we compare the ease of use of SAWN to the more conventional infusion-based ESI methods and demonstrate the ability to generate higher order tandem mass spectral data of lipid A for automated structure assignment using our previously reported hierarchical tandem mass spectrometry (HiTMS) algorithm. The ease of generating SAWN-MS(n) data combined with HiTMS interpretation offers the potential for high throughput lipid A structure analysis.

Determination of lead isotopes in a new Greenland deep ice core at the sub-picogram per gram level by thermal ionization mass spectrometry using an improved decontamination method.

PubMed

Han, Changhee; Burn-Nunes, Laurie J; Lee, Khanghyun; Chang, Chaewon; Kang, Jung-Ho; Han, Yeongcheol; Hur, Soon Do; Hong, Sungmin

2015-08-01

An improved decontamination method and ultraclean analytical procedures have been developed to minimize Pb contamination of processed glacial ice cores and to achieve reliable determination of Pb isotopes in North Greenland Eemian Ice Drilling (NEEM) deep ice core sections with concentrations at the sub-picogram per gram level. A PL-7 (Fuso Chemical) silica-gel activator has replaced the previously used colloidal silica activator produced by Merck and has been shown to provide sufficiently enhanced ion beam intensity for Pb isotope analysis for a few tens of picograms of Pb. Considering the quantities of Pb contained in the NEEM Greenland ice core and a sample weight of 10 g used for the analysis, the blank contribution from the sample treatment was observed to be negligible. The decontamination and analysis of the artificial ice cores and selected NEEM Greenland ice core sections confirmed the cleanliness and effectiveness of the overall analytical process. Copyright © 2015 Elsevier B.V. All rights reserved.

A combined averaging and frequency mixing approach for force identification in weakly nonlinear high-Q oscillators: Atomic force microscope

NASA Astrophysics Data System (ADS)

Sah, Si Mohamed; Forchheimer, Daniel; Borgani, Riccardo; Haviland, David

2018-02-01

We present a polynomial force reconstruction of the tip-sample interaction force in Atomic Force Microscopy. The method uses analytical expressions for the slow-time amplitude and phase evolution, obtained from time-averaging over the rapidly oscillating part of the cantilever dynamics. The slow-time behavior can be easily obtained in either the numerical simulations or the experiment in which a high-Q resonator is perturbed by a weak nonlinearity and a periodic driving force. A direct fit of the theoretical expressions to the simulated and experimental data gives the best-fit parameters for the force model. The method combines and complements previous works (Platz et al., 2013; Forchheimer et al., 2012 [2]) and it allows for computationally more efficient parameter mapping with AFM. Results for the simulated asymmetric piecewise linear force and VdW-DMT force models are compared with the reconstructed polynomial force and show a good agreement. It is also shown that the analytical amplitude and phase modulation equations fit well with the experimental data.

Selected Analytical Methods for Environmental Remediation and Recovery (SAM) - Home

EPA Pesticide Factsheets

The SAM Home page provides access to all information provided in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM), and includes a query function allowing users to search methods by analyte, sample type and instrumentation.

Data Pre-Processing Method to Remove Interference of Gas Bubbles and Cell Clusters During Anaerobic and Aerobic Yeast Fermentations in a Stirred Tank Bioreactor

NASA Astrophysics Data System (ADS)

Princz, S.; Wenzel, U.; Miller, R.; Hessling, M.

2014-11-01

One aerobic and four anaerobic batch fermentations of the yeast Saccharomyces cerevisiae were conducted in a stirred bioreactor and monitored inline by NIR spectroscopy and a transflectance dip probe. From the acquired NIR spectra, chemometric partial least squares regression (PLSR) models for predicting biomass, glucose and ethanol were constructed. The spectra were directly measured in the fermentation broth and successfully inspected for adulteration using our novel data pre-processing method. These adulterations manifested as strong fluctuations in the shape and offset of the absorption spectra. They resulted from cells, cell clusters, or gas bubbles intercepting the optical path of the dip probe. In the proposed data pre-processing method, adulterated signals are removed by passing the time-scanned non-averaged spectra through two filter algorithms with a 5% quantile cutoff. The filtered spectra containing meaningful data are then averaged. A second step checks whether the whole time scan is analyzable. If true, the average is calculated and used to prepare the PLSR models. This new method distinctly improved the prediction results. To dissociate possible correlations between analyte concentrations, such as glucose and ethanol, the feeding analytes were alternately supplied at different concentrations (spiking) at the end of the four anaerobic fermentations. This procedure yielded low-error (anaerobic) PLSR models for predicting analyte concentrations of 0.31 g/l for biomass, 3.41 g/l for glucose, and 2.17 g/l for ethanol. The maximum concentrations were 14 g/l biomass, 167 g/l glucose, and 80 g/l ethanol. Data from the aerobic fermentation, carried out under high agitation and high aeration, were incorporated to realize combined PLSR models, which have not been previously reported to our knowledge.

Simultaneous screening and quantification of 29 drugs of abuse in oral fluid by solid-phase extraction and ultraperformance LC-MS/MS.

PubMed

Badawi, Nora; Simonsen, Kirsten Wiese; Steentoft, Anni; Bernhoft, Inger Marie; Linnet, Kristian

2009-11-01

The European DRUID (Driving under the Influence of Drugs, Alcohol And Medicines) project calls for analysis of oral fluid (OF) samples, collected randomly and anonymously at the roadside from drivers in Denmark throughout 2008-2009. To analyze these samples we developed an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for detection of 29 drugs and illicit compounds in OF. The drugs detected were opioids, amphetamines, cocaine, benzodiazepines, and Delta-9-tetrahydrocannabinol. Solid-phase extraction was performed with a Gilson ASPEC XL4 system equipped with Bond Elut Certify sample cartridges. OF samples (200 mg) diluted with 5 mL of ammonium acetate/methanol (vol/vol 90:10) buffer were applied to the columns and eluted with 3 mL of acetonitrile with aqueous ammonium hydroxide. Target drugs were quantified by use of a Waters ACQUITY UPLC system coupled to a Waters Quattro Premier XE triple quadrupole (positive electrospray ionization mode, multiple reaction monitoring mode). Extraction recoveries were 36%-114% for all analytes, including Delta-9-tetrahydrocannabinol and benzoylecgonine. The lower limit of quantification was 0.5 mug/kg for all analytes. Total imprecision (CV) was 5.9%-19.4%. With the use of deuterated internal standards for most compounds, the performance of the method was not influenced by matrix effects. A preliminary account of OF samples collected at the roadside showed the presence of amphetamine, cocaine, codeine, Delta-9-tetrahydrocannabinol, tramadol, and zopiclone. The UPLC-MS/MS method makes it possible to detect all 29 analytes in 1 chromatographic run (15 min), including Delta-9-tetrahydrocannabinol and benzoylecgonine, which previously have been difficult to incorporate into multicomponent methods.

HPLC-MS method for the quantification of nine anti-HIV drugs from dry plasma spot on glass filter and their long term stability in different conditions.

PubMed

D'Avolio, Antonio; Simiele, Marco; Siccardi, Marco; Baietto, Lorena; Sciandra, Mauro; Bonora, Stefano; Di Perri, Giovanni

2010-09-05

A bioanalytical method for the determination of most commonly prescribed protease inhibitors (saquinavir, atazanavir, amprenavir, darunavir, lopinavir and ritonavir) and non-nucleoside reverse transcriptase inhibitors (etravirine, efavirenz and nevirapine) was developed, modifying our previous HPLC-MS chromatographic run, validated and a complete short and long term stability evaluation was carried out. One hundred microlitres of plasma were distributed on a collection glass paper filter (Glass-Microfibre from Sartorius), then the filter underwent thermal treatment, both for drying and for HIV inactivation, and stored at room temperature, 4 degrees C and -20 degrees C. The analytes were extracted from the filter disc using tert-butylmethylether with basic pH, after the addition of the internal standards quinoxaline. The extract was dried, reconstituted and the chromatographic separation was performed on a reversed-phase C-18 column (150 mm x 2.0 mm) and the analytes were quantified using a single quadrupole mass spectrometer. The method was validated considering the concentration ranges encountered in clinical trials and the routine clinical practice. The assay was linear over the concentration ranges tested. Accuracies ranged from 92.1% to 111.9% and intra-day and inter-day relative standard deviation for all quality control levels ranged from 0.2 to 12.9 and 3.1 to 14.4, respectively. Analytes in dried plasma spots were stable for longer time when dried/inactivation step was carried out before storage compared to samples not dried/inactivated before the analysis. The dried/inactivation step allows shipment of samples at room temperature without any risks, therefore the developed and validated method enables an easy and cheap sample shipment for therapeutic drug monitoring and pharmacokinetic studies. 2010 Elsevier B.V. All rights reserved.

MAGNETO-FRICTIONAL MODELING OF CORONAL NONLINEAR FORCE-FREE FIELDS. I. TESTING WITH ANALYTIC SOLUTIONS

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

Guo, Y.; Keppens, R.; Xia, C.

2016-09-10

We report our implementation of the magneto-frictional method in the Message Passing Interface Adaptive Mesh Refinement Versatile Advection Code (MPI-AMRVAC). The method aims at applications where local adaptive mesh refinement (AMR) is essential to make follow-up dynamical modeling affordable. We quantify its performance in both domain-decomposed uniform grids and block-adaptive AMR computations, using all frequently employed force-free, divergence-free, and other vector comparison metrics. As test cases, we revisit the semi-analytic solution of Low and Lou in both Cartesian and spherical geometries, along with the topologically challenging Titov–Démoulin model. We compare different combinations of spatial and temporal discretizations, and find thatmore » the fourth-order central difference with a local Lax–Friedrichs dissipation term in a single-step marching scheme is an optimal combination. The initial condition is provided by the potential field, which is the potential field source surface model in spherical geometry. Various boundary conditions are adopted, ranging from fully prescribed cases where all boundaries are assigned with the semi-analytic models, to solar-like cases where only the magnetic field at the bottom is known. Our results demonstrate that all the metrics compare favorably to previous works in both Cartesian and spherical coordinates. Cases with several AMR levels perform in accordance with their effective resolutions. The magneto-frictional method in MPI-AMRVAC allows us to model a region of interest with high spatial resolution and large field of view simultaneously, as required by observation-constrained extrapolations using vector data provided with modern instruments. The applications of the magneto-frictional method to observations are shown in an accompanying paper.« less

40 CFR 141.89 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Analytical methods. 141.89 Section 141...) NATIONAL PRIMARY DRINKING WATER REGULATIONS Control of Lead and Copper § 141.89 Analytical methods. (a... shall be conducted with the methods in § 141.23(k)(1). (1) Analyses for alkalinity, calcium...

40 CFR 141.89 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 24 2013-07-01 2013-07-01 false Analytical methods. 141.89 Section 141...) NATIONAL PRIMARY DRINKING WATER REGULATIONS Control of Lead and Copper § 141.89 Analytical methods. (a... shall be conducted with the methods in § 141.23(k)(1). (1) Analyses for alkalinity, calcium...

40 CFR 141.89 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 23 2014-07-01 2014-07-01 false Analytical methods. 141.89 Section 141...) NATIONAL PRIMARY DRINKING WATER REGULATIONS Control of Lead and Copper § 141.89 Analytical methods. (a... shall be conducted with the methods in § 141.23(k)(1). (1) Analyses for alkalinity, calcium...

40 CFR 141.89 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 23 2011-07-01 2011-07-01 false Analytical methods. 141.89 Section 141...) NATIONAL PRIMARY DRINKING WATER REGULATIONS Control of Lead and Copper § 141.89 Analytical methods. (a... shall be conducted with the methods in § 141.23(k)(1). (1) Analyses for alkalinity, calcium...

75 FR 49930 - Stakeholder Meeting Regarding Re-Evaluation of Currently Approved Total Coliform Analytical Methods

Federal Register 2010, 2011, 2012, 2013, 2014

2010-08-16

... Currently Approved Total Coliform Analytical Methods AGENCY: Environmental Protection Agency (EPA). ACTION... of currently approved Total Coliform Rule (TCR) analytical methods. At these meetings, stakeholders will be given an opportunity to discuss potential elements of a method re-evaluation study, such as...

40 CFR 141.89 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 24 2012-07-01 2012-07-01 false Analytical methods. 141.89 Section 141...) NATIONAL PRIMARY DRINKING WATER REGULATIONS Control of Lead and Copper § 141.89 Analytical methods. (a... shall be conducted with the methods in § 141.23(k)(1). (1) Analyses for alkalinity, calcium...

Multiplexed bovine milk oligosaccharide analysis with aminoxy tandem mass tags

PubMed Central

Poulsen, Nina Aagaard; Barile, Daniela

2018-01-01

Milk oligosaccharides (OS) are a key factor that influences the infant gut microbial composition, and their importance in promoting healthy infant development and disease prevention is becoming increasingly apparent. Investigating the structures, properties, and sources of these compounds requires a host of complementary analytical techniques. Relative compound quantification by mass spectral analysis of isobarically labeled samples is a relatively new technique that has been used mainly in the proteomics field. Glycomics applications have so far focused on analysis of protein-linked glycans, while analysis of free milk OS has previously been conducted only on analytical standards. In this paper, we extend the use of isobaric glycan tags to the analysis of bovine milk OS by presenting a method for separation of labeled OS on a porous graphitized carbon liquid chromatographic column with subsequent analysis by quadrupole time-of-flight tandem mass spectrometry. Abundances for 15 OS extracted from mature bovine milk were measured, with replicate injections providing coefficients of variation below 15% for most OS. Isobaric labeling improved ionization efficiency for low-abundance, high-molecular weight fucosylated OS, which are known to exist in bovine milk but have been only sporadically reported in the literature. We compared the abundances of four fucosylated OS in milk from Holstein and Jersey cattle and found that three of the compounds were more abundant in Jersey milk, which is in general agreement with a previous study. This novel method represents an advancement in our ability to characterize milk OS and provides the advantages associated with isobaric labeling, including reduced instrumental analysis time and increased analyte ionization efficiency. This improved ability to measure differences in bioactive OS abundances in large datasets will facilitate exploration of OS from all food sources for the purpose of developing health-guiding products for infants, immune-compromised elderly, and the population at large. PMID:29698512

Ultrasonic isolation of the outer membrane of Escherichia coli with autodisplayed Z-domains.

PubMed

Bong, Ji-Hong; Yoo, Gu; Park, Min; Kang, Min-Jung; Jose, Joachim; Pyun, Jae-Chul

2014-11-01

The outer membrane of Escherichia coli was previously isolated as a liposome-like outer membrane particle using an enzymatic treatment for lysozymes; for immunoassays, the particles were subsequently layered on solid supports via hydrophobic interactions. This work presents an enzyme-free isolation method for the E. coli outer membrane with autodisplayed Z-domains using ultrasonication. First, the properties of the outer membrane particle, such as the particle size, zeta potential, and total protein, were compared with the properties of particles obtained using the previous preparation methods. Compared with the conventional isolation method using an enzyme treatment, the ultrasonic method exhibited a higher efficiency at isolating the outer membrane and less contamination by cytosolic proteins. The isolated outer membrane particles were layered on a gold surface, and the roughness and thickness of the layered outer membrane layers were subsequently analyzed using AFM analysis. Finally, the antibody-binding activity of two outer membrane layers with autodisplayed Z-domains created from particles that were isolated using the enzymatic and ultrasonic isolation methods was measured using fluorescein-labeled antibody as a model analyte, and the activity of the outer membrane layer that was isolated from the ultrasonic method was estimated to be more than 20% higher than that from the conventional enzymatic method. Copyright © 2014 Elsevier Inc. All rights reserved.

GalaxyGPCRloop: Template-Based and Ab Initio Structure Sampling of the Extracellular Loops of G-Protein-Coupled Receptors.

PubMed

Won, Jonghun; Lee, Gyu Rie; Park, Hahnbeom; Seok, Chaok

2018-06-07

The second extracellular loops (ECL2s) of G-protein-coupled receptors (GPCRs) are often involved in GPCR functions, and their structures have important implications in drug discovery. However, structure prediction of ECL2 is difficult because of its long length and the structural diversity among different GPCRs. In this study, a new ECL2 conformational sampling method involving both template-based and ab initio sampling was developed. Inspired by the observation of similar ECL2 structures of closely related GPCRs, a template-based sampling method employing loop structure templates selected from the structure database was developed. A new metric for evaluating similarity of the target loop to templates was introduced for template selection. An ab initio loop sampling method was also developed to treat cases without highly similar templates. The ab initio method is based on the previously developed fragment assembly and loop closure method. A new sampling component that takes advantage of secondary structure prediction was added. In addition, a conserved disulfide bridge restraining ECL2 conformation was predicted and analytically incorporated into sampling, reducing the effective dimension of the conformational search space. The sampling method was combined with an existing energy function for comparison with previously reported loop structure prediction methods, and the benchmark test demonstrated outstanding performance.

Rapid simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and 3,4-methylenedioxyethylamphetamine in urine by solid-phase extraction and GC-MS: a method optimized for high-volume laboratories.

PubMed

Stout, Peter R; Horn, Carl K; Klette, Kevin L

2002-01-01

To facilitate analysis of high sample volumes, an extraction, derivatization and gas chromatographic-mass spectrometric analysis method was developed to simultaneously determine amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxyamphetamine (MDA) 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) in urine. This method utilized a positive-pressure manifold cation-exchange polymer-based solid-phase extraction followed by elution directly into automated liquid sampler (ALS) vials. Rapid derivatization was accomplished using heptafluorobutyric anhydride (HFBA). Recoveries averaged 90% or greater for each of the compounds. Limits of detection were 62.5 ng/mL (AMP and MDEA), 15.6 ng/mL (MAMP), and 31.3 ng/mL (MDA and MDMA) using a 2-mL sample volume. The method was linear to 5000 ng/mL for all compounds using MDMA-d5 and MAMP-d14 as internal standards. Over 200 human urine samples previously determined to contain the target analytes were analyzed using the method. Excellent agreement was seen with previous quantitations. The method was challenged with 75 potentially interfering compounds and no interferences were seen. These interfering compounds included ephedrine, pseudoephedrine, phenylpropanolamine, and phenethylamine. The method resulted in dramatic reductions in processing time and waste production.

A Generalized Pivotal Quantity Approach to Analytical Method Validation Based on Total Error.

PubMed

Yang, Harry; Zhang, Jianchun

2015-01-01

The primary purpose of method validation is to demonstrate that the method is fit for its intended use. Traditionally, an analytical method is deemed valid if its performance characteristics such as accuracy and precision are shown to meet prespecified acceptance criteria. However, these acceptance criteria are not directly related to the method's intended purpose, which is usually a gurantee that a high percentage of the test results of future samples will be close to their true values. Alternate "fit for purpose" acceptance criteria based on the concept of total error have been increasingly used. Such criteria allow for assessing method validity, taking into account the relationship between accuracy and precision. Although several statistical test methods have been proposed in literature to test the "fit for purpose" hypothesis, the majority of the methods are not designed to protect the risk of accepting unsuitable methods, thus having the potential to cause uncontrolled consumer's risk. In this paper, we propose a test method based on generalized pivotal quantity inference. Through simulation studies, the performance of the method is compared to five existing approaches. The results show that both the new method and the method based on β-content tolerance interval with a confidence level of 90%, hereafter referred to as the β-content (0.9) method, control Type I error and thus consumer's risk, while the other existing methods do not. It is further demonstrated that the generalized pivotal quantity method is less conservative than the β-content (0.9) method when the analytical methods are biased, whereas it is more conservative when the analytical methods are unbiased. Therefore, selection of either the generalized pivotal quantity or β-content (0.9) method for an analytical method validation depends on the accuracy of the analytical method. It is also shown that the generalized pivotal quantity method has better asymptotic properties than all of the current methods. Analytical methods are often used to ensure safety, efficacy, and quality of medicinal products. According to government regulations and regulatory guidelines, these methods need to be validated through well-designed studies to minimize the risk of accepting unsuitable methods. This article describes a novel statistical test for analytical method validation, which provides better protection for the risk of accepting unsuitable analytical methods. © PDA, Inc. 2015.

Using the ratio of the magnetic field to the analytic signal of the magnetic gradient tensor in determining the position of simple shaped magnetic anomalies

NASA Astrophysics Data System (ADS)

Karimi, Kurosh; Shirzaditabar, Farzad

2017-08-01

The analytic signal of magnitude of the magnetic field’s components and its first derivatives have been employed for locating magnetic structures, which can be considered as point-dipoles or line of dipoles. Although similar methods have been used for locating such magnetic anomalies, they cannot estimate the positions of anomalies in noisy states with an acceptable accuracy. The methods are also inexact in determining the depth of deep anomalies. In noisy cases and in places other than poles, the maximum points of the magnitude of the magnetic vector components and Az are not located exactly above 3D bodies. Consequently, the horizontal location estimates of bodies are accompanied by errors. Here, the previous methods are altered and generalized to locate deeper models in the presence of noise even at lower magnetic latitudes. In addition, a statistical technique is presented for working in noisy areas and a new method, which is resistant to noise by using a ‘depths mean’ method, is made. Reduction to the pole transformation is also used to find the most possible actual horizontal body location. Deep models are also well estimated. The method is tested on real magnetic data over an urban gas pipeline in the vicinity of Kermanshah province, Iran. The estimated location of the pipeline is accurate in accordance with the result of the half-width method.

Isosteric heat of hydrogen adsorption on MOFs: comparison between adsorption calorimetry, sorption isosteric method, and analytical models

NASA Astrophysics Data System (ADS)

Kloutse, A. F.; Zacharia, R.; Cossement, D.; Chahine, R.; Balderas-Xicohténcatl, R.; Oh, H.; Streppel, B.; Schlichtenmayer, M.; Hirscher, M.

2015-12-01

Isosteric heat of adsorption is an important parameter required to describe the thermal performance of adsorptive storage systems. It is most frequently calculated from adsorption isotherms measured over wide ranges of pressure and temperature, using the so-called adsorption isosteric method. Direct quantitative estimation of isosteric heats on the other hand is possible using the coupled calorimetric-volumetric method, which involves simultaneous measurement of heat and adsorption. In this work, we compare the isosteric heats of hydrogen adsorption on microporous materials measured by both methods. Furthermore, the experimental data are compared with the isosteric heats obtained using the modified Dubinin-Astakhov, Tóth, and Unilan adsorption analytical models to establish the reliability and limitations of simpler methods and assumptions. To this end, we measure the hydrogen isosteric heats on five prototypical metal-organic frameworks: MOF-5, Cu-BTC, Fe-BTC, MIL-53, and MOF-177 using both experimental methods. For all MOFs, we find a very good agreement between the isosteric heats measured using the calorimetric and isosteric methods throughout the range of loading studied. Models' prediction on the other hand deviates from both experiments depending on the MOF studied and the range of loading. Under low-loadings of less than 5 mol kg-1, the isosteric heat of hydrogen adsorption decreases in the order Cu-BTC > MIL-53 > MOF-5 > Fe-BTC > MOF-177. The order of isosteric heats is coherent with the strength of hydrogen interaction revealed from previous thermal desorption spectroscopy measurements.

Integration of Gas Chromatography Mass Spectrometry Methods for Differentiating Ricin Preparation Methods

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

Wunschel, David S.; Melville, Angela M.; Ehrhardt, Christopher J.

2012-05-17

The investigation of crimes involving chemical or biological agents is infrequent, but presents unique analytical challenges. The protein toxin ricin is encountered more frequently than other agents and is found in the seeds of the castor plant Ricinus communis. Typically, the toxin is extracted from castor seeds utilizing a variety of different recipes that result in varying purity of the toxin. Moreover, these various purification steps can also leave or differentially remove a variety of exogenous and endogenous residual components with the toxin that may indicate the type and number of purification steps involved. We have applied three gas chromatographicmore » - mass spectrometric (GC-MS) based analytical methods to measure the variation in seed carbohydrates and castor oil ricinoleic acid as well as the presence of solvents used for purification. These methods were applied to the same samples prepared using four previously identified toxin preparation methods starting from four varieties of castor seeds. The individual data sets for seed carbohydrate profiles, ricinoleic acid or acetone amount each provided information capable of differentiating different types of toxin preparations across seed types. However, the integration of the data sets using multivariate factor analysis provided a clear distinction of all samples based on the preparation method and independent of the seed source. In particular the abundance of mannose, arabinose, fucose, ricinoleic acid and acetone were shown to be important differentiating factors. These complementary tools provide a more confident determination of the method of toxin preparation.« less

40 CFR 158.355 - Enforcement analytical method.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Enforcement analytical method. 158.355 Section 158.355 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.355 Enforcement analytical method. An...

40 CFR 158.355 - Enforcement analytical method.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 25 2012-07-01 2012-07-01 false Enforcement analytical method. 158.355 Section 158.355 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.355 Enforcement analytical method. An...

40 CFR 158.355 - Enforcement analytical method.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 25 2013-07-01 2013-07-01 false Enforcement analytical method. 158.355 Section 158.355 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.355 Enforcement analytical method. An...

40 CFR 158.355 - Enforcement analytical method.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 24 2011-07-01 2011-07-01 false Enforcement analytical method. 158.355 Section 158.355 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS DATA REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.355 Enforcement analytical method. An...

Is a pre-analytical process for urinalysis required?

PubMed

Petit, Morgane; Beaudeux, Jean-Louis; Majoux, Sandrine; Hennequin, Carole

2017-10-01

For the reliable urinary measurement of calcium, phosphate and uric acid, a pre-analytical process by adding acid or base to urine samples at laboratory is recommended in order to dissolve precipitated solutes. Several studies on different kind of samples and analysers have previously shown that a such pre-analytical treatment is useless. The objective was to study the necessity of pre-analytical treatment of urine on samples collected using the V-Monovette ® (Sarstedt) system and measured on the analyser Architect C16000 (Abbott Diagnostics). Sixty urinary samples of hospitalized patients were selected (n=30 for calcium and phosphate, and n=30 for uric acid). After acidification of urine samples for measurement of calcium and phosphate, and alkalinisation for measurement of uric acid respectively, differences between results before and after the pre-analytical treatment were compared to acceptable limits recommended by the French society of clinical biology (SFBC). No difference in concentration between before and after pre-analytical treatment of urine samples exceeded acceptable limits from SFBC for measurement of calcium and uric acid. For phosphate, only one sample exceeded these acceptable limits, showing a result paradoxically lower after acidification. In conclusion, in agreement with previous study, our results show that acidification or alkalinisation of urine samples from 24 h urines or from urination is not a pre-analytical necessity for measurement of calcium, phosphate and uric acid.

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

Hohimer, J.P.

The use of laser-based analytical methods in nuclear-fuel processing plants is considered. The species and locations for accountability, process control, and effluent control measurements in the Coprocessing, Thorex, and reference Purex fuel processing operations are identified and the conventional analytical methods used for these measurements are summarized. The laser analytical methods based upon Raman, absorption, fluorescence, and nonlinear spectroscopy are reviewed and evaluated for their use in fuel processing plants. After a comparison of the capabilities of the laser-based and conventional analytical methods, the promising areas of application of the laser-based methods in fuel processing plants are identified.

Milk Bottom-Up Proteomics: Method Optimization

PubMed Central

Vincent, Delphine; Ezernieks, Vilnis; Elkins, Aaron; Nguyen, Nga; Moate, Peter J.; Cocks, Benjamin G.; Rochfort, Simone

2016-01-01

Milk is a complex fluid whose proteome displays a diverse set of proteins of high abundance such as caseins and medium to low abundance whey proteins such as ß-lactoglobulin, lactoferrin, immunoglobulins, glycoproteins, peptide hormones, and enzymes. A sample preparation method that enables high reproducibility and throughput is key in reliably identifying proteins present or proteins responding to conditions such as a diet, health or genetics. Using skim milk samples from Jersey and Holstein-Friesian cows, we compared three extraction procedures which have not previously been applied to samples of cows' milk. Method A (urea) involved a simple dilution of the milk in a urea-based buffer, method B (TCA/acetone) involved a trichloroacetic acid (TCA)/acetone precipitation, and method C (methanol/chloroform) involved a tri-phasic partition method in chloroform/methanol solution. Protein assays, SDS-PAGE profiling, and trypsin digestion followed by nanoHPLC-electrospray ionization-tandem mass spectrometry (nLC-ESI-MS/MS) analyses were performed to assess their efficiency. Replicates were used at each analytical step (extraction, digestion, injection) to assess reproducibility. Mass spectrometry (MS) data are available via ProteomeXchange with identifier PXD002529. Overall 186 unique accessions, major and minor proteins, were identified with a combination of methods. Method C (methanol/chloroform) yielded the best resolved SDS-patterns and highest protein recovery rates, method A (urea) yielded the greatest number of accessions, and, of the three procedures, method B (TCA/acetone) was the least compatible of all with a wide range of downstream analytical procedures. Our results also highlighted breed differences between the proteins in milk of Jersey and Holstein-Friesian cows. PMID:26793233

Rational Selection, Criticality Assessment, and Tiering of Quality Attributes and Test Methods for Analytical Similarity Evaluation of Biosimilars.

PubMed

Vandekerckhove, Kristof; Seidl, Andreas; Gutka, Hiten; Kumar, Manish; Gratzl, Gyöngyi; Keire, David; Coffey, Todd; Kuehne, Henriette

2018-05-10

Leading regulatory agencies recommend biosimilar assessment to proceed in a stepwise fashion, starting with a detailed analytical comparison of the structural and functional properties of the proposed biosimilar and reference product. The degree of analytical similarity determines the degree of residual uncertainty that must be addressed through downstream in vivo studies. Substantive evidence of similarity from comprehensive analytical testing may justify a targeted clinical development plan, and thus enable a shorter path to licensing. The importance of a careful design of the analytical similarity study program therefore should not be underestimated. Designing a state-of-the-art analytical similarity study meeting current regulatory requirements in regions such as the USA and EU requires a methodical approach, consisting of specific steps that far precede the work on the actual analytical study protocol. This white paper discusses scientific and methodological considerations on the process of attribute and test method selection, criticality assessment, and subsequent assignment of analytical measures to US FDA's three tiers of analytical similarity assessment. Case examples of selection of critical quality attributes and analytical methods for similarity exercises are provided to illustrate the practical implementation of the principles discussed.

Simultaneous Spectrophotometric Determination of Rifampicin, Isoniazid and Pyrazinamide in a Single Step

PubMed Central

Asadpour-Zeynali, Karim; Saeb, Elhameh

2016-01-01

Three antituberculosis medications are investigated in this work consist of rifampicin, isoniazid and pyrazinamide. The ultra violet (UV) spectra of these compounds are overlapped, thus use of suitable chemometric methods are helpful for simultaneous spectrophotometric determination of them. A generalized version of net analyte signal standard addition method (GNASSAM) was used for determination of three antituberculosis medications as a model system. In generalized net analyte signal standard addition method only one standard solution was prepared for all analytes. This standard solution contains a mixture of all analytes of interest, and the addition of such solution to sample, causes increases in net analyte signal of each analyte which are proportional to the concentrations of analytes in added standards solution. For determination of concentration of each analyte in some synthetic mixtures, the UV spectra of pure analytes and each sample were recorded in the range of 210 nm-550 nm. The standard addition procedure was performed for each sample and the UV spectrum was recorded after each addition and finally the results were analyzed by net analyte signal method. Obtained concentrations show acceptable performance of GNASSAM in these cases. PMID:28243267

Analytic redundancy management for SCOLE

NASA Technical Reports Server (NTRS)

Montgomery, Raymond C.

1988-01-01

The objective of this work is to develop a practical sensor analytic redundancy management scheme for flexible spacecraft and to demonstrate it using the SCOLE experimental apparatus. The particular scheme to be used is taken from previous work on the Grid apparatus by Williams and Montgomery.

Adhesive-Bonded Composite Joint Analysis with Delaminated Surface Ply Using Strain-Energy Release Rate

NASA Technical Reports Server (NTRS)

Chadegani, Alireza; Yang, Chihdar; Smeltzer, Stanley S. III

2012-01-01

This paper presents an analytical model to determine the strain energy release rate due to an interlaminar crack of the surface ply in adhesively bonded composite joints subjected to axial tension. Single-lap shear-joint standard test specimen geometry with thick bondline is followed for model development. The field equations are formulated by using the first-order shear-deformation theory in laminated plates together with kinematics relations and force equilibrium conditions. The stress distributions for the adherends and adhesive are determined after the appropriate boundary and loading conditions are applied and the equations for the field displacements are solved. The system of second-order differential equations is solved to using the symbolic computation tool Maple 9.52 to provide displacements fields. The equivalent forces at the tip of the prescribed interlaminar crack are obtained based on interlaminar stress distributions. The strain energy release rate of the crack is then determined by using the crack closure method. Finite element analyses using the J integral as well as the crack closure method are performed to verify the developed analytical model. It has been shown that the results using the analytical method correlate well with the results from the finite element analyses. An attempt is made to predict the failure loads of the joints based on limited test data from the literature. The effectiveness of the inclusion of bondline thickness is justified when compared with the results obtained from the previous model in which a thin bondline and uniform adhesive stresses through the bondline thickness are assumed.

Fast mass spectrometry-based enantiomeric excess determination of proteinogenic amino acids.

PubMed

Fleischer, Heidi; Thurow, Kerstin

2013-03-01

A rapid determination of the enantiomeric excess of proteinogenic amino acids is of great importance in various fields of chemical and biologic research and industries. Owing to their different biologic effects, enantiomers are interesting research subjects in drug development for the design of new and more efficient pharmaceuticals. Usually, the enantiomeric composition of amino acids is determined by conventional analytical methods such as liquid or gas chromatography or capillary electrophoresis. These analytical techniques do not fulfill the requirements of high-throughput screening due to their relative long analysis times. The method presented allows a fast analysis of chiral amino acids without previous time consuming chromatographic separation. The analytical measurements base on parallel kinetic resolution with pseudoenantiomeric mass tagged auxiliaries and were carried out by mass spectrometry with electrospray ionization. All 19 chiral proteinogenic amino acids were tested and Pro, Ser, Trp, His, and Glu were selected as model substrates for verification measurements. The enantiomeric excesses of amino acids with non-polar and aliphatic side chains as well as Trp and Phe (aromatic side chains) were determined with maximum deviations of the expected value less than or equal to 10ee%. Ser, Cys, His, Glu, and Asp were determined with deviations lower or equal to 14ee% and the enantiomeric excess of Tyr were calculated with 17ee% deviation. The total screening process is fully automated from the sample pretreatment to the data processing. The method presented enables fast measurement times about 1.38 min per sample and is applicable in the scope of high-throughput screenings.

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

Daley, P F

The overall objective of this project is the continued development, installation, and testing of continuous water sampling and analysis technologies for application to on-site monitoring of groundwater treatment systems and remediation sites. In a previous project, an on-line analytical system (OLAS) for multistream water sampling was installed at the Fort Ord Operable Unit 2 Groundwater Treatment System, with the objective of developing a simplified analytical method for detection of Compounds of Concern at that plant, and continuous sampling of up to twelve locations in the treatment system, from raw influent waters to treated effluent. Earlier implementations of the water samplingmore » and processing system (Analytical Sampling and Analysis Platform, A A+RT, Milpitas, CA) depended on off-line integrators that produced paper plots of chromatograms, and sent summary tables to a host computer for archiving. We developed a basic LabVIEW (National Instruments, Inc., Austin, TX) based gas chromatography control and data acquisition system that was the foundation for further development and integration with the ASAP system. Advantages of this integration include electronic archiving of all raw chromatographic data, and a flexible programming environment to support development of improved ASAP operation and automated reporting. The initial goals of integrating the preexisting LabVIEW chromatography control system with the ASAP, and demonstration of a simplified, site-specific analytical method were successfully achieved. However, although the principal objective of this system was assembly of an analytical system that would allow plant operators an up-to-the-minute view of the plant's performance, several obstacles remained. Data reduction with the base LabVIEW system was limited to peak detection and simple tabular output, patterned after commercial chromatography integrators, with compound retention times and peak areas. Preparation of calibration curves, method detection limit estimates and trend plotting were performed with spreadsheets and statistics software. Moreover, the analytical method developed was very limited in compound coverage, and unable to closely mirror the standard analytical methods promulgated by the EPA. To address these deficiencies, during this award the original equipment was operated at the OU 2-GTS to further evaluate the use of columns, commercial standard blends and other components to broaden the compound coverage of the chromatography system. A second-generation ASAP was designed and built to replace the original system at the OU 2-GTS, and include provision for introduction of internal standard compounds and surrogates into each sample analyzed. An enhanced, LabVIEW based chromatogram analysis application was written, that manages and archives chemical standards information, and provides a basis for NIST traceability for all analyses. Within this same package, all compound calibration response curves are managed, and different report formats were incorporated, that simplify trend analysis. Test results focus on operation of the original system at the OU 1 Integrated Chemical and Flow Monitoring System, at the OU 1 Fire Drill Area remediation site.« less

Efficient Geometric Probabilities of Multi-transiting Systems, Circumbinary Planets, and Exoplanet Mutual Events

NASA Astrophysics Data System (ADS)

Brakensiek, Joshua; Ragozzine, D.

2012-10-01

The transit method for discovering extra-solar planets relies on detecting regular diminutions of light from stars due to the shadows of planets passing in between the star and the observer. NASA's Kepler Mission has successfully discovered thousands of exoplanet candidates using this technique, including hundreds of stars with multiple transiting planets. In order to estimate the frequency of these valuable systems, our research concerns the efficient calculation of geometric probabilities for detecting multiple transiting extrasolar planets around the same parent star. In order to improve on previous studies that used numerical methods (e.g., Ragozzine & Holman 2010, Tremaine & Dong 2011), we have constructed an efficient, analytical algorithm which, given a collection of conjectured exoplanets orbiting a star, computes the probability that any particular group of exoplanets are transiting. The algorithm applies theorems of elementary differential geometry to compute the areas bounded by circular curves on the surface of a sphere (see Ragozzine & Holman 2010). The implemented algorithm is more accurate and orders of magnitude faster than previous algorithms, based on comparison with Monte Carlo simulations. Expanding this work, we have also developed semi-analytical methods for determining the frequency of exoplanet mutual events, i.e., the geometric probability two planets will transit each other (Planet-Planet Occultation) and the probability that this transit occurs simultaneously as they transit their star (Overlapping Double Transits; see Ragozzine & Holman 2010). The latter algorithm can also be applied to calculating the probability of observing transiting circumbinary planets (Doyle et al. 2011, Welsh et al. 2012). All of these algorithms have been coded in C and will be made publicly available. We will present and advertise these codes and illustrate their value for studying exoplanetary systems.

Stabilizing potentials in bound state analytic continuation methods for electronic resonances in polyatomic molecules

DOE PAGES

White, Alec F.; Head-Gordon, Martin; McCurdy, C. William

2017-01-30

The computation of Siegert energies by analytic continuation of bound state energies has recently been applied to shape resonances in polyatomic molecules by several authors. Here, we critically evaluate a recently proposed analytic continuation method based on low order (type III) Padé approximants as well as an analytic continuation method based on high order (type II) Padé approximants. We compare three classes of stabilizing potentials: Coulomb potentials, Gaussian potentials, and attenuated Coulomb potentials. These methods are applied to a model potential where the correct answer is known exactly and to the 2Π g shape resonance of N 2 - whichmore » has been studied extensively by other methods. Both the choice of stabilizing potential and method of analytic continuation prove to be important to the accuracy of the results. We then conclude that an attenuated Coulomb potential is the most effective of the three for bound state analytic continuation methods. With the proper potential, such methods show promise for algorithmic determination of the positions and widths of molecular shape resonances.« less

Stabilizing potentials in bound state analytic continuation methods for electronic resonances in polyatomic molecules

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

White, Alec F.; Head-Gordon, Martin; McCurdy, C. William

The computation of Siegert energies by analytic continuation of bound state energies has recently been applied to shape resonances in polyatomic molecules by several authors. Here, we critically evaluate a recently proposed analytic continuation method based on low order (type III) Padé approximants as well as an analytic continuation method based on high order (type II) Padé approximants. We compare three classes of stabilizing potentials: Coulomb potentials, Gaussian potentials, and attenuated Coulomb potentials. These methods are applied to a model potential where the correct answer is known exactly and to the 2Π g shape resonance of N 2 - whichmore » has been studied extensively by other methods. Both the choice of stabilizing potential and method of analytic continuation prove to be important to the accuracy of the results. We then conclude that an attenuated Coulomb potential is the most effective of the three for bound state analytic continuation methods. With the proper potential, such methods show promise for algorithmic determination of the positions and widths of molecular shape resonances.« less

A Lagrangian meshfree method applied to linear and nonlinear elasticity.

PubMed

Walker, Wade A

2017-01-01

The repeated replacement method (RRM) is a Lagrangian meshfree method which we have previously applied to the Euler equations for compressible fluid flow. In this paper we present new enhancements to RRM, and we apply the enhanced method to both linear and nonlinear elasticity. We compare the results of ten test problems to those of analytic solvers, to demonstrate that RRM can successfully simulate these elastic systems without many of the requirements of traditional numerical methods such as numerical derivatives, equation system solvers, or Riemann solvers. We also show the relationship between error and computational effort for RRM on these systems, and compare RRM to other methods to highlight its strengths and weaknesses. And to further explain the two elastic equations used in the paper, we demonstrate the mathematical procedure used to create Riemann and Sedov-Taylor solvers for them, and detail the numerical techniques needed to embody those solvers in code.

A Lagrangian meshfree method applied to linear and nonlinear elasticity

PubMed Central

2017-01-01

The repeated replacement method (RRM) is a Lagrangian meshfree method which we have previously applied to the Euler equations for compressible fluid flow. In this paper we present new enhancements to RRM, and we apply the enhanced method to both linear and nonlinear elasticity. We compare the results of ten test problems to those of analytic solvers, to demonstrate that RRM can successfully simulate these elastic systems without many of the requirements of traditional numerical methods such as numerical derivatives, equation system solvers, or Riemann solvers. We also show the relationship between error and computational effort for RRM on these systems, and compare RRM to other methods to highlight its strengths and weaknesses. And to further explain the two elastic equations used in the paper, we demonstrate the mathematical procedure used to create Riemann and Sedov-Taylor solvers for them, and detail the numerical techniques needed to embody those solvers in code. PMID:29045443

Method for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, Gregory C.; Barinaga, Charles J.; Koppenaal, David W.

1998-01-01

A method for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the method has the step of addition of a charge transfer gas to the carrier analyte combination that accepts charge from the carrier gas ions yet minimally accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the method as employed in various analytical instruments including an inductively coupled plasma mass spectrometer.

Method for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, G.C.; Barinaga, C.J.; Koppenaal, D.W.

1998-06-16

A method for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the method has the step of addition of a charge transfer gas to the carrier analyte combination that accepts charge from the carrier gas ions yet minimally accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the method as employed in various analytical instruments including an inductively coupled plasma mass spectrometer. 7 figs.

Temporal abstraction-based clinical phenotyping with Eureka!

PubMed

Post, Andrew R; Kurc, Tahsin; Willard, Richie; Rathod, Himanshu; Mansour, Michel; Pai, Akshatha Kalsanka; Torian, William M; Agravat, Sanjay; Sturm, Suzanne; Saltz, Joel H

2013-01-01

Temporal abstraction, a method for specifying and detecting temporal patterns in clinical databases, is very expressive and performs well, but it is difficult for clinical investigators and data analysts to understand. Such patterns are critical in phenotyping patients using their medical records in research and quality improvement. We have previously developed the Analytic Information Warehouse (AIW), which computes such phenotypes using temporal abstraction but requires software engineers to use. We have extended the AIW's web user interface, Eureka! Clinical Analytics, to support specifying phenotypes using an alternative model that we developed with clinical stakeholders. The software converts phenotypes from this model to that of temporal abstraction prior to data processing. The model can represent all phenotypes in a quality improvement project and a growing set of phenotypes in a multi-site research study. Phenotyping that is accessible to investigators and IT personnel may enable its broader adoption.

An analysis of an optimal selection process for characteristics and technical performance of baseball pitchers.

PubMed

Lin, Wen-Bin; Tung, I-Wu; Chen, Mei-Jung; Chen, Mei-Yen

2011-08-01

Selection of a qualified pitcher has relied previously on qualitative indices; here, both quantitative and qualitative indices including pitching statistics, defense, mental skills, experience, and managers' recognition were collected, and an analytic hierarchy process was used to rank baseball pitchers. The participants were 8 experts who ranked characteristics and statistics of 15 baseball pitchers who comprised the first round of potential representatives for the Chinese Taipei National Baseball team. The results indicated a selection rate that was 91% consistent with the official national team roster, as 11 pitchers with the highest scores who were recommended as optimal choices to be official members of the Chinese Tai-pei National Baseball team actually participated in the 2009 Baseball World Cup. An analytic hierarchy can aid in selection of qualified pitchers, depending on situational and practical needs; the method could be extended to other sports and team-selection situations.

A histogram-free multicanonical Monte Carlo algorithm for the construction of analytical density of states

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

Eisenbach, Markus; Li, Ying Wai

We report a new multicanonical Monte Carlo (MC) algorithm to obtain the density of states (DOS) for physical systems with continuous state variables in statistical mechanics. Our algorithm is able to obtain an analytical form for the DOS expressed in a chosen basis set, instead of a numerical array of finite resolution as in previous variants of this class of MC methods such as the multicanonical (MUCA) sampling and Wang-Landau (WL) sampling. This is enabled by storing the visited states directly in a data set and avoiding the explicit collection of a histogram. This practice also has the advantage ofmore » avoiding undesirable artificial errors caused by the discretization and binning of continuous state variables. Our results show that this scheme is capable of obtaining converged results with a much reduced number of Monte Carlo steps, leading to a significant speedup over existing algorithms.« less

Study of design and control of remote manipulators. Part 2: Vibration considerations in manipulator design

NASA Technical Reports Server (NTRS)

Book, W. J.

1973-01-01

An investigation is reported involving a mathematical procedure using 4 x 4 transformation matrices for analyzing the vibrations of flexible manipulators. Previous studies with the procedure are summarized and the method is extended to include flexible joints as well as links, and to account for the effects of various power transmission schemes. A systematic study of the allocation of structural material and the placement of components such as motors and gearboxes was undertaken using the analytical tools developed. As one step in this direction the variables which relate the vibration parameters of the arm to the task and environment of the arm were isolated and nondimensionalized. The 4 x 4 transformation matrices were also used to develop analytical expressions for the terms of the complete 6 x 6 compliance matrix for the case of two flexible links joined by a rotating joint, flexible about its axis of rotation.

Small-x asymptotics of the quark helicity distribution: Analytic results

DOE PAGES

Kovchegov, Yuri V.; Pitonyak, Daniel; Sievert, Matthew D.

2017-06-15

In this Letter, we analytically solve the evolution equations for the small-x asymptotic behavior of the (flavor singlet) quark helicity distribution in the large- N c limit. Here, these evolution equations form a set of coupled integro-differential equations, which previously could only be solved numerically. This approximate numerical solution, however, revealed simplifying properties of the small-x asymptotics, which we exploit here to obtain an analytic solution.

Method for Operating a Sensor to Differentiate Between Analytes in a Sample

DOEpatents

Kunt, Tekin; Cavicchi, Richard E; Semancik, Stephen; McAvoy, Thomas J

1998-07-28

Disclosed is a method for operating a sensor to differentiate between first and second analytes in a sample. The method comprises the steps of determining a input profile for the sensor which will enhance the difference in the output profiles of the sensor as between the first analyte and the second analyte; determining a first analyte output profile as observed when the input profile is applied to the sensor; determining a second analyte output profile as observed when the temperature profile is applied to the sensor; introducing the sensor to the sample while applying the temperature profile to the sensor, thereby obtaining a sample output profile; and evaluating the sample output profile as against the first and second analyte output profiles to thereby determine which of the analytes is present in the sample.

Angelica sinensis in China-A review of botanical profile, ethnopharmacology, phytochemistry and chemical analysis.

PubMed

Wei, Wen-Long; Zeng, Rui; Gu, Cai-Mei; Qu, Yan; Huang, Lin-Fang

2016-08-22

Angelica sinensis (Oliv.) Diels, known as Dang Gui (in Chinese), is a traditional medicinal and edible plant that has long been used for tonifying, replenishing, and invigorating blood as well as relieving pain, lubricating the intestines, and treating female irregular menstruation and amenorrhea. A. sinensis has also been used as a health product and become increasingly popular in China, Japan, and Korea. This paper aims to provide a systemic review of traditional uses of A. sinensis and its recent advances in the fields of phytochemistry, analytical methods and toxicology. In addition, possible trends, therapeutic potentials, and perspectives for future research of this plant are also briefly discussed. An extensive review of the literature was conducted, and electronic databases including China National Knowledge Infrastructure, PubMed, Google Scholar, Science Direct, and Reaxys were used to assemble the data. Ethnopharmacological literature and digitalised sources of academic libraries were also systematically searched. In addition, information was obtained from local books and The Plant List (TPL, www.theplantlist.org). This study reviews the progress in chemical analysis of A. sinensis and its preparations. Previously and newly established methods, including spectroscopy, thin-layer chromatography (TLC), gas chromatography (GC), high-performance liquid chromatography (HPLC), ultra-performance liquid chromatography(UPLC), and nuclear magnetic resonance analysis (NMR), are summarized. Moreover, identified bioactive components such as polysaccharides, ligustilide and ferulic acid were reviewed, along with analytical methods for quantitative and qualitative determination of target analytes, and fingerprinting authentication, quality evaluation of A. sinensis, and toxicology and pharmacodynamic studies. Scientific reports on crude extracts and pure compounds and formulations revealed a wide range of pharmacological activities, including anti-inflammatory activity, antifibrotic action, antispasmodic activity, antioxidant activities, and neuroprotective action, as well as cardio- and cerebrovascular effects. Within the published scientific literature are numerous reports regarding analytical methods that use various chromatographic and spectrophotometric technologies to monitor various types of components with different physicochemical properties simultaneously. This review discusses the reasonable selection of marker compounds based on high concentrations, analytical methods, and commercial availabilities with the goal of developing quick, accurate, and applicable analytical approaches for quality evaluation and establishing harmonised criteria for the analysis of A. sinensis and its finished products. Compounds isolated from A. sinensis are abundant sources of chemical diversity, from which we can discover active molecules. Thus, more studies on the pharmacological mechanisms of the predominant active compounds of A. sinensis are needed. In addition, given that A. sinensis is one of the most popular traditional herbal medicines, its main therapeutic aspects, toxicity, and adverse effects warrant further investigation in the future. Copyright © 2016. Published by Elsevier Ireland Ltd.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of selected carbamate pesticides in water by high-performance liquid chromatography

USGS Publications Warehouse

Werner, S.L.; Johnson, S.M.

1994-01-01

As part of its primary responsibility concerning water as a national resource, the U.S. Geological Survey collects and analyzes samples of ground water and surface water to determine water quality. This report describes the method used since June 1987 to determine selected total-recoverable carbamate pesticides present in water samples. High- performance liquid chromatography is used to separate N-methyl carbamates, N-methyl carbamoyloximes, and an N-phenyl carbamate which have been extracted from water and concentrated in dichloromethane. Analytes, surrogate compounds, and reference compounds are eluted from the analytical column within 25 minutes. Two modes of analyte detection are used: (1) a photodiode-array detector measures and records ultraviolet-absorbance profiles, and (2) a fluorescence detector measures and records fluorescence from an analyte derivative produced when analyte hydrolysis is combined with chemical derivatization. Analytes are identified and confirmed in a three-stage process by use of chromatographic retention time, ultraviolet (UV) spectral comparison, and derivatization/fluorescence detection. Quantitative results are based on the integration of single-wavelength UV-absorbance chromatograms and on comparison with calibration curves derived from external analyte standards that are run with samples as part of an instrumental analytical sequence. Estimated method detection limits vary for each analyte, depending on the sample matrix conditions, and range from 0.5 microgram per liter to as low as 0.01 microgram per liter. Reporting levels for all analytes have been set at 0.5 microgram per liter for this method. Corrections on the basis of percentage recoveries of analytes spiked into distilled water are not applied to values calculated for analyte concentration in samples. These values for analyte concentrations instead indicate the quantities recovered by the method from a particular sample matrix.

Evaluation of selected methods for determining streamflow during periods of ice effect

USGS Publications Warehouse

Melcher, N.B.; Walker, J.F.

1990-01-01

The methods are classified into two general categories, subjective and analytical, depending on whether individual judgement is necessary for method application. On the basis of results of the evaluation for the three Iowa stations, two of the subjective methods (discharge ratio and hydrographic-and-climatic comparison) were more accurate than the other subjective methods, and approximately as accurate as the best analytical method. Three of the analytical methods (index velocity, adjusted rating curve, and uniform flow) could potentially be used for streamflow-gaging stations where the need for accurate ice-affected discharge estimates justifies the expense of collecting additional field data. One analytical method (ice adjustment factor) may be appropriate for use for stations with extremely stable stage-discharge ratings and measuring sections. Further research is needed to refine the analytical methods. The discharge ratio and multiple regression methods produce estimates of streamflow for varying ice conditions using information obtained from the existing U.S. Geological Survey streamflow-gaging network.

Determination of free cortisol and free cortisone in human urine by on-line turbulent flow chromatography coupled to fused-core chromatography-tandem mass spectrometry (TFC-HPLC-MS/MS).

PubMed

Sánchez-Guijo, Alberto; Hartmann, Michaela F; Shi, Lijie; Remer, Thomas; Wudy, Stefan A

2014-01-01

Urinary free cortisol and urinary free cortisone are decisive markers for the diagnosis of syndromes related to the dysfunction of the adrenal gland or to evaluate certain enzymatic disorders. Here, we present a new method, designed for routine laboratory use, which enables quick determination of these analytes with minor sample workup. Turbulent flow chromatography shortens sample preparation, and connection to a fused-core particle-packed column (rugged amide-embedded C18 phase) permits a rapid and effective separation of the analytes, as well as additional separation from other related and isobaric compounds present in urine. Urinary isobaric compounds were successfully identified. The method requires only 100 μl of urine supernatant per sample. The total time between injections is 9.5 min. The solvents used for both turbulent and analytical chromatography are water and methanol, and the relatively low flows needed during the method resulted in an extended life of the columns. Linearity showed a R (2) > 0.994. Limit of detection and limit of quantification are 0.5 and 1.0 ng/ml for cortisone and 1.0 and 2.0 ng/ml for cortisol. Recoveries ranged from 99.7 to 109.1 % for cortisone and from 98.7 to 102.9 % for cortisol. Accuracy values (relative errors) for intra- and inter-assay experiments were always below 8 %, whereas precision (percent CV) ranged from 3.7 to 10.7 %. No matrix effects were detected during the validation process. The reproducibility for each analyte's retention time was excellent, with a coefficient of variation always below 0.2 %. The final validation step included the study of urine samples from healthy children and from children previously diagnosed with corticoidal disorders. The high selectivity achieved enables quick data handling.

PESTICIDE ANALYTICAL METHODS TO SUPPORT DUPLICATE-DIET HUMAN EXPOSURE MEASUREMENTS

EPA Science Inventory

Historically, analytical methods for determination of pesticides in foods have been developed in support of regulatory programs and are specific to food items or food groups. Most of the available methods have been developed, tested and validated for relatively few analytes an...

Validating Analytical Methods

ERIC Educational Resources Information Center

Ember, Lois R.

1977-01-01

The procedures utilized by the Association of Official Analytical Chemists (AOAC) to develop, evaluate, and validate analytical methods for the analysis of chemical pollutants are detailed. Methods validated by AOAC are used by the EPA and FDA in their enforcement programs and are granted preferential treatment by the courts. (BT)

Analytic Empirical Potentials for all Stable Isotopologues of the Ground X(^1Σ^+) State of ZnO from Purely Rotational Measurements

NASA Astrophysics Data System (ADS)

Dattani, Nikesh S.; Zack, Lindsay; Sun, Ming; Johnson, Erin R.; Le Roy, Robert; Ziurys, Lucy

2014-06-01

We report eight new ultra-high precision (±5 kHz) measurements of purely rotational N(1←0) transitions in several vibrational states of all stable isotopologues of the ground X(11Σ+) -state of ZnO. Combined with previous high-resolution (±50 kHz) measurements of purely rotational transitions between higher rotational states for the same system, we are able to build analytic potentials for 64Zn16O, 66Zn16O, 67Zn16O, 68Zn16O, and 70Zn16O, that are in full agreement with all known spectroscopic measurements of the system. Despite there being absolutely no vibrational information, our empirical potentials are able to determine the size of the vibrational spacings and the bond lengths, each with a precision of more than two orders of magnitude greater than the most precise empirical values previously known. We then use the XDM method to calculate values for the C6, C8, and C10 long-range constants for this molecule, and use these to accurately anchor the long-range regions of the potentials, where no measurements have yet been performed. In the region lying between the short-range measurements and the long-range theory on which our potentials are based, our final analytic global potentials are in very good agreement with state of the art ab initio potentials. L. N. Zack, R. L. Pulliam, L. M. Ziurys, J. Mol. Spec., 256, 186-191 (2009).

Interobserver Agreement on First-Stage Conversation Analytic Transcription

ERIC Educational Resources Information Center

Roberts, Felicia; Robinson, Jeffrey D.

2004-01-01

This investigation assesses interobserver agreement on conversation analytic (CA) transcription. Four professional CA transcribers spent a maximum of 3 hours transcribing 2.5 minutes of a previously unknown, naturally occurring, mundane telephone call. Researchers unitized transcripts into words, sounds, silences, inbreaths, outbreaths, and laugh…

Major advances in testing of dairy products: milk component and dairy product attribute testing.

PubMed

Barbano, D M; Lynch, J M

2006-04-01

Milk component analysis is relatively unusual in the field of quantitative analytical chemistry because an analytical test result determines the allocation of very large amounts of money between buyers and sellers of milk. Therefore, there is high incentive to develop and refine these methods to achieve a level of analytical performance rarely demanded of most methods or laboratory staff working in analytical chemistry. In the last 25 yr, well-defined statistical methods to characterize and validate analytical method performance combined with significant improvements in both the chemical and instrumental methods have allowed achievement of improved analytical performance for payment testing. A shift from marketing commodity dairy products to the development, manufacture, and marketing of value added dairy foods for specific market segments has created a need for instrumental and sensory approaches and quantitative data to support product development and marketing. Bringing together sensory data from quantitative descriptive analysis and analytical data from gas chromatography olfactometry for identification of odor-active compounds in complex natural dairy foods has enabled the sensory scientist and analytical chemist to work together to improve the consistency and quality of dairy food flavors.

Stiffness and Damping Coefficient Estimation of Compliant Surface Gas Bearings for Oil-Free Turbomachinery

NASA Technical Reports Server (NTRS)

DellaCorte, Christopher

2010-01-01

Foil gas bearings are a key technology in many commercial and emerging Oil-Free turbomachinery systems. These bearings are non-linear and have been difficult to analytically model in terms of performance characteristics such as load capacity, power loss, stiffness and damping. Previous investigations led to an empirically derived method, a rule-of-thumb, to estimate load capacity. This method has been a valuable tool in system development. The current paper extends this tool concept to include rules for stiffness and damping coefficient estimation. It is expected that these rules will further accelerate the development and deployment of advanced Oil-Free machines operating on foil gas bearings

Direct S -matrix calculation for diffractive structures and metasurfaces

NASA Astrophysics Data System (ADS)

Shcherbakov, Alexey A.; Stebunov, Yury V.; Baidin, Denis F.; Kämpfe, Thomas; Jourlin, Yves

2018-06-01

The paper presents a derivation of analytical components of S matrices for arbitrary planar diffractive structures and metasurfaces in the Fourier domain. The attained general formulas for S -matrix components can be applied within both formulations in the Cartesian and curvilinear metric. A numerical method based on these results can benefit from all previous improvements of the Fourier domain methods. In addition, we provide expressions for S -matrix calculation in the case of periodically corrugated layers of two-dimensional materials, which are valid for arbitrary corrugation depth-to-period ratios. As an example, the derived equations are used to simulate resonant grating excitation of graphene plasmons and the impact of a silica interlayer on corresponding reflection curves.

ADVANCEMENTS IN TIME-SPECTRA ANALYSIS METHODS FOR LEAD SLOWING-DOWN SPECTROSCOPY

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

Smith, Leon E.; Anderson, Kevin K.; Gesh, Christopher J.

2010-08-11

Direct measurement of Pu in spent nuclear fuel remains a key challenge for safeguarding nuclear fuel cycles of today and tomorrow. Lead slowing-down spectroscopy (LSDS) is an active nondestructive assay method that has the potential to provide independent, direct measurement of Pu and U isotopic mass with an uncertainty lower than the approximately 10 percent typical of today’s confirmatory assay methods. Pacific Northwest National Laboratory’s (PNNL) previous work to assess the viability of LSDS for the assay of pressurized water reactor (PWR) assemblies indicated that the method could provide direct assay of Pu-239 and U-235 (and possibly Pu-240 and Pu-241)more » with uncertainties less than a few percent, assuming suitably efficient instrumentation, an intense pulsed neutron source, and improvements in the time-spectra analysis methods used to extract isotopic information from a complex LSDS signal. This previous simulation-based evaluation used relatively simple PWR fuel assembly definitions (e.g. constant burnup across the assembly) and a constant initial enrichment and cooling time. The time-spectra analysis method was founded on a preliminary analytical model of self-shielding intended to correct for assay-signal nonlinearities introduced by attenuation of the interrogating neutron flux within the assembly.« less

Ultrasensitive analysis of lysergic acid diethylamide and its C-8 isomer in hair by capillary zone electrophoresis in combination with a stacking technique and laser induced fluorescence detection.

PubMed

Airado-Rodríguez, Diego; Cruces-Blanco, Carmen; García-Campaña, Ana M

2015-03-25

This article deals with the development and validation of a novel capillary zone electrophoresis (CZE) with laser induced fluorescence detection method for the analysis of lysergic acid diethylamide (LSD) and its isomer iso-LSD in hair samples. The separation of both analytes has been achieved in less than 13 min in a 72-cm effective length capillary with 75-μm internal diameter. As running buffer 25 mM citrate, pH 6.0 has been employed and separation temperature and voltage of 20 °C and 13 kV respectively, were applied. Field amplified sample injection (FASI) has been employed for on-line sample preconcentration, using ultrapure water containing 117 μM H3PO4 as optimum injection medium. Injection voltage and time have been optimized by means of experimental design, obtaining values of 7 kV and 15s, respectively. Methylergonovine has been employed as internal standard in order to compensate irreproducibility from electrokinetic injection. The analytical method has been applied to hair samples, previous extraction of the target analytes by ultrasound assisted solid-liquid extraction at 40 °C for 2.5 h, employing acetonitrile as extracting solvent. Linear responses were found for LSD and iso-LSD in matrix-matched calibrations from around 0.400 up to 50.0 pg mg(-1). LODs (3 S/N) in the order of 0.100 pg mg(-1) were calculated for both analytes, obtaining satisfactory recovery percentages for this kind of sample. Copyright © 2015 Elsevier B.V. All rights reserved.

Comprehensive analytical strategy for biomonitoring of pesticides in urine by liquid chromatography–orbitrap high resolution masss pectrometry.

PubMed

Roca, M; Leon, N; Pastor, A; Yusà, V

2014-12-29

In this study we propose an analytical strategy that combines a target approach for the quantitative analysis of contemporary pesticide metabolites with a comprehensive post-target screening for the identification of biomarkers of exposure to environmental contaminants in urine using liquid chromatography coupled to high-resolution mass spectrometry (LC–HRMS). The quantitative method for the target analysis of 29 urinary metabolites of organophosphate (OP) insecticides, synthetic pyrethroids, herbicides and fungicides was validated after a previous statistical optimization of the main factors governing the ion source ionization and a fragmentation study using the high energy collision dissociation (HCD) cell. The full scan accurate mass data were acquired with a resolving power of 50,000 FWHM (scan speed, 2 Hz), in both ESI+ and ESI− modes, and with and without HCD-fragmentation. The method – LOQ was lower than 3.2 μg L−1 for the majority of the analytes. For post-target screening a customized theoretical database was built, for the identification of 60 metabolites including pesticides, PAHs, phenols, and other metabolites of environmental pollutants. For identification purposes, accurate exact mass with less than 5 ppm, and diagnostic ions including isotopes and/or fragments were used. The analytical strategy was applied to 20 urine sample collected from children living in Valencia Region. Eleven target metabolites were detected with concentrations ranging from 1.18 to 131 μg L−1. Likewise, several compounds were tentatively identified in the post-target analysis belonging to the families of phthalates, phenols and parabenes. The proposed strategy is suitable for the determination of target pesticide biomarkers in urine in the framework of biomonitoring studies, and appropriate for the identification of other non-target metabolites.

Ochratoxin A in cocoa and chocolate sampled in Canada.

PubMed

Turcotte, A-M; Scott, P M

2011-06-01

In order to determine the levels of ochratoxin A (OTA) in cocoa and cocoa products available in Canada, a previously published analytical method, with minor modifications to the extraction and immunoaffinity clean-up and inclusion of an evaporation step, was initially used (Method I). To improve the low method recoveries (46-61%), 40% methanol was then included in the aqueous sodium bicarbonate extraction solvent (pH 7.8) (Method II). Clean-up was on an Ochratest™ immunoaffinity column and OTA was determined by liquid chromatography (LC) with fluorescence detection. Recoveries of OTA from spiked cocoa powder (0.5 and 5 ng g(-1)) were 75-84%; while recoveries from chocolate were 93-94%. The optimized method was sensitive (limit of quantification (LOQ) = 0.07-0.08 ng g(-1)), accurate (recovery = 75-94%) and precise (coefficient of variation (CV) < 5%). It is applicable to cocoa and chocolate. Analysis of 32 samples of cocoa powder (16 alkalized and 16 natural) for OTA showed an incidence of 100%, with concentrations ranging from 0.25 to 7.8 ng g(-1); in six samples the OTA level exceeded 2 ng g(-1), the previously considered European Union limit for cocoa. The frequency of detection of OTA in 28 chocolate samples (21 dark or baking chocolate and seven milk chocolate) was also 100% with concentrations ranging from 0.05 to 1.4 ng g(-1); one sample had a level higher than the previously considered European Union limit for chocolate (1 ng g(-1)).

Linear modeling of steady-state behavioral dynamics.

PubMed Central

Palya, William L; Walter, Donald; Kessel, Robert; Lucke, Robert

2002-01-01

The observed steady-state behavioral dynamics supported by unsignaled periods of reinforcement within repeating 2,000-s trials were modeled with a linear transfer function. These experiments employed improved schedule forms and analytical methods to improve the precision of the measured transfer function, compared to previous work. The refinements include both the use of multiple reinforcement periods that improve spectral coverage and averaging of independently determined transfer functions. A linear analysis was then used to predict behavior observed for three different test schedules. The fidelity of these predictions was determined. PMID:11831782

Spin bearing retainer design optimization

NASA Technical Reports Server (NTRS)

Boesiger, Edward A.; Warner, Mark H.

1991-01-01

The dynamics behavior of spin bearings for momentum wheels (control-moment gyroscope, reaction wheel assembly) is critical to satellite stability and life. Repeated bearing retainer instabilities hasten lubricant deterioration and can lead to premature bearing failure and/or unacceptable vibration. These instabilities are typically distinguished by increases in torque, temperature, audible noise, and vibration induced by increases into the bearing cartridge. Ball retainer design can be optimized to minimize these occurrences. A retainer was designed using a previously successful smaller retainer as an example. Analytical methods were then employed to predict its behavior and optimize its configuration.

Higher-Order Binding Corrections to the Lamb Shift

NASA Astrophysics Data System (ADS)

Pachucki, K.

1993-08-01

In this work a new analytical method for calculating the one-loop self-energy correction to the Lamb shift is presented in detail. The technique relies on division into the low and the high energy parts. The low energy part is calculated using the multipole expansion and the high energy part is calculated by expanding the Dirac-Coulomb propagator in powers of the Coulomb field. The obtained results are in agreement with those previously known, but are more accurate. A new theoretical value of the Lamb shift is also given.

77 FR 56176 - Analytical Methods Used in Periodic Reporting

Federal Register 2010, 2011, 2012, 2013, 2014

2012-09-12

... POSTAL REGULATORY COMMISSION 39 CFR Part 3001 [Docket No. RM2012-7; Order No. 1459] Analytical Methods Used in Periodic Reporting AGENCY: Postal Regulatory Commission. ACTION: Notice of proposed... analytical methods approved for use in periodic reporting.\\1\\ \\1\\ Petition of the United States Postal...

Introduction to Validation of Analytical Methods: Potentiometric Determination of CO[subscript 2

ERIC Educational Resources Information Center

Hipólito-Nájera, A. Ricardo; Moya-Hernandez, M. Rosario; Gomez-Balderas, Rodolfo; Rojas-Hernandez, Alberto; Romero-Romo, Mario

2017-01-01

Validation of analytical methods is a fundamental subject for chemical analysts working in chemical industries. These methods are also relevant for pharmaceutical enterprises, biotechnology firms, analytical service laboratories, government departments, and regulatory agencies. Therefore, for undergraduate students enrolled in majors in the field…

Analytical Energy Gradients for Excited-State Coupled-Cluster Methods

NASA Astrophysics Data System (ADS)

Wladyslawski, Mark; Nooijen, Marcel

The equation-of-motion coupled-cluster (EOM-CC) and similarity transformed equation-of-motion coupled-cluster (STEOM-CC) methods have been firmly established as accurate and routinely applicable extensions of single-reference coupled-cluster theory to describe electronically excited states. An overview of these methods is provided, with emphasis on the many-body similarity transform concept that is the key to a rationalization of their accuracy. The main topic of the paper is the derivation of analytical energy gradients for such non-variational electronic structure approaches, with an ultimate focus on obtaining their detailed algebraic working equations. A general theoretical framework using Lagrange's method of undetermined multipliers is presented, and the method is applied to formulate the EOM-CC and STEOM-CC gradients in abstract operator terms, following the previous work in [P.G. Szalay, Int. J. Quantum Chem. 55 (1995) 151] and [S.R. Gwaltney, R.J. Bartlett, M. Nooijen, J. Chem. Phys. 111 (1999) 58]. Moreover, the systematics of the Lagrange multiplier approach is suitable for automation by computer, enabling the derivation of the detailed derivative equations through a standardized and direct procedure. To this end, we have developed the SMART (Symbolic Manipulation and Regrouping of Tensors) package of automated symbolic algebra routines, written in the Mathematica programming language. The SMART toolkit provides the means to expand, differentiate, and simplify equations by manipulation of the detailed algebraic tensor expressions directly. The Lagrangian multiplier formulation establishes a uniform strategy to perform the automated derivation in a standardized manner: A Lagrange multiplier functional is constructed from the explicit algebraic equations that define the energy in the electronic method; the energy functional is then made fully variational with respect to all of its parameters, and the symbolic differentiations directly yield the explicit equations for the wavefunction amplitudes, the Lagrange multipliers, and the analytical gradient via the perturbation-independent generalized Hellmann-Feynman effective density matrix. This systematic automated derivation procedure is applied to obtain the detailed gradient equations for the excitation energy (EE-), double ionization potential (DIP-), and double electron affinity (DEA-) similarity transformed equation-of-motion coupled-cluster singles-and-doubles (STEOM-CCSD) methods. In addition, the derivatives of the closed-shell-reference excitation energy (EE-), ionization potential (IP-), and electron affinity (EA-) equation-of-motion coupled-cluster singles-and-doubles (EOM-CCSD) methods are derived. Furthermore, the perturbative EOM-PT and STEOM-PT gradients are obtained. The algebraic derivative expressions for these dozen methods are all derived here uniformly through the automated Lagrange multiplier process and are expressed compactly in a chain-rule/intermediate-density formulation, which facilitates a unified modular implementation of analytic energy gradients for CCSD/PT-based electronic methods. The working equations for these analytical gradients are presented in full detail, and their factorization and implementation into an efficient computer code are discussed.

External Standards or Standard Addition? Selecting and Validating a Method of Standardization

NASA Astrophysics Data System (ADS)

Harvey, David T.

2002-05-01

A common feature of many problem-based laboratories in analytical chemistry is a lengthy independent project involving the analysis of "real-world" samples. Students research the literature, adapting and developing a method suitable for their analyte, sample matrix, and problem scenario. Because these projects encompass the complete analytical process, students must consider issues such as obtaining a representative sample, selecting a method of analysis, developing a suitable standardization, validating results, and implementing appropriate quality assessment/quality control practices. Most textbooks and monographs suitable for an undergraduate course in analytical chemistry, however, provide only limited coverage of these important topics. The need for short laboratory experiments emphasizing important facets of method development, such as selecting a method of standardization, is evident. The experiment reported here, which is suitable for an introductory course in analytical chemistry, illustrates the importance of matrix effects when selecting a method of standardization. Students also learn how a spike recovery is used to validate an analytical method, and obtain a practical experience in the difference between performing an external standardization and a standard addition.

Extensions to decision curve analysis, a novel method for evaluating diagnostic tests, prediction models and molecular markers

PubMed Central

Vickers, Andrew J; Cronin, Angel M; Elkin, Elena B; Gonen, Mithat

2008-01-01

Background Decision curve analysis is a novel method for evaluating diagnostic tests, prediction models and molecular markers. It combines the mathematical simplicity of accuracy measures, such as sensitivity and specificity, with the clinical applicability of decision analytic approaches. Most critically, decision curve analysis can be applied directly to a data set, and does not require the sort of external data on costs, benefits and preferences typically required by traditional decision analytic techniques. Methods In this paper we present several extensions to decision curve analysis including correction for overfit, confidence intervals, application to censored data (including competing risk) and calculation of decision curves directly from predicted probabilities. All of these extensions are based on straightforward methods that have previously been described in the literature for application to analogous statistical techniques. Results Simulation studies showed that repeated 10-fold crossvalidation provided the best method for correcting a decision curve for overfit. The method for applying decision curves to censored data had little bias and coverage was excellent; for competing risk, decision curves were appropriately affected by the incidence of the competing risk and the association between the competing risk and the predictor of interest. Calculation of decision curves directly from predicted probabilities led to a smoothing of the decision curve. Conclusion Decision curve analysis can be easily extended to many of the applications common to performance measures for prediction models. Software to implement decision curve analysis is provided. PMID:19036144

Internal wave energy flux from density perturbations in nonlinear stratifications

NASA Astrophysics Data System (ADS)

Lee, Frank M.; Allshouse, Michael R.; Swinney, Harry L.; Morrison, P. J.

2017-11-01

Tidal flow over the topography at the bottom of the ocean, whose density varies with depth, generates internal gravity waves that have a significant impact on the energy budget of the ocean. Thus, understanding the energy flux (J = p v) is important, but it is difficult to measure simultaneously the pressure and velocity perturbation fields, p and v . In a previous work, a Green's-function-based method was developed to calculate the instantaneous p, v , and thus J , given a density perturbation field for a constant buoyancy frequency N. Here we extend the previous analytic Green's function work to include nonuniform N profiles, namely the tanh-shaped and linear cases, because background density stratifications that occur in the ocean and some experiments are nonlinear. In addition, we present a finite-difference method for the general case where N has an arbitrary profile. Each method is validated against numerical simulations. The methods we present can be applied to measured density perturbation data by using our MATLAB graphical user interface EnergyFlux. PJM was supported by the U.S. Department of Energy Contract DE-FG05-80ET-53088. HLS and MRA were supported by ONR Grant No. N000141110701.

An improved method for estimating capillary pressure from 3D microtomography images and its application to the study of disconnected nonwetting phase

NASA Astrophysics Data System (ADS)

Li, Tianyi; Schlüter, Steffen; Dragila, Maria Ines; Wildenschild, Dorthe

2018-04-01

We present an improved method for estimating interfacial curvatures from x-ray computed microtomography (CMT) data that significantly advances the potential for this tool to unravel the mechanisms and phenomena associated with multi-phase fluid motion in porous media. CMT data, used to analyze the spatial distribution and capillary pressure-saturation (Pc-S) relationships of liquid phases, requires accurate estimates of interfacial curvature. Our improved method for curvature estimation combines selective interface modification and distance weighting approaches. It was verified against synthetic (analytical computer-generated) and real image data sets, demonstrating a vast improvement over previous methods. Using this new tool on a previously published data set (multiphase flow) yielded important new insights regarding the pressure state of the disconnected nonwetting phase during drainage and imbibition. The trapped and disconnected non-wetting phase delimits its own hysteretic Pc-S curve that inhabits the space within the main hysteretic Pc-S loop of the connected wetting phase. Data suggests that the pressure of the disconnected, non-wetting phase is strongly modified by the pore geometry rather than solely by the bulk liquid phase that surrounds it.

Rapid quantification of imidazolium-based ionic liquids by hydrophilic interaction liquid chromatography: Methodology and an investigation of the retention mechanisms.

PubMed

Hawkins, Cory A; Rud, Anna; Guthrie, Margaret L; Dietz, Mark L

2015-06-26

The separation of nine N,N'-dialkylimidazolium-based ionic liquids (ILs) by an isocratic hydrophilic interaction high-performance liquid chromatographic method using an unmodified silica column was investigated. The chosen analytical conditions using a 90:10 acetonitrile-ammonium formate buffer mobile phase on a high-purity, unmodified silica column were found to be efficient, robust, and sensitive for the determination of ILs in a variety of solutions. The retention window (k' = 2-11) was narrower than that of previous methods, resulting in a 7-min runtime for the nine IL homologues. The lower limit of quantification of the method, 2-3 μmol L(-1), was significantly lower than those reported previously for HPLC-UV methods. The effects of systematically modifying the IL cation alkyl chain length, column temperature, and mobile-phase water and buffer content on solute retention were examined. Cation exchange was identified as the dominant retention mechanism for most of the solutes, with a distinct (single methylene group) transition to a dominant partitioning mode at the highest solute polarity. Copyright © 2015 Elsevier B.V. All rights reserved.

Applying Nyquist's method for stability determination to solar wind observations

NASA Astrophysics Data System (ADS)

Klein, Kristopher G.; Kasper, Justin C.; Korreck, K. E.; Stevens, Michael L.

2017-10-01

The role instabilities play in governing the evolution of solar and astrophysical plasmas is a matter of considerable scientific interest. The large number of sources of free energy accessible to such nearly collisionless plasmas makes general modeling of unstable behavior, accounting for the temperatures, densities, anisotropies, and relative drifts of a large number of populations, analytically difficult. We therefore seek a general method of stability determination that may be automated for future analysis of solar wind observations. This work describes an efficient application of the Nyquist instability method to the Vlasov dispersion relation appropriate for hot, collisionless, magnetized plasmas, including the solar wind. The algorithm recovers the familiar proton temperature anisotropy instabilities, as well as instabilities that had been previously identified using fits extracted from in situ observations in Gary et al. (2016). Future proposed applications of this method are discussed.

Analytical method for establishing indentation rolling resistance

NASA Astrophysics Data System (ADS)

Gładysiewicz, Lech; Konieczna, Martyna

2018-01-01

Belt conveyors are highly reliable machines able to work in special operating conditions. Harsh environment, long distance of transporting and great mass of transported martials are cause of high energy usage. That is why research in the field of belt conveyor transportation nowadays focuses on reducing the power consumption without lowering their efficiency. In this paper, previous methods for testing rolling resistance are described, and new method designed by authors was presented. New method of testing rolling resistance is quite simple and inexpensive. Moreover it allows to conduct the experimental tests of the impact of different parameters on the value of indentation rolling resistance such as core design, cover thickness, ambient temperature, idler travel frequency, or load value as well. Finally results of tests of relationship between rolling resistance and idler travel frequency and between rolling resistance and idler travel speed was presented.

No Impact of the Analytical Method Used for Determining Cystatin C on Estimating Glomerular Filtration Rate in Children.

PubMed

Alberer, Martin; Hoefele, Julia; Benz, Marcus R; Bökenkamp, Arend; Weber, Lutz T

2017-01-01

Measurement of inulin clearance is considered to be the gold standard for determining kidney function in children, but this method is time consuming and expensive. The glomerular filtration rate (GFR) is on the other hand easier to calculate by using various creatinine- and/or cystatin C (Cys C)-based formulas. However, for the determination of serum creatinine (Scr) and Cys C, different and non-interchangeable analytical methods exist. Given the fact that different analytical methods for the determination of creatinine and Cys C were used in order to validate existing GFR formulas, clinicians should be aware of the type used in their local laboratory. In this study, we compared GFR results calculated on the basis of different GFR formulas and either used Scr and Cys C values as determined by the analytical method originally employed for validation or values obtained by an alternative analytical method to evaluate any possible effects on the performance. Cys C values determined by means of an immunoturbidimetric assay were used for calculating the GFR using equations in which this analytical method had originally been used for validation. Additionally, these same values were then used in other GFR formulas that had originally been validated using a nephelometric immunoassay for determining Cys C. The effect of using either the compatible or the possibly incompatible analytical method for determining Cys C in the calculation of GFR was assessed in comparison with the GFR measured by creatinine clearance (CrCl). Unexpectedly, using GFR equations that employed Cys C values derived from a possibly incompatible analytical method did not result in a significant difference concerning the classification of patients as having normal or reduced GFR compared to the classification obtained on the basis of CrCl. Sensitivity and specificity were adequate. On the other hand, formulas using Cys C values derived from a compatible analytical method partly showed insufficient performance when compared to CrCl. Although clinicians should be aware of applying a GFR formula that is compatible with the locally used analytical method for determining Cys C and creatinine, other factors might be more crucial for the calculation of correct GFR values.

Review of Research Reporting Guidelines for Radiology Researchers.

PubMed

Cronin, Paul; Rawson, James V

2016-05-01

Prior articles have reviewed reporting guidelines and study evaluation tools for clinical research. However, only some of the many available accepted reporting guidelines at the Enhancing the QUAlity and Transparency Of health Research Network have been discussed in previous reports. In this paper, we review the key Enhancing the QUAlity and Transparency Of health Research reporting guidelines that have not been previously discussed. The study types include diagnostic and prognostic studies, reliability and agreement studies, observational studies, analytical and descriptive, experimental studies, quality improvement studies, qualitative research, health informatics, systematic reviews and meta-analyses, economic evaluations, and mixed methods studies. There are also sections on study protocols, and statistical analyses and methods. In each section, there is a brief overview of the study type, and then the reporting guideline(s) that are most applicable to radiology researchers including radiologists involved in health services research are discussed. Copyright © 2016 The Association of University Radiologists. Published by Elsevier Inc. All rights reserved.

Counteracting moment device for reduction of earthquake-induced excursions of multi-level buildings.

PubMed

Nagaya, K; Fukushima, T; Kosugi, Y

1999-05-01

A vibration-control mechanism for beams and columns was presented in our previous report in which the earthquake force was transformed into a vibration-control force by using a gear train mechanism. In our previous report, however, only the principle of transforming the earthquake force into the control force was presented; the discussion for real structures and the design method were not presented. The present article provides a theoretical analysis of the column which is used in multi-layered buildings. Experimental tests were carried out for a model of multi-layered buildings in the frequency range of a principal earthquake wave. Theoretical results are compared to the experimental data. The optimal design of the control mechanism, which is of importance in the column design, is presented. Numerical calculations are carried out for the optimal design. It is shown that vibrations of the column involving the mechanism are suppressed remarkably. The optimal design method and the analytical results are applicable to the design of the column.

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

Xia, T. Y.; Zhang, Y.

We present an analytical calculation of the spectra of CMB anisotropies and polarizations generated by relic gravitational waves (RGWs). As a substantial extension to the previous studies, three new ingredients are included in this work. First, the analytic C{sub l}{sup TT} and C{sub l}{sup TE} are given; especially the latter can be useful to extract signal of RGWs from the observed data in the zero-multipole method. Second, a fitting formula of the decaying factor on small scales is given, coming from the visibility function around the photon decoupling. Third, the impacts by the neutrino free-streaming (NFS) is examined, a processmore » that occurred in the early universe and leaves observable imprints on CMB via RGWs. It is found that the analytic C{sub l}{sup TT} and C{sub l}{sup TE} have profiles agreeing with the numeric ones, except that C{sub l}{sup TT} in a range l{<=}10 and the first trough of C{sub l}{sup TE} around l{approx}75 have some deviations. With the new damping factor, the analytic C{sub l}{sup EE} and C{sub l}{sup BB} match with the numeric ones with the maximum errors only {approx}3% up to the first three peaks for l{<=}600, improving the previous studies substantially. The correspondence of the positions of peaks of C{sub l}{sup XX} and those of RGWs are also demonstrated explicitly. We also find that NFS reduces the amplitudes of C{sub l}{sup XX} by (20%{approx}35%) for l{approx_equal}(100{approx}600) and shifts slightly their peaks to smaller angles. Detailed analyses show that the zero multipoles l{sub 0}, where C{sub l}{sup TE} crosses 0, are shifted to larger values by NFS. This shifting effect is as important as those caused by different inflation models and different baryon fractions.« less

Change in Minimum Orbit Intersection Distance due to General Relativistic Precession in Small Solar System Bodies

NASA Astrophysics Data System (ADS)

Sekhar, Aswin; Valsecchi, Giovanni B.; Asher, David; Werner, Stephanie; Vaubaillon, Jeremie; Li, Gongjie

2017-06-01

One of the greatest successes of Einstein's General Theory of Relativity (GR) was the correct prediction of the perihelion precession of Mercury. The closed form expression to compute this precession tells us that substantial GR precession would occur only if the bodies have a combination of both moderately small perihelion distance and semi-major axis. Minimum Orbit Intersection Distance (MOID) is a quantity which helps us to understand the closest proximity of two orbits in space. Hence evaluating MOID is crucial to understand close encounters and collision scenarios better. In this work, we look at the possible scenarios where a small GR precession in argument of pericentre can create substantial changes in MOID for small bodies ranging from meteoroids to comets and asteroids.Previous works have looked into neat analytical techniques to understand different collision scenarios and we use those standard expressions to compute MOID analytically. We find the nature of this mathematical function is such that a relatively small GR precession can lead to drastic changes in MOID values depending on the initial value of argument of pericentre. Numerical integrations were done with the MERCURY package incorporating GR code to test the same effects. A numerical approach showed the same interesting relationship (as shown by analytical theory) between values of argument of pericentre and the peaks or dips in MOID values. There is an overall agreement between both analytical and numerical methods.We find that GR precession could play an important role in the calculations pertaining to MOID and close encounter scenarios in the case of certain small solar system bodies (depending on their initial orbital elements) when long term impact risk possibilities are considered. Previous works have looked into impact probabilities and collision scenarios on planets from different small body populations. This work aims to find certain sub-sets of small bodies where GR could play an interesting role. Certain parallels are drawn between the cases of asteroids, comets and small perihelion distance meteoroid streams.

Optimal clinical trial design based on a dichotomous Markov-chain mixed-effect sleep model.

PubMed

Steven Ernest, C; Nyberg, Joakim; Karlsson, Mats O; Hooker, Andrew C

2014-12-01

D-optimal designs for discrete-type responses have been derived using generalized linear mixed models, simulation based methods and analytical approximations for computing the fisher information matrix (FIM) of non-linear mixed effect models with homogeneous probabilities over time. In this work, D-optimal designs using an analytical approximation of the FIM for a dichotomous, non-homogeneous, Markov-chain phase advanced sleep non-linear mixed effect model was investigated. The non-linear mixed effect model consisted of transition probabilities of dichotomous sleep data estimated as logistic functions using piecewise linear functions. Theoretical linear and nonlinear dose effects were added to the transition probabilities to modify the probability of being in either sleep stage. D-optimal designs were computed by determining an analytical approximation the FIM for each Markov component (one where the previous state was awake and another where the previous state was asleep). Each Markov component FIM was weighted either equally or by the average probability of response being awake or asleep over the night and summed to derive the total FIM (FIM(total)). The reference designs were placebo, 0.1, 1-, 6-, 10- and 20-mg dosing for a 2- to 6-way crossover study in six dosing groups. Optimized design variables were dose and number of subjects in each dose group. The designs were validated using stochastic simulation/re-estimation (SSE). Contrary to expectations, the predicted parameter uncertainty obtained via FIM(total) was larger than the uncertainty in parameter estimates computed by SSE. Nevertheless, the D-optimal designs decreased the uncertainty of parameter estimates relative to the reference designs. Additionally, the improvement for the D-optimal designs were more pronounced using SSE than predicted via FIM(total). Through the use of an approximate analytic solution and weighting schemes, the FIM(total) for a non-homogeneous, dichotomous Markov-chain phase advanced sleep model was computed and provided more efficient trial designs and increased nonlinear mixed-effects modeling parameter precision.

Surrogate matrix and surrogate analyte approaches for definitive quantitation of endogenous biomolecules.

PubMed

Jones, Barry R; Schultz, Gary A; Eckstein, James A; Ackermann, Bradley L

2012-10-01

Quantitation of biomarkers by LC-MS/MS is complicated by the presence of endogenous analytes. This challenge is most commonly overcome by calibration using an authentic standard spiked into a surrogate matrix devoid of the target analyte. A second approach involves use of a stable-isotope-labeled standard as a surrogate analyte to allow calibration in the actual biological matrix. For both methods, parallelism between calibration standards and the target analyte in biological matrix must be demonstrated in order to ensure accurate quantitation. In this communication, the surrogate matrix and surrogate analyte approaches are compared for the analysis of five amino acids in human plasma: alanine, valine, methionine, leucine and isoleucine. In addition, methodology based on standard addition is introduced, which enables a robust examination of parallelism in both surrogate analyte and surrogate matrix methods prior to formal validation. Results from additional assays are presented to introduce the standard-addition methodology and to highlight the strengths and weaknesses of each approach. For the analysis of amino acids in human plasma, comparable precision and accuracy were obtained by the surrogate matrix and surrogate analyte methods. Both assays were well within tolerances prescribed by regulatory guidance for validation of xenobiotic assays. When stable-isotope-labeled standards are readily available, the surrogate analyte approach allows for facile method development. By comparison, the surrogate matrix method requires greater up-front method development; however, this deficit is offset by the long-term advantage of simplified sample analysis.

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

Wiedenman, B. J.; White, T. L.; Mahannah, R. N.

Ion Chromatography (IC) is the principal analytical method used to support studies of Sludge Reciept and Adjustment Tank (SRAT) chemistry at DWPF. A series of prior analytical ''Round Robin'' (RR) studies included both supernate and sludge samples from SRAT simulant, previously reported as memos, are tabulated in this report.2,3 From these studies it was determined to standardize IC column size to 4 mm diameter, eliminating the capillary column from use. As a follow on test, the DWPF laboratory, the PSAL laboratory, and the AD laboratory participated in the current analytical RR to determine a suite of anions in SRAT simulantmore » by IC, results also are tabulated in this report. The particular goal was to confirm the laboratories ability to measure and quantitate glycolate ion. The target was + or - 20% inter-lab agreement of the analyte averages for the RR. Each of the three laboratories analyzed a batch of 12 samples. For each laboratory, the percent relative standard deviation (%RSD) of the averages on nitrate, glycolate, and oxalate, was 10% or less. The three laboratories all met the goal of 20% relative agreement for nitrate and glycolate. For oxalate, the PSAL laboratory reported an average value that was 20% higher than the average values reported by the DWPF laboratory and the AD laboratory. Because of this wider window of agreement, it was concluded to continue the practice of an additional acid digestion for total oxalate measurement. It should also be noted that large amounts of glycolate in the SRAT samples will have an impact on detection limits of near eluting peaks, namely Fluoride and Formate. A suite of scoping experiments are presented in the report to identify and isolate other potential interlaboratory disceprancies. Specific ion chromatography inter-laboratory method conditions and differences are tabulated. Most differences were minor but there are some temperature control equipment differences that are significant leading to a recommendation of a heated jacket for analytical columns that are remoted for use in radiohoods. A suggested method improvement would be to implement column temperture control at a temperature slightly above ambient to avoid peak shifting due to temperature fluctuations. Temperature control in this manner would improve short and longer term peak retention time stability. An unknown peak was observed during the analysis of glycolic acid and SRAT simulant. The unknown peak was determined to best match diglycolic acid. The development of a method for acetate is summaraized, and no significant amount of acetate was observed in the SRAT products tested. In addition, an alternative Gas Chromatograph (GC) method for glycolate is summarized.« less

Effect-Based Screening Methods for Water Quality Characterization Will Augment Conventional Analyte-by-Analyte Chemical Methods in Research As Well As Regulatory Monitoring

EPA Science Inventory

Conventional approaches to water quality characterization can provide data on individual chemical components of each water sample. This analyte-by-analyte approach currently serves many useful research and compliance monitoring needs. However these approaches, which require a ...

Fourier Collocation Approach With Mesh Refinement Method for Simulating Transit-Time Ultrasonic Flowmeters Under Multiphase Flow Conditions.

PubMed

Simurda, Matej; Duggen, Lars; Basse, Nils T; Lassen, Benny

2018-02-01

A numerical model for transit-time ultrasonic flowmeters operating under multiphase flow conditions previously presented by us is extended by mesh refinement and grid point redistribution. The method solves modified first-order stress-velocity equations of elastodynamics with additional terms to account for the effect of the background flow. Spatial derivatives are calculated by a Fourier collocation scheme allowing the use of the fast Fourier transform, while the time integration is realized by the explicit third-order Runge-Kutta finite-difference scheme. The method is compared against analytical solutions and experimental measurements to verify the benefit of using mapped grids. Additionally, a study of clamp-on and in-line ultrasonic flowmeters operating under multiphase flow conditions is carried out.

Advances in explosives analysis—part II: photon and neutron methods

DOE PAGES

Brown, Kathryn E.; Greenfield, Margo T.; McGrane, Shawn D.; ...

2015-10-07

The number and capability of explosives detection and analysis methods have increased dramatically since publication of the Analytical and Bioanalytical Chemistry special issue devoted to Explosives Analysis [Moore DS, Goodpaster JV, Anal Bioanal Chem 395:245–246, 2009]. Here we review and critically evaluate the latest (the past five years) important advances in explosives detection, with details of the improvements over previous methods, and suggest possible avenues towards further advances in, e.g., stand-off distance, detection limit, selectivity, and penetration through camouflage or packaging. Our review consists of two parts. Part I discussed methods based on animals, chemicals (including colorimetry, molecularly imprinted polymers,more » electrochemistry, and immunochemistry), ions (both ion-mobility spectrometry and mass spectrometry), and mechanical devices. In Part II, we review methods based on photons, from very energetic photons including X-rays and gamma rays down to the terahertz range, and neutrons.« less

Use of Foodomics for Control of Food Processing and Assessing of Food Safety.

PubMed

Josić, D; Peršurić, Ž; Rešetar, D; Martinović, T; Saftić, L; Kraljević Pavelić, S

Food chain, food safety, and food-processing sectors face new challenges due to globalization of food chain and changes in the modern consumer preferences. In addition, gradually increasing microbial resistance, changes in climate, and human errors in food handling remain a pending barrier for the efficient global food safety management. Consequently, a need for development, validation, and implementation of rapid, sensitive, and accurate methods for assessment of food safety often termed as foodomics methods is required. Even though, the growing role of these high-throughput foodomic methods based on genomic, transcriptomic, proteomic, and metabolomic techniques has yet to be completely acknowledged by the regulatory agencies and bodies. The sensitivity and accuracy of these methods are superior to previously used standard analytical procedures and new methods are suitable to address a number of novel requirements posed by the food production sector and global food market. © 2017 Elsevier Inc. All rights reserved.

Advances in explosives analysis—part I. animal, chemical, ion, and mechanical methods

DOE PAGES

Brown, Kathryn E.; Greenfield, Margo T.; McGrane, Shawn D.; ...

2015-10-13

The number and capability of explosives detection and analysis methods have increased substantially since the publication of the Analytical and Bioanalytical Chemistry special issue devoted to Explosives Analysis (Moore and Goodpaster, Anal Bioanal Chem 395(2):245–246, 2009). We review and critically evaluate the latest (the past five years) important advances in explosives detection, with details of the improvements over previous methods, and suggest possible avenues towards further advances in, e.g., stand-off distance, detection limit, selectivity, and penetration through camouflage or packaging. The review consists of two parts. Moreover, Part I, reviews methods based on animals, chemicals (including colorimetry, molecularly imprinted polymers,more » electrochemistry, and immunochemistry), ions (both ion-mobility spectrometry and mass spectrometry), and mechanical devices. Part II will review methods based on photons, from very energetic photons including X-rays and gamma rays down to the terahertz range, and neutrons.« less

Method of multiplexed analysis using ion mobility spectrometer

DOEpatents

Belov, Mikhail E [Richland, WA; Smith, Richard D [Richland, WA

2009-06-02

A method for analyzing analytes from a sample introduced into a Spectrometer by generating a pseudo random sequence of a modulation bins, organizing each modulation bin as a series of submodulation bins, thereby forming an extended pseudo random sequence of submodulation bins, releasing the analytes in a series of analyte packets into a Spectrometer, thereby generating an unknown original ion signal vector, detecting the analytes at a detector, and characterizing the sample using the plurality of analyte signal subvectors. The method is advantageously applied to an Ion Mobility Spectrometer, and an Ion Mobility Spectrometer interfaced with a Time of Flight Mass Spectrometer.

The importance of quality control in validating concentrations ...

EPA Pesticide Factsheets

A national-scale survey of 247 contaminants of emerging concern (CECs), including organic and inorganic chemical compounds, and microbial contaminants, was conducted in source and treated drinking water samples from 25 treatment plants across the United States. Multiple methods were used to determine these CECs, including six analytical methods to measure 174 pharmaceuticals, personal care products, and pesticides. A three-component quality assurance/quality control (QA/QC) program was designed for the subset of 174 CECs which allowed us to assess and compare performances of the methods used. The three components included: 1) a common field QA/QC protocol and sample design, 2) individual investigator-developed method-specific QA/QC protocols, and 3) a suite of 46 method comparison analytes that were determined in two or more analytical methods. Overall method performance for the 174 organic chemical CECs was assessed by comparing spiked recoveries in reagent, source, and treated water over a two-year period. In addition to the 247 CECs reported in the larger drinking water study, another 48 pharmaceutical compounds measured did not consistently meet predetermined quality standards. Methodologies that did not seem suitable for these analytes are overviewed. The need to exclude analytes based on method performance demonstrates the importance of additional QA/QC protocols. This paper compares the method performance of six analytical methods used to measure 174 emer

Qualitative and quantitative measurement of cannabinoids in cannabis using modified HPLC/DAD method.

PubMed

Patel, Bhupendra; Wene, Daniel; Fan, Zhihua Tina

2017-11-30

This study presents an accurate and high throughput method for the quantitative determination of various cannabinoids in cannabis plant material using high pressure liquid chromatography (HPLC) with a diode array detector (DAD). Sample extraction and chromatographic analysis conditions for the measurement of cannabinoids in the complex cannabis plant material matrix were optimized. The Agilent Poroshell 120 SB-C18 column provided high resolution for all target analytes with a short run time (10minutes) given the core shell technology. The aqueous buffer mobile phase was optimized with ammonium acetate at pH 4.75. The change in the mobile phase and the new column ensured a separation between cannabidiol (CBD and cannabigerol (CBG) along with cannabigerol and tetrahydrocannabinolic acid (THCA), which were not well separated by previous publications, improved buffering capacity, and provided analytical performance stability. Moreover, baseline drifting was significantly minimized by the use of a low concentration buffer solution (25mM ammonium acetate). In addition, evaporation and reconstitution of the sample residue with a methanol-organic pure (OP) water solution (65:35) significantly reduced the matrix interference. The modified extraction produced good recoveries (>91%) for each of the eight cannabinoids. The optimized method was validated for specificity, linearity, sensitivity, precision, accuracy, and stability. The combined relative standard deviation (%RSD) for intra-day and inter-day precision for all eight analytes varied from 2.5% to 5.2% and 0.28% to 5.5%, respectively. The %RSD for the repeatability study varied from 1.1% to 5.5%. The recoveries from spiked cannabis matrix samples were greater than 90% for all analytes, except delta-8-tetrahydrocannabinol (Δ 8 -THC), which was 80%. The recoveries varied from 81% to 107% with a precision of 0.7-8.1%RSD. Delta-9-tetrahydrocannabinol (Δ 9 -THC) in all of the cannabis samples (n=635) was less than 10%, which is in compliance with the NJ Medicinal Marijuana regulation. Analysis of samples from two cultivars, which included ten individual samples, four composite samples, seven calibration standards, and four quality control standards, can be performed within 24hours by this high throughput method. Published by Elsevier B.V.

Co-occurring substance-related and behavioral addiction problems: A person-centered, lay epidemiology approach.

PubMed

Konkolÿ Thege, Barna; Hodgins, David C; Wild, T Cameron

2016-12-01

Background and aims The aims of this study were (a) to describe the prevalence of single versus multiple addiction problems in a large representative sample and (b) to identify distinct subgroups of people experiencing substance-related and behavioral addiction problems. Methods A random sample of 6,000 respondents from Alberta, Canada, completed survey items assessing self-attributed problems experienced in the past year with four substances (alcohol, tobacco, marijuana, and cocaine) and six behaviors (gambling, eating, shopping, sex, video gaming, and work). Hierarchical cluster analyses were used to classify patterns of co-occurring addiction problems on an analytic subsample of 2,728 respondents (1,696 women and 1032 men; M age  = 45.1 years, SD age  = 13.5 years) who reported problems with one or more of the addictive behaviors in the previous year. Results In the total sample, 49.2% of the respondents reported zero, 29.8% reported one, 13.1% reported two, and 7.9% reported three or more addiction problems in the previous year. Cluster-analytic results suggested a 7-group solution. Members of most clusters were characterized by multiple addiction problems; the average number of past year addictive behaviors in cluster members ranged between 1 (Cluster II: excessive eating only) and 2.5 (Cluster VII: excessive video game playing with the frequent co-occurrence of smoking, excessive eating and work). Discussion and conclusions Our findings replicate previous results indicating that about half of the adult population struggles with at least one excessive behavior in a given year; however, our analyses revealed a higher number of co-occurring addiction clusters than typically found in previous studies.

Co-occurring substance-related and behavioral addiction problems: A person-centered, lay epidemiology approach

PubMed Central

Konkolÿ Thege, Barna; Hodgins, David C.; Wild, T. Cameron

2016-01-01

Background and aims The aims of this study were (a) to describe the prevalence of single versus multiple addiction problems in a large representative sample and (b) to identify distinct subgroups of people experiencing substance-related and behavioral addiction problems. Methods A random sample of 6,000 respondents from Alberta, Canada, completed survey items assessing self-attributed problems experienced in the past year with four substances (alcohol, tobacco, marijuana, and cocaine) and six behaviors (gambling, eating, shopping, sex, video gaming, and work). Hierarchical cluster analyses were used to classify patterns of co-occurring addiction problems on an analytic subsample of 2,728 respondents (1,696 women and 1032 men; Mage = 45.1 years, SDage = 13.5 years) who reported problems with one or more of the addictive behaviors in the previous year. Results In the total sample, 49.2% of the respondents reported zero, 29.8% reported one, 13.1% reported two, and 7.9% reported three or more addiction problems in the previous year. Cluster-analytic results suggested a 7-group solution. Members of most clusters were characterized by multiple addiction problems; the average number of past year addictive behaviors in cluster members ranged between 1 (Cluster II: excessive eating only) and 2.5 (Cluster VII: excessive video game playing with the frequent co-occurrence of smoking, excessive eating and work). Discussion and conclusions Our findings replicate previous results indicating that about half of the adult population struggles with at least one excessive behavior in a given year; however, our analyses revealed a higher number of co-occurring addiction clusters than typically found in previous studies. PMID:27829288

Solubilities of crystalline drugs in polymers: an improved analytical method and comparison of solubilities of indomethacin and nifedipine in PVP, PVP/VA, and PVAc.

PubMed

Sun, Ye; Tao, Jing; Zhang, Geoff G Z; Yu, Lian

2010-09-01

A previous method for measuring solubilities of crystalline drugs in polymers has been improved to enable longer equilibration and used to survey the solubilities of indomethacin (IMC) and nifedipine (NIF) in two homo-polymers [polyvinyl pyrrolidone (PVP) and polyvinyl acetate (PVAc)] and their co-polymer (PVP/VA). These data are important for understanding the stability of amorphous drug-polymer dispersions, a strategy actively explored for delivering poorly soluble drugs. Measuring solubilities in polymers is difficult because their high viscosities impede the attainment of solubility equilibrium. In this method, a drug-polymer mixture prepared by cryo-milling is annealed at different temperatures and analyzed by differential scanning calorimetry to determine whether undissolved crystals remain and thus the upper and lower bounds of the equilibrium solution temperature. The new annealing method yielded results consistent with those obtained with the previous scanning method at relatively high temperatures, but revised slightly the previous results at lower temperatures. It also lowered the temperature of measurement closer to the glass transition temperature. For D-mannitol and IMC dissolving in PVP, the polymer's molecular weight has little effect on the weight-based solubility. For IMC and NIF, the dissolving powers of the polymers follow the order PVP > PVP/VA > PVAc. In each polymer studied, NIF is less soluble than IMC. The activities of IMC and NIF dissolved in various polymers are reasonably well fitted to the Flory-Huggins model, yielding the relevant drug-polymer interaction parameters. The new annealing method yields more accurate data than the previous scanning method when solubility equilibrium is slow to achieve. In practice, these two methods can be combined for efficiency. The measured solubilities are not readily anticipated, which underscores the importance of accurate experimental data for developing predictive models.

New analytical solutions to the two-phase water faucet problem

DOE PAGES

Zou, Ling; Zhao, Haihua; Zhang, Hongbin

2016-06-17

Here, the one-dimensional water faucet problem is one of the classical benchmark problems originally proposed by Ransom to study the two-fluid two-phase flow model. With certain simplifications, such as massless gas phase and no wall and interfacial frictions, analytical solutions had been previously obtained for the transient liquid velocity and void fraction distribution. The water faucet problem and its analytical solutions have been widely used for the purposes of code assessment, benchmark and numerical verifications. In our previous study, the Ransom’s solutions were used for the mesh convergence study of a high-resolution spatial discretization scheme. It was found that, atmore » the steady state, an anticipated second-order spatial accuracy could not be achieved, when compared to the existing Ransom’s analytical solutions. A further investigation showed that the existing analytical solutions do not actually satisfy the commonly used two-fluid single-pressure two-phase flow equations. In this work, we present a new set of analytical solutions of the water faucet problem at the steady state, considering the gas phase density’s effect on pressure distribution. This new set of analytical solutions are used for mesh convergence studies, from which anticipated second-order of accuracy is achieved for the 2nd order spatial discretization scheme. In addition, extended Ransom’s transient solutions for the gas phase velocity and pressure are derived, with the assumption of decoupled liquid and gas pressures. Numerical verifications on the extended Ransom’s solutions are also presented.« less

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

Wettability of graphitic-carbon and silicon surfaces: MD modeling and theoretical analysis

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

Ramos-Alvarado, Bladimir; Kumar, Satish; Peterson, G. P.

2015-07-28

The wettability of graphitic carbon and silicon surfaces was numerically and theoretically investigated. A multi-response method has been developed for the analysis of conventional molecular dynamics (MD) simulations of droplets wettability. The contact angle and indicators of the quality of the computations are tracked as a function of the data sets analyzed over time. This method of analysis allows accurate calculations of the contact angle obtained from the MD simulations. Analytical models were also developed for the calculation of the work of adhesion using the mean-field theory, accounting for the interfacial entropy changes. A calibration method is proposed to providemore » better predictions of the respective contact angles under different solid-liquid interaction potentials. Estimations of the binding energy between a water monomer and graphite match those previously reported. In addition, a breakdown in the relationship between the binding energy and the contact angle was observed. The macroscopic contact angles obtained from the MD simulations were found to match those predicted by the mean-field model for graphite under different wettability conditions, as well as the contact angles of Si(100) and Si(111) surfaces. Finally, an assessment of the effect of the Lennard-Jones cutoff radius was conducted to provide guidelines for future comparisons between numerical simulations and analytical models of wettability.« less

Using model-based screening to help discover unknown environmental contaminants.

PubMed

McLachlan, Michael S; Kierkegaard, Amelie; Radke, Michael; Sobek, Anna; Malmvärn, Anna; Alsberg, Tomas; Arnot, Jon A; Brown, Trevor N; Wania, Frank; Breivik, Knut; Xu, Shihe

2014-07-01

Of the tens of thousands of chemicals in use, only a small fraction have been analyzed in environmental samples. To effectively identify environmental contaminants, methods to prioritize chemicals for analytical method development are required. We used a high-throughput model of chemical emissions, fate, and bioaccumulation to identify chemicals likely to have high concentrations in specific environmental media, and we prioritized these for target analysis. This model-based screening was applied to 215 organosilicon chemicals culled from industrial chemical production statistics. The model-based screening prioritized several recognized organosilicon contaminants and generated hypotheses leading to the selection of three chemicals that have not previously been identified as potential environmental contaminants for target analysis. Trace analytical methods were developed, and the chemicals were analyzed in air, sewage sludge, and sediment. All three substances were found to be environmental contaminants. Phenyl-tris(trimethylsiloxy)silane was present in all samples analyzed, with concentrations of ∼50 pg m(-3) in Stockholm air and ∼0.5 ng g(-1) dw in sediment from the Stockholm archipelago. Tris(trifluoropropyl)trimethyl-cyclotrisiloxane and tetrakis(trifluoropropyl)tetramethyl-cyclotetrasiloxane were found in sediments from Lake Mjøsa at ∼1 ng g(-1) dw. The discovery of three novel environmental contaminants shows that models can be useful for prioritizing chemicals for exploratory assessment.

At-line process analytical technology (PAT) for more efficient scale up of biopharmaceutical microfiltration unit operations.

PubMed

Watson, Douglas S; Kerchner, Kristi R; Gant, Sean S; Pedersen, Joseph W; Hamburger, James B; Ortigosa, Allison D; Potgieter, Thomas I

2016-01-01

Tangential flow microfiltration (MF) is a cost-effective and robust bioprocess separation technique, but successful full scale implementation is hindered by the empirical, trial-and-error nature of scale-up. We present an integrated approach leveraging at-line process analytical technology (PAT) and mass balance based modeling to de-risk MF scale-up. Chromatography-based PAT was employed to improve the consistency of an MF step that had been a bottleneck in the process used to manufacture a therapeutic protein. A 10-min reverse phase ultra high performance liquid chromatography (RP-UPLC) assay was developed to provide at-line monitoring of protein concentration. The method was successfully validated and method performance was comparable to previously validated methods. The PAT tool revealed areas of divergence from a mass balance-based model, highlighting specific opportunities for process improvement. Adjustment of appropriate process controls led to improved operability and significantly increased yield, providing a successful example of PAT deployment in the downstream purification of a therapeutic protein. The general approach presented here should be broadly applicable to reduce risk during scale-up of filtration processes and should be suitable for feed-forward and feed-back process control. © 2015 American Institute of Chemical Engineers.

Three-Dimensional Piecewise-Continuous Class-Shape Transformation of Wings

NASA Technical Reports Server (NTRS)

Olson, Erik D.

2015-01-01

Class-Shape Transformation (CST) is a popular method for creating analytical representations of the surface coordinates of various components of aerospace vehicles. A wide variety of two- and three-dimensional shapes can be represented analytically using only a modest number of parameters, and the surface representation is smooth and continuous to as fine a degree as desired. This paper expands upon the original two-dimensional representation of airfoils to develop a generalized three-dimensional CST parametrization scheme that is suitable for a wider range of aircraft wings than previous formulations, including wings with significant non-planar shapes such as blended winglets and box wings. The method uses individual functions for the spanwise variation of airfoil shape, chord, thickness, twist, and reference axis coordinates to build up the complete wing shape. An alternative formulation parameterizes the slopes of the reference axis coordinates in order to relate the spanwise variation to the tangents of the sweep and dihedral angles. Also discussed are methods for fitting existing wing surface coordinates, including the use of piecewise equations to handle discontinuities, and mathematical formulations of geometric continuity constraints. A subsonic transport wing model is used as an example problem to illustrate the application of the methodology and to quantify the effects of piecewise representation and curvature constraints.

Performing both propensity score and instrumental variable analyses in observational studies often leads to discrepant results: a systematic review.

PubMed

Laborde-Castérot, Hervé; Agrinier, Nelly; Thilly, Nathalie

2015-10-01

Propensity score (PS) and instrumental variable (IV) are analytical techniques used to adjust for confounding in observational research. More and more, they seem to be used simultaneously in studies evaluating health interventions. The present review aimed to analyze the agreement between PS and IV results in medical research published to date. Review of all published observational studies that evaluated a clinical intervention using simultaneously PS and IV analyses, as identified in MEDLINE and Web of Science. Thirty-seven studies, most of them published during the previous 5 years, reported 55 comparisons between results from PS and IV analyses. There was a slight/fair agreement between the methods [Cohen's kappa coefficient = 0.21 (95% confidence interval: 0.00, 0.41)]. In 23 cases (42%), results were nonsignificant for one method and significant for the other, and IV analysis results were nonsignificant in most situations (87%). Discrepancies are frequent between PS and IV analyses and can be interpreted in various ways. This suggests that researchers should carefully consider their analytical choices, and readers should be cautious when interpreting results, until further studies clarify the respective roles of the two methods in observational comparative effectiveness research. Copyright © 2015 Elsevier Inc. All rights reserved.

Numeric kinetic energy operators for molecules in polyspherical coordinates

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

Sadri, Keyvan; Meyer, Hans-Dieter; Lauvergnat, David

Generalized curvilinear coordinates, as, e.g., polyspherical coordinates, are in general better adapted to the resolution of the nuclear Schroedinger equation than rectilinear ones like the normal mode coordinates. However, analytical expressions of the kinetic energy operators (KEOs) for molecular systems in polyspherical coordinates may be prohibitively complicated for large systems. In this paper we propose a method to generate a KEO numerically and bring it to a form practicable for dynamical calculations. To examine the new method we calculated vibrational spectra and eigenenergies for nitrous acid (HONO) and compare it with results obtained with an exact analytical KEO derived previouslymore » [F. Richter, P. Rosmus, F. Gatti, and H.-D. Meyer, J. Chem. Phys. 120, 6072 (2004)]. In a second example we calculated {pi}{yields}{pi}* photoabsorption spectrum and eigenenergies of ethene (C{sub 2}H{sub 4}) and compared it with previous work [M. R. Brill, F. Gatti, D. Lauvergnat, and H.-D. Meyer, Chem. Phys. 338, 186 (2007)]. In this ethene study the dimensionality was reduced from 12 to 6 by freezing six internal coordinates. Results for both molecules show that the proposed method for obtaining an approximate KEO is reliable for dynamical calculations. The error in eigenenergies was found to be below 1 cm{sup -1} for most states calculated.« less

A probabilistic and multi-objective analysis of lexicase selection and ε-lexicase selection.

PubMed

Cava, William La; Helmuth, Thomas; Spector, Lee; Moore, Jason H

2018-05-10

Lexicase selection is a parent selection method that considers training cases individually, rather than in aggregate, when performing parent selection. Whereas previous work has demonstrated the ability of lexicase selection to solve difficult problems in program synthesis and symbolic regression, the central goal of this paper is to develop the theoretical underpinnings that explain its performance. To this end, we derive an analytical formula that gives the expected probabilities of selection under lexicase selection, given a population and its behavior. In addition, we expand upon the relation of lexicase selection to many-objective optimization methods to describe the behavior of lexicase selection, which is to select individuals on the boundaries of Pareto fronts in high-dimensional space. We show analytically why lexicase selection performs more poorly for certain sizes of population and training cases, and show why it has been shown to perform more poorly in continuous error spaces. To address this last concern, we propose new variants of ε-lexicase selection, a method that modifies the pass condition in lexicase selection to allow near-elite individuals to pass cases, thereby improving selection performance with continuous errors. We show that ε-lexicase outperforms several diversity-maintenance strategies on a number of real-world and synthetic regression problems.

Determination of nanomolar chromate in drinking water with solid phase extraction and a portable spectrophotometer.

PubMed

Ma, Jian; Yang, Bo; Byrne, Robert H

2012-06-15

Determination of chromate at low concentration levels in drinking water is an important analytical objective for both human health and environmental science. Here we report the use of solid phase extraction (SPE) in combination with a custom-made portable light-emitting diode (LED) spectrophotometer to achieve detection of chromate in the field at nanomolar levels. The measurement chemistry is based on a highly selective reaction between 1,5-diphenylcarbazide (DPC) and chromate under acidic conditions. The Cr-DPC complex formed in the reaction can be extracted on a commercial C18 SPE cartridge. Concentrated Cr-DPC is subsequently eluted with methanol and detected by spectrophotometry. Optimization of analytical conditions involved investigation of reagent compositions and concentrations, eluent type, flow rate (sample loading), sample volume, and stability of the SPE cartridge. Under optimized conditions, detection limits are on the order of 3 nM. Only 50 mL of sample is required for an analysis, and total analysis time is around 10 min. The targeted analytical range of 0-500 nM can be easily extended by changing the sample volume. Compared to previous SPE-based spectrophotometric methods, this analytical procedure offers the benefits of improved sensitivity, reduced sample consumption, shorter analysis time, greater operational convenience, and lower cost. Copyright © 2012 Elsevier B.V. All rights reserved.

Microchip integrating magnetic nanoparticles for allergy diagnosis.

PubMed

Teste, Bruno; Malloggi, Florent; Siaugue, Jean-Michel; Varenne, Anne; Kanoufi, Frederic; Descroix, Stéphanie

2011-12-21

We report on the development of a simple and easy to use microchip dedicated to allergy diagnosis. This microchip combines both the advantages of homogeneous immunoassays i.e. species diffusion and heterogeneous immunoassays i.e. easy separation and preconcentration steps. In vitro allergy diagnosis is based on specific Immunoglobulin E (IgE) quantitation, in that way we have developed and integrated magnetic core-shell nanoparticles (MCSNPs) as an IgE capture nanoplatform in a microdevice taking benefit from both their magnetic and colloidal properties. Integrating such immunosupport allows to perform the target analyte (IgE) capture in the colloidal phase thus increasing the analyte capture kinetics since both immunological partners are diffusing during the immune reaction. This colloidal approach improves 1000 times the analyte capture kinetics compared to conventional methods. Moreover, based on the MCSNPs' magnetic properties and on the magnetic chamber we have previously developed the MCSNPs and therefore the target can be confined and preconcentrated within the microdevice prior to the detection step. The MCSNPs preconcentration factor achieved was about 35,000 and allows to reach high sensitivity thus avoiding catalytic amplification during the detection step. The developed microchip offers many advantages: the analytical procedure was fully integrated on-chip, analyses were performed in short assay time (20 min), the sample and reagents consumption was reduced to few microlitres (5 μL) while a low limit of detection can be achieved (about 1 ng mL(-1)).

Connecting the shadows: probing inner disk geometries using shadows in transitional disks

NASA Astrophysics Data System (ADS)

Min, M.; Stolker, T.; Dominik, C.; Benisty, M.

2017-08-01

Aims: Shadows in transitional disks are generally interpreted as signs of a misaligned inner disk. This disk is usually beyond the reach of current day high contrast imaging facilities. However, the location and morphology of the shadow features allow us to reconstruct the inner disk geometry. Methods: We derive analytic equations of the locations of the shadow features as a function of the orientation of the inner and outer disk and the height of the outer disk wall. In contrast to previous claims in the literature, we show that the position angle of the line connecting the shadows cannot be directly related to the position angle of the inner disk. Results: We show how the analytic framework derived here can be applied to transitional disks with shadow features. We use estimates of the outer disk height to put constraints on the inner disk orientation. In contrast with the results from Long et al. (2017, ApJ, 838, 62), we derive that for the disk surrounding HD 100453 the analytic estimates and interferometric observations result in a consistent picture of the orientation of the inner disk. Conclusions: The elegant consistency in our analytic framework between observation and theory strongly support both the interpretation of the shadow features as coming from a misaligned inner disk as well as the diagnostic value of near infrared interferometry for inner disk geometry.

Selection of infectious medical waste disposal firms by using the analytic hierarchy process and sensitivity analysis.

PubMed

Hsu, Pi-Fang; Wu, Cheng-Ru; Li, Ya-Ting

2008-01-01

While Taiwanese hospitals dispose of large amounts of medical waste to ensure sanitation and personal hygiene, doing so inefficiently creates potential environmental hazards and increases operational expenses. However, hospitals lack objective criteria to select the most appropriate waste disposal firm and evaluate its performance, instead relying on their own subjective judgment and previous experiences. Therefore, this work presents an analytic hierarchy process (AHP) method to objectively select medical waste disposal firms based on the results of interviews with experts in the field, thus reducing overhead costs and enhancing medical waste management. An appropriate weight criterion based on AHP is derived to assess the effectiveness of medical waste disposal firms. The proposed AHP-based method offers a more efficient and precise means of selecting medical waste firms than subjective assessment methods do, thus reducing the potential risks for hospitals. Analysis results indicate that the medical sector selects the most appropriate infectious medical waste disposal firm based on the following rank: matching degree, contractor's qualifications, contractor's service capability, contractor's equipment and economic factors. By providing hospitals with an effective means of evaluating medical waste disposal firms, the proposed AHP method can reduce overhead costs and enable medical waste management to understand the market demand in the health sector. Moreover, performed through use of Expert Choice software, sensitivity analysis can survey the criterion weight of the degree of influence with an alternative hierarchy.

Quantitative analysis of periodontal pathogens by ELISA and real-time polymerase chain reaction.

PubMed

Hamlet, Stephen M

2010-01-01

The development of analytical methods enabling the accurate identification and enumeration of bacterial species colonizing the oral cavity has led to the identification of a small number of bacterial pathogens that are major factors in the etiology of periodontal disease. Further, these methods also underpin more recent epidemiological analyses of the impact of periodontal disease on general health. Given the complex milieu of over 700 species of microorganisms known to exist within the complex biofilms found in the oral cavity, the identification and enumeration of oral periodontopathogens has not been an easy task. In recent years however, some of the intrinsic limitations of the more traditional microbiological analyses previously used have been overcome with the advent of immunological and molecular analytical methods. Of the plethora of methodologies reported in the literature, the enzyme-linked immunosorbent assay (ELISA), which combines the specificity of antibody with the sensitivity of simple enzyme assays and the polymerase chain reaction (PCR), has been widely utilized in both laboratory and clinical applications. Although conventional PCR does not allow quantitation of the target organism, real-time PCR (rtPCR) has the ability to detect amplicons as they accumulate in "real time" allowing subsequent quantitation. These methods enable the accurate quantitation of as few as 10(2) (using rtPCR) to 10(4) (using ELISA) periodontopathogens in dental plaque samples.

Life cycle management of analytical methods.

PubMed

Parr, Maria Kristina; Schmidt, Alexander H

2018-01-05

In modern process management, the life cycle concept gains more and more importance. It focusses on the total costs of the process from invest to operation and finally retirement. Also for analytical procedures an increasing interest for this concept exists in the recent years. The life cycle of an analytical method consists of design, development, validation (including instrumental qualification, continuous method performance verification and method transfer) and finally retirement of the method. It appears, that also regulatory bodies have increased their awareness on life cycle management for analytical methods. Thus, the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH), as well as the United States Pharmacopeial Forum discuss the enrollment of new guidelines that include life cycle management of analytical methods. The US Pharmacopeia (USP) Validation and Verification expert panel already proposed a new General Chapter 〈1220〉 "The Analytical Procedure Lifecycle" for integration into USP. Furthermore, also in the non-regulated environment a growing interest on life cycle management is seen. Quality-by-design based method development results in increased method robustness. Thereby a decreased effort is needed for method performance verification, and post-approval changes as well as minimized risk of method related out-of-specification results. This strongly contributes to reduced costs of the method during its life cycle. Copyright © 2017 Elsevier B.V. All rights reserved.

Horizontal lifelines - review of regulations and simple design method considering anchorage rigidity.

PubMed

Galy, Bertrand; Lan, André

2018-03-01

Among the many occupational risks construction workers encounter every day falling from a height is the most dangerous. The objective of this article is to propose a simple analytical design method for horizontal lifelines (HLLs) that considers anchorage flexibility. The article presents a short review of the standards and regulations/acts/codes concerning HLLs in Canada the USA and Europe. A static analytical approach is proposed considering anchorage flexibility. The analytical results are compared with a series of 42 dynamic fall tests and a SAP2000 numerical model. The experimental results show that the analytical method is a little conservative and overestimates the line tension in most cases with a maximum of 17%. The static SAP2000 results show a maximum 2.1% difference with the analytical method. The analytical method is accurate enough to safely design HLLs and quick design abaci are provided to allow the engineer to make quick on-site verification if needed.

Diagrammatic Monte Carlo study of Fröhlich polaron dispersion in two and three dimensions

NASA Astrophysics Data System (ADS)

Hahn, Thomas; Klimin, Sergei; Tempere, Jacques; Devreese, Jozef T.; Franchini, Cesare

2018-04-01

We present results for the solution of the large polaron Fröhlich Hamiltonian in 3 dimensions (3D) and 2 dimensions (2D) obtained via the diagrammatic Monte Carlo (DMC) method. Our implementation is based on the approach by Mishchenko [A. S. Mishchenko et al., Phys. Rev. B 62, 6317 (2000), 10.1103/PhysRevB.62.6317]. Polaron ground state energies and effective polaron masses are successfully benchmarked with data obtained using Feynman's path integral formalism. By comparing 3D and 2D data, we verify the analytically exact scaling relations for energies and effective masses from 3 D →2 D , which provides a stringent test for the quality of DMC predictions. The accuracy of our results is further proven by providing values for the exactly known coefficients in weak- and strong-coupling expansions. Moreover, we compute polaron dispersion curves which are validated with analytically known lower and upper limits in the small-coupling regime and verify the first-order expansion results for larger couplings, thus disproving previous critiques on the apparent incompatibility of DMC with analytical results and furnishing useful reference for a wide range of coupling strengths.