Keeping It Simple: Can We Estimate Malting Quality Potential Using an Isothermal Mashing Protocol and Common Laboratory Instrumentation?

USDA-ARS?s Scientific Manuscript database

Current methods for generating malting quality metrics have been developed largely to support commercial malting and brewing operations, providing accurate, reproducible analytical data to guide malting and brewing production. Infrastructure to support these analytical operations often involves sub...

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.

Moderate severity heart failure does not involve a downregulation of myocardial fatty acid oxidation

DTIC Science & Technology

2004-10-01

malonyl-CoA-sensitive form of carnitine palmitoyltransferase is not local - ized exclusively in the outer membrane of rat liver mitochondria . J Biol...for the isolation of fresh mitochondria , both subsarcolemmal and interfibrillar. Analytic methods. Detailed analytic methods have been previously cited...populations of mitochondria , the subsarcolemmal and inter- fibrillar, were isolated from hearts of normal and HF dogs using the procedure of Palmer et al

Sustained prediction ability of net analyte preprocessing methods using reduced calibration sets. Theoretical and experimental study involving the spectrophotometric analysis of multicomponent mixtures.

PubMed

Goicoechea, H C; Olivieri, A C

2001-07-01

A newly developed multivariate method involving net analyte preprocessing (NAP) was tested using central composite calibration designs of progressively decreasing size regarding the multivariate simultaneous spectrophotometric determination of three active components (phenylephrine, diphenhydramine and naphazoline) and one excipient (methylparaben) in nasal solutions. Its performance was evaluated and compared with that of partial least-squares (PLS-1). Minimisation of the calibration predicted error sum of squares (PRESS) as a function of a moving spectral window helped to select appropriate working spectral ranges for both methods. The comparison of NAP and PLS results was carried out using two tests: (1) the elliptical joint confidence region for the slope and intercept of a predicted versus actual concentrations plot for a large validation set of samples and (2) the D-optimality criterion concerning the information content of the calibration data matrix. Extensive simulations and experimental validation showed that, unlike PLS, the NAP method is able to furnish highly satisfactory results when the calibration set is reduced from a full four-component central composite to a fractional central composite, as expected from the modelling requirements of net analyte based methods.

Methods for Integrating Moderation and Mediation: A General Analytical Framework Using Moderated Path Analysis

ERIC Educational Resources Information Center

Edwards, Jeffrey R.; Lambert, Lisa Schurer

2007-01-01

Studies that combine moderation and mediation are prevalent in basic and applied psychology research. Typically, these studies are framed in terms of moderated mediation or mediated moderation, both of which involve similar analytical approaches. Unfortunately, these approaches have important shortcomings that conceal the nature of the moderated…

Island Explorations: Discovering Effects of Environmental Research-Based Lab Activities on Analytical Chemistry Students

ERIC Educational Resources Information Center

Tomasik, Janice Hall; LeCaptain, Dale; Murphy, Sarah; Martin, Mary; Knight, Rachel M.; Harke, Maureen A.; Burke, Ryan; Beck, Kara; Acevedo-Polakovich, I. David

2014-01-01

Motivating students in analytical chemistry can be challenging, in part because of the complexity and breadth of topics involved. Some methods that help encourage students and convey real-world relevancy of the material include incorporating environmental issues, research-based lab experiments, and service learning projects. In this paper, we…

Maximum Likelihood Estimation in Meta-Analytic Structural Equation Modeling

ERIC Educational Resources Information Center

Oort, Frans J.; Jak, Suzanne

2016-01-01

Meta-analytic structural equation modeling (MASEM) involves fitting models to a common population correlation matrix that is estimated on the basis of correlation coefficients that are reported by a number of independent studies. MASEM typically consist of two stages. The method that has been found to perform best in terms of statistical…

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

On solving wave equations on fixed bounded intervals involving Robin boundary conditions with time-dependent coefficients

NASA Astrophysics Data System (ADS)

van Horssen, Wim T.; Wang, Yandong; Cao, Guohua

2018-06-01

In this paper, it is shown how characteristic coordinates, or equivalently how the well-known formula of d'Alembert, can be used to solve initial-boundary value problems for wave equations on fixed, bounded intervals involving Robin type of boundary conditions with time-dependent coefficients. A Robin boundary condition is a condition that specifies a linear combination of the dependent variable and its first order space-derivative on a boundary of the interval. Analytical methods, such as the method of separation of variables (SOV) or the Laplace transform method, are not applicable to those types of problems. The obtained analytical results by applying the proposed method, are in complete agreement with those obtained by using the numerical, finite difference method. For problems with time-independent coefficients in the Robin boundary condition(s), the results of the proposed method also completely agree with those as for instance obtained by the method of separation of variables, or by the finite difference method.

METHOD DEVELOPMENT FOR THE DETERMINATION OF FORMALDEHYDE IN SAMPLES OF ENVIRONMENTAL ORIGIN

EPA Science Inventory

An analytical method was developed for the determination of formaldehyde in samples of environmental origin. After a review of the current literature, five candidate methods involving chemical derivatization were chosen for evaluation. The five derivatization reagents studied wer...

Contribution of Electrochemistry to the Biomedical and Pharmaceutical Analytical Sciences.

PubMed

Kauffmann, Jean-Michel; Patris, Stephanie; Vandeput, Marie; Sarakbi, Ahmad; Sakira, Abdul Karim

2016-01-01

All analytical techniques have experienced major progress since the last ten years and electroanalysis is also involved in this trend. The unique characteristics of phenomena occurring at the electrode-solution interface along with the variety of electrochemical methods currently available allow for a broad spectrum of applications. Potentiometric, conductometric, voltammetric and amperometric methods are briefly reviewed with a critical view in terms of performance of the developed instrumentation with special emphasis on pharmaceutical and biomedical applications.

Analytical model for advective-dispersive transport involving flexible boundary inputs, initial distributions and zero-order productions

NASA Astrophysics Data System (ADS)

Chen, Jui-Sheng; Li, Loretta Y.; Lai, Keng-Hsin; Liang, Ching-Ping

2017-11-01

A novel solution method is presented which leads to an analytical model for the advective-dispersive transport in a semi-infinite domain involving a wide spectrum of boundary inputs, initial distributions, and zero-order productions. The novel solution method applies the Laplace transform in combination with the generalized integral transform technique (GITT) to obtain the generalized analytical solution. Based on this generalized analytical expression, we derive a comprehensive set of special-case solutions for some time-dependent boundary distributions and zero-order productions, described by the Dirac delta, constant, Heaviside, exponentially-decaying, or periodically sinusoidal functions as well as some position-dependent initial conditions and zero-order productions specified by the Dirac delta, constant, Heaviside, or exponentially-decaying functions. The developed solutions are tested against an analytical solution from the literature. The excellent agreement between the analytical solutions confirms that the new model can serve as an effective tool for investigating transport behaviors under different scenarios. Several examples of applications, are given to explore transport behaviors which are rarely noted in the literature. The results show that the concentration waves resulting from the periodically sinusoidal input are sensitive to dispersion coefficient. The implication of this new finding is that a tracer test with a periodic input may provide additional information when for identifying the dispersion coefficients. Moreover, the solution strategy presented in this study can be extended to derive analytical models for handling more complicated problems of solute transport in multi-dimensional media subjected to sequential decay chain reactions, for which analytical solutions are not currently available.

LC-MS/MS methods for albendazole analysis in feed and its metabolite residues in fish fillet and a leaching study in feed after an alternative procedure for drug incorporation.

PubMed

Busatto, Zenaís; da Silva, Agnaldo Fernando Baldo; de Freitas, Osvaldo; Paschoal, Jonas Augusto Rizzato

2017-04-01

This paper describes the development of analytical methods for the quantification of albendazole (ABZ) in fish feed and ABZ and its main known metabolites (albendazole sulfoxide, albendazole sulfone and albendazole aminosulfone) in fish fillet employing LC-MS/MS. In order to assess the reliability of the analytical methods, evaluation was undertaken as recommended by related guides proposed by the Brazilian Ministry of Agriculture for analytical method validation. The calibration curve for ABZ quantification in feed showed adequate linearity (r > 0.99), precision (CV < 1.03%) and trueness ranging from 99% to 101%. The method for ABZ residues in fish fillet involving the QuEChERS technique for sample extraction had adequate linearity (r > 0.99) for all analytes, precision (CV < 13%) and trueness around 100%, with CCα < 122 ng g - 1 and CCβ < 145 ng g - 1 . Besides, by aiming to avoid the risk of ABZ leaching from feed into the aquatic environment during fish medication via the oral route, a promising procedure for drug incorporation in the feed involving coating feed pellets with ethyl cellulose polymer containing ABZ was also evaluated. The medicated feed had good homogeneity (CV < 3%) and a lower release of ABZ (< 0.2%) from feed to water when the medicated feed stayed in the water for up to 15 min.

THE DETERMINATION OF NON-PESTICIDAL AND PESTICIDAL ORGANOTIN COMPOUNDS IN WATER BY GAS CHROMATOGRAPHY WITH [PULSED] FLAME PHOTOMETRIC DETECTION (GS/PFPD): THE EFFECTS OF "MASS" DISCRIMINATION

EPA Science Inventory

Capillary gas chromatography with GC/PFPD was used in the development of analytical methodology for determining both non-pesticidal and pesticidal organotin compounds in drinking water and other aqueous matrices. The method involves aqueous ethylation of organotin analytes with ...

Target analyte quantification by isotope dilution LC-MS/MS directly referring to internal standard concentrations--validation for serum cortisol measurement.

PubMed

Maier, Barbara; Vogeser, Michael

2013-04-01

Isotope dilution LC-MS/MS methods used in the clinical laboratory typically involve multi-point external calibration in each analytical series. Our aim was to test the hypothesis that determination of target analyte concentrations directly derived from the relation of the target analyte peak area to the peak area of a corresponding stable isotope labelled internal standard compound [direct isotope dilution analysis (DIDA)] may be not inferior to conventional external calibration with respect to accuracy and reproducibility. Quality control samples and human serum pools were analysed in a comparative validation protocol for cortisol as an exemplary analyte by LC-MS/MS. Accuracy and reproducibility were compared between quantification either involving a six-point external calibration function, or a result calculation merely based on peak area ratios of unlabelled and labelled analyte. Both quantification approaches resulted in similar accuracy and reproducibility. For specified analytes, reliable analyte quantification directly derived from the ratio of peak areas of labelled and unlabelled analyte without the need for a time consuming multi-point calibration series is possible. This DIDA approach is of considerable practical importance for the application of LC-MS/MS in the clinical laboratory where short turnaround times often have high priority.

Comparative analysis of methods for real-time analytical control of chemotherapies preparations.

PubMed

Bazin, Christophe; Cassard, Bruno; Caudron, Eric; Prognon, Patrice; Havard, Laurent

2015-10-15

Control of chemotherapies preparations are now an obligation in France, though analytical control is compulsory. Several methods are available and none of them is presumed as ideal. We wanted to compare them so as to determine which one could be the best choice. We compared non analytical (visual and video-assisted, gravimetric) and analytical (HPLC/FIA, UV/FT-IR, UV/Raman, Raman) methods thanks to our experience and a SWOT analysis. The results of the analysis show great differences between the techniques, but as expected none us them is without defects. However they can probably be used in synergy. Overall for the pharmacist willing to get involved, the implementation of the control for chemotherapies preparations must be widely anticipated, with the listing of every parameter, and remains according to us an analyst's job. Copyright © 2015 Elsevier B.V. All rights reserved.

Analytic Method for Computing Instrument Pointing Jitter

NASA Technical Reports Server (NTRS)

Bayard, David

2003-01-01

A new method of calculating the root-mean-square (rms) pointing jitter of a scientific instrument (e.g., a camera, radar antenna, or telescope) is introduced based on a state-space concept. In comparison with the prior method of calculating the rms pointing jitter, the present method involves significantly less computation. The rms pointing jitter of an instrument (the square root of the jitter variance shown in the figure) is an important physical quantity which impacts the design of the instrument, its actuators, controls, sensory components, and sensor- output-sampling circuitry. Using the Sirlin, San Martin, and Lucke definition of pointing jitter, the prior method of computing the rms pointing jitter involves a frequency-domain integral of a rational polynomial multiplied by a transcendental weighting function, necessitating the use of numerical-integration techniques. In practice, numerical integration complicates the problem of calculating the rms pointing error. In contrast, the state-space method provides exact analytic expressions that can be evaluated without numerical integration.

Computational and analytical methods in nonlinear fluid dynamics

NASA Astrophysics Data System (ADS)

Walker, James

1993-09-01

The central focus of the program was on the application and development of modern analytical and computational methods to the solution of nonlinear problems in fluid dynamics and reactive gas dynamics. The research was carried out within the Division of Engineering Mathematics in the Department of Mechanical Engineering and Mechanics and principally involved Professors P.A. Blythe, E. Varley and J.D.A. Walker. In addition. the program involved various international collaborations. Professor Blythe completed work on reactive gas dynamics with Professor D. Crighton FRS of Cambridge University in the United Kingdom. Professor Walker and his students carried out joint work with Professor F.T. Smith, of University College London, on various problems in unsteady flow and turbulent boundary layers.

An improved 3D MoF method based on analytical partial derivatives

NASA Astrophysics Data System (ADS)

Chen, Xiang; Zhang, Xiong

2016-12-01

MoF (Moment of Fluid) method is one of the most accurate approaches among various surface reconstruction algorithms. As other second order methods, MoF method needs to solve an implicit optimization problem to obtain the optimal approximate surface. Therefore, the partial derivatives of the objective function have to be involved during the iteration for efficiency and accuracy. However, to the best of our knowledge, the derivatives are currently estimated numerically by finite difference approximation because it is very difficult to obtain the analytical derivatives of the object function for an implicit optimization problem. Employing numerical derivatives in an iteration not only increase the computational cost, but also deteriorate the convergence rate and robustness of the iteration due to their numerical error. In this paper, the analytical first order partial derivatives of the objective function are deduced for 3D problems. The analytical derivatives can be calculated accurately, so they are incorporated into the MoF method to improve its accuracy, efficiency and robustness. Numerical studies show that by using the analytical derivatives the iterations are converged in all mixed cells with the efficiency improvement of 3 to 4 times.

Biological Matrix Effects in Quantitative Tandem Mass Spectrometry-Based Analytical Methods: Advancing Biomonitoring

PubMed Central

Panuwet, Parinya; Hunter, Ronald E.; D’Souza, Priya E.; Chen, Xianyu; Radford, Samantha A.; Cohen, Jordan R.; Marder, M. Elizabeth; Kartavenka, Kostya; Ryan, P. Barry; Barr, Dana Boyd

2015-01-01

The ability to quantify levels of target analytes in biological samples accurately and precisely, in biomonitoring, involves the use of highly sensitive and selective instrumentation such as tandem mass spectrometers and a thorough understanding of highly variable matrix effects. Typically, matrix effects are caused by co-eluting matrix components that alter the ionization of target analytes as well as the chromatographic response of target analytes, leading to reduced or increased sensitivity of the analysis. Thus, before the desired accuracy and precision standards of laboratory data are achieved, these effects must be characterized and controlled. Here we present our review and observations of matrix effects encountered during the validation and implementation of tandem mass spectrometry-based analytical methods. We also provide systematic, comprehensive laboratory strategies needed to control challenges posed by matrix effects in order to ensure delivery of the most accurate data for biomonitoring studies assessing exposure to environmental toxicants. PMID:25562585

Bessel function expansion to reduce the calculation time and memory usage for cylindrical computer-generated holograms.

PubMed

Sando, Yusuke; Barada, Daisuke; Jackin, Boaz Jessie; Yatagai, Toyohiko

2017-07-10

This study proposes a method to reduce the calculation time and memory usage required for calculating cylindrical computer-generated holograms. The wavefront on the cylindrical observation surface is represented as a convolution integral in the 3D Fourier domain. The Fourier transformation of the kernel function involving this convolution integral is analytically performed using a Bessel function expansion. The analytical solution can drastically reduce the calculation time and the memory usage without any cost, compared with the numerical method using fast Fourier transform to Fourier transform the kernel function. In this study, we present the analytical derivation, the efficient calculation of Bessel function series, and a numerical simulation. Furthermore, we demonstrate the effectiveness of the analytical solution through comparisons of calculation time and memory usage.

Quantifying the measurement uncertainty of results from environmental analytical methods.

PubMed

Moser, J; Wegscheider, W; Sperka-Gottlieb, C

2001-07-01

The Eurachem-CITAC Guide Quantifying Uncertainty in Analytical Measurement was put into practice in a public laboratory devoted to environmental analytical measurements. In doing so due regard was given to the provisions of ISO 17025 and an attempt was made to base the entire estimation of measurement uncertainty on available data from the literature or from previously performed validation studies. Most environmental analytical procedures laid down in national or international standards are the result of cooperative efforts and put into effect as part of a compromise between all parties involved, public and private, that also encompasses environmental standards and statutory limits. Central to many procedures is the focus on the measurement of environmental effects rather than on individual chemical species. In this situation it is particularly important to understand the measurement process well enough to produce a realistic uncertainty statement. Environmental analytical methods will be examined as far as necessary, but reference will also be made to analytical methods in general and to physical measurement methods where appropriate. This paper describes ways and means of quantifying uncertainty for frequently practised methods of environmental analysis. It will be shown that operationally defined measurands are no obstacle to the estimation process as described in the Eurachem/CITAC Guide if it is accepted that the dominating component of uncertainty comes from the actual practice of the method as a reproducibility standard deviation.

The role of analytical science in natural resource decision making

NASA Astrophysics Data System (ADS)

Miller, Alan

1993-09-01

There is a continuing debate about the proper role of analytical (positivist) science in natural resource decision making. Two diametrically opposed views are evident, arguing for and against a more extended role for scientific information. The debate takes on a different complexion if one recognizes that certain kinds of problem, referred to here as “wicked” or “trans-science” problems, may not be amenable to the analytical process. Indeed, the mistaken application of analytical methods to trans-science problems may not only be a waste of time and money but also serve to hinder policy development. Since many environmental issues are trans-science in nature, then it follows that alternatives to analytical science need to be developed. In this article, the issues involved in the debate are clarified by examining the impact of the use of analytical methods in a particular case, the spruce budworm controversy in New Brunswick. The article ends with some suggestions about a “holistic” approach to the problem.

Performance Evaluation of an Improved GC-MS Method to Quantify Methylmercury in Fish.

PubMed

Watanabe, Takahiro; Kikuchi, Hiroyuki; Matsuda, Rieko; Hayashi, Tomoko; Akaki, Koichi; Teshima, Reiko

2015-01-01

Here, we set out to improve our previously developed methylmercury analytical method, involving phenyl derivatization and gas chromatography-mass spectrometry (GC-MS). In the improved method, phenylation of methylmercury with sodium tetraphenylborate was carried out in a toluene/water two-phase system, instead of in water alone. The modification enabled derivatization at optimum pH, and the formation of by-products was dramatically reduced. In addition, adsorption of methyl phenyl mercury in the GC system was suppressed by co-injection of PEG200, enabling continuous analysis without loss of sensitivity. The performance of the improved analytical method was independently evaluated by three analysts using certified reference materials and methylmercury-spiked fresh fish samples. The present analytical method was validated as suitable for determination of compliance with the provisional regulation value for methylmercury in fish, set in the Food Sanitation haw.

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.

Determining a carbohydrate profile for Hansenula polymorpha

NASA Technical Reports Server (NTRS)

Petersen, G. R.

1985-01-01

The determination of the levels of carbohydrates in the yeast Hansenula polymorpha required the development of new analytical procedures. Existing fractionation and analytical methods were adapted to deal with the problems involved with the lysis of whole cells. Using these new procedures, the complete carbohydrate profiles of H. polymorpha and selected mutant strains were determined and shown to correlate favourably with previously published results.

Procrustes Matching by Congruence Coefficients

ERIC Educational Resources Information Center

Korth, Bruce; Tucker, L. R.

1976-01-01

Matching by Procrustes methods involves the transformation of one matrix to match with another. A special least squares criterion, the congruence coefficient, has advantages as a criterion for some factor analytic interpretations. A Procrustes method maximizing the congruence coefficient is given. (Author/JKS)

Implicit solution of Navier-Stokes equations on staggered curvilinear grids using a Newton-Krylov method with a novel analytical Jacobian.

NASA Astrophysics Data System (ADS)

Borazjani, Iman; Asgharzadeh, Hafez

2015-11-01

Flow simulations involving complex geometries and moving boundaries suffer from time-step size restriction and low convergence rates with explicit and semi-implicit schemes. Implicit schemes can be used to overcome these restrictions. However, implementing implicit solver for nonlinear equations including Navier-Stokes is not straightforward. Newton-Krylov subspace methods (NKMs) are one of the most advanced iterative methods to solve non-linear equations such as implicit descritization of the Navier-Stokes equation. The efficiency of NKMs massively depends on the Jacobian formation method, e.g., automatic differentiation is very expensive, and matrix-free methods slow down as the mesh is refined. Analytical Jacobian is inexpensive method, but derivation of analytical Jacobian for Navier-Stokes equation on staggered grid is challenging. The NKM with a novel analytical Jacobian was developed and validated against Taylor-Green vortex and pulsatile flow in a 90 degree bend. The developed method successfully handled the complex geometries such as an intracranial aneurysm with multiple overset grids, and immersed boundaries. It is shown that the NKM with an analytical Jacobian is 3 to 25 times faster than the fixed-point implicit Runge-Kutta method, and more than 100 times faster than automatic differentiation depending on the grid (size) and the flow problem. The developed methods are fully parallelized with parallel efficiency of 80-90% on the problems tested.

Modern analytical methods for the detection of food fraud and adulteration by food category.

PubMed

Hong, Eunyoung; Lee, Sang Yoo; Jeong, Jae Yun; Park, Jung Min; Kim, Byung Hee; Kwon, Kisung; Chun, Hyang Sook

2017-09-01

This review provides current information on the analytical methods used to identify food adulteration in the six most adulterated food categories: animal origin and seafood, oils and fats, beverages, spices and sweet foods (e.g. honey), grain-based food, and others (organic food and dietary supplements). The analytical techniques (both conventional and emerging) used to identify adulteration in these six food categories involve sensory, physicochemical, DNA-based, chromatographic and spectroscopic methods, and have been combined with chemometrics, making these techniques more convenient and effective for the analysis of a broad variety of food products. Despite recent advances, the need remains for suitably sensitive and widely applicable methodologies that encompass all the various aspects of food adulteration. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Development of a reference material for routine performance monitoring of methods measuring polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and dioxin-like polychlorinated biphenyls.

PubMed

Selliah, S S; Cussion, S; MacPherson, K A; Reiner, E J; Toner, D

2001-06-01

Matrix-matched environmental certified reference materials (CRMs) are one of the most useful tools to validate analytical methods, assess analytical laboratory performance and to assist in the resolution of data conflicts between laboratories. This paper describes the development of a lake sediment as a CRM for polychorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (DLPCBs). The presence of DLPCBs in the environment is of increased concern and analytical methods are being developed internationally for monitoring DLPCBs in the environment. This paper also reports the results of an international interlaboratory study involving thirty-five laboratories from seventeen countries, conducted to characterize and validate levels of a sediment reference material for PCDDs, PCDFs and DLPCBs.

Methods for determination of inorganic substances in water and fluvial sediments

USGS Publications Warehouse

Fishman, Marvin J.; Friedman, Linda C.

1989-01-01

Chapter Al of the laboratory manual contains methods used by the U.S. Geological Survey to analyze samples of water, suspended sediments, and bottom material for their content of inorganic constituents. Included are methods for determining the concentration of dissolved constituents in water, the total recoverable and total of constituents in water-suspended sediment samples, and the recoverable and total concentrations of constituents in samples of bottom material. The introduction to the manual includes essential definitions and a brief discussion of the use of significant figures in calculating and reporting analytical results. Quality control in the water-analysis laboratory is discussed, including the accuracy and precision of analyses, the use of standard-reference water samples, and the operation of an effective quality-assurance program. Methods for sample preparation and pretreatment are given also. A brief discussion of the principles of the analytical techniques involved and their particular application to water and sediment analysis is presented. The analytical methods of these techniques are arranged alphabetically by constituent. For each method, the general topics covered are the application, the principle of the method, the interferences, the apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data, when available. More than 126 methods are given for the determination of 70 inorganic constituents and physical properties of water, suspended sediment, and bottom material.

Analytical method for the fast time-domain reconstruction of fluorescent inclusions in vitro and in vivo.

PubMed

Han, Sung-Ho; Farshchi-Heydari, Salman; Hall, David J

2010-01-20

A novel time-domain optical method to reconstruct the relative concentration, lifetime, and depth of a fluorescent inclusion is described. We establish an analytical method for the estimations of these parameters for a localized fluorescent object directly from the simple evaluations of continuous wave intensity, exponential decay, and temporal position of the maximum of the fluorescence temporal point-spread function. Since the more complex full inversion process is not involved, this method permits a robust and fast processing in exploring the properties of a fluorescent inclusion. This method is confirmed by in vitro and in vivo experiments. Copyright 2010 Biophysical Society. Published by Elsevier Inc. All rights reserved.

Sampling Large Graphs for Anticipatory Analytics

DTIC Science & Technology

2015-05-15

low. C. Random Area Sampling Random area sampling [8] is a “ snowball ” sampling method in which a set of random seed vertices are selected and areas... Sampling Large Graphs for Anticipatory Analytics Lauren Edwards, Luke Johnson, Maja Milosavljevic, Vijay Gadepally, Benjamin A. Miller Lincoln...systems, greater human-in-the-loop involvement, or through complex algorithms. We are investigating the use of sampling to mitigate these challenges

Application of factorial designs to study factors involved in the determination of aldehydes present in beer by on-fiber derivatization in combination with gas chromatography and mass spectrometry.

PubMed

Carrillo, Génesis; Bravo, Adriana; Zufall, Carsten

2011-05-11

With the aim of studying the factors involved in on-fiber derivatization of Strecker aldehydes, furfural, and (E)-2-nonenal with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine in beer, factorial designs were applied. The effect of the temperature, time, and NaCl addition on the analytes' derivatization/extraction efficiency was studied through a factorial 2(3) randomized-block design; all of the factors and their interactions were significant at the 95% confidence level for most of the analytes. The effect of temperature and its interactions separated the analytes in two groups. However, a single sampling condition was selected that optimized response for most aldehydes. The resulting method, combining on-fiber derivatization with gas chromatography-mass spectrometry, was validated. Limits of detections were between 0.015 and 1.60 μg/L, and relative standard deviations were between 1.1 and 12.2%. The efficacy of the internal standardization method was confirmed by recovery percentage (73-117%). The method was applied to the determination of aldehydes in fresh beer and after storage at 28 °C.

Analytical challenges in sports drug testing.

PubMed

Thevis, Mario; Krug, Oliver; Geyer, Hans; Walpurgis, Katja; Baume, Norbert; Thomas, Andreas

2018-03-01

Analytical chemistry represents a central aspect of doping controls. Routine sports drug testing approaches are primarily designed to address the question whether a prohibited substance is present in a doping control sample and whether prohibited methods (for example, blood transfusion or sample manipulation) have been conducted by an athlete. As some athletes have availed themselves of the substantial breadth of research and development in the pharmaceutical arena, proactive and preventive measures are required such as the early implementation of new drug candidates and corresponding metabolites into routine doping control assays, even though these drug candidates are to date not approved for human use. Beyond this, analytical data are also cornerstones of investigations into atypical or adverse analytical findings, where the overall picture provides ample reason for follow-up studies. Such studies have been of most diverse nature, and tailored approaches have been required to probe hypotheses and scenarios reported by the involved parties concerning the plausibility and consistency of statements and (analytical) facts. In order to outline the variety of challenges that doping control laboratories are facing besides providing optimal detection capabilities and analytical comprehensiveness, selected case vignettes involving the follow-up of unconventional adverse analytical findings, urine sample manipulation, drug/food contamination issues, and unexpected biotransformation reactions are thematized.

Evaluation of a multiclass, multiresidue liquid chromatography-tandem mass spectrometry method for analysis of 120 veterinary drugs in bovine kidney

USDA-ARS?s Scientific Manuscript database

Traditionally, regulatory monitoring of veterinary drug residues in food animal tissues involves the use of several single-class methods to cover a wide analytical scope. Multiclass, multiresidue methods of analysis tend to provide greater overall laboratory efficiency than the use of multiple meth...

Laboratory analytical methods for the determination of the hydrocarbon status of soils (a review)

NASA Astrophysics Data System (ADS)

Pikovskii, Yu. I.; Korotkov, L. A.; Smirnova, M. A.; Kovach, R. G.

2017-10-01

Laboratory analytical methods suitable for the determination of the hydrocarbon status of soils (a specific soil characteristic involving information on the total content and qualitative features of soluble (bitumoid) carbonaceous substances and individual hydrocarbons (polycyclic aromatic hydrocarbons, alkanes, etc.) in bitumoid, as well as the composition and content of hydrocarbon gases) have been considered. Among different physicochemical methods of study, attention is focused on the methods suitable for the wide use. Luminescence-bituminological analysis, low-temperature spectrofluorimetry (Shpolskii spectroscopy), infrared (IR) spectroscopy, gas chromatography, chromatography-mass spectrometry, and some other methods have been characterized, as well as sample preparation features. Advantages and limitations of each of these methods are described; their efficiency, instrumental complexity, analysis duration, and accuracy are assessed.

Waveguides for performing enzymatic reactions

DOEpatents

Levene; Michael J. , Korlach; Jonas , Turner; Stephen W. , Craighead; Harold G. , Webb; Watt W.

2007-11-06

The present invention is directed to a method and an apparatus for analysis of an analyte. The method involves providing a zero-mode waveguide which includes a cladding surrounding a core where the cladding is configured to preclude propagation of electromagnetic energy of a frequency less than a cutoff frequency longitudinally through the core of the zero-mode waveguide. The analyte is positioned in the core of the zero-mode waveguide and is then subjected, in the core of the zero-mode wave guide, to activating electromagnetic radiation of a frequency less than the cut-off frequency under conditions effective to permit analysis of the analyte in an effective observation volume which is more compact than if the analysis were carried out in the absence of the zero-mode waveguide.

Zero-mode waveguides

DOEpatents

Levene, Michael J.; Korlach, Jonas; Turner, Stephen W.; Craighead, Harold G.; Webb, Watt W.

2007-02-20

The present invention is directed to a method and an apparatus for analysis of an analyte. The method involves providing a zero-mode waveguide which includes a cladding surrounding a core where the cladding is configured to preclude propagation of electromagnetic energy of a frequency less than a cutoff frequency longitudinally through the core of the zero-mode waveguide. The analyte is positioned in the core of the zero-mode waveguide and is then subjected, in the core of the zero-mode waveguide, to activating electromagnetic radiation of a frequency less than the cut-off frequency under conditions effective to permit analysis of the analyte in an effective observation volume which is more compact than if the analysis were carried out in the absence of the zero-mode waveguide.

Analytical solutions for determining residual stresses in two-dimensional domains using the contour method

PubMed Central

Kartal, Mehmet E.

2013-01-01

The contour method is one of the most prevalent destructive techniques for residual stress measurement. Up to now, the method has involved the use of the finite-element (FE) method to determine the residual stresses from the experimental measurements. This paper presents analytical solutions, obtained for a semi-infinite strip and a finite rectangle, which can be used to calculate the residual stresses directly from the measured data; thereby, eliminating the need for an FE approach. The technique is then used to determine the residual stresses in a variable-polarity plasma-arc welded plate and the results show good agreement with independent neutron diffraction measurements. PMID:24204187

Combining Heterogeneous Correlation Matrices: Simulation Analysis of Fixed-Effects Methods

ERIC Educational Resources Information Center

Hafdahl, Adam R.

2008-01-01

Monte Carlo studies of several fixed-effects methods for combining and comparing correlation matrices have shown that two refinements improve estimation and inference substantially. With rare exception, however, these simulations have involved homogeneous data analyzed using conditional meta-analytic procedures. The present study builds on…

Stress state estimation in multilayer support of vertical shafts, considering off-design cross-sectional deformation

NASA Astrophysics Data System (ADS)

Antsiferov, SV; Sammal, AS; Deev, PV

2018-03-01

To determine the stress-strain state of multilayer support of vertical shafts, including cross-sectional deformation of the tubing rings as against the design, the authors propose an analytical method based on the provision of the mechanics of underground structures and surrounding rock mass as the elements of an integrated deformable system. The method involves a rigorous solution of the corresponding problem of elasticity, obtained using the mathematical apparatus of the theory of analytic functions of a complex variable. The design method is implemented as a software program allowing multivariate applied computation. Examples of the calculation are given.

Gold Nanorods as Plasmonic Sensors for Particle Diffusion.

PubMed

Wulf, Verena; Knoch, Fabian; Speck, Thomas; Sönnichsen, Carsten

2016-12-01

Plasmonic gold nanoparticles are normally used as sensor to detect analytes permanently bound to their surface. If the interaction between the analyte and the nanosensor surface is negligible, it only diffuses through the sensor's sensing volume, causing a small temporal shift of the plasmon resonance position. By using a very sensitive and fast detection scheme, we are able to detect these small fluctuations in the plasmon resonance. With the help of a theoretical model consistent with our detection geometry, we determine the analyte's diffusion coefficient. The method is verified by observing the trends upon changing diffusor size and medium viscosity, and the diffusion coefficients obtained were found to reflect reduced diffusion close to a solid interface. Our method, which we refer to as NanoPCS (for nanoscale plasmon correlation spectroscopy), is of practical importance for any application involving the diffusion of analytes close to nanoparticles.

HR-ICPMS ANALYTICAL METHODS DEVELOPMENT

EPA Science Inventory

Recent HEASD studies involving atmospheric sampling in remote areas (Barrow, Alaska; Cheeka Peak, Washington; Mauna Loa, Hawaii; Ny-Alesund, Norway; aircraft measurements off Florida's Atlantic coast) and low volume personal exposure monitoring (Baltimore, Maryland; Fresno, Calif...

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.

A two-dimensional analytical model of vapor intrusion involving vertical heterogeneity.

PubMed

Yao, Yijun; Verginelli, Iason; Suuberg, Eric M

2017-05-01

In this work, we present an analytical chlorinated vapor intrusion (CVI) model that can estimate source-to-indoor air concentration attenuation by simulating two-dimensional (2-D) vapor concentration profile in vertically heterogeneous soils overlying a homogenous vapor source. The analytical solution describing the 2-D soil gas transport was obtained by applying a modified Schwarz-Christoffel mapping method. A partial field validation showed that the developed model provides results (especially in terms of indoor emission rates) in line with the measured data from a case involving a building overlying a layered soil. In further testing, it was found that the new analytical model can very closely replicate the results of three-dimensional (3-D) numerical models at steady state in scenarios involving layered soils overlying homogenous groundwater sources. By contrast, by adopting a two-layer approach (capillary fringe and vadose zone) as employed in the EPA implementation of the Johnson and Ettinger model, the spatially and temporally averaged indoor concentrations in the case of groundwater sources can be higher than the ones estimated by the numerical model up to two orders of magnitude. In short, the model proposed in this work can represent an easy-to-use tool that can simulate the subsurface soil gas concentration in layered soils overlying a homogenous vapor source while keeping the simplicity of an analytical approach that requires much less computational effort.

Quantification of HCV RNA in Liver Tissue by bDNA Assay.

PubMed

Dailey, P J; Collins, M L; Urdea, M S; Wilber, J C

1999-01-01

With this statement, Sherlock and Dooley have described two of the three major challenges involved in quantitatively measuring any analyte in tissue samples: the distribution of the analyte in the tissue; and the standard of reference, or denominator, with which to make comparisons between tissue samples. The third challenge for quantitative measurement of an analyte in tissue is to ensure reproducible and quantitative recovery of the analyte on extraction from tissue samples. This chapter describes a method that can be used to measure HCV RNA quantitatively in liver biopsy and tissue samples using the bDNA assay. All three of these challenges-distribution, denominator, and recovery-apply to the measurement of HCV RNA in liver biopsies.

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.

On a class of integrals of Legendre polynomials with complicated arguments--with applications in electrostatics and biomolecular modeling.

PubMed

Yu, Yi-Kuo

2003-08-15

The exact analytical result for a class of integrals involving (associated) Legendre polynomials of complicated argument is presented. The method employed can in principle be generalized to integrals involving other special functions. This class of integrals also proves useful in the electrostatic problems in which dielectric spheres are involved, which is of importance in modeling the dynamics of biological macromolecules. In fact, with this solution, a more robust foundation is laid for the Generalized Born method in modeling the dynamics of biomolecules. c2003 Elsevier B.V. All rights reserved.

Progressive damage, fracture predictions and post mortem correlations for fiber composites

NASA Technical Reports Server (NTRS)

1985-01-01

Lewis Research Center is involved in the development of computational mechanics methods for predicting the structural behavior and response of composite structures. In conjunction with the analytical methods development, experimental programs including post failure examination are conducted to study various factors affecting composite fracture such as laminate thickness effects, ply configuration, and notch sensitivity. Results indicate that the analytical capabilities incorporated in the CODSTRAN computer code are effective in predicting the progressive damage and fracture of composite structures. In addition, the results being generated are establishing a data base which will aid in the characterization of composite fracture.

Cell bioprocessing in space - Applications of analytical cytology

NASA Technical Reports Server (NTRS)

Todd, P.; Hymer, W. C.; Goolsby, C. L.; Hatfield, J. M.; Morrison, D. R.

1988-01-01

Cell bioprocessing experiments in space are reviewed and the development of on-board cell analytical cytology techniques that can serve such experiments is discussed. Methods and results of experiments involving the cultivation and separation of eukaryotic cells in space are presented. It is suggested that an advanced cytometer should be developed for the quantitative analysis of large numbers of specimens of suspended eukaryotic cells and bioparticles in experiments on the Space Station.

Pythagorean fuzzy analytic hierarchy process to multi-criteria decision making

NASA Astrophysics Data System (ADS)

Mohd, Wan Rosanisah Wan; Abdullah, Lazim

2017-11-01

A numerous approaches have been proposed in the literature to determine the criteria of weight. The weight of criteria is very significant in the process of decision making. One of the outstanding approaches that used to determine weight of criteria is analytic hierarchy process (AHP). This method involves decision makers (DMs) to evaluate the decision to form the pair-wise comparison between criteria and alternatives. In classical AHP, the linguistic variable of pairwise comparison is presented in terms of crisp value. However, this method is not appropriate to present the real situation of the problems because it involved the uncertainty in linguistic judgment. For this reason, AHP has been extended by incorporating the Pythagorean fuzzy sets. In addition, no one has found in the literature proposed how to determine the weight of criteria using AHP under Pythagorean fuzzy sets. In order to solve the MCDM problem, the Pythagorean fuzzy analytic hierarchy process is proposed to determine the criteria weight of the evaluation criteria. Using the linguistic variables, pairwise comparison for evaluation criteria are made to the weights of criteria using Pythagorean fuzzy numbers (PFNs). The proposed method is implemented in the evaluation problem in order to demonstrate its applicability. This study shows that the proposed method provides us with a useful way and a new direction in solving MCDM problems with Pythagorean fuzzy context.

What we-authors, reviewers and editors of scientific work-can learn from the analytical history of biological 3-nitrotyrosine.

PubMed

Tsikas, Dimitrios

2017-07-15

Tyrosine and tyrosine residues in proteins are attacked by the reactive oxygen and nitrogen species peroxynitrite (O=N-OO - ) to generate 3-nitrotyrosine (3-NT) and 3-nitrotyrosine-proteins (3-NTProt), respectively. 3-NT and 3-NTProt are widely accepted as biomarkers of nitr(os)ative stress. Over the years many different analytical methods have been reported for 3-NT and 3-NTProt. Reported concentrations often differ by more than three orders of magnitude, indicative of serious analytical problems. Strategies to overcome pre-analytical and analytical shortcomings and pitfalls have been proposed. The present review investigated whether recently published work on the quantitative measurement of biological 3-nitrotyrosine did adequately consider the analytical past of this biomolecule. 3-Nitrotyrosine was taken as a representative of biomolecules that occur in biological samples in the pM-to-nM concentration range. This examination revealed that in many cases the main protagonists involved in the publication of scientific work, i.e., authors, reviewers and editors, failed to do so. Learning from the analytical history of 3-nitrotyrosine means advancing analytical and biological science and implies the following key issues. (1) Choosing the most reliable analytical approach in terms of sensitivity and accuracy; presently this is best feasible by stable-isotope dilution tandem mass spectrometry coupled with gas chromatography (GC-MS/MS) or liquid chromatography (LC-MS/MS). (2) Minimizing artificial formation of 3-nitrotyrosine during sample work up, a major pitfall in 3-nitrotyrosine analysis. (3) Validating adequately the final method in the intendent biological matrix and the established concentration range. (4) Inviting experts in the field for critical evaluation of the novelty and reliability of the proposed analytical method, placing special emphasis on the compliance of the analytical outcome with 3-nitrotyrosine concentrations obtained by validated GC-MS/MS and LC-MS/MS methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultraviolet, Visible, and Fluorescence Spectroscopy

NASA Astrophysics Data System (ADS)

Penner, Michael H.

Spectroscopy in the ultraviolet-visible (UV-Vis) range is one of the most commonly encountered laboratory techniques in food analysis. Diverse examples, such as the quantification of macrocomponents (total carbohydrate by the phenol-sulfuric acid method), quantification of microcomponents, (thiamin by the thiochrome fluorometric procedure), estimates of rancidity (lipid oxidation status by the thiobarbituric acid test), and surveillance testing (enzyme-linked immunoassays), are presented in this text. In each of these cases, the analytical signal for which the assay is based is either the emission or absorption of radiation in the UV-Vis range. This signal may be inherent in the analyte, such as the absorbance of radiation in the visible range by pigments, or a result of a chemical reaction involving the analyte, such as the colorimetric copper-based Lowry method for the analysis of soluble protein.

Zero-mode clad waveguides for performing spectroscopy with confined effective observation volumes

DOEpatents

Levene, Michael J.; Korlach, Jonas; Turner, Stephen W.; Craighead, Harold G.; Webb, Watt W.

2005-07-12

The present invention is directed to a method and an apparatus for analysis of an analyte. The method involves providing a zero-mode waveguide which includes a cladding surrounding a core where the cladding is configured to preclude propagation of electromagnetic energy of a frequency less than a cutoff frequency longitudinally through the core of the zero-mode waveguide. The analyte is positioned in the core of the zero-mode waveguide and is then subjected, in the core of the zero-mode waveguide, to activating electromagnetic radiation of a frequency less than the cut-off frequency under conditions effective to permit analysis of the analyte in an effective observation volume which is more compact than if the analysis were carried out in the absence of the zero-mode waveguide.

Waveguides for performing spectroscopy with confined effective observation volumes

DOEpatents

Levene, Michael J.; Korlach, Jonas; Turner, Stephen W.; Craighead, Harold G.; Webb, Watt W.

2006-03-14

The present invention is directed to a method and an apparatus for analysis of an analyte. The method involves providing a zero-mode waveguide which includes a cladding surrounding a core where the cladding is configured to preclude propagation of electromagnetic energy of a frequency less than a cutoff frequency longitudinally through the core of the zero-mode waveguide. The analyte is positioned in the core of the zero-mode waveguide and is then subjected, in the core of the zero-mode waveguide, to activating electromagnetic radiation of a frequency less than the cut-off frequency under conditions effective to permit analysis of the analyte in an effective observation volume which is more compact than if the analysis were carried out in the absence of the zero-mode waveguide.

Monitoring occupational exposure to cancer chemotherapy drugs

NASA Technical Reports Server (NTRS)

Baker, E. S.; Connor, T. H.

1996-01-01

Reports of the health effects of handling cytotoxic drugs and compliance with guidelines for handling these agents are briefly reviewed, and studies using analytical and biological methods of detecting exposure are evaluated. There is little conclusive evidence of detrimental health effects from occupational exposure to cytotoxic drugs. Work practices have improved since the issuance of guidelines for handling these drugs, but compliance with the recommended practices is still inadequate. Of 64 reports published since 1979 on studies of workers' exposure to these drugs, 53 involved studies of changes in cellular or molecular endpoints (biological markers) and 12 described chemical analyses of drugs or their metabolites in urine (2 involved both, and 2 reported the same study). The primary biological markers used were urine mutagenicity, sister chromatid exchange, and chromosomal aberrations; other studies involved formation of micronuclei and measurements of urinary thioethers. The studies had small sample sizes, and the methods were qualitative, nonspecific, subject to many confounders, and possibly not sensitive enough to detect most occupational exposures. Since none of the currently available biological and analytical methods is sufficiently reliable or reproducible for routine monitoring of exposure in the workplace, further studies using these methods are not recommended; efforts should focus instead on wide-spread implementation of improved practices for handling cytotoxic drugs.

Applications of computer algebra to distributed parameter systems

NASA Technical Reports Server (NTRS)

Storch, Joel A.

1993-01-01

In the analysis of vibrations of continuous elastic systems, one often encounters complicated transcendental equations with roots directly related to the system's natural frequencies. Typically, these equations contain system parameters whose values must be specified before a numerical solution can be obtained. The present paper presents a method whereby the fundamental frequency can be obtained in analytical form to any desired degree of accuracy. The method is based upon truncation of rapidly converging series involving inverse powers of the system natural frequencies. A straightforward method to developing these series and summing them in closed form is presented. It is demonstrated how Computer Algebra can be exploited to perform the intricate analytical procedures which otherwise would render the technique difficult to apply in practice. We illustrate the method by developing two analytical approximations to the fundamental frequency of a vibrating cantilever carrying a rigid tip body. The results are compared to the numerical solution of the exact (transcendental) frequency equation over a range of system parameters.

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…

On Manpower Forecasting. Methods for Manpower Analysis, No.2.

ERIC Educational Resources Information Center

Morton, J.E.

Some of the problems and techniques involved in manpower forecasting are discussed. This non-technical introduction to the field aims at reducing fears of data manipulation methods and at increasing respect for conceptual, logical, and analytical issues. The major approaches to manpower forecasting are explicated and evaluated under the headings:…

Evaluation of two methods to determine glyphosate and AMPA in soils of Argentina

NASA Astrophysics Data System (ADS)

De Geronimo, Eduardo; Lorenzon, Claudio; Iwasita, Barbara; Faggioli, Valeria; Aparicio, Virginia; Costa, Jose Luis

2017-04-01

Argentine agricultural production is fundamentally based on a technological package combining no-tillage and the dependence of glyphosate applications to control weeds in transgenic crops (soybean, maize and cotton). Therefore, glyphosate is the most employed herbicide in the country, where 180 to 200 million liters are applied every year. Due to its widespread use, it is important to assess its impact on the environment and, therefore, reliable analytical methods are mandatory. Glyphosate molecule exhibits unique physical and chemical characteristics which difficult its quantification, especially in soils with high organic matter content, such as the central eastern Argentine soils, where strong interferences are normally observed. The objective of this work was to compare two methods for extraction and quantification of glyphosate and AMPA in samples of 8 representative soils of Argentina. The first analytical method (method 1) was based on the use of phosphate buffer as extracting solution and dichloromethane to minimize matrix organic content. In the second method (method 2), potassium hydroxide was used to extract the analytes followed by a clean-up step using solid phase extraction (SPE) to minimize strong interferences. Sensitivity, recoveries, matrix effects and robustness were evaluated. Both methodologies involved a derivatization with 9-fluorenyl-methyl-chloroformate (FMOC) in borate buffer and detection based on ultra-high-pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Recoveries obtained from soil samples spiked at 0.1 and 1 mg kg-1 and were satisfactory in both methods (70% - 120%). However, there was a remarkable difference regarding the matrix effect, being the SPE clean-up step (method 2) insufficient to remove the interferences. Whereas the dilution and the clean-up with dichloromethane (method 1) were more effective minimizing the ionic suppression. Moreover, method 1 had fewer steps in the protocol of sample processing than method 2. This can be highly valuable in the routine lab work due to the reduction of potential undesired errors such as the loss of analyte or sample contamination. In addition, the substitution of SPE by another alternative involved a considerable reduction of analytical costs in method 1. We conclude that method 1 seemed to be simpler and cheaper than method 2, as well as reliable to quantify glyphosate in Argentinean soils. We hope that this experience can be useful to simplify the protocols of glyphosate quantification and contribute to the understanding of the fate of this herbicide in the environment.

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

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.

Students' science process skill and analytical thinking ability in chemistry learning

NASA Astrophysics Data System (ADS)

Irwanto, Rohaeti, Eli; Widjajanti, Endang; Suyanta

2017-08-01

Science process skill and analytical thinking ability are needed in chemistry learning in 21st century. Analytical thinking is related with science process skill which is used by students to solve complex and unstructured problems. Thus, this research aims to determine science process skill and analytical thinking ability of senior high school students in chemistry learning. The research was conducted in Tiga Maret Yogyakarta Senior High School, Indonesia, at the middle of the first semester of academic year 2015/2016 is using the survey method. The survey involved 21 grade XI students as participants. Students were given a set of test questions consists of 15 essay questions. The result indicated that the science process skill and analytical thinking ability were relatively low ie. 30.67%. Therefore, teachers need to improve the students' cognitive and psychomotor domains effectively in learning process.

Student Receivables Management: Opportunities for Improved Practices.

ERIC Educational Resources Information Center

Jacquin, Jules C.; Goyal, Anil K.

1995-01-01

The college or university's business office can help reduce problems with student receivables through procedural review of the tuition revenue process, application of analytical methods, and improved operating practices. Admissions, financial aid, and billing offices must all be involved. (MSE)

Triangular dislocation: an analytical, artefact-free solution

NASA Astrophysics Data System (ADS)

Nikkhoo, Mehdi; Walter, Thomas R.

2015-05-01

Displacements and stress-field changes associated with earthquakes, volcanoes, landslides and human activity are often simulated using numerical models in an attempt to understand the underlying processes and their governing physics. The application of elastic dislocation theory to these problems, however, may be biased because of numerical instabilities in the calculations. Here, we present a new method that is free of artefact singularities and numerical instabilities in analytical solutions for triangular dislocations (TDs) in both full-space and half-space. We apply the method to both the displacement and the stress fields. The entire 3-D Euclidean space {R}3 is divided into two complementary subspaces, in the sense that in each one, a particular analytical formulation fulfils the requirements for the ideal, artefact-free solution for a TD. The primary advantage of the presented method is that the development of our solutions involves neither numerical approximations nor series expansion methods. As a result, the final outputs are independent of the scale of the input parameters, including the size and position of the dislocation as well as its corresponding slip vector components. Our solutions are therefore well suited for application at various scales in geoscience, physics and engineering. We validate the solutions through comparison to other well-known analytical methods and provide the MATLAB codes.

Analytical solutions for tomato peeling with combined heat flux and convective boundary conditions

NASA Astrophysics Data System (ADS)

Cuccurullo, G.; Giordano, L.; Metallo, A.

2017-11-01

Peeling of tomatoes by radiative heating is a valid alternative to steam or lye, which are expensive and pollutant methods. Suitable energy densities are required in order to realize short time operations, thus involving only a thin layer under the tomato surface. This paper aims to predict the temperature field in rotating tomatoes exposed to the source irradiation. Therefore, a 1D unsteady analytical model is presented, which involves a semi-infinite slab subjected to time dependent heating while convective heat transfer takes place on the exposed surface. In order to account for the tomato rotation, the heat source is described as the positive half-wave of a sinusoidal function. The problem being linear, the solution is derived following the Laplace Transform Method. In addition, an easy-to-handle solution for the problem at hand is presented, which assumes a differentiable function for approximating the source while neglecting convective cooling, the latter contribution turning out to be negligible for the context at hand. A satisfying agreement between the two analytical solutions is found, therefore, an easy procedure for a proper design of the dry heating system can be set up avoiding the use of numerical simulations.

Separation-oriented derivatization of native fluorescent compounds through fluorous labeling followed by liquid chromatography with fluorous-phase.

PubMed

Sakaguchi, Yohei; Yoshida, Hideyuki; Todoroki, Kenichiro; Nohta, Hitoshi; Yamaguchi, Masatoshi

2009-06-15

We have developed a new and simple method based on "fluorous derivatization" for LC of native fluorescent compounds. This method involves the use of a column with a fluorous stationary phase. Native fluorescent analytes with target functional groups are precolumn derivatized with a nonfluorescent fluorous tag, and the fluorous-labeled analytes are retained in the column, whereas underivatized substances are not. Only the retained fluorescent analytes are detected fluorometrically at appropriate retention times, and retained substrates without fluorophores are not detected. In this study, biologically important carboxylic acids (homovanillic acid, vanillylmandelic acid, and 5-hydroxyindoleacetic acid) and drugs (naproxen, felbinac, flurbiprofen, and etodolac) were used as model native fluorescent compounds. Experimental results indicate that the fluorous-phase column can selectively retain fluorous compounds including fluorous-labeled analytes on the basis of fluorous separation. We believe that separation-oriented derivatization presented here is the first step toward the introduction of fluorous derivatization in quantitative LC analysis.

Prediction of turning stability using receptance coupling

NASA Astrophysics Data System (ADS)

Jasiewicz, Marcin; Powałka, Bartosz

2018-01-01

This paper presents an issue of machining stability prediction of dynamic "lathe - workpiece" system evaluated using receptance coupling method. Dynamic properties of the lathe components (the spindle and the tailstock) are assumed to be constant and can be determined experimentally based on the results of the impact test. Hence, the variable of the system "machine tool - holder - workpiece" is the machined part, which can be easily modelled analytically. The method of receptance coupling enables a synthesis of experimental (spindle, tailstock) and analytical (machined part) models, so impact testing of the entire system becomes unnecessary. The paper presents methodology of analytical and experimental models synthesis, evaluation of the stability lobes and experimental validation procedure involving both the determination of the dynamic properties of the system and cutting tests. In the summary the experimental verification results would be presented and discussed.

Analytical Glycobiology at High Sensitivity: Current Approaches and Directions

PubMed Central

Novotny, Milos V.; Alley, William R.; Mann, Benjamin F.

2013-01-01

This review summarizes the analytical advances made during the last several years in the structural and quantitative determinations of glycoproteins in complex biological mixtures. The main analytical techniques used in the fields of glycomics and glycoproteomics involve different modes of mass spectrometry and their combinations with capillary separation methods such as microcolumn liquid chromatography and capillary electrophoresis. The needs for high-sensitivity measurements have been emphasized in the oligosaccharide profiling used in the field of biomarker discovery through MALDI mass spectrometry. High-sensitivity profiling of both glycans and glycopeptides from biological fluids and tissue extracts has been aided significantly through lectin preconcentration and the uses of affinity chromatography. PMID:22945852

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.

Quantification of astaxanthin in shrimp waste hydrolysate by HPLC.

PubMed

López-Cervantes, J; Sánchez-Machado, D I; Gutiérrez-Coronado, M A; Ríos-Vázquez, N J

2006-10-01

In the present study, a simple and rapid reversed-phase HPLC method for the determination of astaxanthin in shrimp waste hydrolysate has been developed and validated. The analytical procedure involves the direct extraction of astaxanthin from the lipid fraction with methanol. The analytical column, SS Exil ODS, was operated at 25C. The mobile phase consisted of a mixture of water:methanol:dichloromethane:acetonitrile (4.5:28:22:45.5 v/v/v/v) at a flow rate of 1.0 mL/min. Detection and identification were performed using a photodiode array detector (lambda(detection) = 476 nm). The proposed HPLC method showed adequate linearity, repeatability and accuracy.

Qualitative methods in quantum theory

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

Migdal, A.B.

The author feels that the solution of most problems in theoretical physics begins with the application of qualitative methods - dimensional estimates and estimates made from simple models, the investigation of limiting cases, the use of the analytic properties of physical quantities, etc. This book proceeds in this spirit, rather than in a formal, mathematical way with no traces of the sweat involved in the original work left to show. The chapters are entitled Dimensional and model approximations, Various types of perturbation theory, The quasi-classical approximation, Analytic properties of physical quantities, Methods in the many-body problem, and Qualitative methods inmore » quantum field theory. Each chapter begins with a detailed introduction, in which the physical meaning of the results obtained in that chapter is explained in a simple way. 61 figures. (RWR)« less

Handling Missing Data in Educational Research Using SPSS

ERIC Educational Resources Information Center

Cheema, Jehanzeb

2012-01-01

This study looked at the effect of a number of factors such as the choice of analytical method, the handling method for missing data, sample size, and proportion of missing data, in order to evaluate the effect of missing data treatment on accuracy of estimation. In order to accomplish this a methodological approach involving simulated data was…

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.

Comparison of three sampling and analytical methods for the determination of airborne hexavalent chromium.

PubMed

Boiano, J M; Wallace, M E; Sieber, W K; Groff, J H; Wang, J; Ashley, K

2000-08-01

A field study was conducted with the goal of comparing the performance of three recently developed or modified sampling and analytical methods for the determination of airborne hexavalent chromium (Cr(VI)). The study was carried out in a hard chrome electroplating facility and in a jet engine manufacturing facility where airborne Cr(VI) was expected to be present. The analytical methods evaluated included two laboratory-based procedures (OSHA Method ID-215 and NIOSH Method 7605) and a field-portable method (NIOSH Method 7703). These three methods employ an identical sampling methodology: collection of Cr(VI)-containing aerosol on a polyvinyl chloride (PVC) filter housed in a sampling cassette, which is connected to a personal sampling pump calibrated at an appropriate flow rate. The basis of the analytical methods for all three methods involves extraction of the PVC filter in alkaline buffer solution, chemical isolation of the Cr(VI) ion, complexation of the Cr(VI) ion with 1,5-diphenylcarbazide, and spectrometric measurement of the violet chromium diphenylcarbazone complex at 540 nm. However, there are notable specific differences within the sample preparation procedures used in three methods. To assess the comparability of the three measurement protocols, a total of 20 side-by-side air samples were collected, equally divided between a chromic acid electroplating operation and a spray paint operation where water soluble forms of Cr(VI) were used. A range of Cr(VI) concentrations from 0.6 to 960 microg m(-3), with Cr(VI) mass loadings ranging from 0.4 to 32 microg, was measured at the two operations. The equivalence of the means of the log-transformed Cr(VI) concentrations obtained from the different analytical methods was compared. Based on analysis of variance (ANOVA) results, no statistically significant differences were observed between mean values measured using each of the three methods. Small but statistically significant differences were observed between results obtained from performance evaluation samples for the NIOSH field method and the OSHA laboratory method.

Method and means for dynamic measurement of rates of adsorption from solutions

DOEpatents

Slomka, Bogdan J.; Buttermore, William H.

1992-05-05

A method and apparatus for dynamic measurement of rates of absorption from solutions. The method has the advantage of avoiding the use of solvent normally used to establish a baseline. The method involves pre-evacuating the adsorbent contained in an adsorbent cell and thereafter rapidly contacting the adsorbent with analytical solution, all without prior exposure of adsorbent to pure solvent. The result is a sharp characteristic adsorption line.

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.

Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

PubMed

Goudarzi, Nasser

2009-02-11

A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples.

Development of NIRS method for quality control of drug combination artesunate–azithromycin for the treatment of severe malaria

PubMed Central

Boyer, Chantal; Gaudin, Karen; Kauss, Tina; Gaubert, Alexandra; Boudis, Abdelhakim; Verschelden, Justine; Franc, Mickaël; Roussille, Julie; Boucher, Jacques; Olliaro, Piero; White, Nicholas J.; Millet, Pascal; Dubost, Jean-Pierre

2012-01-01

Near infrared spectroscopy (NIRS) methods were developed for the determination of analytical content of an antimalarial-antibiotic (artesunate and azithromycin) co-formulation in hard gelatin capsule (HGC). The NIRS consists of pre-processing treatment of spectra (raw spectra and first-derivation of two spectral zones), a unique principal component analysis model to ensure the specificity and then two partial least-squares regression models for the determination content of each active pharmaceutical ingredient. The NIRS methods were developed and validated with no reference method, since the manufacturing process of HGC is basically mixed excipients with active pharmaceutical ingredients. The accuracy profiles showed β-expectation tolerance limits within the acceptance limits (±5%). The analytical control approach performed by reversed phase (HPLC) required two different methods involving two different preparation and chromatographic methods. NIRS offers advantages in terms of lower costs of equipment and procedures, time saving, environmentally friendly. PMID:22579599

Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

NASA Astrophysics Data System (ADS)

Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

2006-12-01

A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

Benchmark Comparison of Cloud Analytics Methods Applied to Earth Observations

NASA Technical Reports Server (NTRS)

Lynnes, Chris; Little, Mike; Huang, Thomas; Jacob, Joseph; Yang, Phil; Kuo, Kwo-Sen

2016-01-01

Cloud computing has the potential to bring high performance computing capabilities to the average science researcher. However, in order to take full advantage of cloud capabilities, the science data used in the analysis must often be reorganized. This typically involves sharding the data across multiple nodes to enable relatively fine-grained parallelism. This can be either via cloud-based file systems or cloud-enabled databases such as Cassandra, Rasdaman or SciDB. Since storing an extra copy of data leads to increased cost and data management complexity, NASA is interested in determining the benefits and costs of various cloud analytics methods for real Earth Observation cases. Accordingly, NASA's Earth Science Technology Office and Earth Science Data and Information Systems project have teamed with cloud analytics practitioners to run a benchmark comparison on cloud analytics methods using the same input data and analysis algorithms. We have particularly looked at analysis algorithms that work over long time series, because these are particularly intractable for many Earth Observation datasets which typically store data with one or just a few time steps per file. This post will present side-by-side cost and performance results for several common Earth observation analysis operations.

Benchmark Comparison of Cloud Analytics Methods Applied to Earth Observations

NASA Astrophysics Data System (ADS)

Lynnes, C.; Little, M. M.; Huang, T.; Jacob, J. C.; Yang, C. P.; Kuo, K. S.

2016-12-01

Cloud computing has the potential to bring high performance computing capabilities to the average science researcher. However, in order to take full advantage of cloud capabilities, the science data used in the analysis must often be reorganized. This typically involves sharding the data across multiple nodes to enable relatively fine-grained parallelism. This can be either via cloud-based filesystems or cloud-enabled databases such as Cassandra, Rasdaman or SciDB. Since storing an extra copy of data leads to increased cost and data management complexity, NASA is interested in determining the benefits and costs of various cloud analytics methods for real Earth Observation cases. Accordingly, NASA's Earth Science Technology Office and Earth Science Data and Information Systems project have teamed with cloud analytics practitioners to run a benchmark comparison on cloud analytics methods using the same input data and analysis algorithms. We have particularly looked at analysis algorithms that work over long time series, because these are particularly intractable for many Earth Observation datasets which typically store data with one or just a few time steps per file. This post will present side-by-side cost and performance results for several common Earth observation analysis operations.

Use of LC-HRMS in full scan-XIC mode for multi-analyte urine drug testing - a step towards a 'black-box' solution?

PubMed

Stephanson, N N; Signell, P; Helander, A; Beck, O

2017-08-01

The influx of new psychoactive substances (NPS) has created a need for improved methods for drug testing in toxicology laboratories. The aim of this work was to design, validate and apply a multi-analyte liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method for screening of 148 target analytes belonging to the NPS class, plant alkaloids and new psychoactive therapeutic drugs. The analytical method used a fivefold dilution of urine with nine deuterated internal standards and injection of 2 μl. The LC system involved a 2.0 μm 100 × 2.0 mm YMC-UltraHT Hydrosphere-C 18 column and gradient elution with a flow rate of 0.5 ml/min and a total analysis time of 6.0 min. Solvent A consisted of 10 mmol/l ammonium formate and 0.005% formic acid, pH 4.8, and Solvent B was methanol with 10 mmol/l ammonium formate and 0.005% formic acid. The HRMS (Q Exactive, Thermo Scientific) used a heated electrospray interface and was operated in positive mode with 70 000 resolution. The scan range was 100-650 Da, and data for extracted ion chromatograms used ± 10 ppm tolerance. Product ion monitoring was applied for confirmation analysis and for some selected analytes also for screening. Method validation demonstrated limited influence from urine matrix, linear response within the measuring range (typically 0.1-1.0 μg/ml) and acceptable imprecision in quantification (CV <15%). A few analytes were found to be unstable in urine upon storage. The method was successfully applied for routine drug testing of 17 936 unknown samples, of which 2715 (15%) contained 52 of the 148 analytes. It is concluded that the method design based on simple dilution of urine and using LC-HRMS in extracted ion chromatogram mode may offer an analytical system for urine drug testing that fulfils the requirement of a 'black box' solution and can replace immunochemical screening applied on autoanalyzers. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Multiresidue analytical method for pharmaceuticals and personal care products in sewage and sewage sludge by online direct immersion SPME on-fiber derivatization - GCMS.

PubMed

López-Serna, Rebeca; Marín-de-Jesús, David; Irusta-Mata, Rubén; García-Encina, Pedro Antonio; Lebrero, Raquel; Fdez-Polanco, María; Muñoz, Raúl

2018-08-15

The work here presented aimed at developing an analytical method for the simultaneous determination of 22 pharmaceuticals and personal care products, including 3 transformation products, in sewage and sludge. A meticulous method optimization, involving an experimental design, was carried out. The developed method was fully automated and consisted of the online extraction of 17 mL of water sample by Direct Immersion Solid Phase MicroExtraction followed by On-fiber Derivatization coupled to Gas Chromatography - Mass Spectrometry (DI-SPME - On-fiber Derivatization - GC - MS). This methodology was validated for 12 of the initial compounds as a reliable (relative recoveries above 90% for sewage and 70% for sludge; repeatability as %RSD below 10% in all cases), sensitive (LODs below 20 ng L -1 in sewage and 10 ng g -1 in sludge), versatile (sewage and sewage-sludge samples up to 15,000 ng L -1 and 900 ng g -1 , respectively) and green analytical alternative for many medium-tech routine laboratories around the world to keep up with both current and forecast environmental regulations requirements. The remaining 10 analytes initially considered showed insufficient suitability to be included in the final method. The methodology was successfully applied to real samples generated in a pilot scale sewage treatment reactor. Copyright © 2018 Elsevier B.V. All rights reserved.

Recommendations for accreditation of laboratories in molecular biology of hematologic malignancies.

PubMed

Flandrin-Gresta, Pascale; Cornillet, Pascale; Hayette, Sandrine; Gachard, Nathalie; Tondeur, Sylvie; Mauté, Carole; Cayuela, Jean-Michel

2015-01-01

Over recent years, the development of molecular biology techniques has improved the hematological diseases diagnostic and follow-up. Consequently, these techniques are largely used in the biological screening of these diseases; therefore the Hemato-oncology molecular diagnostics laboratories must be actively involved in the accreditation process according the ISO 15189 standard. The French group of molecular biologists (GBMHM) provides requirements for the implementation of quality assurance for the medical molecular laboratories. This guideline states the recommendations for the pre-analytical, analytical (methods validation procedures, quality controls, reagents), and post-analytical conditions. In addition, herein we state a strategy for the internal quality control management. These recommendations will be regularly updated.

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.

Statistical Discourse Analysis: A Method for Modelling Online Discussion Processes

ERIC Educational Resources Information Center

Chiu, Ming Ming; Fujita, Nobuko

2014-01-01

Online forums (synchronous and asynchronous) offer exciting data opportunities to analyze how people influence one another through their interactions. However, researchers must address several analytic difficulties involving the data (missing values, nested structure [messages within topics], non-sequential messages), outcome variables (discrete…

40 CFR 63.90 - Program overview.

Code of Federal Regulations, 2012 CFR

2012-07-01

... calibration gases or test cells; (4) Use of an analytical technology that differs from that specified by a... “proven technology” (generally accepted by the scientific community as equivalent or better) that is... enforceable test method involving “proven technology” (generally accepted by the scientific community as...

40 CFR 63.90 - Program overview.

Code of Federal Regulations, 2013 CFR

2013-07-01

... calibration gases or test cells; (4) Use of an analytical technology that differs from that specified by a... “proven technology” (generally accepted by the scientific community as equivalent or better) that is... enforceable test method involving “proven technology” (generally accepted by the scientific community as...

40 CFR 63.90 - Program overview.

Code of Federal Regulations, 2014 CFR

2014-07-01

... calibration gases or test cells; (4) Use of an analytical technology that differs from that specified by a... “proven technology” (generally accepted by the scientific community as equivalent or better) that is... enforceable test method involving “proven technology” (generally accepted by the scientific community as...

Delving Deeper: Transforming Shapes Physically and Analytically

ERIC Educational Resources Information Center

Rathouz, Margaret; Novak, Christopher; Clifford, John

2013-01-01

Constructing formulas "from scratch" for calculating geometric measurements of shapes--for example, the area of a triangle--involves reasoning deductively and drawing connections between different methods (Usnick, Lamphere, and Bright 1992). Visual and manipulative models also play a role in helping students understand the underlying…

Method and means for dynamic measurement of rates of adsorption from solutions

DOEpatents

Slomka, B.J.; Buttermore, W.H.

1992-05-05

A method and apparatus are described for the dynamic measurement of rates of absorption from solutions. The method has the advantage of avoiding the use of solvent normally used to establish a baseline. The method involves pre-evacuating the adsorbent contained in an adsorbent cell and thereafter rapidly contacting the adsorbent with analytical solution, all without prior exposure of adsorbent to pure solvent. The result is a sharp characteristic adsorption line. 5 figs.

Analytical and Biological Methods for Probing the Blood-Brain Barrier

PubMed Central

Sloan, Courtney D. Kuhnline; Nandi, Pradyot; Linz, Thomas H.; Aldrich, Jane V.; Audus, Kenneth L.; Lunte, Susan M.

2013-01-01

The blood-brain barrier (BBB) is an important interface between the peripheral and central nervous systems. It protects the brain against the infiltration of harmful substances and regulates the permeation of beneficial endogenous substances from the blood into the extracellular fluid of the brain. It can also present a major obstacle in the development of drugs that are targeted for the central nervous system. Several methods have been developed to investigate the transport and metabolism of drugs, peptides, and endogenous compounds at the BBB. In vivo methods include intravenous injection, brain perfusion, positron emission tomography, and microdialysis sampling. Researchers have also developed in vitro cell-culture models that can be employed to investigate transport and metabolism at the BBB without the complication of systemic involvement. All these methods require sensitive and selective analytical methods to monitor the transport and metabolism of the compounds of interest at the BBB. PMID:22708905

Ion-pairing HPLC methods to determine EDTA and DTPA in small molecule and biological pharmaceutical formulations.

PubMed

Wang, George; Tomasella, Frank P

2016-06-01

Ion-pairing high-performance liquid chromatography-ultraviolet (HPLC-UV) methods were developed to determine two commonly used chelating agents, ethylenediaminetetraacetic acid (EDTA) in Abilify® (a small molecule drug with aripiprazole as the active pharmaceutical ingredient) oral solution and diethylenetriaminepentaacetic acid (DTPA) in Yervoy® (a monoclonal antibody drug with ipilimumab as the active pharmaceutical ingredient) intravenous formulation. Since the analytes, EDTA and DTPA, do not contain chromophores, transition metal ions (Cu 2+ , Fe 3+ ) which generate highly stable metallocomplexes with the chelating agents were added into the sample preparation to enhance UV detection. The use of metallocomplexes with ion-pairing chromatography provides the ability to achieve the desired sensitivity and selectivity in the development of the method. Specifically, the sample preparation involving metallocomplex formation allowed sensitive UV detection. Copper was utilized for the determination of EDTA and iron was utilized for the determination of DTPA. In the case of EDTA, a gradient mobile phase separated the components of the formulation from the analyte. In the method for DTPA, the active drug substance, ipilimumab, was eluted in the void. In addition, the optimization of the concentration of the ion-pairing reagent was discussed as a means of enhancing the retention of the aminopolycarboxylic acids (APCAs) including EDTA and DTPA and the specificity of the method. The analytical method development was designed based on the chromatographic properties of the analytes, the nature of the sample matrix and the intended purpose of the method. Validation data were presented for the two methods. Finally, both methods were successfully utilized in determining the fate of the chelates.

Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water.

PubMed

Tobiszewski, Marek; Orłowski, Aleksander

2015-03-27

The study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists--decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as an example) were selected as input alternatives to MCDA analysis. Nine different criteria describing the alternatives were chosen from different groups--metrological, economical and the most importantly--environmental impact. The weights for each criterion were obtained from questionnaires that were sent to experts, giving three different scenarios for MCDA results. The results of analysis show that PROMETHEE is very promising tool to choose the analytical procedure with respect to its greenness. The rankings for all three scenarios placed solid phase microextraction and liquid phase microextraction--based procedures high, while liquid-liquid extraction, solid phase extraction and stir bar sorptive extraction--based procedures were placed low in the ranking. The results show that although some of the experts do not intentionally choose green analytical chemistry procedures, their MCDA choice is in accordance with green chemistry principles. The PROMETHEE ranking results were compared with more widely accepted green analytical chemistry tools--NEMI and Eco-Scale. As PROMETHEE involved more different factors than NEMI, the assessment results were only weakly correlated. Oppositely, the results of Eco-Scale assessment were well-correlated as both methodologies involved similar criteria of assessment. Copyright © 2015 Elsevier B.V. All rights reserved.

Tiered analytics for purity assessment of macrocyclic peptides in drug discovery: Analytical consideration and method development.

PubMed

Qian Cutrone, Jingfang Jenny; Huang, Xiaohua Stella; Kozlowski, Edward S; Bao, Ye; Wang, Yingzi; Poronsky, Christopher S; Drexler, Dieter M; Tymiak, Adrienne A

2017-05-10

Synthetic macrocyclic peptides with natural and unnatural amino acids have gained considerable attention from a number of pharmaceutical/biopharmaceutical companies in recent years as a promising approach to drug discovery, particularly for targets involving protein-protein or protein-peptide interactions. Analytical scientists charged with characterizing these leads face multiple challenges including dealing with a class of complex molecules with the potential for multiple isomers and variable charge states and no established standards for acceptable analytical characterization of materials used in drug discovery. In addition, due to the lack of intermediate purification during solid phase peptide synthesis, the final products usually contain a complex profile of impurities. In this paper, practical analytical strategies and methodologies were developed to address these challenges, including a tiered approach to assessing the purity of macrocyclic peptides at different stages of drug discovery. Our results also showed that successful progression and characterization of a new drug discovery modality benefited from active analytical engagement, focusing on fit-for-purpose analyses and leveraging a broad palette of analytical technologies and resources. Copyright © 2017. Published by Elsevier B.V.

Shedding light on food fraud: spectrophotometric and spectroscopic methods as a tool against economically motivated adulteration of food

NASA Astrophysics Data System (ADS)

Petronijević, R. B.; Velebit, B.; Baltić, T.

2017-09-01

Intentional modification of food or substitution of food ingredients with the aim of gaining profit is food fraud or economically motivated adulteration (EMA). EMA appeared in the food supply chain, and following the global expansion of the food market, has become a world-scale problem for the global economy. Food frauds have involved oils, milk and meat products, infant formula, honey, juices, spices, etc. New legislation was enacted in the last decade in order to fight EMA. Effective analytical methods for food fraud detection are few and still in development. The majority of the methods in common use today for EMA detection are time consuming and inappropriate for use on the production line or out of the laboratory. The next step in the evolution of analytical techniques to combat food fraud is development of fast, accurate methods applicable using portable or handheld devices. Spectrophotometric and spectroscopic methods combined with chemometric analysis, and perhaps in combination with other rapid physico-chemical techniques, could be the answer. This review discusses some analytical techniques based on spectrophotometry and spectroscopy, which are used to reveal food fraud and EMA.

Bio-analytical method development and validation of Rasagiline by high performance liquid chromatography tandem mass spectrometry detection and its application to pharmacokinetic study

PubMed Central

Konda, Ravi Kumar; Chandu, Babu Rao; Challa, B.R.; Kothapalli, Chandrasekhar B.

2012-01-01

The most suitable bio-analytical method based on liquid–liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mm×50 mm, 3.5 μm) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-4000 system. The total run time was 3.0 min. The proposed method has been validated with the linear range of 5–12000 pg/mL for Rasagiline. The intra-run and inter-run precision values were within 1.3%–2.9% and 1.6%–2.2% respectively for Rasagiline. The overall recovery for Rasagiline and Rasagiline-13C3 mesylate analog was 96.9% and 96.7% respectively. This validated method was successfully applied to the bioequivalence and pharmacokinetic study of human volunteers under fasting condition. PMID:29403764

On-Site Detection as a Countermeasure to Chemical Warfare/Terrorism.

PubMed

Seto, Y

2014-01-01

On-site monitoring and detection are necessary in the crisis and consequence management of wars and terrorism involving chemical warfare agents (CWAs) such as sarin. The analytical performance required for on-site detection is mainly determined by the fatal vapor concentration and volatility of the CWAs involved. The analytical performance for presently available on-site technologies and commercially available on-site equipment for detecting CWAs interpreted and compared in this review include: classical manual methods, photometric methods, ion mobile spectrometry, vibrational spectrometry, gas chromatography, mass spectrometry, sensors, and other methods. Some of the data evaluated were obtained from our experiments using authentic CWAs. We concluded that (a) no technologies perfectly fulfill all of the on-site detection requirements and (b) adequate on-site detection requires (i) a combination of the monitoring-tape method and ion-mobility spectrometry for point detection and (ii) a combination of the monitoring-tape method, atmospheric pressure chemical ionization mass spectrometry with counterflow introduction, and gas chromatography with a trap and special detectors for continuous monitoring. The basic properties of CWAs, the concept of on-site detection, and the sarin gas attacks in Japan as well as the forensic investigations thereof, are also explicated in this article. Copyright © 2014 Central Police University.

Magnetic scavengers as carriers of analytes for flowing atmospheric pressure afterglow mass spectrometry (FAPA-MS).

PubMed

Cegłowski, Michał; Kurczewska, Joanna; Smoluch, Marek; Reszke, Edward; Silberring, Jerzy; Schroeder, Grzegorz

2015-09-07

In this paper, a procedure for the preconcentration and transport of mixtures of acids, bases, and drug components to a mass spectrometer using magnetic scavengers is presented. Flowing atmospheric pressure afterglow mass spectrometry (FAPA-MS) was used as an analytical method for identification of the compounds by thermal desorption from the scavengers. The proposed procedure is fast and cheap, and does not involve time-consuming purification steps. The developed methodology can be applied for trapping harmful substances in minute quantities, to transport them to specialized, remotely located laboratories.

New analytical exact solutions of time fractional KdV-KZK equation by Kudryashov methods

NASA Astrophysics Data System (ADS)

S Saha, Ray

2016-04-01

In this paper, new exact solutions of the time fractional KdV-Khokhlov-Zabolotskaya-Kuznetsov (KdV-KZK) equation are obtained by the classical Kudryashov method and modified Kudryashov method respectively. For this purpose, the modified Riemann-Liouville derivative is used to convert the nonlinear time fractional KdV-KZK equation into the nonlinear ordinary differential equation. In the present analysis, the classical Kudryashov method and modified Kudryashov method are both used successively to compute the analytical solutions of the time fractional KdV-KZK equation. As a result, new exact solutions involving the symmetrical Fibonacci function, hyperbolic function and exponential function are obtained for the first time. The methods under consideration are reliable and efficient, and can be used as an alternative to establish new exact solutions of different types of fractional differential equations arising from mathematical physics. The obtained results are exhibited graphically in order to demonstrate the efficiencies and applicabilities of these proposed methods of solving the nonlinear time fractional KdV-KZK equation.

Direct /sup 125/I-radioligand assays for serum progesterone compared with assays involving extraction of serum

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

Ratcliffe, W.A.; Corrie, J.E.; Dalziel, A.H.

1982-06-01

Researchers compared two direct radioimmunoassays for progesterone in 50 microL of unextracted serum or plasma with assays involving extraction of serum. The direct assays include the use of either danazol at pH 7.4 or 8-anilino-1-naphthalenesulfonic acid at pH 4.0 to displace progesterone from serum binding-proteins. Progesterone is then assayed by using an antiserum to a progesterone 11 alpha hemisuccinyl conjugate and the radioligand /sup 125/I-labeled progesterone 11 alpha-glucuronyl tyramine, with separation by double-antibody techniques. Direct assays with either displacing agent gave good analytical recovery of progesterone added to human serum, and progesterone values for patients' specimens correlated well (r greatermore » than 0.96) with results of assays involving extraction of serum. Precision was similar with each displacing agent over the working range 2.5-100 nmol/L and superior to that of extraction assays. Researchers conclude that these direct assays of progesterone are analytically valid and more robust, precise, and technically convenient than many conventional methods involving extraction of serum.« less

Direct /sup 125/I-radioligand assays for serum progesterone compared with assays involving extraction of serum

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

Ratcliffe, W.A.; Corrie, J.E.T.; Dalziel, A.H.

1982-06-01

Two direct radioimmunoassays for progesterone in 50 ..mu..L of unextracted serum or plasma with assays involving extraction of serum were compared. The direct assays include the use of either danazol at pH 7.4 or 8-anilino-1-naphthalenesulfonic acid at pH 4.0 to displace progesterone from serum binding-proteins. Progesterone is then assayed by using an antiserum to a progesterone 11..cap alpha..-hemisuccinyl conjugate and the radioligand /sup 125/I-labeled progesterone 11..cap alpha..-glucuronyl tyramine, with separation by double-antibody techniques. Direct assays with either displacing agent gave good analytical recovery of progesterone added to human serum, and progesterone values for patients' specimens correlated well (r > 0.96)more » with results of assays involving extraction of serum. Precision was similar with each displacing agent over the working range 2.5-100 nmol/L and superior to that of extraction assays. We conclude that these direct assays of progesterone are analytically valid and more robust, precise, and technically convenient than many conventional methods involving extraction of serum.« less

Topics in Chemical Instrumentation: An Introduction to Supercritical Fluid Chromatography--Part 2. Applications and Future Trends.

ERIC Educational Resources Information Center

Palmieri, Margo D.

1989-01-01

Discussed are selected application and future trends in supercritical fluid chromatography (SFC). The greatest application for SFC involves those analytes that are difficult to separate using GC or LC methods. Optimum conditions for SFC are examined. Provided are several example chromatograms. (MVL)

An Application of Latent Variable Structural Equation Modeling for Experimental Research in Educational Technology

ERIC Educational Resources Information Center

Lee, Hyeon Woo

2011-01-01

As the technology-enriched learning environments and theoretical constructs involved in instructional design become more sophisticated and complex, a need arises for equally sophisticated analytic methods to research these environments, theories, and models. Thus, this paper illustrates a comprehensive approach for analyzing data arising from…

Functional Communication Training: A Contemporary Behavior Analytic Intervention for Problem Behaviors.

ERIC Educational Resources Information Center

Durand, V. Mark; Merges, Eileen

2001-01-01

This article describes functional communication training (FCT) with students who have autism. FCT involves teaching alternative communication strategies to replace problem behaviors. The article reviews the conditions under which this intervention is successful and compares the method with other behavioral approaches. It concludes that functional…

ANALYSIS OF THE ENANTIOMERS OF CHIRAL PESTICIDES AND OTHER POLLUTANTS IN ENVIRONMENTAL SAMPLES BY CAPILLARY ELECTROPHORESIS

EPA Science Inventory

The generic method described here involves typical capillary electrophoresis (CE) techniques, with the addition of cyclodextrin chiral selectors to the electrolyte for enantiomer separation and also, in the case of neutral analytes, the further addition of a micelle forming comp...

A Guide to Job Analysis for the Preparation of Job Training Programmes.

ERIC Educational Resources Information Center

Ceramics, Glass, and Mineral Products Industry Training Board, Harrow (England).

The paper deals with job analysis for the preparation of job training programs. The analytical approach involves five steps: enlisting support, examining the job, describing the job, analyzing training requirements, and planning the programs. Appendixes include methods of producing training schemes--the simple job breakdown, straightforward…

Teacher Acquisition of Functional Analysis Methods Using Pyramidal Training

ERIC Educational Resources Information Center

Pence, Sacha T.; St. Peter, Claire C.; Giles, Aimee F.

2014-01-01

Pyramidal training involves an experienced professional training a subset of individuals who, in turn, train additional individuals. Pyramidal training is effective for training a variety of behavior-analytic skills with direct-care staff, parents, and teachers. As teachers' roles in behavioral assessment increase, pyramidal training may be…

Mathematical modeling and pharmaceutical pricing: analyses used to inform in-licensing and developmental go/No-Go decisions.

PubMed

Vernon, John A; Hughen, W Keener; Johnson, Scott J

2005-05-01

In the face of significant real healthcare cost inflation, pressured budgets, and ongoing launches of myriad technology of uncertain value, payers have formalized new valuation techniques that represent a barrier to entry for drugs. Cost-effectiveness analysis predominates among these methods, which involves differencing a new technological intervention's marginal costs and benefits with a comparator's, and comparing the resulting ratio to a payer's willingness-to-pay threshold. In this paper we describe how firms are able to model the feasible range of future product prices when making in-licensing and developmental Go/No-Go decisions by considering payers' use of the cost-effectiveness method. We illustrate this analytic method with a simple deterministic example and then incorporate stochastic assumptions using both analytic and simulation methods. Using this strategic approach, firms may reduce product development and in-licensing risk.

Advances in Instrumental Analysis of Brominated Flame Retardants: Current Status and Future Perspectives

PubMed Central

2014-01-01

This review aims to highlight the recent advances and methodological improvements in instrumental techniques applied for the analysis of different brominated flame retardants (BFRs). The literature search strategy was based on the recent analytical reviews published on BFRs. The main selection criteria involved the successful development and application of analytical methods for determination of the target compounds in various environmental matrices. Different factors affecting chromatographic separation and mass spectrometric detection of brominated analytes were evaluated and discussed. Techniques using advanced instrumentation to achieve outstanding results in quantification of different BFRs and their metabolites/degradation products were highlighted. Finally, research gaps in the field of BFR analysis were identified and recommendations for future research were proposed. PMID:27433482

Method for fabricating non-detonable explosive simulants

DOEpatents

Simpson, Randall L.; Pruneda, Cesar O.

1995-01-01

A simulator which is chemically equivalent to an explosive, but is not detonable. The simulator has particular use in the training of explosives detecting dogs and calibrating sensitive analytical instruments. The explosive simulants may be fabricated by different techniques, a first involves the use of standard slurry coatings to produce a material with a very high binder to explosive ratio without masking the explosive vapor, and the second involves coating inert beads with thin layers of explosive molecules.

Liquid-cooling technology for gas turbines - Review and status

NASA Technical Reports Server (NTRS)

Van Fossen, G. J., Jr.; Stepka, F. S.

1978-01-01

After a brief review of past efforts involving the forced-convection cooling of gas turbines, the paper surveys the state of the art of the liquid cooling of gas turbines. Emphasis is placed on thermosyphon methods of cooling, including those utilizing closed, open, and closed-loop thermosyphons; other methods, including sweat, spray and stator cooling, are also discussed. The more significant research efforts, design data, correlations, and analytical methods are mentioned and voids in technology are summarized.

Speciation of butyltin compounds in marine sediments with headspace solid phase microextraction and gas chromatography mass spectrometry.

PubMed

Cardellicchio, N; Giandomenico, S; Decataldo, A; Di Leo, A

2001-03-01

A method for the determination of organotin compounds (monobutyl = MBT, dibutyl = DBT, and tributyltin = TBT) in marine sediments by headspace Solid Phase Microextraction (SPME) has been developed. The analytical procedure involved 1) extraction of TBT, DBT and MBT from sediments with HCl and methanol mixture, 2) in situ derivatization with sodium tetraethylborate and 3) headspace SPME extraction using a fiber coated with poly(dimethylsiloxane). The derivatized organotin compounds were desorbed into the splitless injector and simultaneously analyzed by gas chromatography - mass spectrometry. The analytical method was optimized with respect to derivatization reaction and extraction conditions. The detection limits obtained for MBT, DBT and TBT ranged from 730 to 969 pg/g as Sn dry weight. Linear calibration curves were obtained for all analytes in the range of 30-1000 ng/L as Sn. Analysis of a standard reference sediment (CRM 462) demonstrates the suitability of this method for the determination of butyltin compounds in marine sediments. The application to the determination of TBT, DBT and MBT in a coastal marine sediment is shown.

Potential role of gold nanoparticles for improved analytical methods: an introduction to characterizations and applications.

PubMed

Wu, Chung-Shu; Liu, Fu-Ken; Ko, Fu-Hsiang

2011-01-01

Nanoparticle-based material is a revolutionary scientific and engineering venture that will invariably impact the existing analytical separation and preconcentration for a variety of analytes. Nanoparticles can be regarded as a hybrid between small molecule and bulk material. A material on the nanoscale produces considerable changes on various properties, making them size- and shape-dependent. Gold nanoparticles (Au NPs), one of the wide variety of core materials available, coupled with tunable surface properties in the form of inorganic or inorganic-organic hybrid have been reported as an excellent platform for a broad range of analytical methods. This review aims to introduce the basic principles, examples, and descriptions of methods for the characterization of Au NPs by using chromatography, electrophoresis, and self-assembly strategies for separation science. Some of the latest important applications of using Au NPs as stationary phases toward open-tubular capillary electrochromatography, gas chromatography, and liquid chromatography as well as roles of run buffer additive to enhance separation and preconcentration in the field of chromatographic, electrophoretic and in chip-based systems are reviewed. Additionally, we review Au NPs-assisted state-of-the-art techniques involving the use of micellar electrokinetic chromatography, an online diode array detector, solid-phase extraction, and mass spectrometry for the preconcentration of some chemical compounds and biomolecules.

LIBS-LIF-Raman: a new tool for the future E-RIHS

NASA Astrophysics Data System (ADS)

Detalle, Vincent; Bai, Xueshi; Bourguignon, Elsa; Menu, Michel; Pallot-Frossard, Isabelle

2017-07-01

France is one of the countries involved in the future E-RIHS - European Research Infrastructure for Heritage Science. The research infrastructure dedicated to the study of materials of cultural and natural heritage will provide transnational access to state-of-the-art technologies (synchrotron, ion beams, lasers, portable methods, etc.) and scientific archives. E-RIHS addresses the experimental problems of knowledge and conservation of heritage materials (collections of art and natural museums, monuments, archaeological sites, archives, libraries, etc.). The cultural artefacts are characterized by complementary methods at multi-scales. The variety and the hybrid are specific of these artefacts and induce complex problems that are not expected in traditional Natural Science: paints, ceramics and glasses, metals, palaeontological specimens, lithic materials, graphic documents, etc. E-RIHS develops in that purpose transnational access to distributed platforms in many European countries. Five complementary accesses are in this way available: FIXLAB (access to fixed platforms for synchrotron, neutrons, ion beams, lasers, etc.), MOLAB (access to mobile examination and analytical methods to study the works in situ), ARCHLAB (access to scientific archives kept in the cultural institutions), DIGILAB (access to a digital infrastructure for the processing of quantitative data, implementing a policy on (re)use of data, choice of data formats, etc.) and finally EXPERTLAB (panels of experts for the implementation of collaborative and multidisciplinary projects for the study, the analysis and the conservation of heritage works).Thus E-RIHS is specifically involved in complex studies for the development of advanced high-resolution analytical and imaging tools. The privileged field of intervention of the infrastructure is that of the study of large corpora, collections and architectural ensembles. Based on previous I3 European program, and especially IPERION-CH program that support the creation of new mobile instrumentation, the French institutions are involved in the development of LIBS/LIF/RAMAN portable instrumentation. After a presentation of the challenge and the multiple advantages in building the European Infrastructure and of the French E-RIHS hub, the major interests of associating the three lasers based on analytical methods for a more global and precise characterization of the heritage objects taking into account their precious characters and their specific constraints. Lastly some preliminary results will be presented in order to give a first idea of the power of this analytical tool.

Simultaneous quantitation of hydroxychloroquine and its metabolites in mouse blood and tissues using LC-ESI-MS/MS: An application for pharmacokinetic studies.

PubMed

Chhonker, Yashpal S; Sleightholm, Richard L; Li, Jing; Oupický, David; Murry, Daryl J

2018-01-01

Hydroxychloroquine (HCQ) has been shown to disrupt autophagy and sensitize cancer cells to radiation and chemotherapeutic agents. However, the optimal delivery method, dose, and tumor concentrations required for these effects are not known. This is in part due to a lack of sensitive and reproducible analytical methods for HCQ quantitation in small animals. As such, we developed and validated a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method for simultaneous quantitation of hydroxychloroquine and its metabolites in mouse blood and tissues. The chromatographic separation and detection of analytes were achieved on a reversed phase Thermo Aquasil C 18 (50×4.6mm, 3μ) column, with gradient elution using 0.2% formic acid and 0.1% formic acid in methanol as mobile phase at a flow rate of 0.5mL/min. Simple protein precipitation was utilized for extraction of analytes from the desired matrix. Analytes were separated and quantitated using MS/MS with an electrospray ionization source in positive multiple reaction monitoring (MRM) mode. The MS/MS response was linear over the concentration range from 1 to 2000ng/mL for all analytes with a correlation coefficient (R 2 ) of 0.998 or better. The within- and between-day precision (relative standard deviation, % RSD) and accuracy were within the acceptable limits per FDA guidelines. The validated method was successfully applied to a preclinical pharmacokinetic mouse study involving low volume blood and tissue samples for hydroxychloroquine and metabolites. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantum State Tomography via Linear Regression Estimation

PubMed Central

Qi, Bo; Hou, Zhibo; Li, Li; Dong, Daoyi; Xiang, Guoyong; Guo, Guangcan

2013-01-01

A simple yet efficient state reconstruction algorithm of linear regression estimation (LRE) is presented for quantum state tomography. In this method, quantum state reconstruction is converted into a parameter estimation problem of a linear regression model and the least-squares method is employed to estimate the unknown parameters. An asymptotic mean squared error (MSE) upper bound for all possible states to be estimated is given analytically, which depends explicitly upon the involved measurement bases. This analytical MSE upper bound can guide one to choose optimal measurement sets. The computational complexity of LRE is O(d4) where d is the dimension of the quantum state. Numerical examples show that LRE is much faster than maximum-likelihood estimation for quantum state tomography. PMID:24336519

Numerical investigation of finite-volume effects for the HVP

NASA Astrophysics Data System (ADS)

Boyle, Peter; Gülpers, Vera; Harrison, James; Jüttner, Andreas; Portelli, Antonin; Sachrajda, Christopher

2018-03-01

It is important to correct for finite-volume (FV) effects in the presence of QED, since these effects are typically large due to the long range of the electromagnetic interaction. We recently made the first lattice calculation of electromagnetic corrections to the hadronic vacuum polarisation (HVP). For the HVP, an analytical derivation of FV corrections involves a two-loop calculation which has not yet been carried out. We instead calculate the universal FV corrections numerically, using lattice scalar QED as an effective theory. We show that this method gives agreement with known analytical results for scalar mass FV effects, before applying it to calculate FV corrections for the HVP. This method for numerical calculation of FV effects is also widely applicable to quantities beyond the HVP.

Validation of chemistry models employed in a particle simulation method

NASA Technical Reports Server (NTRS)

Haas, Brian L.; Mcdonald, Jeffrey D.

1991-01-01

The chemistry models employed in a statistical particle simulation method, as implemented in the Intel iPSC/860 multiprocessor computer, are validated and applied. Chemical relaxation of five-species air in these reservoirs involves 34 simultaneous dissociation, recombination, and atomic-exchange reactions. The reaction rates employed in the analytic solutions are obtained from Arrhenius experimental correlations as functions of temperature for adiabatic gas reservoirs in thermal equilibrium. Favorable agreement with the analytic solutions validates the simulation when applied to relaxation of O2 toward equilibrium in reservoirs dominated by dissociation and recombination, respectively, and when applied to relaxation of air in the temperature range 5000 to 30,000 K. A flow of O2 over a circular cylinder at high Mach number is simulated to demonstrate application of the method to multidimensional reactive flows.

Petermann I and II spot size: Accurate semi analytical description involving Nelder-Mead method of nonlinear unconstrained optimization and three parameter fundamental modal field

NASA Astrophysics Data System (ADS)

Roy Choudhury, Raja; Roy Choudhury, Arundhati; Kanti Ghose, Mrinal

2013-01-01

A semi-analytical model with three optimizing parameters and a novel non-Gaussian function as the fundamental modal field solution has been proposed to arrive at an accurate solution to predict various propagation parameters of graded-index fibers with less computational burden than numerical methods. In our semi analytical formulation the optimization of core parameter U which is usually uncertain, noisy or even discontinuous, is being calculated by Nelder-Mead method of nonlinear unconstrained minimizations as it is an efficient and compact direct search method and does not need any derivative information. Three optimizing parameters are included in the formulation of fundamental modal field of an optical fiber to make it more flexible and accurate than other available approximations. Employing variational technique, Petermann I and II spot sizes have been evaluated for triangular and trapezoidal-index fibers with the proposed fundamental modal field. It has been demonstrated that, the results of the proposed solution identically match with the numerical results over a wide range of normalized frequencies. This approximation can also be used in the study of doped and nonlinear fiber amplifier.

Comparison of FDTD numerical computations and analytical multipole expansion method for plasmonics-active nanosphere dimers.

PubMed

Dhawan, Anuj; Norton, Stephen J; Gerhold, Michael D; Vo-Dinh, Tuan

2009-06-08

This paper describes a comparative study of finite-difference time-domain (FDTD) and analytical evaluations of electromagnetic fields in the vicinity of dimers of metallic nanospheres of plasmonics-active metals. The results of these two computational methods, to determine electromagnetic field enhancement in the region often referred to as "hot spots" between the two nanospheres forming the dimer, were compared and a strong correlation observed for gold dimers. The analytical evaluation involved the use of the spherical-harmonic addition theorem to relate the multipole expansion coefficients between the two nanospheres. In these evaluations, the spacing between two nanospheres forming the dimer was varied to obtain the effect of nanoparticle spacing on the electromagnetic fields in the regions between the nanostructures. Gold and silver were the metals investigated in our work as they exhibit substantial plasmon resonance properties in the ultraviolet, visible, and near-infrared spectral regimes. The results indicate excellent correlation between the two computational methods, especially for gold nanosphere dimers with only a 5-10% difference between the two methods. The effect of varying the diameters of the nanospheres forming the dimer, on the electromagnetic field enhancement, was also studied.

Part-2: Analytical Expressions of Concentrations of Glucose, Oxygen, and Gluconic Acid in a Composite Membrane for Closed-Loop Insulin Delivery for the Non-steady State Conditions.

PubMed

Mehala, N; Rajendran, L; Meena, V

2017-02-01

A mathematical model developed by Abdekhodaie and Wu (J Membr Sci 335:21-31, 2009), which describes a dynamic process involving an enzymatic reaction and diffusion of reactants and product inside glucose-sensitive composite membrane has been discussed. This theoretical model depicts a system of non-linear non-steady state reaction diffusion equations. These equations have been solved using new approach of homotopy perturbation method and analytical solutions pertaining to the concentrations of glucose, oxygen, and gluconic acid are derived. These analytical results are compared with the numerical results, and limiting case results for steady state conditions and a good agreement is observed. The influence of various kinetic parameters involved in the model has been presented graphically. Theoretical evaluation of the kinetic parameters like the maximal reaction velocity (V max ) and Michaelis-Menten constants for glucose and oxygen (K g and K ox ) is also reported. This predicted model is very much useful for designing the glucose-responsive composite membranes for closed-loop insulin delivery.

High-order moments of spin-orbit energy in a multielectron configuration

NASA Astrophysics Data System (ADS)

Na, Xieyu; Poirier, M.

2016-07-01

In order to analyze the energy-level distribution in complex ions such as those found in warm dense plasmas, this paper provides values for high-order moments of the spin-orbit energy in a multielectron configuration. Using second-quantization results and standard angular algebra or fully analytical expressions, explicit values are given for moments up to 10th order for the spin-orbit energy. Two analytical methods are proposed, using the uncoupled or coupled orbital and spin angular momenta. The case of multiple open subshells is considered with the help of cumulants. The proposed expressions for spin-orbit energy moments are compared to numerical computations from Cowan's code and agree with them. The convergence of the Gram-Charlier expansion involving these spin-orbit moments is analyzed. While a spectrum with infinitely thin components cannot be adequately represented by such an expansion, a suitable convolution procedure ensures the convergence of the Gram-Charlier series provided high-order terms are accounted for. A corrected analytical formula for the third-order moment involving both spin-orbit and electron-electron interactions turns out to be in fair agreement with Cowan's numerical computations.

On Nonconvex Decentralized Gradient Descent

DTIC Science & Technology

2016-08-01

and J. Bolte, On the convergence of the proximal algorithm for nonsmooth functions involving analytic features, Math . Program., 116: 5-16, 2009. [2] H...splitting, and regularized Gauss-Seidel methods, Math . Pro- gram., Ser. A, 137: 91-129, 2013. [3] P. Bianchi and J. Jakubowicz, Convergence of a multi-agent...subgradient method under random communication topologies , IEEE J. Sel. Top. Signal Process., 5:754-771, 2011. [11] A. Nedic and A. Ozdaglar, Distributed

A Newton-Krylov method with an approximate analytical Jacobian for implicit solution of Navier-Stokes equations on staggered overset-curvilinear grids with immersed boundaries.

PubMed

Asgharzadeh, Hafez; Borazjani, Iman

2017-02-15

The explicit and semi-implicit schemes in flow simulations involving complex geometries and moving boundaries suffer from time-step size restriction and low convergence rates. Implicit schemes can be used to overcome these restrictions, but implementing them to solve the Navier-Stokes equations is not straightforward due to their non-linearity. Among the implicit schemes for nonlinear equations, Newton-based techniques are preferred over fixed-point techniques because of their high convergence rate but each Newton iteration is more expensive than a fixed-point iteration. Krylov subspace methods are one of the most advanced iterative methods that can be combined with Newton methods, i.e., Newton-Krylov Methods (NKMs) to solve non-linear systems of equations. The success of NKMs vastly depends on the scheme for forming the Jacobian, e.g., automatic differentiation is very expensive, and matrix-free methods without a preconditioner slow down as the mesh is refined. A novel, computationally inexpensive analytical Jacobian for NKM is developed to solve unsteady incompressible Navier-Stokes momentum equations on staggered overset-curvilinear grids with immersed boundaries. Moreover, the analytical Jacobian is used to form preconditioner for matrix-free method in order to improve its performance. The NKM with the analytical Jacobian was validated and verified against Taylor-Green vortex, inline oscillations of a cylinder in a fluid initially at rest, and pulsatile flow in a 90 degree bend. The capability of the method in handling complex geometries with multiple overset grids and immersed boundaries is shown by simulating an intracranial aneurysm. It was shown that the NKM with an analytical Jacobian is 1.17 to 14.77 times faster than the fixed-point Runge-Kutta method, and 1.74 to 152.3 times (excluding an intensively stretched grid) faster than automatic differentiation depending on the grid (size) and the flow problem. In addition, it was shown that using only the diagonal of the Jacobian further improves the performance by 42 - 74% compared to the full Jacobian. The NKM with an analytical Jacobian showed better performance than the fixed point Runge-Kutta because it converged with higher time steps and in approximately 30% less iterations even when the grid was stretched and the Reynold number was increased. In fact, stretching the grid decreased the performance of all methods, but the fixed-point Runge-Kutta performance decreased 4.57 and 2.26 times more than NKM with a diagonal Jacobian when the stretching factor was increased, respectively. The NKM with a diagonal analytical Jacobian and matrix-free method with an analytical preconditioner are the fastest methods and the superiority of one to another depends on the flow problem. Furthermore, the implemented methods are fully parallelized with parallel efficiency of 80-90% on the problems tested. The NKM with the analytical Jacobian can guide building preconditioners for other techniques to improve their performance in the future.

A Newton–Krylov method with an approximate analytical Jacobian for implicit solution of Navier–Stokes equations on staggered overset-curvilinear grids with immersed boundaries

PubMed Central

Asgharzadeh, Hafez; Borazjani, Iman

2016-01-01

The explicit and semi-implicit schemes in flow simulations involving complex geometries and moving boundaries suffer from time-step size restriction and low convergence rates. Implicit schemes can be used to overcome these restrictions, but implementing them to solve the Navier-Stokes equations is not straightforward due to their non-linearity. Among the implicit schemes for nonlinear equations, Newton-based techniques are preferred over fixed-point techniques because of their high convergence rate but each Newton iteration is more expensive than a fixed-point iteration. Krylov subspace methods are one of the most advanced iterative methods that can be combined with Newton methods, i.e., Newton-Krylov Methods (NKMs) to solve non-linear systems of equations. The success of NKMs vastly depends on the scheme for forming the Jacobian, e.g., automatic differentiation is very expensive, and matrix-free methods without a preconditioner slow down as the mesh is refined. A novel, computationally inexpensive analytical Jacobian for NKM is developed to solve unsteady incompressible Navier-Stokes momentum equations on staggered overset-curvilinear grids with immersed boundaries. Moreover, the analytical Jacobian is used to form preconditioner for matrix-free method in order to improve its performance. The NKM with the analytical Jacobian was validated and verified against Taylor-Green vortex, inline oscillations of a cylinder in a fluid initially at rest, and pulsatile flow in a 90 degree bend. The capability of the method in handling complex geometries with multiple overset grids and immersed boundaries is shown by simulating an intracranial aneurysm. It was shown that the NKM with an analytical Jacobian is 1.17 to 14.77 times faster than the fixed-point Runge-Kutta method, and 1.74 to 152.3 times (excluding an intensively stretched grid) faster than automatic differentiation depending on the grid (size) and the flow problem. In addition, it was shown that using only the diagonal of the Jacobian further improves the performance by 42 – 74% compared to the full Jacobian. The NKM with an analytical Jacobian showed better performance than the fixed point Runge-Kutta because it converged with higher time steps and in approximately 30% less iterations even when the grid was stretched and the Reynold number was increased. In fact, stretching the grid decreased the performance of all methods, but the fixed-point Runge-Kutta performance decreased 4.57 and 2.26 times more than NKM with a diagonal Jacobian when the stretching factor was increased, respectively. The NKM with a diagonal analytical Jacobian and matrix-free method with an analytical preconditioner are the fastest methods and the superiority of one to another depends on the flow problem. Furthermore, the implemented methods are fully parallelized with parallel efficiency of 80–90% on the problems tested. The NKM with the analytical Jacobian can guide building preconditioners for other techniques to improve their performance in the future. PMID:28042172

A Newton-Krylov method with an approximate analytical Jacobian for implicit solution of Navier-Stokes equations on staggered overset-curvilinear grids with immersed boundaries

NASA Astrophysics Data System (ADS)

Asgharzadeh, Hafez; Borazjani, Iman

2017-02-01

The explicit and semi-implicit schemes in flow simulations involving complex geometries and moving boundaries suffer from time-step size restriction and low convergence rates. Implicit schemes can be used to overcome these restrictions, but implementing them to solve the Navier-Stokes equations is not straightforward due to their non-linearity. Among the implicit schemes for non-linear equations, Newton-based techniques are preferred over fixed-point techniques because of their high convergence rate but each Newton iteration is more expensive than a fixed-point iteration. Krylov subspace methods are one of the most advanced iterative methods that can be combined with Newton methods, i.e., Newton-Krylov Methods (NKMs) to solve non-linear systems of equations. The success of NKMs vastly depends on the scheme for forming the Jacobian, e.g., automatic differentiation is very expensive, and matrix-free methods without a preconditioner slow down as the mesh is refined. A novel, computationally inexpensive analytical Jacobian for NKM is developed to solve unsteady incompressible Navier-Stokes momentum equations on staggered overset-curvilinear grids with immersed boundaries. Moreover, the analytical Jacobian is used to form a preconditioner for matrix-free method in order to improve its performance. The NKM with the analytical Jacobian was validated and verified against Taylor-Green vortex, inline oscillations of a cylinder in a fluid initially at rest, and pulsatile flow in a 90 degree bend. The capability of the method in handling complex geometries with multiple overset grids and immersed boundaries is shown by simulating an intracranial aneurysm. It was shown that the NKM with an analytical Jacobian is 1.17 to 14.77 times faster than the fixed-point Runge-Kutta method, and 1.74 to 152.3 times (excluding an intensively stretched grid) faster than automatic differentiation depending on the grid (size) and the flow problem. In addition, it was shown that using only the diagonal of the Jacobian further improves the performance by 42-74% compared to the full Jacobian. The NKM with an analytical Jacobian showed better performance than the fixed point Runge-Kutta because it converged with higher time steps and in approximately 30% less iterations even when the grid was stretched and the Reynold number was increased. In fact, stretching the grid decreased the performance of all methods, but the fixed-point Runge-Kutta performance decreased 4.57 and 2.26 times more than NKM with a diagonal and full Jacobian, respectivley, when the stretching factor was increased. The NKM with a diagonal analytical Jacobian and matrix-free method with an analytical preconditioner are the fastest methods and the superiority of one to another depends on the flow problem. Furthermore, the implemented methods are fully parallelized with parallel efficiency of 80-90% on the problems tested. The NKM with the analytical Jacobian can guide building preconditioners for other techniques to improve their performance in the future.

Micro-separation toward systems biology.

PubMed

Liu, Bi-Feng; Xu, Bo; Zhang, Guisen; Du, Wei; Luo, Qingming

2006-02-17

Current biology is experiencing transformation in logic or philosophy that forces us to reevaluate the concept of cell, tissue or entire organism as a collection of individual components. Systems biology that aims at understanding biological system at the systems level is an emerging research area, which involves interdisciplinary collaborations of life sciences, computational and mathematical sciences, systems engineering, and analytical technology, etc. For analytical chemistry, developing innovative methods to meet the requirement of systems biology represents new challenges as also opportunities and responsibility. In this review, systems biology-oriented micro-separation technologies are introduced for comprehensive profiling of genome, proteome and metabolome, characterization of biomolecules interaction and single cell analysis such as capillary electrophoresis, ultra-thin layer gel electrophoresis, micro-column liquid chromatography, and their multidimensional combinations, parallel integrations, microfabricated formats, and nano technology involvement. Future challenges and directions are also suggested.

Analytical surveillance of emerging drugs of abuse and drug formulations

PubMed Central

Thomas, Brian F.; Pollard, Gerald T.; Grabenauer, Megan

2012-01-01

Uncontrolled recreational drugs are proliferating in number and variety. Effects of long-term use are unknown, and regulation is problematic, as efforts to control one chemical often lead to several other structural analogs. Advanced analytical instrumentation and methods are continuing to be developed to identify drugs, chemical constituents of products, and drug substances and metabolites in biological fluids. Several mass spectrometry based approaches appear promising, particularly those that involve high resolution chromatographic and mass spectrometric methods that allow unbiased data acquisition and sophisticated data interrogation. Several of these techniques are shown to facilitate both targeted and broad spectrum analysis, which is often of particular benefit when dealing with misleadingly labeled products or assessing a biological matrix for illicit drugs and metabolites. The development and application of novel analytical approaches such as these will help to assess the nature and degree of exposure and risk and, where necessary, inform forensics and facilitate implementation of specific regulation and control measures. PMID:23154240

Environmental monitoring of phenolic pollutants in water by cloud point extraction prior to micellar electrokinetic chromatography.

PubMed

Stege, Patricia W; Sombra, Lorena L; Messina, Germán A; Martinez, Luis D; Silva, María F

2009-05-01

Many aromatic compounds can be found in the environment as a result of anthropogenic activities and some of them are highly toxic. The need to determine low concentrations of pollutants requires analytical methods with high sensitivity, selectivity, and resolution for application to soil, sediment, water, and other environmental samples. Complex sample preparation involving analyte isolation and enrichment is generally necessary before the final analysis. The present paper outlines a novel, simple, low-cost, and environmentally friendly method for the simultaneous determination of p-nitrophenol (PNP), p-aminophenol (PAP), and hydroquinone (HQ) by micellar electrokinetic capillary chromatography after preconcentration by cloud point extraction. Enrichment factors of 180 to 200 were achieved. The limits of detection of the analytes for the preconcentration of 50-ml sample volume were 0.10 microg L(-1) for PNP, 0.20 microg L(-1) for PAP, and 0.16 microg L(-1) for HQ. The optimized procedure was applied to the determination of phenolic pollutants in natural waters from San Luis, Argentina.

Separation techniques for the clean-up of radioactive mixed waste for ICP-AES/ICP-MS analysis

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

Swafford, A.M.; Keller, J.M.

1993-03-17

Two separation techniques were investigated for the clean-up of typical radioactive mixed waste samples requiring elemental analysis by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). These measurements frequently involve regulatory or compliance criteria which include the determination of elements on the EPA Target Analyte List (TAL). These samples usually consist of both an aqueous phase and a solid phase which is mostly an inorganic sludge. Frequently, samples taken from the waste tanks contain high levels of uranium and thorium which can cause spectral interferences in ICP-AES or ICP-MS analysis. The removal of these interferences ismore » necessary to determine the presence of the EPA TAL elements in the sample. Two clean-up methods were studied on simulated aqueous waste samples containing the EPA TAL elements. The first method studied was a classical procedure based upon liquid-liquid extraction using tri-n- octylphosphine oxide (TOPO) dissolved in cyclohexane. The second method investigated was based on more recently developed techniques using extraction chromatography; specifically the use of a commercially available Eichrom TRU[center dot]Spec[trademark] column. Literature on these two methods indicates the efficient removal of uranium and thorium from properly prepared samples and provides considerable qualitative information on the extraction behavior of many other elements. However, there is a lack of quantitative data on the extraction behavior of elements on the EPA Target Analyte List. Experimental studies on these two methods consisted of determining whether any of the analytes were extracted by these methods and the recoveries obtained. Both methods produced similar results; the EPA target analytes were only slightly or not extracted. Advantages and disadvantages of each method were evaluated and found to be comparable.« less

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

Meinke, Rainer B.; Goodzeit, Carl L.; Ball, Millicent J.

This research project advanced the development of reliable, cost-effective arrays of superconducting quadrupole magnets for use in multi-beam inertial fusion accelerators. The field in each array cell must be identical and meet stringent requirements for field quality and strength. An optimized compact array design using flat double-layer pancake coils was developed. Analytical studies of edge termination methods showed that it is feasible to meet the requirements for field uniformity in all cells and elimination of stray external field in several ways: active methods that involve placement of field compensating coils on the periphery of the array or a passive methodmore » that involves use of iron shielding.« less

Microbial ecology laboratory procedures manual NASA/MSFC

NASA Technical Reports Server (NTRS)

Huff, Timothy L.

1990-01-01

An essential part of the efficient operation of any microbiology laboratory involved in sample analysis is a standard procedures manual. The purpose of this manual is to provide concise and well defined instructions on routine technical procedures involving sample analysis and methods for monitoring and maintaining quality control within the laboratory. Of equal importance is the safe operation of the laboratory. This manual outlines detailed procedures to be followed in the microbial ecology laboratory to assure safety, analytical control, and validity of results.

Method for fabricating non-detonable explosive simulants

DOEpatents

Simpson, R.L.; Pruneda, C.O.

1995-05-09

A simulator is disclosed which is chemically equivalent to an explosive, but is not detonable. The simulator has particular use in the training of explosives detecting dogs and calibrating sensitive analytical instruments. The explosive simulants may be fabricated by different techniques, a first involves the use of standard slurry coatings to produce a material with a very high binder to explosive ratio without masking the explosive vapor, and the second involves coating inert beads with thin layers of explosive molecules. 5 figs.

System of Systems Analytic Workbench - 2017

DTIC Science & Technology

2017-08-31

and transitional activities with key collaborators. The tools include: System Operational Dependency Analysis/System Developmental Dependency Analysis...in the methods of the SoS-AWB involve the following: 1. System Operability Dependency Analysis (SODA)/System Development Dependency Analysis...available f. Development of standard dependencies with combinations of low-medium-high parameters Report No. SERC-2017-TR-111

Detection, characterization and quantification of inorganic engineered nanomaterials: A review of techniques and methodological approaches for the analysis of complex samples.

PubMed

Laborda, Francisco; Bolea, Eduardo; Cepriá, Gemma; Gómez, María T; Jiménez, María S; Pérez-Arantegui, Josefina; Castillo, Juan R

2016-01-21

The increasing demand of analytical information related to inorganic engineered nanomaterials requires the adaptation of existing techniques and methods, or the development of new ones. The challenge for the analytical sciences has been to consider the nanoparticles as a new sort of analytes, involving both chemical (composition, mass and number concentration) and physical information (e.g. size, shape, aggregation). Moreover, information about the species derived from the nanoparticles themselves and their transformations must also be supplied. Whereas techniques commonly used for nanoparticle characterization, such as light scattering techniques, show serious limitations when applied to complex samples, other well-established techniques, like electron microscopy and atomic spectrometry, can provide useful information in most cases. Furthermore, separation techniques, including flow field flow fractionation, capillary electrophoresis and hydrodynamic chromatography, are moving to the nano domain, mostly hyphenated to inductively coupled plasma mass spectrometry as element specific detector. Emerging techniques based on the detection of single nanoparticles by using ICP-MS, but also coulometry, are in their way to gain a position. Chemical sensors selective to nanoparticles are in their early stages, but they are very promising considering their portability and simplicity. Although the field is in continuous evolution, at this moment it is moving from proofs-of-concept in simple matrices to methods dealing with matrices of higher complexity and relevant analyte concentrations. To achieve this goal, sample preparation methods are essential to manage such complex situations. Apart from size fractionation methods, matrix digestion, extraction and concentration methods capable of preserving the nature of the nanoparticles are being developed. This review presents and discusses the state-of-the-art analytical techniques and sample preparation methods suitable for dealing with complex samples. Single- and multi-method approaches applied to solve the nanometrological challenges posed by a variety of stakeholders are also presented. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of environmental regulatory proposals: Its your chance to influence policy

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

Veil, J.A.

1994-03-02

As part of the regulatory development process, the US Envirorunental Protection Agency (EPA) collects data, makes various assumptions about the data, and analyzes the data. Although EPA acts in good faith, the agency cannot always be aware of all relevant data, make only appropriate assumptions, and use applicable analytical methods. Regulated industries must carefully must carefully review every component of the regulatory decision-making process to identify misunderstandings and errors and to supply additional data that is relevant to the regulatory action. This paper examines three examples of how EPA`s data, assumptions, and analytical methods have been critiqued. The first twomore » examples involve EPA`s cost-effectiveness (CE) analyses prepared for the offshore oil and gas effluent limitations guidelines and as part of EPA Region 6`s general permit for coastal waters of Texas and Louisiana. A CE analysis regulations to the incremental amount of pollutants that would be removed by the recommended treatment processes. The third example, although not involving a CE analysis, demonstrates how the use of non-representative data can influence the outcome of an analysis.« less

Transient modeling/analysis of hyperbolic heat conduction problems employing mixed implicit-explicit alpha method

NASA Technical Reports Server (NTRS)

Tamma, Kumar K.; D'Costa, Joseph F.

1991-01-01

This paper describes the evaluation of mixed implicit-explicit finite element formulations for hyperbolic heat conduction problems involving non-Fourier effects. In particular, mixed implicit-explicit formulations employing the alpha method proposed by Hughes et al. (1987, 1990) are described for the numerical simulation of hyperbolic heat conduction models, which involves time-dependent relaxation effects. Existing analytical approaches for modeling/analysis of such models involve complex mathematical formulations for obtaining closed-form solutions, while in certain numerical formulations the difficulties include severe oscillatory solution behavior (which often disguises the true response) in the vicinity of the thermal disturbances, which propagate with finite velocities. In view of these factors, the alpha method is evaluated to assess the control of the amount of numerical dissipation for predicting the transient propagating thermal disturbances. Numerical test models are presented, and pertinent conclusions are drawn for the mixed-time integration simulation of hyperbolic heat conduction models involving non-Fourier effects.

Metformin: A Review of Characteristics, Properties, Analytical Methods and Impact in the Green Chemistry.

PubMed

da Trindade, Mariana Teixeira; Kogawa, Ana Carolina; Salgado, Hérida Regina Nunes

2018-01-02

Diabetes mellitus (DM) is considered a public health problem. The initial treatment consists of improving the lifestyle and making changes in the diet. When these changes are not enough, the use of medication becomes necessary. The metformin aims to reduce the hepatic production of glucose and is the preferred treatment for type 2. The objective is to survey the characteristics and properties of metformin, as well as hold a discussion on the existing analytical methods to green chemistry and their impacts for both the operator and the environment. For the survey, data searches were conducted by scientific papers in the literature as well as in official compendium. The characteristics and properties are shown, also, methods using liquid chromatography techniques, titration, absorption spectrophotometry in the ultraviolet and the infrared region. Most of the methods presented are not green chemistry oriented. It is necessary the awareness of everyone involved in the optimization of the methods applied through the implementation of green chemistry to determine the metformin.

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

Ultrasonic inspection of carbon fiber reinforced plastic by means of sample-recognition methods

NASA Technical Reports Server (NTRS)

Bilgram, R.

1985-01-01

In the case of carbon fiber reinforced plastic (CFRP), it has not yet been possible to detect nonlocal defects and material degradation related to aging with the aid of nondestructive inspection method. An approach for overcoming difficulties regarding such an inspection involves an extension of the ultrasonic inspection procedure on the basis of a use of signal processing and sample recognition methods. The basic concept involved in this approach is related to the realization that the ultrasonic signal contains information regarding the medium which is not utilized in conventional ultrasonic inspection. However, the analytical study of the phyiscal processes involved is very complex. For this reason, an empirical approach is employed to make use of the information which has not been utilized before. This approach uses reference signals which can be obtained with material specimens of different quality. The implementation of these concepts for the supersonic inspection of CFRP laminates is discussed.

Solution of Grad-Shafranov equation by the method of fundamental solutions

NASA Astrophysics Data System (ADS)

Nath, D.; Kalra, M. S.; Kalra

2014-06-01

In this paper we have used the Method of Fundamental Solutions (MFS) to solve the Grad-Shafranov (GS) equation for the axisymmetric equilibria of tokamak plasmas with monomial sources. These monomials are the individual terms appearing on the right-hand side of the GS equation if one expands the nonlinear terms into polynomials. Unlike the Boundary Element Method (BEM), the MFS does not involve any singular integrals and is a meshless boundary-alone method. Its basic idea is to create a fictitious boundary around the actual physical boundary of the computational domain. This automatically removes the involvement of singular integrals. The results obtained by the MFS match well with the earlier results obtained using the BEM. The method is also applied to Solov'ev profiles and it is found that the results are in good agreement with analytical results.

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.

Analytical solutions of the two-dimensional Dirac equation for a topological channel intersection

NASA Astrophysics Data System (ADS)

Anglin, J. R.; Schulz, A.

2017-01-01

Numerical simulations in a tight-binding model have shown that an intersection of topologically protected one-dimensional chiral channels can function as a beam splitter for noninteracting fermions on a two-dimensional lattice [Qiao, Jung, and MacDonald, Nano Lett. 11, 3453 (2011), 10.1021/nl201941f; Qiao et al., Phys. Rev. Lett. 112, 206601 (2014), 10.1103/PhysRevLett.112.206601]. Here we confirm this result analytically in the corresponding continuum k .p model, by solving the associated two-dimensional Dirac equation, in the presence of a "checkerboard" potential that provides a right-angled intersection between two zero-line modes. The method by which we obtain our analytical solutions is systematic and potentially generalizable to similar problems involving intersections of one-dimensional systems.

A General Simulation Method for Multiple Bodies in Proximate Flight

NASA Technical Reports Server (NTRS)

Meakin, Robert L.

2003-01-01

Methods of unsteady aerodynamic simulation for an arbitrary number of independent bodies flying in close proximity are considered. A novel method to efficiently detect collision contact points is described. A method to compute body trajectories in response to aerodynamic loads, applied loads, and inter-body collisions is also given. The physical correctness of the methods are verified by comparison to a set of analytic solutions. The methods, combined with a Navier-Stokes solver, are used to demonstrate the possibility of predicting the unsteady aerodynamics and flight trajectories of moving bodies that involve rigid-body collisions.

Approximate Solution of Time-Fractional Advection-Dispersion Equation via Fractional Variational Iteration Method

PubMed Central

İbiş, Birol

2014-01-01

This paper aims to obtain the approximate solution of time-fractional advection-dispersion equation (FADE) involving Jumarie's modification of Riemann-Liouville derivative by the fractional variational iteration method (FVIM). FVIM provides an analytical approximate solution in the form of a convergent series. Some examples are given and the results indicate that the FVIM is of high accuracy, more efficient, and more convenient for solving time FADEs. PMID:24578662

The role of light microscopy in aerospace analytical laboratories

NASA Technical Reports Server (NTRS)

Crutcher, E. R.

1977-01-01

Light microscopy has greatly reduced analytical flow time and added new dimensions to laboratory capability. Aerospace analytical laboratories are often confronted with problems involving contamination, wear, or material inhomogeneity. The detection of potential problems and the solution of those that develop necessitate the most sensitive and selective applications of sophisticated analytical techniques and instrumentation. This inevitably involves light microscopy. The microscope can characterize and often identify the cause of a problem in 5-15 minutes with confirmatory tests generally less than one hour. Light microscopy has and will make a very significant contribution to the analytical capabilities of aerospace laboratories.

A new method for determining acoustic-liner admittance in a rectangular duct with grazing flow from experimental data

NASA Technical Reports Server (NTRS)

Watson, W. R.

1984-01-01

A method is developed for determining acoustic liner admittance in a rectangular duct with grazing flow. The axial propagation constant, cross mode order, and mean flow profile is measured. These measured data are then input into an analytical program which determines the unknown admittance value. The analytical program is based upon a finite element discretization of the acoustic field and a reposing of the unknown admittance value as a linear eigenvalue problem on the admittance value. Gaussian elimination is employed to solve this eigenvalue problem. The method used is extendable to grazing flows with boundary layers in both transverse directions of an impedance tube (or duct). Predicted admittance values are compared both with exact values that can be obtained for uniform mean flow profiles and with those from a Runge Kutta integration technique for cases involving a one dimensional boundary layer.

An approach to estimate spatial distribution of analyte within cells using spectrally-resolved fluorescence microscopy.

PubMed

Sharma, Dharmendar Kumar; Irfanullah, Mir; Basu, Santanu Kumar; Madhu, Sheri; De, Suman; Jadhav, Sameer; Ravikanth, Mangalampalli; Chowdhury, Arindam

2017-01-18

While fluorescence microscopy has become an essential tool amongst chemists and biologists for the detection of various analyte within cellular environments, non-uniform spatial distribution of sensors within cells often restricts extraction of reliable information on relative abundance of analytes in different subcellular regions. As an alternative to existing sensing methodologies such as ratiometric or FRET imaging, where relative proportion of analyte with respect to the sensor can be obtained within cells, we propose a methodology using spectrally-resolved fluorescence microscopy, via which both the relative abundance of sensor as well as their relative proportion with respect to the analyte can be simultaneously extracted for local subcellular regions. This method is exemplified using a BODIPY sensor, capable of detecting mercury ions within cellular environments, characterized by spectral blue-shift and concurrent enhancement of emission intensity. Spectral emission envelopes collected from sub-microscopic regions allowed us to compare the shift in transition energies as well as integrated emission intensities within various intracellular regions. Construction of a 2D scatter plot using spectral shifts and emission intensities, which depend on the relative amount of analyte with respect to sensor and the approximate local amounts of the probe, respectively, enabled qualitative extraction of relative abundance of analyte in various local regions within a single cell as well as amongst different cells. Although the comparisons remain semi-quantitative, this approach involving analysis of multiple spectral parameters opens up an alternative way to extract spatial distribution of analyte in heterogeneous systems. The proposed method would be especially relevant for fluorescent probes that undergo relatively nominal shift in transition energies compared to their emission bandwidths, which often restricts their usage for quantitative ratiometric imaging in cellular media due to strong cross-talk between energetically separated detection channels.

An approach to estimate spatial distribution of analyte within cells using spectrally-resolved fluorescence microscopy

NASA Astrophysics Data System (ADS)

Sharma, Dharmendar Kumar; Irfanullah, Mir; Basu, Santanu Kumar; Madhu, Sheri; De, Suman; Jadhav, Sameer; Ravikanth, Mangalampalli; Chowdhury, Arindam

2017-03-01

While fluorescence microscopy has become an essential tool amongst chemists and biologists for the detection of various analyte within cellular environments, non-uniform spatial distribution of sensors within cells often restricts extraction of reliable information on relative abundance of analytes in different subcellular regions. As an alternative to existing sensing methodologies such as ratiometric or FRET imaging, where relative proportion of analyte with respect to the sensor can be obtained within cells, we propose a methodology using spectrally-resolved fluorescence microscopy, via which both the relative abundance of sensor as well as their relative proportion with respect to the analyte can be simultaneously extracted for local subcellular regions. This method is exemplified using a BODIPY sensor, capable of detecting mercury ions within cellular environments, characterized by spectral blue-shift and concurrent enhancement of emission intensity. Spectral emission envelopes collected from sub-microscopic regions allowed us to compare the shift in transition energies as well as integrated emission intensities within various intracellular regions. Construction of a 2D scatter plot using spectral shifts and emission intensities, which depend on the relative amount of analyte with respect to sensor and the approximate local amounts of the probe, respectively, enabled qualitative extraction of relative abundance of analyte in various local regions within a single cell as well as amongst different cells. Although the comparisons remain semi-quantitative, this approach involving analysis of multiple spectral parameters opens up an alternative way to extract spatial distribution of analyte in heterogeneous systems. The proposed method would be especially relevant for fluorescent probes that undergo relatively nominal shift in transition energies compared to their emission bandwidths, which often restricts their usage for quantitative ratiometric imaging in cellular media due to strong cross-talk between energetically separated detection channels. Dedicated to Professor Kankan Bhattacharyya.

Development of an 19F NMR method for the analysis of fluorinated acids in environmental water samples.

PubMed

Ellis, D A; Martin, J W; Muir, D C; Mabury, S A

2000-02-15

This investigation was carried out to evaluate 19F NMR as an analytical tool for the measurement of trifluoroacetic acid (TFA) and other fluorinated acids in the aquatic environment. A method based upon strong anionic exchange (SAX) chromatography was also optimized for the concentration of the fluoro acids prior to NMR analysis. Extraction of the analyte from the SAX column was carried out directly in the NMR solvent in the presence of the strong organic base, DBU. The method allowed the analysis of the acid without any prior cleanup steps being involved. Optimal NMR sensitivity based upon T1 relaxation times was investigated for seven fluorinated compounds in four different NMR solvents. The use of the relaxation agent chromium acetylacetonate, Cr(acac)3, within these solvent systems was also evaluated. Results show that the optimal NMR solvent differs for each fluorinated analyte. Cr(acac)3 was shown to have pronounced effects on the limits of detection of the analyte. Generally, the optimal sensitivity condition appears to be methanol-d4/2M DBU in the presence of 4 mg/mL of Cr-(acac)3. The method was validated through spike and recovery for five fluoro acids from environmentally relevant waters. Results are presented for the analysis of TFA in Toronto rainwater, which ranged from < 16 to 850 ng/L. The NMR results were confirmed by GC-MS selected-ion monitoring of the fluoroanalide derivative.

Analytic Methods for Evaluating Patterns of Multiple Congenital Anomalies in Birth Defect Registries.

PubMed

Agopian, A J; Evans, Jane A; Lupo, Philip J

2018-01-15

It is estimated that 20 to 30% of infants with birth defects have two or more birth defects. Among these infants with multiple congenital anomalies (MCA), co-occurring anomalies may represent either chance (i.e., unrelated etiologies) or pathogenically associated patterns of anomalies. While some MCA patterns have been recognized and described (e.g., known syndromes), others have not been identified or characterized. Elucidating these patterns may result in a better understanding of the etiologies of these MCAs. This article reviews the literature with regard to analytic methods that have been used to evaluate patterns of MCAs, in particular those using birth defect registry data. A popular method for MCA assessment involves a comparison of the observed to expected ratio for a given combination of MCAs, or one of several modified versions of this comparison. Other methods include use of numerical taxonomy or other clustering techniques, multiple regression analysis, and log-linear analysis. Advantages and disadvantages of these approaches, as well as specific applications, were outlined. Despite the availability of multiple analytic approaches, relatively few MCA combinations have been assessed. The availability of large birth defects registries and computing resources that allow for automated, big data strategies for prioritizing MCA patterns may provide for new avenues for better understanding co-occurrence of birth defects. Thus, the selection of an analytic approach may depend on several considerations. Birth Defects Research 110:5-11, 2018. © 2017 Wiley Periodicals, Inc. © 2017 Wiley Periodicals, Inc.

Transfer of analytical procedures: a panel of strategies selected for risk management, with emphasis on an integrated equivalence-based comparative testing approach.

PubMed

Agut, C; Caron, A; Giordano, C; Hoffman, D; Ségalini, A

2011-09-10

In 2001, a multidisciplinary team made of analytical scientists and statisticians at Sanofi-aventis has published a methodology which has governed, from that time, the transfers from R&D sites to Manufacturing sites of the release monographs. This article provides an overview of the recent adaptations brought to this original methodology taking advantage of our experience and the new regulatory framework, and, in particular, the risk management perspective introduced by ICH Q9. Although some alternate strategies have been introduced in our practices, the comparative testing one, based equivalence testing as statistical approach, remains the standard for assays lying on very critical quality attributes. This is conducted with the concern to control the most important consumer's risk involved at two levels in analytical decisions in the frame of transfer studies: risk, for the receiving laboratory, to take poor release decisions with the analytical method and risk, for the sending laboratory, to accredit such a receiving laboratory on account of its insufficient performances with the method. Among the enhancements to the comparative studies, the manuscript presents the process settled within our company for a better integration of the transfer study into the method life-cycle, just as proposals of generic acceptance criteria and designs for assay and related substances methods. While maintaining rigor and selectivity of the original approach, these improvements tend towards an increased efficiency in the transfer operations. Copyright © 2011 Elsevier B.V. All rights reserved.

Relative frequencies of constrained events in stochastic processes: An analytical approach.

PubMed

Rusconi, S; Akhmatskaya, E; Sokolovski, D; Ballard, N; de la Cal, J C

2015-10-01

The stochastic simulation algorithm (SSA) and the corresponding Monte Carlo (MC) method are among the most common approaches for studying stochastic processes. They relies on knowledge of interevent probability density functions (PDFs) and on information about dependencies between all possible events. Analytical representations of a PDF are difficult to specify in advance, in many real life applications. Knowing the shapes of PDFs, and using experimental data, different optimization schemes can be applied in order to evaluate probability density functions and, therefore, the properties of the studied system. Such methods, however, are computationally demanding, and often not feasible. We show that, in the case where experimentally accessed properties are directly related to the frequencies of events involved, it may be possible to replace the heavy Monte Carlo core of optimization schemes with an analytical solution. Such a replacement not only provides a more accurate estimation of the properties of the process, but also reduces the simulation time by a factor of order of the sample size (at least ≈10(4)). The proposed analytical approach is valid for any choice of PDF. The accuracy, computational efficiency, and advantages of the method over MC procedures are demonstrated in the exactly solvable case and in the evaluation of branching fractions in controlled radical polymerization (CRP) of acrylic monomers. This polymerization can be modeled by a constrained stochastic process. Constrained systems are quite common, and this makes the method useful for various applications.

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.

Advances in spatial epidemiology and geographic information systems.

PubMed

Kirby, Russell S; Delmelle, Eric; Eberth, Jan M

2017-01-01

The field of spatial epidemiology has evolved rapidly in the past 2 decades. This study serves as a brief introduction to spatial epidemiology and the use of geographic information systems in applied research in epidemiology. We highlight technical developments and highlight opportunities to apply spatial analytic methods in epidemiologic research, focusing on methodologies involving geocoding, distance estimation, residential mobility, record linkage and data integration, spatial and spatio-temporal clustering, small area estimation, and Bayesian applications to disease mapping. The articles included in this issue incorporate many of these methods into their study designs and analytical frameworks. It is our hope that these studies will spur further development and utilization of spatial analysis and geographic information systems in epidemiologic research. Copyright © 2016 Elsevier Inc. All rights reserved.

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

PubMed

Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

2000-02-11

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

Miniaturized Temperature-Controlled Planar Chromatography (Micro-TLC) as a Versatile Technique for Fast Screening of Micropollutants and Biomarkers Derived from Surface Water Ecosystems and During Technological Processes of Wastewater Treatment.

PubMed

Ślączka-Wilk, Magdalena M; Włodarczyk, Elżbieta; Kaleniecka, Aleksandra; Zarzycki, Paweł K

2017-07-01

There is increasing interest in the development of simple analytical systems enabling the fast screening of target components in complex samples. A number of newly invented protocols are based on quasi separation techniques involving microfluidic paper-based analytical devices and/or micro total analysis systems. Under such conditions, the quantification of target components can be performed mainly due to selective detection. The main goal of this paper is to demonstrate that miniaturized planar chromatography has the capability to work as an efficient separation and quantification tool for the analysis of multiple targets within complex environmental samples isolated and concentrated using an optimized SPE method. In particular, we analyzed various samples collected from surface water ecosystems (lakes, rivers, and the Baltic Sea of Middle Pomerania in the northern part of Poland) in different seasons, as well as samples collected during key wastewater technological processes (originating from the "Jamno" wastewater treatment plant in Koszalin, Poland). We documented that the multiple detection of chromatographic spots on RP-18W microplates-under visible light, fluorescence, and fluorescence quenching conditions, and using the visualization reagent phosphomolybdic acid-enables fast and robust sample classification. The presented data reveal that the proposed micro-TLC system is useful, inexpensive, and can be considered as a complementary method for the fast control of treated sewage water discharged by a municipal wastewater treatment plant, particularly for the detection of low-molecular mass micropollutants with polarity ranging from estetrol to progesterone, as well as chlorophyll-related dyes. Due to the low consumption of mobile phases composed of water-alcohol binary mixtures (less than 1 mL/run for the simultaneous separation of up to nine samples), this method can be considered an environmentally friendly and green chemistry analytical tool. The described analytical protocol can be complementary to those involving classical column chromatography (HPLC) or various planar microfluidic devices.

General method of solving the Schroedinger equation of atoms and molecules

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

Nakatsuji, Hiroshi

2005-12-15

We propose a general method of solving the Schroedinger equation of atoms and molecules. We first construct the wave function having the exact structure, using the ICI (iterative configuration or complement interaction) method and then optimize the variables involved by the variational principle. Based on the scaled Schroedinger equation and related principles, we can avoid the singularity problem of atoms and molecules and formulate a general method of calculating the exact wave functions in an analytical expansion form. We choose initial function {psi}{sub 0} and scaling g function, and then the ICI method automatically generates the wave function that hasmore » the exact structure by using the Hamiltonian of the system. The Hamiltonian contains all the information of the system. The free ICI method provides a flexible and variationally favorable procedure of constructing the exact wave function. We explain the computational procedure of the analytical ICI method routinely performed in our laboratory. Simple examples are given using hydrogen atom for the nuclear singularity case, the Hooke's atom for the electron singularity case, and the helium atom for both cases.« less

Do placebo based validation standards mimic real batch products behaviour? Case studies.

PubMed

Bouabidi, A; Talbi, M; Bouklouze, A; El Karbane, M; Bourichi, H; El Guezzar, M; Ziemons, E; Hubert, Ph; Rozet, E

2011-06-01

Analytical methods validation is a mandatory step to evaluate the ability of developed methods to provide accurate results for their routine application. Validation usually involves validation standards or quality control samples that are prepared in placebo or reconstituted matrix made of a mixture of all the ingredients composing the drug product except the active substance or the analyte under investigation. However, one of the main concerns that can be made with this approach is that it may lack an important source of variability that come from the manufacturing process. The question that remains at the end of the validation step is about the transferability of the quantitative performance from validation standards to real authentic drug product samples. In this work, this topic is investigated through three case studies. Three analytical methods were validated using the commonly spiked placebo validation standards at several concentration levels as well as using samples coming from authentic batch samples (tablets and syrups). The results showed that, depending on the type of response function used as calibration curve, there were various degrees of differences in the results accuracy obtained with the two types of samples. Nonetheless the use of spiked placebo validation standards was showed to mimic relatively well the quantitative behaviour of the analytical methods with authentic batch samples. Adding these authentic batch samples into the validation design may help the analyst to select and confirm the most fit for purpose calibration curve and thus increase the accuracy and reliability of the results generated by the method in routine application. Copyright © 2011 Elsevier B.V. All rights reserved.

Sampling and sample processing in pesticide residue analysis.

PubMed

Lehotay, Steven J; Cook, Jo Marie

2015-05-13

Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

Sample normalization methods in quantitative metabolomics.

PubMed

Wu, Yiman; Li, Liang

2016-01-22

To reveal metabolomic changes caused by a biological event in quantitative metabolomics, it is critical to use an analytical tool that can perform accurate and precise quantification to examine the true concentration differences of individual metabolites found in different samples. A number of steps are involved in metabolomic analysis including pre-analytical work (e.g., sample collection and storage), analytical work (e.g., sample analysis) and data analysis (e.g., feature extraction and quantification). Each one of them can influence the quantitative results significantly and thus should be performed with great care. Among them, the total sample amount or concentration of metabolites can be significantly different from one sample to another. Thus, it is critical to reduce or eliminate the effect of total sample amount variation on quantification of individual metabolites. In this review, we describe the importance of sample normalization in the analytical workflow with a focus on mass spectrometry (MS)-based platforms, discuss a number of methods recently reported in the literature and comment on their applicability in real world metabolomics applications. Sample normalization has been sometimes ignored in metabolomics, partially due to the lack of a convenient means of performing sample normalization. We show that several methods are now available and sample normalization should be performed in quantitative metabolomics where the analyzed samples have significant variations in total sample amounts. Copyright © 2015 Elsevier B.V. All rights reserved.

DETERMINATION OF CHLORDANE IN SOIL BY LC/GC/ECD AND LC/GC/EC NIMS WITH COMPARISON OF ASE, SFE, AND SOXHLET EXTRACTION

EPA Science Inventory

Chlordane is a polychlorinated mixture that was used as a long-lived pesticide and now is considered a potential endocrine-disrupting compound. The Environmental Sciences Division is involved in modernizing methods for a number of analytes that are potential target substances for...

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…

Confronting Analytical Dilemmas for Understanding Complex Human Interactions in Design-Based Research from a Cultural-Historical Activity Theory (CHAT) Framework

ERIC Educational Resources Information Center

Yamagata-Lynch, Lisa C.

2007-01-01

Understanding human activity in real-world situations often involves complicated data collection, analysis, and presentation methods. This article discusses how Cultural-Historical Activity Theory (CHAT) can inform design-based research practices that focus on understanding activity in real-world situations. I provide a sample data set with…

An Analytical Chemistry Experiment in Simultaneous Spectrophotometric Determination of Fe(III) and Cu(II) with Hexacyanoruthenate(II) Reagent.

ERIC Educational Resources Information Center

Mehra, M. C.; Rioux, J.

1982-01-01

Experimental procedures, typical observations, and results for the simultaneous analysis of Fe(III) and Cu(II) in a solution are discussed. The method is based on selective interaction between the two ions and potassium hexacyanoruthenate(II) in acid solution involving no preliminary sample preparations. (Author/JN)

The Gran Plot Analysis of an Acid Mixture. An Undergraduate Experiment to Highlight this Alternate Method.

ERIC Educational Resources Information Center

Boiani, James A.

1986-01-01

Describes an experiment which uses the Gran plot for analyzing free ions as well as those involved in an equilibrium. Discusses the benefits of using Gran plots in the study of acids, as well as other analytes in solutions. Presents background theory along with a description of the experimental procedures. (TW)

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.

The Hazardous-Drums Project: A Multiweek Laboratory Exercise for General Chemistry Involving Environmental, Quality Control, and Cost Evaluation

ERIC Educational Resources Information Center

Hayes, David; Widanski, Bozena

2013-01-01

A laboratory experiment is described that introduces students to "real-world" hazardous waste management issues chemists face. The students are required to define an analytical problem, choose a laboratory analysis method, investigate cost factors, consider quality-control issues, interpret the meaning of results, and provide management…

Chemometrics-based process analytical technology (PAT) tools: applications and adaptation in pharmaceutical and biopharmaceutical industries.

PubMed

Challa, Shruthi; Potumarthi, Ravichandra

2013-01-01

Process analytical technology (PAT) is used to monitor and control critical process parameters in raw materials and in-process products to maintain the critical quality attributes and build quality into the product. Process analytical technology can be successfully implemented in pharmaceutical and biopharmaceutical industries not only to impart quality into the products but also to prevent out-of-specifications and improve the productivity. PAT implementation eliminates the drawbacks of traditional methods which involves excessive sampling and facilitates rapid testing through direct sampling without any destruction of sample. However, to successfully adapt PAT tools into pharmaceutical and biopharmaceutical environment, thorough understanding of the process is needed along with mathematical and statistical tools to analyze large multidimensional spectral data generated by PAT tools. Chemometrics is a chemical discipline which incorporates both statistical and mathematical methods to obtain and analyze relevant information from PAT spectral tools. Applications of commonly used PAT tools in combination with appropriate chemometric method along with their advantages and working principle are discussed. Finally, systematic application of PAT tools in biopharmaceutical environment to control critical process parameters for achieving product quality is diagrammatically represented.

Green analytical determination of emerging pollutants in environmental waters using excitation-emission photoinduced fluorescence data and multivariate calibration.

PubMed

Hurtado-Sánchez, María Del Carmen; Lozano, Valeria A; Rodríguez-Cáceres, María Isabel; Durán-Merás, Isabel; Escandar, Graciela M

2015-03-01

An eco-friendly strategy for the simultaneous quantification of three emerging pharmaceutical contaminants is presented. The proposed analytical method, which involves photochemically induced fluorescence matrix data combined with second-order chemometric analysis, was used for the determination of carbamazepine, ofloxacin and piroxicam in water samples of different complexity without the need of chromatographic separation. Excitation-emission photoinduced fluorescence matrices were obtained after UV irradiation, and processed with second-order algorithms. Only one of the tested algorithms was able to overcome the strong spectral overlapping among the studied pollutants and allowed their successful quantitation in very interferent media. The method sensitivity in superficial and underground water samples was enhanced by a simple solid-phase extraction with C18 membranes, which was successful for the extraction/preconcentration of the pollutants at trace levels. Detection limits in preconcentrated (1:125) real water samples ranged from 0.04 to 0.3 ng mL(-1). Relative prediction errors around 10% were achieved. The proposed strategy is significantly simpler and greener than liquid chromatography-mass spectrometry methods, without compromising the analytical quality of the results. Copyright © 2014 Elsevier B.V. All rights reserved.

Surface Plasmon Resonance: New Biointerface Designs and High-Throughput Affinity Screening

NASA Astrophysics Data System (ADS)

Linman, Matthew J.; Cheng, Quan Jason

Surface plasmon resonance (SPR) is a surface optical technique that measures minute changes in refractive index at a metal-coated surface. It has become increasingly popular in the study of biological and chemical analytes because of its label-free measurement feature. In addition, SPR allows for both quantitative and qualitative assessment of binding interactions in real time, making it ideally suited for probing weak interactions that are often difficult to study with other methods. This chapter presents the biosensor development in the last 3 years or so utilizing SPR as the principal analytical technique, along with a concise background of the technique itself. While SPR has demonstrated many advantages, it is a nonselective method and so, building reproducible and functional interfaces is vital to sensing applications. This chapter, therefore, focuses mainly on unique surface chemistries and assay approaches to examine biological interactions with SPR. In addition, SPR imaging for high-throughput screening based on microarrays and novel hyphenated techniques involving the coupling of SPR to other analytical methods is discussed. The chapter concludes with a commentary on the current state of SPR biosensing technology and the general direction of future biosensor research.

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

PubMed

Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-06-01

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

Analytic Formulation and Numerical Implementation of an Acoustic Pressure Gradient Prediction

NASA Technical Reports Server (NTRS)

Lee, Seongkyu; Brentner, Kenneth S.; Farassat, F.; Morris, Philip J.

2008-01-01

Two new analytical formulations of the acoustic pressure gradient have been developed and implemented in the PSU-WOPWOP rotor noise prediction code. The pressure gradient can be used to solve the boundary condition for scattering problems and it is a key aspect to solve acoustic scattering problems. The first formulation is derived from the gradient of the Ffowcs Williams-Hawkings (FW-H) equation. This formulation has a form involving the observer time differentiation outside the integrals. In the second formulation, the time differentiation is taken inside the integrals analytically. This formulation avoids the numerical time differentiation with respect to the observer time, which is computationally more efficient. The acoustic pressure gradient predicted by these new formulations is validated through comparison with available exact solutions for a stationary and moving monopole sources. The agreement between the predictions and exact solutions is excellent. The formulations are applied to the rotor noise problems for two model rotors. A purely numerical approach is compared with the analytical formulations. The agreement between the analytical formulations and the numerical method is excellent for both stationary and moving observer cases.

Rapid analysis of aminoglycoside antibiotics in bovine tissues using disposable pipette extraction and ultrahigh performance liquid chromatography-tandem mass spectrometry.

PubMed

Lehotay, Steven J; Mastovska, Katerina; Lightfield, Alan R; Nuñez, Alberto; Dutko, Terry; Ng, Chilton; Bluhm, Louis

2013-10-25

A high-throughput qualitative screening and identification method for 9 aminoglycosides of regulatory interest has been developed, validated, and implemented for bovine kidney, liver, and muscle tissues. The method involves extraction at previously validated conditions, cleanup using disposable pipette extraction, and analysis by a 3 min ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method. The drug analytes include neomycin, streptomycin, dihydrosptreptomycin, and spectinomycin, which have residue tolerances in bovine in the US, and kanamicin, gentamicin, apramycin, amikacin, and hygromycin, which do not have US tolerances established in bovine tissues. Tobramycin was used as an internal standard. An additional drug, paromomycin also was validated in the method, but it was dropped during implementation due to conversion of neomycin into paromomycin. Proposed fragmentation patterns for the monitored ions of each analyte were elucidated with the aid of high resolution MS using a quadrupole-time-of-flight instrument. Recoveries from spiking experiments at regulatory levels of concern showed that all analytes averaged 70-120% recoveries in all tissues, except hygromycin averaged 61% recovery. Lowest calibrated levels were as low as 0.005 μg/g in matrix extracts, which approximately corresponded to the limit of detection for screening purposes. Drug identifications at levels <0.05 μg/g were made in spiked and/or real samples for all analytes and tissues tested. Analyses of 60 samples from 20 slaughtered cattle previously screened positive for aminoglycosides showed that this method worked well in practice. The UHPLC-MS/MS method has several advantages compared to the previous microbial inhibition screening assay, especially for distinguishing individual drugs from a mixture and improving identification of gentamicin in tissue samples. Published by Elsevier B.V.

Quantitative Methods Based on Twisted Nematic Liquid Crystals for Mapping Surfaces Patterned with Bio/Chemical Functionality Relevant to Bioanalytical Assays

PubMed Central

Lowe, Aaron M.; Bertics, Paul J.; Abbott, Nicholas L.

2009-01-01

We report methods for the acquisition and analysis of optical images formed by thin films of twisted nematic liquid crystals (LCs) placed into contact with surfaces patterned with bio/chemical functionality relevant to surface-based assays. The methods are simple to implement and are shown to provide easily interpreted maps of chemical transformations on surfaces that are widely exploited in the preparation of analytic devices. The methods involve acquisition of multiple images of the LC as a function of the orientation of a polarizer; data analysis condenses the information present in the stack of images into a spatial map of the twist angle of the LC on the analytic surface. The potential utility of the methods is illustrated by mapping (i) the displacement of a monolayer formed from one alkanethiol on a gold film by a second thiol in solution, (ii) coadsorption of mixtures of amine-terminated and ethyleneglycol-terminated alkanethiols on gold films, which leads to a type of mixed monolayer that is widely exploited for immobilization of proteins on analytic surfaces, and (iii) patterns of antibodies printed onto surfaces. These results show that maps of the twist angle of the LC constructed from families of optical images can be used to reveal surface features that are not apparent in a single image of the LC film. Furthermore, the twist angles of the LC can be used to quantify the energy of interaction of the LC with the surface with a spatial resolution of <10 µm. When combined, the results described in this paper suggest non-destructive methods to monitor and validate chemical transformations on surfaces of the type that are routinely employed in the preparation of surface-based analytic technologies. PMID:18355089

Irregular analytical errors in diagnostic testing - a novel concept.

PubMed

Vogeser, Michael; Seger, Christoph

2018-02-23

In laboratory medicine, routine periodic analyses for internal and external quality control measurements interpreted by statistical methods are mandatory for batch clearance. Data analysis of these process-oriented measurements allows for insight into random analytical variation and systematic calibration bias over time. However, in such a setting, any individual sample is not under individual quality control. The quality control measurements act only at the batch level. Quantitative or qualitative data derived for many effects and interferences associated with an individual diagnostic sample can compromise any analyte. It is obvious that a process for a quality-control-sample-based approach of quality assurance is not sensitive to such errors. To address the potential causes and nature of such analytical interference in individual samples more systematically, we suggest the introduction of a new term called the irregular (individual) analytical error. Practically, this term can be applied in any analytical assay that is traceable to a reference measurement system. For an individual sample an irregular analytical error is defined as an inaccuracy (which is the deviation from a reference measurement procedure result) of a test result that is so high it cannot be explained by measurement uncertainty of the utilized routine assay operating within the accepted limitations of the associated process quality control measurements. The deviation can be defined as the linear combination of the process measurement uncertainty and the method bias for the reference measurement system. Such errors should be coined irregular analytical errors of the individual sample. The measurement result is compromised either by an irregular effect associated with the individual composition (matrix) of the sample or an individual single sample associated processing error in the analytical process. Currently, the availability of reference measurement procedures is still highly limited, but LC-isotope-dilution mass spectrometry methods are increasingly used for pre-market validation of routine diagnostic assays (these tests also involve substantial sets of clinical validation samples). Based on this definition/terminology, we list recognized causes of irregular analytical error as a risk catalog for clinical chemistry in this article. These issues include reproducible individual analytical errors (e.g. caused by anti-reagent antibodies) and non-reproducible, sporadic errors (e.g. errors due to incorrect pipetting volume due to air bubbles in a sample), which can both lead to inaccurate results and risks for patients.

A rapid method for estimation of Pu-isotopes in urine samples using high volume centrifuge.

PubMed

Kumar, Ranjeet; Rao, D D; Dubla, Rupali; Yadav, J R

2017-07-01

The conventional radio-analytical technique used for estimation of Pu-isotopes in urine samples involves anion exchange/TEVA column separation followed by alpha spectrometry. This sequence of analysis consumes nearly 3-4 days for completion. Many a times excreta analysis results are required urgently, particularly under repeat and incidental/emergency situations. Therefore, there is need to reduce the analysis time for the estimation of Pu-isotopes in bioassay samples. This paper gives the details of standardization of a rapid method for estimation of Pu-isotopes in urine samples using multi-purpose centrifuge, TEVA resin followed by alpha spectrometry. The rapid method involves oxidation of urine samples, co-precipitation of plutonium along with calcium phosphate followed by sample preparation using high volume centrifuge and separation of Pu using TEVA resin. Pu-fraction was electrodeposited and activity estimated using 236 Pu tracer recovery by alpha spectrometry. Ten routine urine samples of radiation workers were analyzed and consistent radiochemical tracer recovery was obtained in the range 47-88% with a mean and standard deviation of 64.4% and 11.3% respectively. With this newly standardized technique, the whole analytical procedure is completed within 9h (one working day hour). Copyright © 2017 Elsevier Ltd. All rights reserved.

Projected Regression Methods for Inverting Fredholm Integrals: Formalism and Application to Analytical Continuation

NASA Astrophysics Data System (ADS)

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

We present a machine learning-based statistical regression approach to the inversion of Fredholm integrals of the first kind by studying an important example for the quantum materials community, the analytical continuation problem of quantum many-body physics. It involves reconstructing the frequency dependence of physical excitation spectra from data obtained at specific points in the complex frequency plane. The approach provides a natural regularization in cases where the inverse of the Fredholm kernel is ill-conditioned and yields robust error metrics. The stability of the forward problem permits the construction of a large database of input-output pairs. Machine learning methods applied to this database generate approximate solutions which are projected onto the subspace of functions satisfying relevant constraints. We show that for low input noise the method performs as well or better than Maximum Entropy (MaxEnt) under standard error metrics, and is substantially more robust to noise. We expect the methodology to be similarly effective for any problem involving a formally ill-conditioned inversion, provided that the forward problem can be efficiently solved. AJM was supported by the Office of Science of the U.S. Department of Energy under Subcontract No. 3F-3138 and LFA by the Columbia Univeristy IDS-ROADS project, UR009033-05 which also provided part support to RN and LH.

PPM mixtures of formaldehyde in gas cylinders: Stability and analysis

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

Wong, K.C.; Miller, S.B.; Patterson, L.M.

1999-07-01

Scott Specialty Gases has been successful in producing stable calibration gases of formaldehyde at low concentration. Critical to this success has been the development of a treatment process for high pressure aluminum cylinders. Formaldehyde cylinders having concentrations of 20ppm and 4ppm were found to show only small decline in concentrations over a period of approximately 12 months. Since no NIST traceable formaldehyde standards (or Standard Reference Material) are available, all Scott's formaldehyde cylinders were originally certified by traditional impinger method. This method involves an extremely tedious purification procedure for 2,4-dinitrophenylhydrazine (2,4-DNPH). A modified version of the impinger method has beenmore » developed and does not require extensive reagent purification for formaldehyde analysis. Extremely low formaldehyde blanks have been obtained with the modified method. The HPLC conditions in the original method were used for chromatographic separations. The modified method results in a lower analytical uncertainty for the formaldehyde standard mixtures. Consequently, it is possible to discern small differences between analytical results that are important for stability study.« less

Simultaneous determination of fumonisins B1 and B2 in different types of maize by matrix solid phase dispersion and HPLC-MS/MS.

PubMed

de Oliveira, Gabriel Barros; de Castro Gomes Vieira, Carolyne Menezes; Orlando, Ricardo Mathias; Faria, Adriana Ferreira

2017-10-15

This work involved the optimization and validation of a method, according to Directive 2002/657/EC and the Analytical Quality Assurance Manual of Ministério da Agricultura, Pecuária e Abastecimento, Brazil, for simultaneous extraction and determination of fumonisins B1 and B2 in maize. The extraction procedure was based on a matrix solid phase dispersion approach, the optimization of which employed a sequence of different factorial designs. A liquid chromatography-tandem mass spectrometry method was developed for determining these analytes using the selected reaction monitoring mode. The optimized method employed only 1g of silica gel for dispersion and elution with 70% ammonium formate aqueous buffer (50mmolL -1 , pH 9), representing a simple, cheap and chemically friendly sample preparation method. Trueness (recoveries: 86-106%), precision (RSD ≤19%), decision limits, detection capabilities and measurement uncertainties were calculated for the validated method. The method scope was expanded to popcorn kernels, white maize kernels and yellow maize grits. Copyright © 2017 Elsevier Ltd. All rights reserved.

Accurate Estimate of Some Propagation Characteristics for the First Higher Order Mode in Graded Index Fiber with Simple Analytic Chebyshev Method

NASA Astrophysics Data System (ADS)

Dutta, Ivy; Chowdhury, Anirban Roy; Kumbhakar, Dharmadas

2013-03-01

Using Chebyshev power series approach, accurate description for the first higher order (LP11) mode of graded index fibers having three different profile shape functions are presented in this paper and applied to predict their propagation characteristics. These characteristics include fractional power guided through the core, excitation efficiency and Petermann I and II spot sizes with their approximate analytic formulations. We have shown that where two and three Chebyshev points in LP11 mode approximation present fairly accurate results, the values based on our calculations involving four Chebyshev points match excellently with available exact numerical results.

HPLC detection of soluble carbohydrates involved in mannitol and trehalose metabolism in the edible mushroom Agaricus bisporus.

PubMed

Wannet, W J; Hermans, J H; van Der Drift, C; Op Den Camp, H J

2000-02-01

A convenient and sensitive method was developed to separate and detect various types of carbohydrates (polyols, mono- and disaccharides, and phosphorylated sugars) simultaneously using high-performance liquid chromatography (HPLC). The method consists of a chromatographic separation on a CarboPac PA1 anion-exchange analytical column followed by pulsed amperometric detection. In a single run (43 min) 13 carbohydrates were readily resolved. Calibration plots were linear over the ranges of 5-25 microM to 1. 0-1.5 mM. The reliable and fast analysis technique, avoiding derivatization steps and long run times, was used to determine the levels of carbohydrates involved in mannitol and trehalose metabolism in the edible mushroom Agaricus bisporus. Moreover, the method was used to study the trehalose phosphorylase reaction.

On-matrix derivatization extraction of chemical weapons convention relevant alcohols from soil.

PubMed

Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Dubey, D K; Pardasani, Deepak

2013-10-11

Present study deals with the on-matrix derivatization-extraction of aminoalcohols and thiodiglycols, which are important precursors and/or degradation products of VX analogues and vesicants class of chemical warfare agents (CWAs). The method involved hexamethyldisilazane (HMDS) mediated in situ silylation of analytes on the soil. Subsequent extraction and gas chromatography-mass spectrometry analysis of derivatized analytes offered better recoveries in comparison to the procedure recommended by the Organization for the Prohibition of Chemical Weapons (OPCW). Various experimental conditions such as extraction solvent, reagent and catalyst amount, reaction time and temperature were optimized. Best recoveries of analytes ranging from 45% to 103% were obtained with DCM solvent containing 5%, v/v HMDS and 0.01%, w/v iodine as catalyst. The limits of detection (LOD) and limit of quantification (LOQ) with selected analytes ranged from 8 to 277 and 21 to 665ngmL(-1), respectively, in selected ion monitoring mode. Copyright © 2013 Elsevier B.V. All rights reserved.

Analytical approximations for the oscillators with anti-symmetric quadratic nonlinearity

NASA Astrophysics Data System (ADS)

Alal Hosen, Md.; Chowdhury, M. S. H.; Yeakub Ali, Mohammad; Faris Ismail, Ahmad

2017-12-01

A second-order ordinary differential equation involving anti-symmetric quadratic nonlinearity changes sign. The behaviour of the oscillators with an anti-symmetric quadratic nonlinearity is assumed to oscillate different in the positive and negative directions. In this reason, Harmonic Balance Method (HBM) cannot be directly applied. The main purpose of the present paper is to propose an analytical approximation technique based on the HBM for obtaining approximate angular frequencies and the corresponding periodic solutions of the oscillators with anti-symmetric quadratic nonlinearity. After applying HBM, a set of complicated nonlinear algebraic equations is found. Analytical approach is not always fruitful for solving such kinds of nonlinear algebraic equations. In this article, two small parameters are found, for which the power series solution produces desired results. Moreover, the amplitude-frequency relationship has also been determined in a novel analytical way. The presented technique gives excellent results as compared with the corresponding numerical results and is better than the existing ones.

Analytic materials

PubMed Central

2016-01-01

The theory of inhomogeneous analytic materials is developed. These are materials where the coefficients entering the equations involve analytic functions. Three types of analytic materials are identified. The first two types involve an integer p. If p takes its maximum value, then we have a complete analytic material. Otherwise, it is incomplete analytic material of rank p. For two-dimensional materials, further progress can be made in the identification of analytic materials by using the well-known fact that a 90° rotation applied to a divergence-free field in a simply connected domain yields a curl-free field, and this can then be expressed as the gradient of a potential. Other exact results for the fields in inhomogeneous media are reviewed. Also reviewed is the subject of metamaterials, as these materials provide a way of realizing desirable coefficients in the equations. PMID:27956882

An isocratic HPLC method for the simultaneous determination of cholesterol, cardiolipin, and DOPC in lyophilized lipids and liposomal formulations.

PubMed

Simonzadeh, Ninus

2009-04-01

Phospholipids, such as 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC), and 1,1',2,2'-tetramyristoyl cardiolipin, along with cholesterol, form liposomes in aqueous media and have been investigated at NeoPharm (Lake Bluff, IL) as drug-delivery systems. To accurately assess the effectiveness of various formulations involving the use of aforementioned phospholipids and cholesterol, their quantitative determination is essential. An isocratic high-performance liquid chromatographic method for the simultaneous determination of cholesterol, cardiolipin, and DOPC in various pharmaceutical formulations containing the active drug substance has consequently been developed and is presented here. The current method utilizes an ASTEC-diol analytical column and is shown to be stability-indicating and free from interference from any of the formulation excipients, such as sucrose, sodium chloride, and sodium lactate. The analytes are detected using an evaporative light scattering detector (Alltech or Polymer Laboratories). The quantitation of each lipid component is performed using non-linear regression analysis. The retention characteristics of the analytes are examined as a function of eluent composition (e.g., pH, salt content, organic to aqueous phase ratio) and column temperature. The method was validated and was found to be sensitive, specific, rugged, and cost-effective. The current method provides enhanced chromatographic separation for lipid components as well as degradation products as compared to similar methods reported in the literature. It is also inherently simpler than other similar methods reported in the literature that typically use complex gradient elution.

Prediction of jump phenomena in rotationally-coupled maneuvers of aircraft, including nonlinear aerodynamic effects

NASA Technical Reports Server (NTRS)

Young, J. W.; Schy, A. A.; Johnson, K. G.

1977-01-01

An analytical method has been developed for predicting critical control inputs for which nonlinear rotational coupling may cause sudden jumps in aircraft response. The analysis includes the effect of aerodynamics which are nonlinear in angle of attack. The method involves the simultaneous solution of two polynomials in roll rate, whose coefficients are functions of angle of attack and the control inputs. Results obtained using this procedure are compared with calculated time histories to verify the validity of the method for predicting jump-like instabilities.

Status of Rifaximin: A Review of Characteristics, Uses and Analytical Methods.

PubMed

Kogawa, Ana Carolina; Salgado, Hérida Regina Nunes

2018-11-02

Rifaximin, an oral antimicrobial, has many advantages because it is selective intestine, has minimal adverse effects and is used for the treatment of some diseases such as hepatic encephalopathy, irritable bowel syndrome, travelers' diarrhea, ulcerative colitis, Clostridium difficile and acute diarrhea. Rifaximin in the form of 200 mg tablets is commercially available. The crystalline α form is therapeutically safe and effective. In most of the official compendia, rifaximin has no monograph and in none of them is there a monograph for rifaximin tablets. The literature, however, contemplates this gap with varied methods. The literature presents some methods for evaluation of rifaximin in both biological fluid and pharmaceutical product. High performance liquid chromatography stands out for the evaluation of rifaximin. Most of the methods reported in the literature are for pharmaceuticals products. They use (1) toxic organic solvents, harmful to the operator and the environment, and/or (2) buffer solution, which has a shorter service life and requires time-consuming washes of the chromatographic system generating more waste. So, this work aims to discuss (i) properties; (ii) applications; (iii) polymorphism and (iv) analytical methods of rifaximin by the look of green chemistry. This review shows an extremely current topic of great importance to the chemical-pharmaceutical area and everything it involves, since the analytical process until the impact on the environment in which it is embedded.

Fractional Order and Dynamic Simulation of a System Involving an Elastic Wide Plate

NASA Astrophysics Data System (ADS)

David, S. A.; Balthazar, J. M.; Julio, B. H. S.; Oliveira, C.

2011-09-01

Numerous researchers have studied about nonlinear dynamics in several areas of science and engineering. However, in most cases, these concepts have been explored mainly from the standpoint of analytical and computational methods involving integer order calculus (IOC). In this paper we have examined the dynamic behavior of an elastic wide plate induced by two electromagnets of a point of view of the fractional order calculus (FOC). The primary focus of this study is on to help gain a better understanding of nonlinear dynamic in fractional order systems.

Tracking Matrix Effects in the Analysis of DNA Adducts of Polycyclic Aromatic Hydrocarbons

PubMed Central

Klaene, Joshua J.; Flarakos, Caroline; Glick, James; Barret, Jennifer T.; Zarbl, Helmut; Vouros, Paul

2015-01-01

LC-MS using electrospray ionization is currently the method of choice in bio-organic analysis covering a wide range of applications in a broad spectrum of biological media. The technique is noted for its high sensitivity but one major limitation which hinders achievement of its optimal sensitivity is the signal suppression due to matrix inferences introduced by the presence of co-extracted compounds during the sample preparation procedure. The analysis of DNA adducts of common environmental carcinogens is particularly sensitive to such matrix effects as sample preparation is a multistep process which involves “contamination” of the sample due to the addition of enzymes and other reagents for digestion of the DNA in order to isolate the analyte(s). This problem is further exacerbated by the need to reach low levels of quantitation (LOQ in the ppb level) while also working with limited (2-5 μg) quantities of sample. We report here on the systematic investigation of ion signal suppression contributed by each individual step involved in the sample preparation associated with the analysis of DNA adducts of polycyclic aromatic hydrocarbon (PAH) using as model analyte dG-BaP, the deoxyguanosine adduct of benzo[a]pyrene (BaP). The individual matrix contribution of each one of these sources to analyte signal was systematically addressed as were any interactive effects. The information was used to develop a validated analytical protocol for the target biomarker at levels typically encountered in vivo using as little as 2 μg of DNA and applied to a dose response study using a metabolically competent cell line. PMID:26607319

New procedure of quantitative mapping of Ti and Al released from dental implant and Mg, Ca, Fe, Zn, Cu, Mn as physiological elements in oral mucosa by LA-ICP-MS.

PubMed

Sajnóg, Adam; Hanć, Anetta; Koczorowski, Ryszard; Barałkiewicz, Danuta

2017-12-01

A new procedure for determination of elements derived from titanium implants and physiological elements in soft tissues by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is presented. The analytical procedure was developed which involved preparation of in-house matrix matched solid standards with analyte addition based on certified reference material (CRM) MODAS-4 Cormorant Tissue. Addition of gelatin, serving as a binding agent, essentially improved physical properties of standards. Performance of the analytical method was assayed and validated by calculating parameters like precision, detection limits, trueness and recovery of analyte addition using additional CRM - ERM-BB184 Bovine Muscle. Analyte addition was additionally confirmed by microwave digestion of solid standards and analysis by solution nebulization ICP-MS. The detection limits are in range 1.8μgg -1 to 450μgg -1 for Mn and Ca respectively. The precision values range from 7.3% to 42% for Al and Zn respectively. The estimated recoveries of analyte addition line within scope of 83%-153% for Mn and Cu respectively. Oral mucosa samples taken from patients treated with titanium dental implants were examined using developed analytical method. Standards and tissue samples were cryocut into 30µm thin sections. LA-ICP-MS allowed to obtain two-dimensional maps of distribution of elements in tested samples which revealed high content of Ti and Al derived from implants. Photographs from optical microscope displayed numerous particles with µm size in oral mucosa samples which suggests that they are residues from implantation procedure. Copyright © 2017 Elsevier B.V. All rights reserved.

A Review of Interface Electronic Systems for AT-cut Quartz Crystal Microbalance Applications in Liquids

PubMed Central

Arnau, Antonio

2008-01-01

From the first applications of AT-cut quartz crystals as sensors in solutions more than 20 years ago, the so-called quartz crystal microbalance (QCM) sensor is becoming into a good alternative analytical method in a great deal of applications such as biosensors, analysis of biomolecular interactions, study of bacterial adhesion at specific interfaces, pathogen and microorganism detection, study of polymer film-biomolecule or cell-substrate interactions, immunosensors and an extensive use in fluids and polymer characterization and electrochemical applications among others. The appropriate evaluation of this analytical method requires recognizing the different steps involved and to be conscious of their importance and limitations. The first step involved in a QCM system is the accurate and appropriate characterization of the sensor in relation to the specific application. The use of the piezoelectric sensor in contact with solutions strongly affects its behavior and appropriate electronic interfaces must be used for an adequate sensor characterization. Systems based on different principles and techniques have been implemented during the last 25 years. The interface selection for the specific application is important and its limitations must be known to be conscious of its suitability, and for avoiding the possible error propagation in the interpretation of results. This article presents a comprehensive overview of the different techniques used for AT-cut quartz crystal microbalance in in-solution applications, which are based on the following principles: network or impedance analyzers, decay methods, oscillators and lock-in techniques. The electronic interfaces based on oscillators and phase-locked techniques are treated in detail, with the description of different configurations, since these techniques are the most used in applications for detection of analytes in solutions, and in those where a fast sensor response is necessary. PMID:27879713

One-step patterning of hollow microstructures in paper by laser cutting to create microfluidic analytical devices.

PubMed

Nie, Jinfang; Liang, Yuanzhi; Zhang, Yun; Le, Shangwang; Li, Dunnan; Zhang, Songbai

2013-01-21

In this paper, we report a simple, low-cost method for rapid, highly reproductive fabrication of paper-based microfluidics by using a commercially available, minitype CO(2) laser cutting/engraving machine. This method involves only one operation of cutting a piece of paper by laser according to a predesigned pattern. The hollow microstructures formed in the paper are used as the 'hydrophobic barriers' to define the hydrophilic flowing paths. A typical paper device on a 4 cm × 4 cm piece of paper can be fabricated within ∼7-20 s; it is ready for use once the cutting process is finished. The main fabrication parameters such as the applied current and cutting rate of the laser were optimized. The fabrication resolution and multiplexed analytical capability of the hollow microstructure-patterned paper were also characterized.

Kinetic Titration Series with Biolayer Interferometry

PubMed Central

Frenzel, Daniel; Willbold, Dieter

2014-01-01

Biolayer interferometry is a method to analyze protein interactions in real-time. In this study, we illustrate the usefulness to quantitatively analyze high affinity protein ligand interactions employing a kinetic titration series for characterizing the interactions between two pairs of interaction patterns, in particular immunoglobulin G and protein G B1 as well as scFv IC16 and amyloid beta (1–42). Kinetic titration series are commonly used in surface plasmon resonance and involve sequential injections of analyte over a desired concentration range on a single ligand coated sensor chip without waiting for complete dissociation between the injections. We show that applying this method to biolayer interferometry is straightforward and i) circumvents problems in data evaluation caused by unavoidable sensor differences, ii) saves resources and iii) increases throughput if screening a multitude of different analyte/ligand combinations. PMID:25229647

Kinetic titration series with biolayer interferometry.

PubMed

Frenzel, Daniel; Willbold, Dieter

2014-01-01

Biolayer interferometry is a method to analyze protein interactions in real-time. In this study, we illustrate the usefulness to quantitatively analyze high affinity protein ligand interactions employing a kinetic titration series for characterizing the interactions between two pairs of interaction patterns, in particular immunoglobulin G and protein G B1 as well as scFv IC16 and amyloid beta (1-42). Kinetic titration series are commonly used in surface plasmon resonance and involve sequential injections of analyte over a desired concentration range on a single ligand coated sensor chip without waiting for complete dissociation between the injections. We show that applying this method to biolayer interferometry is straightforward and i) circumvents problems in data evaluation caused by unavoidable sensor differences, ii) saves resources and iii) increases throughput if screening a multitude of different analyte/ligand combinations.

A Review of Current Methods for Analysis of Mycotoxins in Herbal Medicines

PubMed Central

Zhang, Lei; Dou, Xiao-Wen; Zhang, Cheng; Logrieco, Antonio F.; Yang, Mei-Hua

2018-01-01

The presence of mycotoxins in herbal medicines is an established problem throughout the entire world. The sensitive and accurate analysis of mycotoxin in complicated matrices (e.g., herbs) typically involves challenging sample pretreatment procedures and an efficient detection instrument. However, although numerous reviews have been published regarding the occurrence of mycotoxins in herbal medicines, few of them provided a detailed summary of related analytical methods for mycotoxin determination. This review focuses on analytical techniques including sampling, extraction, cleanup, and detection for mycotoxin determination in herbal medicines established within the past ten years. Dedicated sections of this article address the significant developments in sample preparation, and highlight the importance of this procedure in the analytical technology. This review also summarizes conventional chromatographic techniques for mycotoxin qualification or quantitation, as well as recent studies regarding the development and application of screening assays such as enzyme-linked immunosorbent assays, lateral flow immunoassays, aptamer-based lateral flow assays, and cytometric bead arrays. The present work provides a good insight regarding the advanced research that has been done and closes with an indication of future demand for the emerging technologies. PMID:29393905

Analytical methods involving separation techniques for determination of low-molecular-weight biothiols in human plasma and blood.

PubMed

Isokawa, Muneki; Kanamori, Takahiro; Funatsu, Takashi; Tsunoda, Makoto

2014-08-01

Low-molecular-weight biothiols such as homocysteine, cysteine, and glutathione are metabolites of the sulfur cycle and play important roles in biological processes such as the antioxidant defense network, methionine cycle, and protein synthesis. Thiol concentrations in human plasma and blood are related to diseases such as cardiovascular disease, neurodegenerative disease, and cancer. The concentrations of homocysteine, cysteine, and glutathione in plasma samples from healthy human subjects are approximately in the range of 5-15, 200-300, and 1-5 μM, respectively. Glutathione concentration in the whole blood is in the millimolar range. Measurement of biothiol levels in plasma and blood is thought to be important for understanding the physiological roles and biomarkers for certain diseases. This review summarizes the relationship of biothiols with certain disease as well as pre-analytical treatment and analytical methods for determination of biothiols in human plasma and blood by using high-performance liquid chromatography and capillary electrophoresis coupled with ultraviolet, fluorescence, or chemiluminescence detection; or mass spectrometry. Copyright © 2014 Elsevier B.V. All rights reserved.

Beyond Antibodies as Binding Partners: The Role of Antibody Mimetics in Bioanalysis.

PubMed

Yu, Xiaowen; Yang, Yu-Ping; Dikici, Emre; Deo, Sapna K; Daunert, Sylvia

2017-06-12

The emergence of novel binding proteins or antibody mimetics capable of binding to ligand analytes in a manner analogous to that of the antigen-antibody interaction has spurred increased interest in the biotechnology and bioanalytical communities. The goal is to produce antibody mimetics designed to outperform antibodies with regard to binding affinities, cellular and tumor penetration, large-scale production, and temperature and pH stability. The generation of antibody mimetics with tailored characteristics involves the identification of a naturally occurring protein scaffold as a template that binds to a desired ligand. This scaffold is then engineered to create a superior binder by first creating a library that is then subjected to a series of selection steps. Antibody mimetics have been successfully used in the development of binding assays for the detection of analytes in biological samples, as well as in separation methods, cancer therapy, targeted drug delivery, and in vivo imaging. This review describes recent advances in the field of antibody mimetics and their applications in bioanalytical chemistry, specifically in diagnostics and other analytical methods.

Evaluation of Analytical Errors in a Clinical Chemistry Laboratory: A 3 Year Experience

PubMed Central

Sakyi, AS; Laing, EF; Ephraim, RK; Asibey, OF; Sadique, OK

2015-01-01

Background: Proficient laboratory service is the cornerstone of modern healthcare systems and has an impact on over 70% of medical decisions on admission, discharge, and medications. In recent years, there is an increasing awareness of the importance of errors in laboratory practice and their possible negative impact on patient outcomes. Aim: We retrospectively analyzed data spanning a period of 3 years on analytical errors observed in our laboratory. The data covered errors over the whole testing cycle including pre-, intra-, and post-analytical phases and discussed strategies pertinent to our settings to minimize their occurrence. Materials and Methods: We described the occurrence of pre-analytical, analytical and post-analytical errors observed at the Komfo Anokye Teaching Hospital clinical biochemistry laboratory during a 3-year period from January, 2010 to December, 2012. Data were analyzed with Graph Pad Prism 5(GraphPad Software Inc. CA USA). Results: A total of 589,510 tests was performed on 188,503 outpatients and hospitalized patients. The overall error rate for the 3 years was 4.7% (27,520/58,950). Pre-analytical, analytical and post-analytical errors contributed 3.7% (2210/58,950), 0.1% (108/58,950), and 0.9% (512/58,950), respectively. The number of tests reduced significantly over the 3-year period, but this did not correspond with a reduction in the overall error rate (P = 0.90) along with the years. Conclusion: Analytical errors are embedded within our total process setup especially pre-analytical and post-analytical phases. Strategic measures including quality assessment programs for staff involved in pre-analytical processes should be intensified. PMID:25745569

Patterns of Work and Family Involvement among Single and Dual Earner Couples: Two Competing Analytical Approaches.

ERIC Educational Resources Information Center

Yogev, Sara; Brett, Jeanne

This paper offers a conceptual framework for the intersection of work and family roles based on the constructs of work involvement and family involvement. The theoretical and empirical literature on the intersection of work and family roles is reviewed from two analytical approaches. From the individual level of analysis, the literature reviewed…

Retention prediction and separation optimization under multilinear gradient elution in liquid chromatography with Microsoft Excel macros.

PubMed

Fasoula, S; Zisi, Ch; Gika, H; Pappa-Louisi, A; Nikitas, P

2015-05-22

A package of Excel VBA macros have been developed for modeling multilinear gradient retention data obtained in single or double gradient elution mode by changing organic modifier(s) content and/or eluent pH. For this purpose, ten chromatographic models were used and four methods were adopted for their application. The methods were based on (a) the analytical expression of the retention time, provided that this expression is available, (b) the retention times estimated using the Nikitas-Pappa approach, (c) the stepwise approximation, and (d) a simple numerical approximation involving the trapezoid rule for integration of the fundamental equation for gradient elution. For all these methods, Excel VBA macros have been written and implemented using two different platforms; the fitting and the optimization platform. The fitting platform calculates not only the adjustable parameters of the chromatographic models, but also the significance of these parameters and furthermore predicts the analyte elution times. The optimization platform determines the gradient conditions that lead to the optimum separation of a mixture of analytes by using the Solver evolutionary mode, provided that proper constraints are set in order to obtain the optimum gradient profile in the minimum gradient time. The performance of the two platforms was tested using experimental and artificial data. It was found that using the proposed spreadsheets, fitting, prediction, and optimization can be performed easily and effectively under all conditions. Overall, the best performance is exhibited by the analytical and Nikitas-Pappa's methods, although the former cannot be used under all circumstances. Copyright © 2015 Elsevier B.V. All rights reserved.

The Social Life of Learning Analytics: Cluster Analysis and the 'Performance' of Algorithmic Education

ERIC Educational Resources Information Center

Perrotta, Carlo; Williamson, Ben

2018-01-01

This paper argues that methods used for the classification and measurement of online education are not neutral and objective, but involved in the creation of the educational realities they claim to measure. In particular, the paper draws on material semiotics to examine cluster analysis as a 'performative device' that, to a significant extent,…

Do Specialty Courts Achieve Better Outcomes for Children in Foster Care than General Courts?

ERIC Educational Resources Information Center

Sloan, Frank A.; Gifford, Elizabeth J.; Eldred, Lindsey M.; Acquah, Kofi F.; Blevins, Claire E.

2013-01-01

Objective: This study assessed the effects of unified family and drug treatment courts (DTCs) on the resolution of cases involving foster care children and the resulting effects on school performance. Method: The first analytic step was to assess the impacts of presence of unified and DTCs in North Carolina counties on time children spent in…

A framework for performing workplace hazard and risk analysis: a participative ergonomics approach.

PubMed

Morag, Ido; Luria, Gil

2013-01-01

Despite the unanimity among researchers about the centrality of workplace analysis based on participatory ergonomics (PE) as a basis for preventive interventions, there is still little agreement about the necessary of a theoretical framework for providing practical guidance. In an effort to develop a conceptual PE framework, the authors, focusing on 20 studies, found five primary dimensions for characterising an analytical structure: (1) extent of workforce involvement; (2) analysis duration; (3) diversity of reporter role types; (4) scope of analysis and (5) supportive information system for analysis management. An ergonomics analysis carried out in a chemical manufacturing plant serves as a case study for evaluating the proposed framework. The study simultaneously demonstrates the five dimensions and evaluates their feasibility. The study showed that managerial leadership was fundamental to the successful implementation of the analysis; that all job holders should participate in analysing their own workplace and simplified reporting methods contributed to a desirable outcome. This paper seeks to clarify the scope of workplace ergonomics analysis by offering a theoretical and structured framework for providing practical advice and guidance. Essential to successfully implementing the analytical framework are managerial involvement, participation of all job holders and simplified reporting methods.

Standardless quantification by parameter optimization in electron probe microanalysis

NASA Astrophysics Data System (ADS)

Limandri, Silvina P.; Bonetto, Rita D.; Josa, Víctor Galván; Carreras, Alejo C.; Trincavelli, Jorge C.

2012-11-01

A method for standardless quantification by parameter optimization in electron probe microanalysis is presented. The method consists in minimizing the quadratic differences between an experimental spectrum and an analytical function proposed to describe it, by optimizing the parameters involved in the analytical prediction. This algorithm, implemented in the software POEMA (Parameter Optimization in Electron Probe Microanalysis), allows the determination of the elemental concentrations, along with their uncertainties. The method was tested in a set of 159 elemental constituents corresponding to 36 spectra of standards (mostly minerals) that include trace elements. The results were compared with those obtained with the commercial software GENESIS Spectrum® for standardless quantification. The quantifications performed with the method proposed here are better in the 74% of the cases studied. In addition, the performance of the method proposed is compared with the first principles standardless analysis procedure DTSA for a different data set, which excludes trace elements. The relative deviations with respect to the nominal concentrations are lower than 0.04, 0.08 and 0.35 for the 66% of the cases for POEMA, GENESIS and DTSA, respectively.

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.

Pharmaceutical cocrystals, salts and polymorphs: Advanced characterization techniques.

PubMed

Pindelska, Edyta; Sokal, Agnieszka; Kolodziejski, Waclaw

2017-08-01

The main goal of a novel drug development is to obtain it with optimal physiochemical, pharmaceutical and biological properties. Pharmaceutical companies and scientists modify active pharmaceutical ingredients (APIs), which often are cocrystals, salts or carefully selected polymorphs, to improve the properties of a parent drug. To find the best form of a drug, various advanced characterization methods should be used. In this review, we have described such analytical methods, dedicated to solid drug forms. Thus, diffraction, spectroscopic, thermal and also pharmaceutical characterization methods are discussed. They all are necessary to study a solid API in its intrinsic complexity from bulk down to the molecular level, gain information on its structure, properties, purity and possible transformations, and make the characterization efficient, comprehensive and complete. Furthermore, these methods can be used to monitor and investigate physical processes, involved in the drug development, in situ and in real time. The main aim of this paper is to gather information on the current advancements in the analytical methods and highlight their pharmaceutical relevance. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of a class of boundary value problems depending on left and right Caputo fractional derivatives

NASA Astrophysics Data System (ADS)

Antunes, Pedro R. S.; Ferreira, Rui A. C.

2017-07-01

In this work we study boundary value problems associated to a nonlinear fractional ordinary differential equation involving left and right Caputo derivatives. We discuss the regularity of the solutions of such problems and, in particular, give precise necessary conditions so that the solutions are C1([0, 1]). Taking into account our analytical results, we address the numerical solution of those problems by the augmented -RBF method. Several examples illustrate the good performance of the numerical method.

Gain Switching for a Detection System to Accommodate a Newly Developed MALDI-Based Quantification Method

NASA Astrophysics Data System (ADS)

Ahn, Sung Hee; Hyeon, Taeghwan; Kim, Myung Soo; Moon, Jeong Hee

2017-09-01

In matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF), matrix-derived ions are routinely deflected away to avoid problems with ion detection. This, however, limits the use of a quantification method that utilizes the analyte-to-matrix ion abundance ratio. In this work, we will show that it is possible to measure this ratio by a minor instrumental modification of a simple form of MALDI-TOF. This involves detector gain switching. [Figure not available: see fulltext.

Task-based image quality evaluation of iterative reconstruction methods for low dose CT using computer simulations

NASA Astrophysics Data System (ADS)

Xu, Jingyan; Fuld, Matthew K.; Fung, George S. K.; Tsui, Benjamin M. W.

2015-04-01

Iterative reconstruction (IR) methods for x-ray CT is a promising approach to improve image quality or reduce radiation dose to patients. The goal of this work was to use task based image quality measures and the channelized Hotelling observer (CHO) to evaluate both analytic and IR methods for clinical x-ray CT applications. We performed realistic computer simulations at five radiation dose levels, from a clinical reference low dose D0 to 25% D0. A fixed size and contrast lesion was inserted at different locations into the liver of the XCAT phantom to simulate a weak signal. The simulated data were reconstructed on a commercial CT scanner (SOMATOM Definition Flash; Siemens, Forchheim, Germany) using the vendor-provided analytic (WFBP) and IR (SAFIRE) methods. The reconstructed images were analyzed by CHOs with both rotationally symmetric (RS) and rotationally oriented (RO) channels, and with different numbers of lesion locations (5, 10, and 20) in a signal known exactly (SKE), background known exactly but variable (BKEV) detection task. The area under the receiver operating characteristic curve (AUC) was used as a summary measure to compare the IR and analytic methods; the AUC was also used as the equal performance criterion to derive the potential dose reduction factor of IR. In general, there was a good agreement in the relative AUC values of different reconstruction methods using CHOs with RS and RO channels, although the CHO with RO channels achieved higher AUCs than RS channels. The improvement of IR over analytic methods depends on the dose level. The reference dose level D0 was based on a clinical low dose protocol, lower than the standard dose due to the use of IR methods. At 75% D0, the performance improvement was statistically significant (p < 0.05). The potential dose reduction factor also depended on the detection task. For the SKE/BKEV task involving 10 lesion locations, a dose reduction of at least 25% from D0 was achieved.

Are Higher Education Institutions Prepared for Learning Analytics?

ERIC Educational Resources Information Center

Ifenthaler, Dirk

2017-01-01

Higher education institutions and involved stakeholders can derive multiple benefits from learning analytics by using different data analytics strategies to produce summative, real-time, and predictive insights and recommendations. However, are institutions and academic as well as administrative staff prepared for learning analytics? A learning…

Analytic study of a rolling sphere on a rough surface

NASA Astrophysics Data System (ADS)

Florea, Olivia A.; Rosca, Ileana C.

2016-11-01

In this paper it is realized an analytic study of the rolling's sphere on a rough horizontal plane under the action of its own gravity. The necessities of integration of the system of dynamical equations of motion lead us to find a reference system where the motion equations should be transformed into simpler expressions and which, in the presence of some significant hypothesis to permit the application of some original methods of analytical integration. In technical applications, the bodies may have a free rolling motion or a motion constrained by geometrical relations in assemblies of parts and machine parts. This study involves a lot of investigations in the field of tribology and of applied dynamics accompanied by experiments. Multiple recordings of several trajectories of the sphere, as well as their treatment of images, also followed by statistical processing experimental data allowed highlighting a very good agreement between the theoretical findings and experimental results.

Shared decision-making – transferring research into practice: the Analytic Hierarchy Process (AHP)

PubMed Central

Dolan, James G.

2008-01-01

Objective To illustrate how the Analytic Hierarchy Process (AHP) can be used to promote shared decision-making and enhance clinician-patient communication. Methods Tutorial review. Results The AHP promotes shared decision making by creating a framework that is used to define the decision, summarize the information available, prioritize information needs, elicit preferences and values, and foster meaningful communication among decision stakeholders. Conclusions The AHP and related multi-criteria methods have the potential for improving the quality of clinical decisions and overcoming current barriers to implementing shared decision making in busy clinical settings. Further research is needed to determine the best way to implement these tools and to determine their effectiveness. Practice Implications Many clinical decisions involve preference-based trade-offs between competing risks and benefits. The AHP is a well-developed method that provides a practical approach for improving patient-provider communication, clinical decision-making, and the quality of patient care in these situations. PMID:18760559

Chemoselective synthesis and analysis of naturally occurring phosphorylated cysteine peptides

PubMed Central

Bertran-Vicente, Jordi; Penkert, Martin; Nieto-Garcia, Olaia; Jeckelmann, Jean-Marc; Schmieder, Peter; Krause, Eberhard; Hackenberger, Christian P. R.

2016-01-01

In contrast to protein O-phosphorylation, studying the function of the less frequent N- and S-phosphorylation events have lagged behind because they have chemical features that prevent their manipulation through standard synthetic and analytical methods. Here we report on the development of a chemoselective synthetic method to phosphorylate Cys side-chains in unprotected peptides. This approach makes use of a reaction between nucleophilic phosphites and electrophilic disulfides accessible by standard methods. We achieve the stereochemically defined phosphorylation of a Cys residue and verify the modification using electron-transfer higher-energy dissociation (EThcD) mass spectrometry. To demonstrate the use of the approach in resolving biological questions, we identify an endogenous Cys phosphorylation site in IICBGlc, which is known to be involved in the carbohydrate uptake from the bacterial phosphotransferase system (PTS). This new chemical and analytical approach finally allows further investigating the functions and significance of Cys phosphorylation in a wide range of crucial cellular processes. PMID:27586301

Validation of an analytical method for the quantitative determination of selenium in bacterial biomass by ultraviolet-visible spectrophotometry.

PubMed

Mörschbächer, Ana Paula; Dullius, Anja; Dullius, Carlos Henrique; Bandt, Cassiano Ricardo; Kuhn, Daniel; Brietzke, Débora Tairini; Malmann Kuffel, Fernando José; Etgeton, Henrique Pretto; Altmayer, Taciélen; Gonçalves, Tamara Engelmann; Oreste, Eliézer Quadro; Ribeiro, Anderson Schwingel; de Souza, Claucia Fernanda Volken; Hoehne, Lucélia

2018-07-30

The present paper describes the validation of a spectrophotometry method involving molecular absorption in the visible ultraviolet-visible (UV-Vis) region for selenium (Se) determination in the bacterial biomass produced by lactic acid bacteria (LAB). The method was found to be suitable for the target application and presented a linearity range from 0.025 to 0.250 mg/L Se. The angular and linear coefficients of the linear equation were 1.0678 and 0.0197 mg/L Se, respectively, and the linear correlation coefficient (R 2 ) was 0.9991. Analyte recovery exceeded 96% with a relative standard deviation (RSD) below 3%. The Se contents in LAB ranged from 0.01 to 20 mg/g. The Se contents in the bacterial biomass determined by UV-Vis were not significantly different (p > 0.05) those determined by graphite furnace atomic absorption spectrometry. Thus, Se can be quantified in LAB biomass using this relatively simpler technique. Copyright © 2018 Elsevier Ltd. All rights reserved.

Just the two of us: misalignment of theory and methods in examining dyadic phenomena.

PubMed

Krasikova, Dina V; LeBreton, James M

2012-07-01

Many organizational phenomena such as leader-member exchange, mentoring, coaching, interpersonal conflict and cooperation, negotiation, performance appraisal, and the employment interview involve inherently dyadic relationships and interactions. Even when theories explicitly acknowledge the dyadic nature of such phenomena, it is not uncommon to observe a disconnection or misalignment between the level of theory and method. Our purpose in the current paper is to discuss how organizational scholars might better align these components of their research endeavors. We discuss how recent developments involving the actor-partner interdependence model (APIM) and reciprocal one-with-many (OWM) models are applicable to studying dyadic phenomena in organizations. The emphasis is on preanalytic considerations associated with collecting and organizing reciprocal dyadic data, types of research questions that APIM and reciprocal OWM models can help answer, and specific analytic techniques involved in testing dyadic hypotheses. (PsycINFO Database Record (c) 2012 APA, all rights reserved).

Multiclass screening method based on solvent extraction and liquid chromatography-tandem mass spectrometry for the determination of antimicrobials and mycotoxins in egg.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; Piovesana, Susy; Samperi, Roberto; Laganà, Aldo

2012-12-14

A QuEChERS (Quick Easy Cheap Effective Rugged Safe)-like extraction method was developed for the simultaneous analysis of veterinary drugs and mycotoxins in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray (ESI) source. Various classes of antimicrobials (tetracyclines, ionophores, coccidiostats, penicillins, cephalosporins, fluoroquinolones, sulfonamides) and mycotoxins (enniatins, beauvericin, ochratoxins, aflatoxins) were considered for the development of this method. Particular attention was devoted to extraction optimization: different solvents (acetone, acetonitrile and methanol), different pH values and different sample to extracting volume ratios were tested and evaluated in terms of recovery, relative standard deviation (RSD) and ESI signal suppression due to matrix effect. Chromatographic and mass spectrometric conditions were optimized to obtain the best instrumental performances for most of the analytes. Quantitative analysis was performed by means of matrix-matched calibration, in a range that varied depending on the analyte and its established maximum limit, when there was one. Recoveries at 100 μg kg(-1) spiking level were >62% (3

Simultaneous determination of sixteen metabolites related to neural tube defects in maternal serum by liquid chromatography coupling with electrospray tandem mass spectrometry.

PubMed

Liang, Xiao-Ping; Liang, Qiong-Lin; Xia, Jian-Fei; Wang, Yong; Hu, Ping; Wang, Yi-Ming; Zheng, Xiao-Ying; Zhang, Ting; Luo, Guo-An

2009-06-15

Disturbances in maternal folate, homocysteine, and glutathione metabolism have been reported to be associated with neural tube defects (NTDs). However, the role played by specific components in the metabolic pathways leading to NTDs remains unclear. Thus an analytical method for simultaneous measurement of sixteen compounds involved in such three metabolic pathways by high performance liquid chromatography-tandem mass spectrometry was developed. The use of hydrophilic chromatography column improved the separation of polar analytes and the detection mode of multiple-reaction monitoring (MRM) enhanced the specificity and sensitivity so as to achieve simultaneous determination of three class of metabolites which have much variance in polarity and contents. The influence of parameters such as temperature, pH, flow rate on the performance of the analytes were studied to get an optimal condition. The method was validated for its linearity, accuracy, and precision, and also used for the analysis of serum samples of NTDs-affected pregnancies and normal women. The result showed that the present method is sensitive and reliable for simultaneous determination of as many as sixteen interesting metabolites which may provide a new means to study the underlying mechanism of NTDs as well as to discover new potential biomarkers.

An analytical framework to assist decision makers in the use of forest ecosystem model predictions

USGS Publications Warehouse

Larocque, Guy R.; Bhatti, Jagtar S.; Ascough, J.C.; Liu, J.; Luckai, N.; Mailly, D.; Archambault, L.; Gordon, Andrew M.

2011-01-01

The predictions from most forest ecosystem models originate from deterministic simulations. However, few evaluation exercises for model outputs are performed by either model developers or users. This issue has important consequences for decision makers using these models to develop natural resource management policies, as they cannot evaluate the extent to which predictions stemming from the simulation of alternative management scenarios may result in significant environmental or economic differences. Various numerical methods, such as sensitivity/uncertainty analyses, or bootstrap methods, may be used to evaluate models and the errors associated with their outputs. However, the application of each of these methods carries unique challenges which decision makers do not necessarily understand; guidance is required when interpreting the output generated from each model. This paper proposes a decision flow chart in the form of an analytical framework to help decision makers apply, in an orderly fashion, different steps involved in examining the model outputs. The analytical framework is discussed with regard to the definition of problems and objectives and includes the following topics: model selection, identification of alternatives, modelling tasks and selecting alternatives for developing policy or implementing management scenarios. Its application is illustrated using an on-going exercise in developing silvicultural guidelines for a forest management enterprise in Ontario, Canada.

GC-MS analyses of the volatiles of Houttuynia cordata Thunb.

PubMed

Yang, Zhan-Nan; Luo, Shi-Qiong; Ma, Jing; Wu, Dan; Hong, Liang; Yu, Zheng-Wen

2016-09-01

GC-MS is the basis of analysis of plant volatiles. Several protocols employed for the assay have resulted in inconsistent results in the literature. We developed a GC-MS method, which were applied to analyze 25 volatiles (α-pinene, camphene, β-pinene, 2-methyl-2-pentenal, myrcene, (+)-limonene, eucalyptol, trans-2-hexenal, γ-terpinene, cis-3-hexeneyl-acetate, 1-hexanol, α-pinene oxide, cis-3-hexen-1-ol, trans-2-hexen-1-ol, decanal, linalool, acetyl-borneol, β-caryophyllene, 2-undecanone, 4-terpineol, borneol, decanol, eugenol, isophytol and phytol) of Houttuynia cordata Thunb. Linear behaviors for all analytes were observed with a linear regression relationship (r2>0.9991) at the concentrations tested. Recoveries of the 25 analytes were 98.56-103.77% with RSDs <3.0%. Solution extraction (SE), which involved addition of an internal standard, could avoid errors for factors in sample preparation by steam distillation (SD) and solidphase micro extraction (SPME). Less sample material (≍0.05g fresh leaves of H. cordata) could be used to determine the contents of 25 analytes by our proposed method and, after collection, did not affect the normal physiological activity or growth of H. cordata. This method can be used to monitor the metabolic accumulation of H. cordata volatiles.

Liquid chromatography tandem mass spectrometry for the simultaneous determination of mequindox and its metabolites in porcine tissues.

PubMed

Zeng, Dongping; Shen, Xiangguang; He, Limin; Ding, Huanzhong; Tang, Youzhi; Sun, Yongxue; Fang, Binghu; Zeng, Zhenling

2012-06-01

A rapid liquid chromatography tandem mass spectrometric method was developed for the simultaneous determination of mequindox and its five metabolites (2-isoethanol mequindox, 2-isoethanol 1-desoxymequindox, 1-desoxymequindox, 1,4-bisdesoxymequindox, and 2-isoethanol bisdesoxymequindox) in porcine muscle, liver, and kidney, fulfilling confirmation criteria with two transitions for each compound with acceptable relative ion intensities. The method involved acid hydrolysis, purification by solid-phase extraction, and subsequent analysis with liquid chromatography tandem mass spectrometry using electrospray ionization operated in positive polarity with a total run time of 15 min. The decision limit values of five analytes in porcine tissues ranged from 0.6 to 2.9 μg/kg, and the detection capability values ranged from 1.2 to 5.7 μg/kg. The results of the inter-day study, which was performed by fortifying porcine muscle (2, 4, and 8 μg/kg), liver, and kidney (10, 20, and 40 μg/kg) samples on three separate days, showed that the accuracy of the method for the various analytes ranged between 75.3 and 107.2% with relative standard deviation less than 12% for each analyte. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development, validation and application of a sensitive analytical method for residue determination and dissipation of imidacloprid in sugarcane under tropical field condition.

PubMed

Ramasubramanian, T; Paramasivam, M; Nirmala, R

2016-06-01

A simple and sensitive analytical method has been developed and validated for the determination of trace amounts of imidacloprid in/on sugarcane sett, stalk and leaf. The method optimized in the present study requires less volume of organic solvent and time. Hence, this method is suitable for high-throughput analyses involving large number of samples. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.003 and 0.01 mg/kg, respectively. The recovery and relative standard deviation were more than 93 % and less than 4 %, respectively. Thus, it is obvious that the analytical method standardized in this study is more precise and accurate enough to determine the residues of imidacloprid in sugarcane sett, stalk and leaf. The dissipation and translocation of imidacloprid residues from treated cane setts to leaf and stalk were studied by adopting this method. In sugarcane setts, the residues of imidacloprid persisted up to 120 days with half-life of 15.4 days at its recommended dose (70 g a.i./ha). The residues of imidacloprid were found to be translocated from setts to stalk and leaf. The imidacloprid residues were detected up to 105 days in both leaf and stalk. Dipping of sugarcane setts in imidacloprid at its recommended dose may result in better protection of cane setts and established crop because of higher initial deposit (>100 mg/kg) and longer persistence (>120 days).

Single-cell MALDI-MS as an analytical tool for studying intrapopulation metabolic heterogeneity of unicellular organisms.

PubMed

Amantonico, Andrea; Urban, Pawel L; Fagerer, Stephan R; Balabin, Roman M; Zenobi, Renato

2010-09-01

Heterogeneity is a characteristic feature of all populations of living organisms. Here we make an attempt to validate a single-cell mass spectrometric method for detection of changes in metabolite levels occurring in populations of unicellular organisms. Selected metabolites involved in central metabolism (ADP, ATP, GTP, and UDP-Glucose) could readily be detected in single cells of Closterium acerosum by means of negative-mode matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS). The analytical capabilities of this approach were characterized using standard compounds. The method was then used to study populations of individual cells with different levels of the chosen metabolites. With principal component analysis and support vector machine algorithms, it was possible to achieve a clear separation of individual C. acerosum cells in different metabolic states. This study demonstrates the suitability of mass spectrometric analysis of metabolites in single cells to measure cell-population heterogeneity.

Stakeholder prioritization of zoonoses in Japan with analytic hierarchy process method.

PubMed

Kadohira, M; Hill, G; Yoshizaki, R; Ota, S; Yoshikawa, Y

2015-05-01

There exists an urgent need to develop iterative risk assessment strategies of zoonotic diseases. The aim of this study is to develop a method of prioritizing 98 zoonoses derived from animal pathogens in Japan and to involve four major groups of stakeholders: researchers, physicians, public health officials, and citizens. We used a combination of risk profiling and analytic hierarchy process (AHP). Profiling risk was accomplished with semi-quantitative analysis of existing public health data. AHP data collection was performed by administering questionnaires to the four stakeholder groups. Results showed that researchers and public health officials focused on case fatality as the chief important factor, while physicians and citizens placed more weight on diagnosis and prevention, respectively. Most of the six top-ranked diseases were similar among all stakeholders. Transmissible spongiform encephalopathy, severe acute respiratory syndrome, and Ebola fever were ranked first, second, and third, respectively.

Green's functions in equilibrium and nonequilibrium from real-time bold-line Monte Carlo

NASA Astrophysics Data System (ADS)

Cohen, Guy; Gull, Emanuel; Reichman, David R.; Millis, Andrew J.

2014-03-01

Green's functions for the Anderson impurity model are obtained within a numerically exact formalism. We investigate the limits of analytical continuation for equilibrium systems, and show that with real time methods even sharp high-energy features can be reliably resolved. Continuing to an Anderson impurity in a junction, we evaluate two-time correlation functions, spectral properties, and transport properties, showing how the correspondence between the spectral function and the differential conductance breaks down when nonequilibrium effects are taken into account. Finally, a long-standing dispute regarding this model has involved the voltage splitting of the Kondo peak, an effect which was predicted over a decade ago by approximate analytical methods but never successfully confirmed by numerics. We settle the issue by demonstrating in an unbiased manner that this splitting indeed occurs. Yad Hanadiv-Rothschild Foundation, TG-DMR120085, TG-DMR130036, NSF CHE-1213247, NSF DMR 1006282, DOE ER 46932.

A new approach to exact optical soliton solutions for the nonlinear Schrödinger equation

NASA Astrophysics Data System (ADS)

Morales-Delgado, V. F.; Gómez-Aguilar, J. F.; Baleanu, Dumitru

2018-05-01

By using the modified homotopy analysis transform method, we construct the analytical solutions of the space-time generalized nonlinear Schrödinger equation involving a new fractional conformable derivative in the Liouville-Caputo sense and the fractional-order derivative with the Mittag-Leffler law. Employing theoretical parameters, we present some numerical simulations and compare the solutions obtained.

Using predictive analytics and big data to optimize pharmaceutical outcomes.

PubMed

Hernandez, Inmaculada; Zhang, Yuting

2017-09-15

The steps involved, the resources needed, and the challenges associated with applying predictive analytics in healthcare are described, with a review of successful applications of predictive analytics in implementing population health management interventions that target medication-related patient outcomes. In healthcare, the term big data typically refers to large quantities of electronic health record, administrative claims, and clinical trial data as well as data collected from smartphone applications, wearable devices, social media, and personal genomics services; predictive analytics refers to innovative methods of analysis developed to overcome challenges associated with big data, including a variety of statistical techniques ranging from predictive modeling to machine learning to data mining. Predictive analytics using big data have been applied successfully in several areas of medication management, such as in the identification of complex patients or those at highest risk for medication noncompliance or adverse effects. Because predictive analytics can be used in predicting different outcomes, they can provide pharmacists with a better understanding of the risks for specific medication-related problems that each patient faces. This information will enable pharmacists to deliver interventions tailored to patients' needs. In order to take full advantage of these benefits, however, clinicians will have to understand the basics of big data and predictive analytics. Predictive analytics that leverage big data will become an indispensable tool for clinicians in mapping interventions and improving patient outcomes. Copyright © 2017 by the American Society of Health-System Pharmacists, Inc. All rights reserved.

Analytical study of temperature distribution in a rectangular porous fin considering both insulated and convective tip

NASA Astrophysics Data System (ADS)

Deshamukhya, Tuhin; Bhanja, Dipankar; Nath, Sujit; Maji, Ambarish; Choubey, Gautam

2017-07-01

The following study is concerned with determination of temperature distribution of porous fins under convective and insulated tip conditions. The authors have made an effort to study the effect of various important parameters involved in the transfer of heat through porous fins as well as the temperature distribution along the fin length subjected to both convective as well as insulated ends. The non-linear equation obtained has been solved by Adomian Decomposition method and validated with a numerical scheme called Finite Difference method by using a central difference scheme and Gauss Siedel Iterative method.

In Vitro Electrochemistry of Biological Systems

PubMed Central

Adams, Kelly L.; Puchades, Maja; Ewing, Andrew G.

2009-01-01

This article reviews recent work involving electrochemical methods for in vitro analysis of biomolecules, with an emphasis on detection and manipulation at and of single cells and cultures of cells. The techniques discussed include constant potential amperometry, chronoamperometry, cellular electroporation, scanning electrochemical microscopy, and microfluidic platforms integrated with electrochemical detection. The principles of these methods are briefly described, followed in most cases with a short description of an analytical or biological application and its significance. The use of electrochemical methods to examine specific mechanistic issues in exocytosis is highlighted, as a great deal of recent work has been devoted to this application. PMID:20151038

Optimization of magnet end-winding geometry

NASA Astrophysics Data System (ADS)

Reusch, Michael F.; Weissenburger, Donald W.; Nearing, James C.

1994-03-01

A simple, almost entirely analytic, method for the optimization of stress-reduced magnet-end winding paths for ribbon-like superconducting cable is presented. This technique is based on characterization of these paths as developable surfaces, i.e., surfaces whose intrinsic geometry is flat. The method is applicable to winding mandrels of arbitrary geometry. Computational searches for optimal winding paths are easily implemented via the technique. Its application to the end configuration of cylindrical Superconducting Super Collider (SSC)-type magnets is discussed. The method may be useful for other engineering problems involving the placement of thin sheets of material.

High Throughput Determination of VX in Drinking Water by ...

EPA Pesticide Factsheets

Methods Report This document provides the standard operating procedure for determination of the chemical warfare agent VX (O-Ethyl S-2-Diisopropylamino-Ethyl Methylphosphonothioate) in drinking water by isotope dilution liquid chromatography tandem mass spectrometer (LC/MS/MS). This method was adapted from one that was initially developed by the Centers for Disease Control and Prevention, in the National Center for Environmental Health for the determination and quantitation of VX in aqueous matrices. This method is designed to support site-specific cleanup goals of environmental remediation activities following a homeland security incident involving this analyte.

Adulterants in Urine Drug Testing.

PubMed

Fu, S

Urine drug testing plays an important role in monitoring licit and illicit drug use for both medico-legal and clinical purposes. One of the major challenges of urine drug testing is adulteration, a practice involving manipulation of a urine specimen with chemical adulterants to produce a false negative test result. This problem is compounded by the number of easily obtained chemicals that can effectively adulterate a urine specimen. Common adulterants include some household chemicals such as hypochlorite bleach, laundry detergent, table salt, and toilet bowl cleaner and many commercial products such as UrinAid (glutaraldehyde), Stealth® (containing peroxidase and peroxide), Urine Luck (pyridinium chlorochromate, PCC), and Klear® (potassium nitrite) available through the Internet. These adulterants can invalidate a screening test result, a confirmatory test result, or both. To counteract urine adulteration, drug testing laboratories have developed a number of analytical methods to detect adulterants in a urine specimen. While these methods are useful in detecting urine adulteration when such activities are suspected, they do not reveal what types of drugs are being concealed. This is particularly the case when oxidizing urine adulterants are involved as these oxidants are capable of destroying drugs and their metabolites in urine, rendering the drug analytes undetectable by any testing technology. One promising approach to address this current limitation has been the use of unique oxidation products formed from reaction of drug analytes with oxidizing adulterants as markers for monitoring drug misuse and urine adulteration. This novel approach will ultimately improve the effectiveness of the current urine drug testing programs. © 2016 Elsevier Inc. All rights reserved.

Confocal Raman imaging and chemometrics applied to solve forensic document examination involving crossed lines and obliteration cases by a depth profiling study.

PubMed

Borba, Flávia de Souza Lins; Jawhari, Tariq; Saldanha Honorato, Ricardo; de Juan, Anna

2017-03-27

This article describes a non-destructive analytical method developed to solve forensic document examination problems involving crossed lines and obliteration. Different strategies combining confocal Raman imaging and multivariate curve resolution-alternating least squares (MCR-ALS) are presented. Multilayer images were acquired at subsequent depth layers into the samples. It is the first time that MCR-ALS is applied to multilayer images for forensic purposes. In this context, this method provides a single set of pure spectral ink signatures and related distribution maps for all layers examined from the sole information in the raw measurement. Four cases were investigated, namely, two concerning crossed lines with different degrees of ink similarity and two related to obliteration, where previous or no knowledge about the identity of the obliterated ink was available. In the crossing line scenario, MCR-ALS analysis revealed the ink nature and the chronological order in which strokes were drawn. For obliteration cases, results making active use of information about the identity of the obliterated ink in the chemometric analysis were of similar quality as those where the identity of the obliterated ink was unknown. In all obliteration scenarios, the identity of inks and the obliterated text were satisfactorily recovered. The analytical methodology proposed is of general use for analytical forensic document examination problems, and considers different degrees of complexity and prior available information. Besides, the strategies of data analysis proposed can be applicable to any other kind of problem in which multilayer Raman images from multicomponent systems have to be interpreted.

Determination of benzo[a]pyrene in edible oils using phase-transfer-catalyst-assisted saponification and supramolecular solvent microextraction coupled to HPLC with fluorescence detection.

PubMed

Wang, Jin; Liu, Laping; Shi, Ludi; Yi, Tingquan; Wen, Yuxia; Wang, Juanli; Liu, Shuhui

2017-01-01

For the analysis of edible oils, saponification is well known as a useful method for eliminating oil matrices. The conventional approach is conducted with alcoholic alkali; it consumes a large volume of organic solvents and impedes the retrieval of analytes by microextraction. In this study, a low-organic-solvent-consuming method has been developed for the analysis of benzo[a]pyrene in edible oils by high-performance liquid chromatography with fluorescence detection. Sample treatment involves aqueous alkaline saponification, assisted by a phase-transfer catalyst, and selective in situ extraction of the analyte with a supramolecular solvent. Comparison of the chromatograms of the oil extracts obtained by different microextraction methods showed that the supramolecular solvent has a better clean-up effect for the unsaponifiable matter from oil matrices. The method offered excellent linearity over a range of 0.03- 5.0 ng mL -1 (r > 0.999). Recovery rates varied from 94 to 102% (RSDs <5.0%). The detection limit and quantification limit were 0.06 and 0.19 μg kg -1 , respectively. The proposed method was applied for the analysis of 52 edible oils collected online in China; the analyte contents of 23 tested oil samples exceeded the maximum limit of 2 μg kg -1 for benzo[a]pyrene set by the Commission Regulation of the European Union. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A sensitive LC-MS/MS method for simultaneous determination of R-bambuterol and its active metabolite R-terbutaline in human plasma and urine with application to a clinical pharmacokinetic study.

PubMed

Zhou, Ting; Zhao, Ting; Cheng, Qing; Liu, Shan; Xu, Ling; Tan, Wen

2014-07-01

A sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of R-bambuterol and its active metabolite R-terbutaline in human plasma and urine was established. The inhibition for the biotransformation of R-bambuterol in plasma was fully investigated. Plasma samples were prepared on ice and neostigmine metilsulfate added as a cholinesterase inhibitor immediately after sample collection. All samples were extracted with ethyl acetate and separated on a C₁₈ column under gradient elution with a mobile phase consisting of methanol and water containing 5 mm ammonium acetate at a flow rate of 0.6 mL/min. The analytes were detected by an API 4000 tandem mass spectrometer with positive electrospray ionization in multiple reaction monitoring mode. The established method was highly sensitive with the lower limit of quantification (LLOQ) of 10.00 pg/mL for each analyte in plasma. In urine samples, the LLOQs were 20.00 and 500.0 pg/mL for R-bambuterol and R-terbutaline, respectively. The intra- and inter-day precisions were <12.7 and <8.6% for plasma and urine, respectively. The analytical runtime within 6.0 min per sample made this method suitable for high-throughput determination. The validated method has been successfully applied to the human pharmacokinetic study of R-bambuterol involving 10 healthy volunteers. Copyright © 2013 John Wiley & Sons, Ltd.

Trends of non-destructive analytical methods for identification of biodiesel feedstock in diesel-biodiesel blend according to European Commission Directive 2012/0288/EC and detecting diesel-biodiesel blend adulteration: A brief review.

PubMed

Mazivila, Sarmento Júnior

2018-04-01

Discrimination of biodiesel feedstock present in diesel-biodiesel blend is challenging due to the great similarity in the spectral profile as well as digital image profile of each type of feedstock employed in biodiesel production. Once the marketed diesel-biodiesel blend is subsidized, in which motivates adulteration in biofuel blend by cheaper supplies with high solubility to obtain profits associated with the subsidies involved in biodiesel production. Non-destructive analytical methods based on qualitative and quantitative analysis for detecting marketed diesel-biodiesel blend adulteration are reviewed. Therefore, at the end is discussed the advantage of the qualitative analysis over quantitative analysis, when the systems require immediate decisions such as to know if the marketed diesel-biodiesel blend is unadulterated or adulterated in order to aid the analyst in selecting the most appropriate green analytical procedure for detecting diesel-biodiesel blend adulteration proceeding in fast way. This critical review provides a brief review on the non-destructive analytical methods reported in scientific literature based on different first-order multivariate calibration models coupled with spectroscopy data and digital image data to identify the type of biodiesel feedstock present in diesel-biodiesel blend in order to meets the strategies adopted by European Commission Directive 2012/0288/EC as well as to monitoring diesel-biodiesel adulteration. According to that Directive, from 2020 biodiesel produced from first-generation feedstock, that is, oils employed in human food such as sunflower, soybean, rapeseed, palm oil, among other oils should not be subsidized. Therefore, those non-destructive analytical methods here reviewed are helpful for discrimination of biodiesel feedstock present in diesel-biodiesel blend according to European Commission Directive 2012/0288/EC as well as for detecting diesel-biodiesel blend adulteration. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical method development for the determination of emerging contaminants in water using supercritical-fluid chromatography coupled with diode-array detection.

PubMed

Del Carmen Salvatierra-Stamp, Vilma; Ceballos-Magaña, Silvia G; Gonzalez, Jorge; Ibarra-Galván, Valentin; Muñiz-Valencia, Roberto

2015-05-01

An analytical method using supercritical-fluid chromatography coupled with diode-array detection for the determination of seven emerging contaminants-two pharmaceuticals (carbamazepine and glyburide), three endocrine disruptors (17α-ethinyl estradiol, bisphenol A, and 17β-estradiol), one bactericide (triclosan), and one pesticide (diuron)-was developed and validated. These contaminants were chosen because of their frequency of use and their toxic effects on both humans and the environment. The optimized chromatographic separation on a Viridis BEH 2-EP column achieved baseline resolution for all compounds in less than 10 min. This separation was applied to environmental water samples after sample preparation. The optimized sample treatment involved a preconcentration step by means of solid-phase extraction using C18-OH cartridges. The proposed method was validated, finding recoveries higher than 94 % and limits of detection and limits of quantification in the range of 0.10-1.59 μg L(-1) and 0.31-4.83 μg L(-1), respectively. Method validation established the proposed method to be selective, linear, accurate, and precise. Finally, the method was successfully applied to environmental water samples.

Testing and Validation of the Dynamic Inertia Measurement Method

NASA Technical Reports Server (NTRS)

Chin, Alexander W.; Herrera, Claudia Y.; Spivey, Natalie D.; Fladung, William A.; Cloutier, David

2015-01-01

The Dynamic Inertia Measurement (DIM) method uses a ground vibration test setup to determine the mass properties of an object using information from frequency response functions. Most conventional mass properties testing involves using spin tables or pendulum-based swing tests, which for large aerospace vehicles becomes increasingly difficult and time-consuming, and therefore expensive, to perform. The DIM method has been validated on small test articles but has not been successfully proven on large aerospace vehicles. In response, the National Aeronautics and Space Administration Armstrong Flight Research Center (Edwards, California) conducted mass properties testing on an "iron bird" test article that is comparable in mass and scale to a fighter-type aircraft. The simple two-I-beam design of the "iron bird" was selected to ensure accurate analytical mass properties. Traditional swing testing was also performed to compare the level of effort, amount of resources, and quality of data with the DIM method. The DIM test showed favorable results for the center of gravity and moments of inertia; however, the products of inertia showed disagreement with analytical predictions.

Experimental and theoretical study of an integrated silicon Mach-Zehnder interferometer for chemical sensing applications

NASA Astrophysics Data System (ADS)

Hor, Yew Fong

2002-08-01

This thesis involves the design, fabrication and characterization of an integrated optical waveguide sensor. Prior to fabrication, design parameters of the waveguide need to be determined and optimized. The waveguide parameters such as waveguide dimension and the refractive index of the core and cladding are obtained from the single-mode cutoff frequency calculated using either analytical or numerical methods. In this thesis, details of analytical calculations to determine the cutoff frequency in terms of the waveguide parameters will be presented. The method discussed here is Marcatili's approximation. The purpose is to solve the scalar wave equation derived from Maxwell's equations because it describes the mode properties inside the waveguides. The Finite Element Method is used to simulate the electric and magnetic fields inside the waveguides and to determine the propagation characteristics in optical waveguides. This method is suited for problems involving complicated geometries and variable index of refraction. Fabrication of the Integrated Mach-Zehnder Interferometer sensor involves several important standard processes such as Chemical Vapor Deposition (CVD) for thin film fabrication, photolithography for mask transfer, and etching for ridge waveguide formation. The detailed fabrication procedures of the tested Mach-Zehnder Interferometer sensors are discussed. After completion of the sensor fabrication processes, the characterizations were carried out for the thin film of SiO2 and PSG, the waveguides and the Y-junction separately. The waveguides were analyzed to make sure that the sensors are working as expected. The experimental testing on the separated waveguide portions of the first batch Integrated Mach-Zehnder Interferometer (MZI) sensors are described. These testing procedures were also performed for the subsequent fabricated batches of the integrated MZI sensors until optimum performance is achieved. A new concept has been proposed for chemical sensing applications. The novelty of the approach is mainly based on utilizing the multi-wavelength or broadband source instead of single wavelength input to the integrated MZI. The shifting of output spectra resulting from the interference has shown the ability of the MZI to analyze the different concentrations of a chemical analyte. The sensitivity of the sensor is also determined from the plot of intensity versus concentration, which is around 0.013 (%ml)-1 and 0.007 (%ml)-l for the white light source and the 1.5 mum broadband source, respectively, while the lowest detectable concentration of ethanol for the sensor detection is around 8% using a intensity variation method and 0.6% using a peak wavelength variation method.

New trends in the analytical determination of emerging contaminants and their transformation products in environmental waters.

PubMed

Agüera, Ana; Martínez Bueno, María Jesús; Fernández-Alba, Amadeo R

2013-06-01

Since the so-called emerging contaminants were established as a new group of pollutants of environmental concern, a great effort has been devoted to the knowledge of their distribution, fate and effects in the environment. After more than 20 years of work, a significant improvement in knowledge about these contaminants has been achieved, but there is still a large gap of information on the growing number of new potential contaminants that are appearing and especially of their unpredictable transformation products. Although the environmental problem arising from emerging contaminants must be addressed from an interdisciplinary point of view, it is obvious that analytical chemistry plays an important role as the first step of the study, as it allows establishing the presence of chemicals in the environment, estimate their concentration levels, identify sources and determine their degradation pathways. These tasks involve serious difficulties requiring different analytical solutions adjusted to purpose. Thus, the complexity of the matrices requires highly selective analytical methods; the large number and variety of compounds potentially present in the samples demands the application of wide scope methods; the low concentrations at which these contaminants are present in the samples require a high detection sensitivity, and high demands on the confirmation and high structural information are needed for the characterisation of unknowns. New developments on analytical instrumentation have been applied to solve these difficulties. Furthermore and not less important has been the development of new specific software packages intended for data acquisition and, in particular, for post-run analysis. Thus, the use of sophisticated software tools has allowed successful screening analysis, determining several hundreds of analytes, and assisted in the structural elucidation of unknown compounds in a timely manner.

An automated ranking platform for machine learning regression models for meat spoilage prediction using multi-spectral imaging and metabolic profiling.

PubMed

Estelles-Lopez, Lucia; Ropodi, Athina; Pavlidis, Dimitris; Fotopoulou, Jenny; Gkousari, Christina; Peyrodie, Audrey; Panagou, Efstathios; Nychas, George-John; Mohareb, Fady

2017-09-01

Over the past decade, analytical approaches based on vibrational spectroscopy, hyperspectral/multispectral imagining and biomimetic sensors started gaining popularity as rapid and efficient methods for assessing food quality, safety and authentication; as a sensible alternative to the expensive and time-consuming conventional microbiological techniques. Due to the multi-dimensional nature of the data generated from such analyses, the output needs to be coupled with a suitable statistical approach or machine-learning algorithms before the results can be interpreted. Choosing the optimum pattern recognition or machine learning approach for a given analytical platform is often challenging and involves a comparative analysis between various algorithms in order to achieve the best possible prediction accuracy. In this work, "MeatReg", a web-based application is presented, able to automate the procedure of identifying the best machine learning method for comparing data from several analytical techniques, to predict the counts of microorganisms responsible of meat spoilage regardless of the packaging system applied. In particularly up to 7 regression methods were applied and these are ordinary least squares regression, stepwise linear regression, partial least square regression, principal component regression, support vector regression, random forest and k-nearest neighbours. MeatReg" was tested with minced beef samples stored under aerobic and modified atmosphere packaging and analysed with electronic nose, HPLC, FT-IR, GC-MS and Multispectral imaging instrument. Population of total viable count, lactic acid bacteria, pseudomonads, Enterobacteriaceae and B. thermosphacta, were predicted. As a result, recommendations of which analytical platforms are suitable to predict each type of bacteria and which machine learning methods to use in each case were obtained. The developed system is accessible via the link: www.sorfml.com. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

IBM Watson Analytics: Automating Visualization, Descriptive, and Predictive Statistics

PubMed Central

2016-01-01

Background We live in an era of explosive data generation that will continue to grow and involve all industries. One of the results of this explosion is the need for newer and more efficient data analytics procedures. Traditionally, data analytics required a substantial background in statistics and computer science. In 2015, International Business Machines Corporation (IBM) released the IBM Watson Analytics (IBMWA) software that delivered advanced statistical procedures based on the Statistical Package for the Social Sciences (SPSS). The latest entry of Watson Analytics into the field of analytical software products provides users with enhanced functions that are not available in many existing programs. For example, Watson Analytics automatically analyzes datasets, examines data quality, and determines the optimal statistical approach. Users can request exploratory, predictive, and visual analytics. Using natural language processing (NLP), users are able to submit additional questions for analyses in a quick response format. This analytical package is available free to academic institutions (faculty and students) that plan to use the tools for noncommercial purposes. Objective To report the features of IBMWA and discuss how this software subjectively and objectively compares to other data mining programs. Methods The salient features of the IBMWA program were examined and compared with other common analytical platforms, using validated health datasets. Results Using a validated dataset, IBMWA delivered similar predictions compared with several commercial and open source data mining software applications. The visual analytics generated by IBMWA were similar to results from programs such as Microsoft Excel and Tableau Software. In addition, assistance with data preprocessing and data exploration was an inherent component of the IBMWA application. Sensitivity and specificity were not included in the IBMWA predictive analytics results, nor were odds ratios, confidence intervals, or a confusion matrix. Conclusions IBMWA is a new alternative for data analytics software that automates descriptive, predictive, and visual analytics. This program is very user-friendly but requires data preprocessing, statistical conceptual understanding, and domain expertise. PMID:27729304

Recent Advances in Paper-Based Sensors

PubMed Central

Liana, Devi D.; Raguse, Burkhard; Gooding, J. Justin; Chow, Edith

2012-01-01

Paper-based sensors are a new alternative technology for fabricating simple, low-cost, portable and disposable analytical devices for many application areas including clinical diagnosis, food quality control and environmental monitoring. The unique properties of paper which allow passive liquid transport and compatibility with chemicals/biochemicals are the main advantages of using paper as a sensing platform. Depending on the main goal to be achieved in paper-based sensors, the fabrication methods and the analysis techniques can be tuned to fulfill the needs of the end-user. Current paper-based sensors are focused on microfluidic delivery of solution to the detection site whereas more advanced designs involve complex 3-D geometries based on the same microfluidic principles. Although paper-based sensors are very promising, they still suffer from certain limitations such as accuracy and sensitivity. However, it is anticipated that in the future, with advances in fabrication and analytical techniques, that there will be more new and innovative developments in paper-based sensors. These sensors could better meet the current objectives of a viable low-cost and portable device in addition to offering high sensitivity and selectivity, and multiple analyte discrimination. This paper is a review of recent advances in paper-based sensors and covers the following topics: existing fabrication techniques, analytical methods and application areas. Finally, the present challenges and future outlooks are discussed. PMID:23112667

Determination of neonicotinoid insecticides and their metabolites in honey bee and honey by liquid chromatography tandem mass spectrometry.

PubMed

Gbylik-Sikorska, Malgorzata; Sniegocki, Tomasz; Posyniak, Andrzej

2015-05-15

The original analytical method for the simultaneous determination and confirmation of neonicotinoids insecticides (imidacloprid, clothianidin, acetamiprid, thiametoxam, thiacloprid, nitenpyram, dinotefuran) and some of their metabolites (imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, desnitro-imidacloprid hydrochloride, thiacloprid-amid and acetamiprid-N-desmethyl) in honey bee and honey was developed. Preparation of honey bee samples involves the extraction with mixture of acetonitrile and ethyl acetate followed by cleaned up using the Sep-Pak Alumina N Plus Long cartridges. Honey samples were dissolved in 1% mixture of acetonitrile and ethyl acetate with addition of TEA, then extracts were cleaned up with Strata X-CW cartridges. The identity of analytes was confirmed using liquid chromatography tandem mass spectrometry. All compounds were separated on a Luna C18 column with gradient elution. The whole procedure was validated according to the requirements of SANCO 12571/2013. The average recoveries of the analytes ranged from 85.3% to 112.0%, repeatabilities were in the range of 2.8-11.2%, within-laboratory reproducibility was in the range of 3.3-14.6%, the limits of quantitation were in the range of 0.1-0.5μgkg(-1), depending of analyte and matrices. The validated method was successfully applied for the determination of clothianidin, imidacloprid and imidacloprid urea in real incurred honey bee samples and clothianidin in honey. Copyright © 2015 Elsevier B.V. All rights reserved.

Analytical Derivation: An Epistemic Game for Solving Mathematically Based Physics Problems

ERIC Educational Resources Information Center

Bajracharya, Rabindra R.; Thompson, John R.

2016-01-01

Problem solving, which often involves multiple steps, is an integral part of physics learning and teaching. Using the perspective of the epistemic game, we documented a specific game that is commonly pursued by students while solving mathematically based physics problems: the "analytical derivation" game. This game involves deriving an…

HPLC-DAD method development and validation for the quantification of hydroxymethylfurfural in corn chips by means of response surface optimisation.

PubMed

Salvatierra Virgen, Sara; Ceballos-Magaña, Silvia Guillermina; Salvatierra-Stamp, Vilma Del Carmen; Sumaya-Martínez, Maria Teresa; Martínez-Martínez, Francisco Javier; Muñiz-Valencia, Roberto

2017-12-01

In recent years, there has been an increased concern about the presence of toxic compounds derived from the Maillard reaction produced during food cooking at high temperatures. The main toxic compounds derived from this reaction are acrylamide and hydroxymethylfurfural (HMF). The majority of analytical methods require sample treatments using solvents which are highly polluting for the environment. The difficulty of quantifying HMF in complex fried food matrices encourages the development of new analytical methods. This paper provides a rapid, sensitive and environmentally-friendly analytical method for the quantification of HMF in corn chips using HPLC-DAD. Chromatographic separation resulted in a baseline separation for HMF in 3.7 min. Sample treatment for corn chip samples first involved a leaching process using water and afterwards a solid-phase extraction (SPE) using HLB-Oasis polymeric cartridges. Sample treatment optimisation was carried out by means of Box-Behnken fractional factorial design and Response Surface Methodolog y to examine the effects of four variables (sample weight, pH, sonication time and elution volume) on HMF extraction from corn chips. The SPE-HPLC-DAD method was validated. The limits of detection and quantification were 0.82 and 2.20 mg kg -1 , respectively. Method precision was evaluated in terms of repeatability and reproducibility as relative standard deviations (RSDs) using three concentration levels. For repeatability, RSD values were 6.9, 3.6 and 2.0%; and for reproducibility 18.8, 7.9 and 2.9%. For a ruggedness study the Yuden test was applied and the result demonstrated the method as robust. The method was successfully applied to different corn chip samples.

Analysis of Bisphenol A, Alkylphenols, and Alkylphenol Ethoxylates in NIST SRM 2585 and Indoor House Dust by Gas Chromatography-Tandem Mass Spectrometry (GC/MS/MS).

PubMed

Fan, Xinghua; Kubwabo, Cariton; Wu, Fang; Rasmussen, Pat E

2018-06-26

Background: Ingestion of house dust has been demonstrated to be an important exposure pathway to several contaminants in young children. These compounds include bisphenol A (BPA), alkylphenols (APs), and alkylphenol ethoxylates (APEOs). Analysis of these compounds in house dust is challenging because of the complex composition of the sample matrix. Objective: The objective was to develop a simple and sensitive method to measure BPA, APs, and APEOs in indoor house dust. Methods: An integrated method that involved solvent extraction using sonication, sample cleanup by solid-phase extraction, derivatization by 2,2,2-trifluoro- N -methyl- N -(trimethylsilyl)acetamide, and analysis by GC coupled with tandem MS was developed for the simultaneous determination of BPA, APs, and APEOs in NIST Standard Reference Material (SRM) 2585 (Organic contaminants in house dust) and in settled house dust samples. Results: Target analytes included BPA, 4- tert -octylphenol (OP), OP monoethoxylate, OP diethoxylate, 4- n -nonylphenol (4 n NP), 4 n NP monoethoxylate (4 n NP 1 EO), branched nonylphenol (NP), NP monoethoxylate, NP diethoxylate, NP triethoxylate, and NP tetraethoxylate. The method was sensitive, with method detection limits ranging from 0.05 to 5.1 μg/g, and average recoveries between 82 and 115%. All target analytes were detected in SRM 2585 and house dust except 4 n NP and 4 n NP 1 EO. Conclusions: The method is simple and fast, with high sensitivity and good reproducibility. It is applicable to the analysis of target analytes in similar matrixes, such as sediments, soil, and biosolids. Highlights: Values measured in SRM 2585 will be useful for future research in method development and method comparison.

Measuring salivary analytes from free-ranging monkeys

PubMed Central

Higham, James P.; Vitale, Alison; Rivera, Adaris Mas; Ayala, James E.; Maestripieri, Dario

2014-01-01

Studies of large free-ranging mammals have been revolutionized by non-invasive methods for assessing physiology, which usually involve the measurement of fecal or urinary biomarkers. However, such techniques are limited by numerous factors. To expand the range of physiological variables measurable non-invasively from free-ranging primates, we developed techniques for sampling monkey saliva by offering monkeys ropes with oral swabs sewn on the ends. We evaluated different attractants for encouraging individuals to offer samples, and proportions of individuals in different age/sex categories willing to give samples. We tested the saliva samples we obtained in three commercially available assays: cortisol, Salivary Alpha Amylase, and Secretory Immunoglobulin A. We show that habituated free-ranging rhesus macaques will give saliva samples voluntarily without training, with 100% of infants, and over 50% of adults willing to chew on collection devices. Our field methods are robust even for analytes that show poor recovery from cotton, and/or that have concentrations dependent on salivary flow rate. We validated the cortisol and SAA assays for use in rhesus macaques by showing aspects of analytical validation, such as that samples dilute linearly and in parallel to assay standards. We also found that values measured correlated with biologically meaningful characteristics of sampled individuals (age and dominance rank). The SIgA assay tested did not react to samples. Given the wide range of analytes measurable in saliva but not in feces or urine, our methods considerably improve our ability to study physiological aspects of the behavior and ecology of free-ranging primates, and are also potentially adaptable to other mammalian taxa. PMID:20837036

Quantification of Methylphenidate, Dexamphetamine, and Atomoxetine in Human Serum and Oral Fluid by HPLC With Fluorescence Detection.

PubMed

Stegmann, Benedikt; Dörfelt, Anett; Haen, Ekkehard

2016-02-01

For psychostimulants, a marked individual variability in the dose-response relationship and large differences in plasma concentrations after similar doses are known. Therefore, optimizing the efficacy of these drugs is at present the most promising way to exploit their full pharmacological potential. Moreover, it seems important to examine oral fluid as less invasive biological matrix for its benefit in therapeutic drug monitoring for patients with hyperkinetic disorder. A high-performance liquid chromatography method for quantification of methylphenidate (MPH), dexamphetamine (DXA), and atomoxetine in serum and oral fluid has been developed and validated. The analytical procedure involves liquid-liquid extraction, derivatization with 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride as a label and chromatographic separation on a Phenomenex Gemini-NX C18 analytical column using gradient elution with water-acetonitrile. The derivatized analytes were detected at 330 nm (excitation wavelength) and 440 nm (emission wavelength). To examine the oral fluid/serum ratios, oral fluid samples were collected simultaneously to blood samples from patients with hyperkinetic disorder. The method allows quantification of all analytes in serum and oral fluid within 16 minutes under the same or similar conditions. Oral fluid/serum ratios for MPH and DXA were highly variable and showed an accumulation of these drugs in oral fluid. The developed method covers the determination of MPH, DXA, and atomoxetine concentrations in serum and oral fluid after the intake of therapeutic doses. Oral fluid samples are useful for the qualitative detection of MPH and DXA.

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.

Protecting Privacy of Shared Epidemiologic Data without Compromising Analysis Potential

DOE PAGES

Cologne, John; Grant, Eric J.; Nakashima, Eiji; ...

2012-01-01

Objective . Ensuring privacy of research subjects when epidemiologic data are shared with outside collaborators involves masking (modifying) the data, but overmasking can compromise utility (analysis potential). Methods of statistical disclosure control for protecting privacy may be impractical for individual researchers involved in small-scale collaborations. Methods . We investigated a simple approach based on measures of disclosure risk and analytical utility that are straightforward for epidemiologic researchers to derive. The method is illustrated using data from the Japanese Atomic-bomb Survivor population. Results . Masking by modest rounding did not adequately enhance security but rounding to remove several digits of relativemore » accuracy effectively reduced the risk of identification without substantially reducing utility. Grouping or adding random noise led to noticeable bias. Conclusions . When sharing epidemiologic data, it is recommended that masking be performed using rounding. Specific treatment should be determined separately in individual situations after consideration of the disclosure risks and analysis needs.« less

Protecting Privacy of Shared Epidemiologic Data without Compromising Analysis Potential

PubMed Central

Cologne, John; Grant, Eric J.; Nakashima, Eiji; Chen, Yun; Funamoto, Sachiyo; Katayama, Hiroaki

2012-01-01

Objective. Ensuring privacy of research subjects when epidemiologic data are shared with outside collaborators involves masking (modifying) the data, but overmasking can compromise utility (analysis potential). Methods of statistical disclosure control for protecting privacy may be impractical for individual researchers involved in small-scale collaborations. Methods. We investigated a simple approach based on measures of disclosure risk and analytical utility that are straightforward for epidemiologic researchers to derive. The method is illustrated using data from the Japanese Atomic-bomb Survivor population. Results. Masking by modest rounding did not adequately enhance security but rounding to remove several digits of relative accuracy effectively reduced the risk of identification without substantially reducing utility. Grouping or adding random noise led to noticeable bias. Conclusions. When sharing epidemiologic data, it is recommended that masking be performed using rounding. Specific treatment should be determined separately in individual situations after consideration of the disclosure risks and analysis needs. PMID:22505949

Specter: linear deconvolution for targeted analysis of data-independent acquisition mass spectrometry proteomics.

PubMed

Peckner, Ryan; Myers, Samuel A; Jacome, Alvaro Sebastian Vaca; Egertson, Jarrett D; Abelin, Jennifer G; MacCoss, Michael J; Carr, Steven A; Jaffe, Jacob D

2018-05-01

Mass spectrometry with data-independent acquisition (DIA) is a promising method to improve the comprehensiveness and reproducibility of targeted and discovery proteomics, in theory by systematically measuring all peptide precursors in a biological sample. However, the analytical challenges involved in discriminating between peptides with similar sequences in convoluted spectra have limited its applicability in important cases, such as the detection of single-nucleotide polymorphisms (SNPs) and alternative site localizations in phosphoproteomics data. We report Specter (https://github.com/rpeckner-broad/Specter), an open-source software tool that uses linear algebra to deconvolute DIA mixture spectra directly through comparison to a spectral library, thus circumventing the problems associated with typical fragment-correlation-based approaches. We validate the sensitivity of Specter and its performance relative to that of other methods, and show that Specter is able to successfully analyze cases involving highly similar peptides that are typically challenging for DIA analysis methods.

Meta-Analyzing a Complex Correlational Dataset: A Case Study Using Correlations That Measure the Relationship between Parental Involvement and Academic Achievement

ERIC Educational Resources Information Center

Polanin, Joshua R.; Wilson, Sandra Jo

2014-01-01

The purpose of this project is to demonstrate the practical methods developed to utilize a dataset consisting of both multivariate and multilevel effect size data. The context for this project is a large-scale meta-analytic review of the predictors of academic achievement. This project is guided by three primary research questions: (1) How do we…

The Effect of Multispectral Image Fusion Enhancement on Human Efficiency

DTIC Science & Technology

2017-03-20

human visual system by applying a technique commonly used in visual percep- tion research : ideal observer analysis. Using this approach, we establish...applications, analytic tech- niques, and procedural methods used across studies. This paper uses ideal observer analysis to establish a frame- work that allows...augmented similarly to incorpo- rate research involving more complex stimulus content. Additionally, the ideal observer can be adapted for a number of

Identification and Quantification of N-Acyl Homoserine Lactones Involved in Bacterial Communication by Small-Scale Synthesis of Internal Standards and Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry.

PubMed

Leipert, Jan; Treitz, Christian; Leippe, Matthias; Tholey, Andreas

2017-12-01

N-acyl homoserine lactones (AHL) are small signal molecules involved in the quorum sensing of many gram-negative bacteria, and play an important role in biofilm formation and pathogenesis. Present analytical methods for identification and quantification of AHL require time-consuming sample preparation steps and are hampered by the lack of appropriate standards. By aiming at a fast and straightforward method for AHL analytics, we investigated the applicability of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). Suitable MALDI matrices, including crystalline and ionic liquid matrices, were tested and the fragmentation of different AHL in collision-induced dissociation MS/MS was studied, providing information about characteristic marker fragments ions. Employing small-scale synthesis protocols, we established a versatile and cost-efficient procedure for fast generation of isotope-labeled AHL standards, which can be used without extensive purification and yielded accurate standard curves. Quantitative analysis was possible in the low pico-molar range, with lower limits of quantification reaching from 1 to 5 pmol for different AHL. The developed methodology was successfully applied in a quantitative MALDI MS analysis of low-volume culture supernatants of Pseudomonas aeruginosa. Graphical abstract ᅟ.

Identification and Quantification of N-Acyl Homoserine Lactones Involved in Bacterial Communication by Small-Scale Synthesis of Internal Standards and Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry

NASA Astrophysics Data System (ADS)

Leipert, Jan; Treitz, Christian; Leippe, Matthias; Tholey, Andreas

2017-12-01

N-acyl homoserine lactones (AHL) are small signal molecules involved in the quorum sensing of many gram-negative bacteria, and play an important role in biofilm formation and pathogenesis. Present analytical methods for identification and quantification of AHL require time-consuming sample preparation steps and are hampered by the lack of appropriate standards. By aiming at a fast and straightforward method for AHL analytics, we investigated the applicability of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). Suitable MALDI matrices, including crystalline and ionic liquid matrices, were tested and the fragmentation of different AHL in collision-induced dissociation MS/MS was studied, providing information about characteristic marker fragments ions. Employing small-scale synthesis protocols, we established a versatile and cost-efficient procedure for fast generation of isotope-labeled AHL standards, which can be used without extensive purification and yielded accurate standard curves. Quantitative analysis was possible in the low pico-molar range, with lower limits of quantification reaching from 1 to 5 pmol for different AHL. The developed methodology was successfully applied in a quantitative MALDI MS analysis of low-volume culture supernatants of Pseudomonas aeruginosa. [Figure not available: see fulltext.

Using design of experiments to optimize derivatization with methyl chloroformate for quantitative analysis of the aqueous phase from hydrothermal liquefaction of biomass.

PubMed

Madsen, René Bjerregaard; Jensen, Mads Mørk; Mørup, Anders Juul; Houlberg, Kasper; Christensen, Per Sigaard; Klemmer, Maika; Becker, Jacob; Iversen, Bo Brummerstedt; Glasius, Marianne

2016-03-01

Hydrothermal liquefaction is a promising technique for the production of bio-oil. The process produces an oil phase, a gas phase, a solid residue, and an aqueous phase. Gas chromatography coupled with mass spectrometry is used to analyze the complex aqueous phase. Especially small organic acids and nitrogen-containing compounds are of interest. The efficient derivatization reagent methyl chloroformate was used to make analysis of the complex aqueous phase from hydrothermal liquefaction of dried distillers grains with solubles possible. A circumscribed central composite design was used to optimize the responses of both derivatized and nonderivatized analytes, which included small organic acids, pyrazines, phenol, and cyclic ketones. Response surface methodology was used to visualize significant factors and identify optimized derivatization conditions (volumes of methyl chloroformate, NaOH solution, methanol, and pyridine). Twenty-nine analytes of small organic acids, pyrazines, phenol, and cyclic ketones were quantified. An additional three analytes were pseudoquantified with use of standards with similar mass spectra. Calibration curves with high correlation coefficients were obtained, in most cases R (2)  > 0.991. Method validation was evaluated with repeatability, and spike recoveries of all 29 analytes were obtained. The 32 analytes were quantified in samples from the commissioning of a continuous flow reactor and in samples from recirculation experiments involving the aqueous phase. The results indicated when the steady-state condition of the flow reactor was obtained and the effects of recirculation. The validated method will be especially useful for investigations of the effect of small organic acids on the hydrothermal liquefaction process.

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...

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...

Statistical process control in nursing research.

PubMed

Polit, Denise F; Chaboyer, Wendy

2012-02-01

In intervention studies in which randomization to groups is not possible, researchers typically use quasi-experimental designs. Time series designs are strong quasi-experimental designs but are seldom used, perhaps because of technical and analytic hurdles. Statistical process control (SPC) is an alternative analytic approach to testing hypotheses about intervention effects using data collected over time. SPC, like traditional statistical methods, is a tool for understanding variation and involves the construction of control charts that distinguish between normal, random fluctuations (common cause variation), and statistically significant special cause variation that can result from an innovation. The purpose of this article is to provide an overview of SPC and to illustrate its use in a study of a nursing practice improvement intervention. Copyright © 2011 Wiley Periodicals, Inc.

Comparison of Analysis with Test for Static Loading of Two Hypersonic Inflatable Aerodynamic Decelerator Concepts

NASA Technical Reports Server (NTRS)

Lyle, Karen H.

2015-01-01

Acceptance of new spacecraft structural architectures and concepts requires validated design methods to minimize the expense involved with technology demonstration via flight-testing. Hypersonic Inflatable Aerodynamic Decelerator (HIAD) architectures are attractive for spacecraft deceleration because they are lightweight, store compactly, and utilize the atmosphere to decelerate a spacecraft during entry. However, designers are hesitant to include these inflatable approaches for large payloads or spacecraft because of the lack of flight validation. This publication summarizes results comparing analytical results with test data for two concepts subjected to representative entry, static loading. The level of agreement and ability to predict the load distribution is considered sufficient to enable analytical predictions to be used in the design process.

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.

Analytical Solutions, Moments, and Their Asymptotic Behaviors for the Time-Space Fractional Cable Equation

NASA Astrophysics Data System (ADS)

Li, Can; Deng, Wei-Hua

2014-07-01

Following the fractional cable equation established in the letter [B.I. Henry, T.A.M. Langlands, and S.L. Wearne, Phys. Rev. Lett. 100 (2008) 128103], we present the time-space fractional cable equation which describes the anomalous transport of electrodiffusion in nerve cells. The derivation is based on the generalized fractional Ohm's law; and the temporal memory effects and spatial-nonlocality are involved in the time-space fractional model. With the help of integral transform method we derive the analytical solutions expressed by the Green's function; the corresponding fractional moments are calculated; and their asymptotic behaviors are discussed. In addition, the explicit solutions of the considered model with two different external current injections are also presented.

Some subclasses of multivalent functions involving a certain linear operator

NASA Astrophysics Data System (ADS)

Srivastava, H. M.; Patel, J.

2005-10-01

The authors investigate various inclusion and other properties of several subclasses of the class of normalized p-valent analytic functions in the open unit disk, which are defined here by means of a certain linear operator. Problems involving generalized neighborhoods of analytic functions in the class are investigated. Finally, some applications of fractional calculus operators are considered.

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...

Liquid chromatographic tandem mass spectrometric assay for quantification of 97/78 and its metabolite 97/63: a promising trioxane antimalarial in monkey plasma.

PubMed

Singh, R P; Sabarinath, S; Gautam, N; Gupta, R C; Singh, S K

2009-07-15

The present manuscript describes development and validation of LC-MS/MS assay for the simultaneous quantitation of 97/78 and its active in-vivo metabolite 97/63 in monkey plasma using alpha-arteether as internal standard (IS). The method involves a single step protein precipitation using acetonitrile as extraction method. The analytes were separated on a Columbus C(18) (50 mm x 2 mm i.d., 5 microm particle size) column by isocratic elution with acetonitrile:ammonium acetate buffer (pH 4, 10 mM) (80:20 v/v) at a flow rate of 0.45 mL/min, and analyzed by mass spectrometry in multiple reaction-monitoring (MRM) positive ion mode. The chromatographic run time was 4.0 min and the weighted (1/x(2)) calibration curves were linear over a range of 1.56-200 ng/mL. The method was linear for both the analytes with correlation coefficients >0.995. The intra-day and inter-day accuracy (% bias) and precisions (% RSD) of the assay were less than 6.27%. Both analytes were stable after three freeze-thaw cycles (% deviation <8.2) and also for 30 days in plasma (% deviation <6.7). The absolute recoveries of 97/78, 97/63 and internal standard (IS), from spiked plasma samples were >90%. The validated assay method, described here, was successfully applied to the pharmacokinetic study of 97/78 and its active in-vivo metabolite 97/63 in Rhesus monkeys.

Development of a highly sensitive methodology for quantitative determination of fexofenadine in a microdose study by multiple injection method using ultra-high performance liquid chromatography with tandem mass spectrometry.

PubMed

Tanaka, Yukari; Yoshikawa, Yutaka; Yasui, Hiroyuki

2012-01-01

An ultra high-sensitivity method for quantifying fexofenadine concentration in rat plasma samples by multiple injection method (MIM) was developed for a microdose study. In this study, MIM involved continuous injections of multiple samples containing the single compound into a column of the ultra-HPLC (UHPLC) system, and then, temporary trapping of the analyte at the column head. This was followed by elution of the compound from the column and detection by mass spectrometer. Fexofenadine, used as a model compound in this study, was extracted from the plasma samples by a protein precipitation method. Chromatographic separation was achieved on a reversed-phase C18 column by using a gradient method with 0.1% formic acid and 0.1% formic acid in acetonitrile as the mobile phase. The analyte was quantified in the positive-ion electrospray ionization mode using selected reaction monitoring. In this study, the analytical time per fexofenadine sample was approximately 2 min according to the UHPLC system. The method exhibited the linear dynamic ranges of 5-5000 pg/mL for fexofenadine in rat plasma. The intra-day precisions were from 3.2 to 8.7% and the accuracy range was 95.2-99.3%. The inter-day precisions and accuracies ranged from 3.5 to 8.4% and from 98.6 to 102.6%, respectively. The validated MIM was successfully applied to a microdose study in the rats that received oral administration of 100 µg/kg fexofenadine. We suggest that this method might be beneficial for the quantification of fexofenadine concentrations in a microdose clinical study.

Evaluation of an analytic linear Boltzmann transport equation solver for high-density inhomogeneities

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

Lloyd, S. A. M.; Ansbacher, W.; Department of Physics and Astronomy, University of Victoria, Victoria, British Columbia V8W 3P6

2013-01-15

Purpose: Acuros external beam (Acuros XB) is a novel dose calculation algorithm implemented through the ECLIPSE treatment planning system. The algorithm finds a deterministic solution to the linear Boltzmann transport equation, the same equation commonly solved stochastically by Monte Carlo methods. This work is an evaluation of Acuros XB, by comparison with Monte Carlo, for dose calculation applications involving high-density materials. Existing non-Monte Carlo clinical dose calculation algorithms, such as the analytic anisotropic algorithm (AAA), do not accurately model dose perturbations due to increased electron scatter within high-density volumes. Methods: Acuros XB, AAA, and EGSnrc based Monte Carlo are usedmore » to calculate dose distributions from 18 MV and 6 MV photon beams delivered to a cubic water phantom containing a rectangular high density (4.0-8.0 g/cm{sup 3}) volume at its center. The algorithms are also used to recalculate a clinical prostate treatment plan involving a unilateral hip prosthesis, originally evaluated using AAA. These results are compared graphically and numerically using gamma-index analysis. Radio-chromic film measurements are presented to augment Monte Carlo and Acuros XB dose perturbation data. Results: Using a 2% and 1 mm gamma-analysis, between 91.3% and 96.8% of Acuros XB dose voxels containing greater than 50% the normalized dose were in agreement with Monte Carlo data for virtual phantoms involving 18 MV and 6 MV photons, stainless steel and titanium alloy implants and for on-axis and oblique field delivery. A similar gamma-analysis of AAA against Monte Carlo data showed between 80.8% and 87.3% agreement. Comparing Acuros XB and AAA evaluations of a clinical prostate patient plan involving a unilateral hip prosthesis, Acuros XB showed good overall agreement with Monte Carlo while AAA underestimated dose on the upstream medial surface of the prosthesis due to electron scatter from the high-density material. Film measurements support the dose perturbations demonstrated by Monte Carlo and Acuros XB data. Conclusions: Acuros XB is shown to perform as well as Monte Carlo methods and better than existing clinical algorithms for dose calculations involving high-density volumes.« less

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...

Development and validation of a simple UHPLC-MS/MS method for the simultaneous determination of trimethylamine N-oxide, choline, and betaine in human plasma and urine.

PubMed

Ocque, Andrew J; Stubbs, Jason R; Nolin, Thomas D

2015-05-10

A simple, sensitive, and precise ultra-high performance liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of trimethylamine N-oxide, choline, and betaine in human plasma and urine. Sample preparation involved protein precipitation with methanol containing internal standards. Chromatographic separation was achieved using an Acquity BEH Amide (2.1mm×50mm, 1.7μm) analytical column with gradient elution of solvent A (10mM ammonium formate, pH 3.5) and solvent B (acetonitrile). The flow rate was 0.4mL/min and the total run time was 5min. Detection of analytes was performed using heated electrospray ionization (positive mode) and selected reaction monitoring. Excellent linearity was observed over the standard curve concentration ranges of 0.010-5.00μg/mL (plasma) and 1.00-150μg/mL (urine) for all analytes. The intra- and inter-day accuracy and precision for all quality controls were within ±10%. Excellent recovery was observed. The method is rapid, accurate and reproducible, and was successfully applied to a pilot study of markers of atherosclerosis in patients with kidney disease who underwent successful kidney transplantation. Copyright © 2015 Elsevier B.V. All rights reserved.

A fully coupled method for massively parallel simulation of hydraulically driven fractures in 3-dimensions: FULLY COUPLED PARALLEL SIMULATION OF HYDRAULIC FRACTURES IN 3-D

DOE PAGES

Settgast, Randolph R.; Fu, Pengcheng; Walsh, Stuart D. C.; ...

2016-09-18

This study describes a fully coupled finite element/finite volume approach for simulating field-scale hydraulically driven fractures in three dimensions, using massively parallel computing platforms. The proposed method is capable of capturing realistic representations of local heterogeneities, layering and natural fracture networks in a reservoir. A detailed description of the numerical implementation is provided, along with numerical studies comparing the model with both analytical solutions and experimental results. The results demonstrate the effectiveness of the proposed method for modeling large-scale problems involving hydraulically driven fractures in three dimensions.

A fully coupled method for massively parallel simulation of hydraulically driven fractures in 3-dimensions: FULLY COUPLED PARALLEL SIMULATION OF HYDRAULIC FRACTURES IN 3-D

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

Settgast, Randolph R.; Fu, Pengcheng; Walsh, Stuart D. C.

This study describes a fully coupled finite element/finite volume approach for simulating field-scale hydraulically driven fractures in three dimensions, using massively parallel computing platforms. The proposed method is capable of capturing realistic representations of local heterogeneities, layering and natural fracture networks in a reservoir. A detailed description of the numerical implementation is provided, along with numerical studies comparing the model with both analytical solutions and experimental results. The results demonstrate the effectiveness of the proposed method for modeling large-scale problems involving hydraulically driven fractures in three dimensions.

Some important considerations in the development of stress corrosion cracking test methods.

NASA Technical Reports Server (NTRS)

Wei, R. P.; Novak, S. R.; Williams, D. P.

1972-01-01

Discussion of some of the precaution needs the development of fracture-mechanics based test methods for studying stress corrosion cracking involves. Following a review of pertinent analytical fracture mechanics considerations and of basic test methods, the implications for test corrosion cracking studies of the time-to-failure determining kinetics of crack growth and life are examined. It is shown that the basic assumption of the linear-elastic fracture mechanics analyses must be clearly recognized and satisfied in experimentation and that the effects of incubation and nonsteady-state crack growth must also be properly taken into account in determining the crack growth kinetics, if valid data are to be obtained from fracture-mechanics based test methods.

Overcoming the challenges of conventional dispersive liquid-liquid microextraction: analysis of THMs in chlorinated swimming pools.

PubMed

Faraji, Hakim; Helalizadeh, Masoumeh; Kordi, Mohammad Reza

2018-01-01

A rapid, simple, and sensitive approach to the analysis of trihalomethanes (THMs) in swimming pool water samples has been developed. The main goal of this study was to overcome or to improve the shortcomings of conventional dispersive liquid-liquid microextraction (DLLME) and to maximize the realization of green analytical chemistry principles. The method involves a simple vortex-assisted microextraction step, in the absence of the dispersive solvent, followed by salting-out effect for the elimination of the centrifugation step. A bell-shaped device and a solidifiable solvent were used to simplify the extraction solvent collection after phase separation. Optimization of the independent variables was performed by using chemometric methods in three steps. The method was statistically validated based on authentic guidance documents. The completion time for extraction was less than 8 min, and the limits of detection were in the range between 4 and 72 ng L -1 . Using this method, good linearity and precision were achieved. The results of THMs determination in different real samples showed that in some cases the concentration of total THMs was more than threshold values of THMs determined by accredited healthcare organizations. This method indicated satisfactory analytical figures of merit. Graphical Abstract A novel green microextraction technique for overcoming the challenges of conventional DLLME. The proposed procedure complies with the principles of green/sustainable analytical chemistry, comprising decreasing the sample size, making easy automation of the process, reducing organic waste, diminishing energy consumption, replacing toxic reagents with safer reagents, and enhancing operator safety.

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...

Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

PubMed

Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

2016-08-12

A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A Development Strategy for Creating a Suite of Reference Materials for the in-situ Microanalysis of Non-conventional Raw Materials

NASA Astrophysics Data System (ADS)

Renno, A. D.; Merchel, S.; Michalak, P. P.; Munnik, F.; Wiedenbeck, M.

2010-12-01

Recent economic trends regarding the supply of rare metals readily justify scientific research into non-conventional raw materials, where a particular need is a better understanding of the relationship between mineralogy, microstructure and the distribution of key metals within ore deposits (geometallurgy). Achieving these goals will require an extensive usage of in-situ microanalytical techniques capable of spatially resolving material heterogeneities which can be key for understanding better resource utilization. The availability of certified reference materials (CRMs) is an essential prerequisite for (1) validating new analytical methods, (2) demonstrating data quality to the contracting authorities, (3) supporting method development and instrument calibration, and (4) establishing traceability between new analytical approaches and existing data sets. This need has led to the granting of funding by the European Union and the German Free State of Saxony for a program to develop such reference materials . This effort will apply the following strategies during the selection of the phases: (1) will use exclusively synthetic minerals, thereby providing large volumes of homogeneous starting material. (2) will focus on matrices which are capable of incorporating many ‘important’ elements while avoid exotic compositions which would not be optimal matrix matches. (3) will emphasise those phases which remain stable during the various microanalytical procedure. This initiative will assess the homogeneity of the reference materials at sampling sizes ranging between 50 and 1 µm; it is also intended to document crystal structural homogeneity too, as this too may potentially impact specific analytical methods. As far as possible both definitive methods as well as methods involving matrix corrections will be used for determining the compositions of the of the individual materials. A critical challenge will be the validation of the determination of analytes concentrations as sub-µg sampling masses. It is planned to cooperate with those who are interested in the development of such reference materials and we invite them to take part in round-robin exercises.

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.

Square-wave adsorptive stripping voltammetric determination of nanomolar levels of bezafibrate using a glassy carbon electrode modified with multi-walled carbon nanotubes within a dihexadecyl hydrogen phosphate film.

PubMed

Ardila, Jorge Armando; Oliveira, Geiser Gabriel; Medeiros, Roberta Antigo; Fatibello-Filho, Orlando

2014-04-07

A highly sensitive method for bezafibrate determination using a glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes within a dihexadecyl hydrogen phosphate film based on square-wave adsorptive stripping voltammetry (SWAdSV) is proposed. The electrochemical behaviour of bezafibrate has been studied by cyclic voltammetry, showing an irreversible anodic peak at a potential of 1.09 V in 0.1 mol L(-1) phosphate buffer solution (pH 2.0). A study of the scan rate showed that the oxidation of bezafibrate is an adsorptive-controlled process, involving the transfer of two electrons and two protons per molecule. The analytical curve was linear over a bezafibrate concentration range from 50 to 910 nmol L(-1), with a detection limit of 16 nmol L(-1). This analytical method was successfully applied for benzafibrate determination in pharmaceutical formulations, with results showing good agreement with those obtained using a comparative spectrophotometric method, and has the potential for field application.

Scaling Laws Applied to a Modal Formulation of the Aeroservoelastic Equations

NASA Technical Reports Server (NTRS)

Pototzky, Anthony S.

2002-01-01

A method of scaling is described that easily converts the aeroelastic equations of motion of a full-sized aircraft into ones of a wind-tunnel model. To implement the method, a set of rules is provided for the conversion process involving matrix operations with scale factors. In addition, a technique for analytically incorporating a spring mounting system into the aeroelastic equations is also presented. As an example problem, a finite element model of a full-sized aircraft is introduced from the High Speed Research (HSR) program to exercise the scaling method. With a set of scale factor values, a brief outline is given of a procedure to generate the first-order aeroservoelastic analytical model representing the wind-tunnel model. To verify the scaling process as applied to the example problem, the root-locus patterns from the full-sized vehicle and the wind-tunnel model are compared to see if the root magnitudes scale with the frequency scale factor value. Selected time-history results are given from a numerical simulation of an active-controlled wind-tunnel model to demonstrate the utility of the scaling process.

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.

Analysis of multiple quaternary ammonium compounds in the brain using tandem capillary column separation and high resolution mass spectrometric detection.

PubMed

Falasca, Sara; Petruzziello, Filomena; Kretz, Robert; Rainer, Gregor; Zhang, Xiaozhe

2012-06-08

Endogenous quaternary ammonium compounds are involved in various physiological processes in the central nervous system. In the present study, eleven quaternary ammonium compounds, including acetylcholine, choline, carnitine, acetylcarnitine and seven other acylcarnitines of low polarity, were analyzed from brain extracts using a two dimension capillary liquid chromatography-Fourier transform mass spectrometry method. To deal with their large difference in hydrophobicities, tandem coupling between reversed phase and hydrophilic interaction chromatography columns was used to separate all the targeted quaternary ammonium compounds. Using high accuracy mass spectrometry in selected ion monitoring mode, all the compounds could be detected from each brain sample with high selectivity. The developed method was applied for the relative quantification of these quaternary ammonium compounds in three different brain regions of tree shrews: prefrontal cortex, striatum, and hippocampus. The comparative analysis showed that quaternary ammonium compounds were differentially distributed across the three brain areas. The analytical method proved to be highly sensitive and reliable for simultaneous determination of all the targeted analytes from brain samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Dynamic leaching and fractionation of trace elements from environmental solids exploiting a novel circulating-flow platform.

PubMed

Mori, Masanobu; Nakano, Koji; Sasaki, Masaya; Shinozaki, Haruka; Suzuki, Shiho; Okawara, Chitose; Miró, Manuel; Itabashi, Hideyuki

2016-02-01

A dynamic flow-through microcolumn extraction system based on extractant re-circulation is herein proposed as a novel analytical approach for simplification of bioaccessibility tests of trace elements in sediments. On-line metal leaching is undertaken in the format of all injection (AI) analysis, which is a sequel of flow injection analysis, but involving extraction under steady-state conditions. The minimum circulation times and flow rates required to determine the maximum bioaccessible pools of target metals (viz., Cu, Zn, Cd, and Pb) from lake and river sediment samples were estimated using Tessier's sequential extraction scheme and an acid single extraction test. The on-line AIA method was successfully validated by mass balance studies of CRM and real sediment samples. Tessier's test in on-line AI format demonstrated to be carried out by one third of extraction time (6h against more than 17 h by the conventional method), with better analytical precision (<9.2% against >15% by the conventional method) and significant decrease in blank readouts as compared with the manual batch counterpart. Copyright © 2015 Elsevier B.V. All rights reserved.

Analytical display design for flight tasks conducted under instrument meteorological conditions. [human factors engineering of pilot performance for display device design in instrument landing systems

NASA Technical Reports Server (NTRS)

Hess, R. A.

1976-01-01

Paramount to proper utilization of electronic displays is a method for determining pilot-centered display requirements. Display design should be viewed fundamentally as a guidance and control problem which has interactions with the designer's knowledge of human psychomotor activity. From this standpoint, reliable analytical models of human pilots as information processors and controllers can provide valuable insight into the display design process. A relatively straightforward, nearly algorithmic procedure for deriving model-based, pilot-centered display requirements was developed and is presented. The optimal or control theoretic pilot model serves as the backbone of the design methodology, which is specifically directed toward the synthesis of head-down, electronic, cockpit display formats. Some novel applications of the optimal pilot model are discussed. An analytical design example is offered which defines a format for the electronic display to be used in a UH-1H helicopter in a landing approach task involving longitudinal and lateral degrees of freedom.

Methods for integrating moderation and mediation: a general analytical framework using moderated path analysis.

PubMed

Edwards, Jeffrey R; Lambert, Lisa Schurer

2007-03-01

Studies that combine moderation and mediation are prevalent in basic and applied psychology research. Typically, these studies are framed in terms of moderated mediation or mediated moderation, both of which involve similar analytical approaches. Unfortunately, these approaches have important shortcomings that conceal the nature of the moderated and the mediated effects under investigation. This article presents a general analytical framework for combining moderation and mediation that integrates moderated regression analysis and path analysis. This framework clarifies how moderator variables influence the paths that constitute the direct, indirect, and total effects of mediated models. The authors empirically illustrate this framework and give step-by-step instructions for estimation and interpretation. They summarize the advantages of their framework over current approaches, explain how it subsumes moderated mediation and mediated moderation, and describe how it can accommodate additional moderator and mediator variables, curvilinear relationships, and structural equation models with latent variables. (c) 2007 APA, all rights reserved.

Forensic Investigation of Formaldehyde in Illicit Products for Hair Treatment by DAD-HPLC: A Case Study.

PubMed

Oiye, Erica N; Ribeiro, Maria Fernanda M; Okumura, Leonardo L; Saczk, Adelir A; Ciancaglini, Pietro; de Oliveira, Marcelo F

2016-07-01

The illegal use of formalin (commercial formaldehyde) in cosmetic products harms the health of individuals exposed to this substance. Over the last years, the commercial availability of these products, especially those containing irregular dosage of formaldehyde, has increased in Brazil. This work analyzes some products for hair treatment available in the Brazilian market and verifies their safety. The adopted analytical methodology involved sample derivatization with 2,4-dinitrophenylhydrazine, followed by high-performance liquid chromatography with ultraviolet detection (UV-VIS) at λ = 365 nm. The limit of quantification is 2.5 × 10 -3% w/w, and the recovery tests were around 93%. Some of the samples contained high and illegal formaldehyde levels ranging from 9% to 19% (w/w) and others presented suitable concentrations of the analyte. On the basis of the results, this work discusses the efficiency and practicality of this analytical method for forensic purposes. © 2016 American Academy of Forensic Sciences.

Exact solution of three-dimensional transport problems using one-dimensional models. [in semiconductor devices

NASA Technical Reports Server (NTRS)

Misiakos, K.; Lindholm, F. A.

1986-01-01

Several parameters of certain three-dimensional semiconductor devices including diodes, transistors, and solar cells can be determined without solving the actual boundary-value problem. The recombination current, transit time, and open-circuit voltage of planar diodes are emphasized here. The resulting analytical expressions enable determination of the surface recombination velocity of shallow planar diodes. The method involves introducing corresponding one-dimensional models having the same values of these parameters.

Aquatic sediments

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

DePinto, J.V.; Young, T.C.; Booty, W.G.

1984-06-01

This literature review includes conference proceedings on the interactions of PCBs. Papers range from the adsorption/desorption behavior of PCBs to the influence of suspended and benthic sediments on fate and transport modeling of PCBs in the Great Lakes. Other papers are included in the review which involve analytical and sampling methods, paleolimnology, and modeling and sediment transport. Two papers presented the results of using radionuclides (Pb-210, Ru-106, Cs-137) in the study of lake-sediment dynamics. 111 references.

Pseudopotential Method for Higher Partial Wave Scattering

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

Idziaszek, Zbigniew; Centrum Fizyki Teoretycznej, Polska Akademia Nauk, 02-668 Warsaw; Calarco, Tommaso

2006-01-13

We present a zero-range pseudopotential applicable for all partial wave interactions between neutral atoms. For p and d waves, we derive effective pseudopotentials, which are useful for problems involving anisotropic external potentials. Finally, we consider two nontrivial applications of the p-wave pseudopotential: we solve analytically the problem of two interacting spin-polarized fermions confined in a harmonic trap, and we analyze the scattering of p-wave interacting particles in a quasi-two-dimensional system.

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.

The determination of mercury in mushrooms by CV-AAS and ICP-AES techniques.

PubMed

Jarzynska, Grazyna; Falandysz, Jerzy

2011-01-01

This research presents an example of an excellent applied study on analytical problems due to hazardous mercury determination in environmental materials and validity of published results on content of this element in wild growing mushrooms. The total mercury content has been analyzed in a several species of wild-grown mushrooms and some herbal origin certified reference materials, using two analytical methods. One method was commonly known and well validated the cold-vapour atomic absorption spectroscopy (CV-AAS) after a direct sample pyrolysis coupled to the gold wool trap, which was a reference method. A second method was a procedure that involved a final mercury measurement using the inductively-coupled plasma atomic emission spectroscopy (ICP-AES) at λ 194.163 nm, which was used by some authors to report on a high mercury content of a large sets of wild-grown mushrooms. We found that the method using the ICP-AES at λ 194.163 nm gave inaccurate and imprecise results. The results of this study imply that because of unsuitability of total mercury determination using the ICP-AES at λ 194.163 nm, the reports on great concentrations of this metal in a large sets of wild-grown mushrooms, when examined using this method, have to be studied with caution, since data are highly biased.

Rapid determination of amino acids in neonatal blood samples based on derivatization with isobutyl chloroformate followed by solid-phase microextraction and gas chromatography/mass spectrometry.

PubMed

Deng, Chunhui; Li, Ning; Zhang, Xiangmin

2004-01-01

The purpose of this study was to develop a simple, rapid and sensitive analytical method for determination of amino acids in neonatal blood samples. The developed method involves the employment of derivatization and a solid-phase microextraction (SPME) technique together with gas chromatography/mass spectrometry (GC/MS). Amino acids in blood samples were derivatized by a mixture of isobutyl chloroformate, methanol and pyridine, and the N(O,S)-alkoxycarbonyl alkyl esters thus formed were headspace extracted by a SPME fiber. Finally, the extracted analytes on the fiber were desorbed and detected by GC/MS in electron impact (EI) mode. L-Valine, L-leucine, L-isoleucine, L-phenylanaline and L-tyrosine in blood samples were quantitatively analyzed by measurement of the corresponding N(O,S)-alkoxycarbonyl alkyl esters using an external standard method. SPME conditions were optimized, and the method was validated. The method was applied to diagnosis of neonatal phenylkenuria (PKU) and maple syrup urine disease (MSUD) by the analyses of five amino acids in blood samples. The results showed that the proposed method is a potentially powerful tool for simultaneous screening for neonatal PKU and MSUD. Copyright (c) 2004 John Wiley & Sons, Ltd.

Lax-Wendroff and TVD finite volume methods for unidimensional thermomechanical numerical simulations of impacts on elastic-plastic solids

NASA Astrophysics Data System (ADS)

Heuzé, Thomas

2017-10-01

We present in this work two finite volume methods for the simulation of unidimensional impact problems, both for bars and plane waves, on elastic-plastic solid media within the small strain framework. First, an extension of Lax-Wendroff to elastic-plastic constitutive models with linear and nonlinear hardenings is presented. Second, a high order TVD method based on flux-difference splitting [1] and Superbee flux limiter [2] is coupled with an approximate elastic-plastic Riemann solver for nonlinear hardenings, and follows that of Fogarty [3] for linear ones. Thermomechanical coupling is accounted for through dissipation heating and thermal softening, and adiabatic conditions are assumed. This paper essentially focuses on one-dimensional problems since analytical solutions exist or can easily be developed. Accordingly, these two numerical methods are compared to analytical solutions and to the explicit finite element method on test cases involving discontinuous and continuous solutions. This allows to study in more details their respective performance during the loading, unloading and reloading stages. Particular emphasis is also paid to the accuracy of the computed plastic strains, some differences being found according to the numerical method used. Lax-Wendoff two-dimensional discretization of a one-dimensional problem is also appended at the end to demonstrate the extensibility of such numerical scheme to multidimensional problems.

Finite-difference time-domain modelling of through-the-Earth radio signal propagation

NASA Astrophysics Data System (ADS)

Ralchenko, M.; Svilans, M.; Samson, C.; Roper, M.

2015-12-01

This research seeks to extend the knowledge of how a very low frequency (VLF) through-the-Earth (TTE) radio signal behaves as it propagates underground, by calculating and visualizing the strength of the electric and magnetic fields for an arbitrary geology through numeric modelling. To achieve this objective, a new software tool has been developed using the finite-difference time-domain method. This technique is particularly well suited to visualizing the distribution of electromagnetic fields in an arbitrary geology. The frequency range of TTE radio (400-9000 Hz) and geometrical scales involved (1 m resolution for domains a few hundred metres in size) involves processing a grid composed of millions of cells for thousands of time steps, which is computationally expensive. Graphics processing unit acceleration was used to reduce execution time from days and weeks, to minutes and hours. Results from the new modelling tool were compared to three cases for which an analytic solution is known. Two more case studies were done featuring complex geologic environments relevant to TTE communications that cannot be solved analytically. There was good agreement between numeric and analytic results. Deviations were likely caused by numeric artifacts from the model boundaries; however, in a TTE application in field conditions, the uncertainty in the conductivity of the various geologic formations will greatly outweigh these small numeric errors.

The WOMBAT Attack Attribution Method: Some Results

NASA Astrophysics Data System (ADS)

Dacier, Marc; Pham, Van-Hau; Thonnard, Olivier

In this paper, we present a new attack attribution method that has been developed within the WOMBAT project. We illustrate the method with some real-world results obtained when applying it to almost two years of attack traces collected by low interaction honeypots. This analytical method aims at identifying large scale attack phenomena composed of IP sources that are linked to the same root cause. All malicious sources involved in a same phenomenon constitute what we call a Misbehaving Cloud (MC). The paper offers an overview of the various steps the method goes through to identify these clouds, providing pointers to external references for more detailed information. Four instances of misbehaving clouds are then described in some more depth to demonstrate the meaningfulness of the concept.

On integrating Jungian and other theories.

PubMed

Sedgwick, David

2015-09-01

This paper consists of reflections on some of the processes, subtleties, and 'eros' involved in attempting to integrate Jungian and other analytic perspectives. Assimilation of other theoretical viewpoints has a long history in analytical psychology, beginning when Jung met Freud. Since its inception, the Journal of Analytical Psychology has provided a forum for theoretical syntheses and comparative psychoanalysis. Such attempts at synthesizing other theories represent analytical psychology itself trying to individuate. © 2015, The Society of Analytical Psychology.

A decision support system using analytical hierarchy process (AHP) for the optimal environmental reclamation of an open-pit mine

NASA Astrophysics Data System (ADS)

Bascetin, A.

2007-04-01

The selection of an optimal reclamation method is one of the most important factors in open-pit design and production planning. It also affects economic considerations in open-pit design as a function of plan location and depth. Furthermore, the selection is a complex multi-person, multi-criteria decision problem. The group decision-making process can be improved by applying a systematic and logical approach to assess the priorities based on the inputs of several specialists from different functional areas within the mine company. The analytical hierarchy process (AHP) can be very useful in involving several decision makers with different conflicting objectives to arrive at a consensus decision. In this paper, the selection of an optimal reclamation method using an AHP-based model was evaluated for coal production in an open-pit coal mine located at Seyitomer region in Turkey. The use of the proposed model indicates that it can be applied to improve the group decision making in selecting a reclamation method that satisfies optimal specifications. Also, it is found that the decision process is systematic and using the proposed model can reduce the time taken to select a optimal method.

Study of a two-dimension transient heat propagation in cylindrical coordinates by means of two finite difference methods

NASA Astrophysics Data System (ADS)

Dumencu, A.; Horbaniuc, B.; Dumitraşcu, G.

2016-08-01

The analytical approach of unsteady conduction heat transfer under actual conditions represent a very difficult (if not insurmountable) problem due to the issues related to finding analytical solutions for the conduction heat transfer equation. Various techniques have been developed in order to overcome these difficulties, among which the alternate directions method and the decomposition method. Both of them are particularly suited for two-dimension heat propagation. The paper deals with both techniques in order to verify whether the results provided are in good accordance. The studied case consists of a long hollow cylinder, and considers that the time-dependent temperature field varies both in the radial and the axial directions. The implicit technique is used in both methods and involves the simultaneous solving of a set of equations for all of the nodes for each time step successively for each of the two directions. Gauss elimination is used to obtain the solution of the set, representing the nodal temperatures. After using the two techniques the results show a very good agreement, and since the decomposition is easier to use in terms of computer code and running time, this technique seems to be more recommendable.

Category 1 external quality assessment program for serum creatinine.

PubMed

González-Lao, Elisabet; Díaz-Garzón, Jorge; Corte, Zoraida; Ricós, Carmen; Perich, Carmen; Álvarez, Virtudes; Simón, Margarita; Minchinela, Joana; García-Lario, José Vicente; Boned, Beatriz; Biosca, Carmen; Cava, Fernando; Fernández-Fernández, Pilar; Fernández-Calle, Pilar

2017-03-01

The Commission of Analytical Quality and the Committee of External Quality Programs of Spanish Society of Laboratory Medicine (SEQC) in collaboration with the Dutch Foundation for the Quality organized the first national category 1 External Quality Assessment Programs (EQAP) pilot study. The aim is to evaluate the standardization of serum creatinine measurements in the Spanish laboratories through a category 1 external quality assurance program with commutable material and reference method assigned values. A total of 87 Spanish laboratories were involved in this program in 2015. Each day a sample control was measured by duplicate during 6 consecutive days. Percentage deviations and coefficients of variation obtained were compared with quality specifications derived from biological variation. A total of 1044 creatinine results were obtained. Laboratories were coded in 11 different method-traceability combinations. Only enzymatic methods get all results within the acceptability limits. To participate in a category 1 EQAP is a valuable tool to assess the standardization degree in our country; a big effort should be made to promote laboratories to change their procedures and to use enzymatic creatinine methods, in order to achieve a satisfactory standardization degree for this important analyte.

Purification of Carbon Nanotubes: Alternative Methods

NASA Technical Reports Server (NTRS)

Files, Bradley; Scott, Carl; Gorelik, Olga; Nikolaev, Pasha; Hulse, Lou; Arepalli, Sivaram

2000-01-01

Traditional carbon nanotube purification process involves nitric acid refluxing and cross flow filtration using surfactant TritonX. This is believed to result in damage to nanotubes and surfactant residue on nanotube surface. Alternative purification procedures involving solvent extraction, thermal zone refining and nitric acid refiuxing are used in the current study. The effect of duration and type of solvent to dissolve impurities including fullerenes and P ACs (polyaromatic compounds) are monitored by nuclear magnetic reasonance, high performance liquid chromatography, and thermogravimetric analysis. Thermal zone refining yielded sample areas rich in nanotubes as seen by scanning electric microscopy. Refluxing in boiling nitric acid seem to improve the nanotube content. Different procedural steps are needed to purify samples produced by laser process compared to arc process. These alternative methods of nanotube purification will be presented along with results from supporting analytical techniques.

[Forced displacement, childhood and adolescence: scenarios regarding socioeconomic stability].

PubMed

Patiño, Gonzalo A; Herrán, Oscar F

2012-06-01

Describing and analysing socio-economic stabilisation scenarios for populations which have been forcibly displaced paying special attention to the situation of children and adolescents. The analytic hierarchy process (AHP) multi-criteria decision-making method developed by Professor Thomas Saaty was used through expert workshops, involving researchers, leaders of NGOs and displaced communities living in the city of Bucaramanga. The partial result of this research showed that some elderly adults from forcibly displaced communities preferred to adapt themselves to urban centres, rather than return to their places of origin, particularly when it came to protecting younger children and dealing with their welfare. The method's consistency index and consistency ratio came within the expected parameters. Government-promoted social and economic stabilisation programmes must be rethought regarding forcibly displaced populations, particularly when situations are envisaged involving the welfare of children and adolescents.

Non-detonable and non-explosive explosive simulators

DOEpatents

Simpson, Randall L.; Pruneda, Cesar O.

1997-01-01

A simulator which is chemically equivalent to an explosive, but is not detonable or explodable. The simulator is a combination of an explosive material with an inert material, either in a matrix or as a coating, where the explosive has a high surface ratio but small volume ratio. The simulator has particular use in the training of explosives detecting dogs, calibrating analytical instruments which are sensitive to either vapor or elemental composition, or other applications where the hazards associated with explosives is undesirable but where chemical and/or elemental equivalence is required. The explosive simulants may be fabricated by different techniques. A first method involves the use of standard slurry coatings to produce a material with a very high binder to explosive ratio without masking the explosive vapor, and a second method involves coating inert substrates with thin layers of explosive.

Understanding Education Involving Geovisual Analytics

ERIC Educational Resources Information Center

Stenliden, Linnea

2013-01-01

Handling the vast amounts of data and information available in contemporary society is a challenge. Geovisual Analytics provides technology designed to increase the effectiveness of information interpretation and analytical task solving. To date, little attention has been paid to the role such tools can play in education and to the extent to which…

The uncertainty of nitrous oxide emissions from grazed grasslands: A New Zealand case study

NASA Astrophysics Data System (ADS)

Kelliher, Francis M.; Henderson, Harold V.; Cox, Neil R.

2017-01-01

Agricultural soils emit nitrous oxide (N2O), a greenhouse gas and the primary source of nitrogen oxides which deplete stratospheric ozone. Agriculture has been estimated to be the largest anthropogenic N2O source. In New Zealand (NZ), pastoral agriculture uses half the land area. To estimate the annual N2O emissions from NZ's agricultural soils, the nitrogen (N) inputs have been determined and multiplied by an emission factor (EF), the mass fraction of N inputs emitted as N2Osbnd N. To estimate the associated uncertainty, we developed an analytical method. For comparison, another estimate was determined by Monte Carlo numerical simulation. For both methods, expert judgement was used to estimate the N input uncertainty. The EF uncertainty was estimated by meta-analysis of the results from 185 NZ field trials. For the analytical method, assuming a normal distribution and independence of the terms used to calculate the emissions (correlation = 0), the estimated 95% confidence limit was ±57%. When there was a normal distribution and an estimated correlation of 0.4 between N input and EF, the latter inferred from experimental data involving six NZ soils, the analytical method estimated a 95% confidence limit of ±61%. The EF data from 185 NZ field trials had a logarithmic normal distribution. For the Monte Carlo method, assuming a logarithmic normal distribution for EF, a normal distribution for the other terms and independence of all terms, the estimated 95% confidence limits were -32% and +88% or ±60% on average. When there were the same distribution assumptions and a correlation of 0.4 between N input and EF, the Monte Carlo method estimated 95% confidence limits were -34% and +94% or ±64% on average. For the analytical and Monte Carlo methods, EF uncertainty accounted for 95% and 83% of the emissions uncertainty when the correlation between N input and EF was 0 and 0.4, respectively. As the first uncertainty analysis of an agricultural soils N2O emissions inventory using "country-specific" field trials to estimate EF uncertainty, this can be a potentially informative case study for the international scientific community.

Fast batch injection analysis of H(2)O(2) using an array of Pt-modified gold microelectrodes obtained from split electronic chips.

PubMed

Pacheco, Bruno D; Valério, Jaqueline; Angnes, Lúcio; Pedrotti, Jairo J

2011-06-24

A fast and robust analytical method for amperometric determination of hydrogen peroxide (H(2)O(2)) based on batch injection analysis (BIA) on an array of gold microelectrodes modified with platinum is proposed. The gold microelectrode array (n=14) was obtained from electronic chips developed for surface mounted device technology (SMD), whose size offers advantages to adapt them in batch cells. The effect of the dispensing rate, volume injected, distance between the platinum microelectrodes and the pipette tip, as well as the volume of solution in the cell on the analytical response were evaluated. The method allows the H(2)O(2) amperometric determination in the concentration range from 0.8 μmolL(-1) to 100 μmolL(-1). The analytical frequency can attain 300 determinations per hour and the detection limit was estimated in 0.34 μmolL(-1) (3σ). The anodic current peaks obtained after a series of 23 successive injections of 50 μL of 25 μmolL(-1) H(2)O(2) showed an RSD<0.9%. To ensure the good selectivity to detect H(2)O(2), its determination was performed in a differential mode, with selective destruction of the H(2)O(2) with catalase in 10 mmolL(-1) phosphate buffer solution. Practical application of the analytical procedure involved H(2)O(2) determination in rainwater of São Paulo City. A comparison of the results obtained by the proposed amperometric method with another one which combines flow injection analysis (FIA) with spectrophotometric detection showed good agreement. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

The Superior Lambert Algorithm

NASA Astrophysics Data System (ADS)

der, G.

2011-09-01

Lambert algorithms are used extensively for initial orbit determination, mission planning, space debris correlation, and missile targeting, just to name a few applications. Due to the significance of the Lambert problem in Astrodynamics, Gauss, Battin, Godal, Lancaster, Gooding, Sun and many others (References 1 to 15) have provided numerous formulations leading to various analytic solutions and iterative methods. Most Lambert algorithms and their computer programs can only work within one revolution, break down or converge slowly when the transfer angle is near zero or 180 degrees, and their multi-revolution limitations are either ignored or barely addressed. Despite claims of robustness, many Lambert algorithms fail without notice, and the users seldom have a clue why. The DerAstrodynamics lambert2 algorithm, which is based on the analytic solution formulated by Sun, works for any number of revolutions and converges rapidly at any transfer angle. It provides significant capability enhancements over every other Lambert algorithm in use today. These include improved speed, accuracy, robustness, and multirevolution capabilities as well as implementation simplicity. Additionally, the lambert2 algorithm provides a powerful tool for solving the angles-only problem without artificial singularities (pointed out by Gooding in Reference 16), which involves 3 lines of sight captured by optical sensors, or systems such as the Air Force Space Surveillance System (AFSSS). The analytic solution is derived from the extended Godal’s time equation by Sun, while the iterative method of solution is that of Laguerre, modified for robustness. The Keplerian solution of a Lambert algorithm can be extended to include the non-Keplerian terms of the Vinti algorithm via a simple targeting technique (References 17 to 19). Accurate analytic non-Keplerian trajectories can be predicted for satellites and ballistic missiles, while performing at least 100 times faster in speed than most numerical integration methods.

MRMPlus: an open source quality control and assessment tool for SRM/MRM assay development.

PubMed

Aiyetan, Paul; Thomas, Stefani N; Zhang, Zhen; Zhang, Hui

2015-12-12

Selected and multiple reaction monitoring involves monitoring a multiplexed assay of proteotypic peptides and associated transitions in mass spectrometry runs. To describe peptide and associated transitions as stable, quantifiable, and reproducible representatives of proteins of interest, experimental and analytical validation is required. However, inadequate and disparate analytical tools and validation methods predispose assay performance measures to errors and inconsistencies. Implemented as a freely available, open-source tool in the platform independent Java programing language, MRMPlus computes analytical measures as recommended recently by the Clinical Proteomics Tumor Analysis Consortium Assay Development Working Group for "Tier 2" assays - that is, non-clinical assays sufficient enough to measure changes due to both biological and experimental perturbations. Computed measures include; limit of detection, lower limit of quantification, linearity, carry-over, partial validation of specificity, and upper limit of quantification. MRMPlus streamlines assay development analytical workflow and therefore minimizes error predisposition. MRMPlus may also be used for performance estimation for targeted assays not described by the Assay Development Working Group. MRMPlus' source codes and compiled binaries can be freely downloaded from https://bitbucket.org/paiyetan/mrmplusgui and https://bitbucket.org/paiyetan/mrmplusgui/downloads respectively.

Determination of artificial sweeteners in beverages with green mobile phases and high temperature liquid chromatography-tandem mass spectrometry.

PubMed

Ordoñez, Edgar Y; Rodil, Rosario; Quintana, José Benito; Cela, Rafael

2015-02-15

A new analytical procedure involving the use of water and a low percentage of ethanol combined to high temperature liquid chromatography-tandem mass spectrometry has been developed for the determination of nine high-intensity sweeteners in a variety of drink samples. The method permitted the analysis in 23min (including column reequilibration) and consuming only 0.85mL of a green organic solvent (ethanol). This methodology provided limits of detection (after 50-fold dilution) in the 0.05-10mg/L range, with recoveries (obtained from five different types of beverages) being in the 86-110% range and relative standard deviation values lower than 12%. Finally, the method was applied to 25 different samples purchased in Spain, where acesulfame and sucralose were the most frequently detected analytes (>50% of the samples) and cyclamate was found over the legislation limit set by the European Union in a sample and at the regulation boundary in three others. Copyright © 2014 Elsevier Ltd. All rights reserved.

Method and apparatus for automated processing and aliquoting of whole blood samples for analysis in a centrifugal fast analyzer

DOEpatents

Burtis, Carl A.; Johnson, Wayne F.; Walker, William A.

1988-01-01

A rotor and disc assembly for use in a centrifugal fast analyzer. The assembly is designed to process multiple samples of whole blood followed by aliquoting of the resultant serum into precisely measured samples for subsequent chemical analysis. The assembly requires minimal operator involvement with no mechanical pipetting. The system comprises (1) a whole blood sample disc, (2) a serum sample disc, (3) a sample preparation rotor, and (4) an analytical rotor. The blood sample disc and serum sample disc are designed with a plurality of precision bore capillary tubes arranged in a spoked array. Samples of blood are loaded into the blood sample disc in capillary tubes filled by capillary action and centrifugally discharged into cavities of the sample preparation rotor where separation of serum and solids is accomplished. The serum is loaded into the capillaries of the serum sample disc by capillary action and subsequently centrifugally expelled into cuvettes of the analytical rotor for analysis by conventional methods.

BetaScint{trademark} fiber-optic sensor for detecting strontium-90 and uranium-238 in soil. Innovative technology summary report

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

NONE

1998-12-01

Accurate measurements of radioactivity in soils contaminated with Strontium-90 (Sr-90) or Uranium-238 (U-238) are essential for many DOE site remediation programs. These crucial measurements determine if excavation and soil removal is necessary, where remediation efforts should be focused, and/or if a site has reached closure. Measuring soil contamination by standard EPA laboratory methods typically takes a week (accelerated analytical test turnaround) or a month (standard analytical test turnaround). The time delay extends to operations involving heavy excavation equipment and associated personnel which are the main costs of remediation. This report describes an application of the BetaScint{trademark} fiber-optic sensor that measuresmore » Sr-90 or U-238 contamination in soil samples on site in about 20 minutes, at a much lower cost than time-consuming laboratory methods, to greatly facilitate remediation. This report describes the technology, its performance, its uses, cost, regulatory and policy issues, and lessons learned.« less

Rapid determination of minoxidil in human plasma using ion-pair HPLC.

PubMed

Zarghi, A; Shafaati, A; Foroutan, S M; Khoddam, A

2004-10-29

A rapid, simple and sensitive ion-pair high-performance liquid chromatography (HPLC) method has been developed for quantification of minoxidil in plasma. The assay enables the measurement of minoxidil for therapeutic drug monitoring with a minimum detectable limit of 0.5 ng ml(-1). The method involves simple, one-step extraction procedure and analytical recovery was complete. The separation was performed on an analytical 150 x 4.6 mm i.d. microbondapak C18 column. The wavelength was set at 281 nm. The mobile phase was a mixture of 0.01 M sodium dihydrogen phosphate buffer and acetonitrile (60:40, v/v) containing 2.5 mM sodium dodecyl sulphate adjusted to pH 3.5 at a flow rate of 1 ml/min. The column temperature was set at 50 degrees C. The calibration curve was linear over the concentration range 2-100 ng ml(-1). The coefficients of variation for inter-day and intra-day assay were found to be less than 8%.

Towards the authentication of European sea bass origin through a combination of biometric measurements and multiple analytical techniques.

PubMed

Farabegoli, Federica; Pirini, Maurizio; Rotolo, Magda; Silvi, Marina; Testi, Silvia; Ghidini, Sergio; Zanardi, Emanuela; Remondini, Daniel; Bonaldo, Alessio; Parma, Luca; Badiani, Anna

2018-06-08

The authenticity of fish products has become an imperative issue for authorities involved in the protection of consumers against fraudulent practices and in the market stabilization. The present study aimed to provide a method for authentication of European sea bass (Dicentrarchus labrax) according to the requirements for seafood labels (Regulation 1379/2013/EU). Data on biometric traits, fatty acid profile, elemental composition, and isotopic abundance of wild and reared (intensively, semi-intensively and extensively) specimens from 18 Southern European sources (n = 160) were collected and clustered in 6 sets of parameters, then subjected to multivariate analysis. Correct allocations of subjects according to their production method, origin and stocking density were demonstrated with good approximation rates (94%, 92% and 92%, respectively) using fatty acid profiles. Less satisfying results were obtained using isotopic abundance, biometric traits, and elemental composition. The multivariate analysis also revealed that extensively reared subjects cannot be analytically discriminated from wild ones.

Rapid classification of biological components

DOEpatents

Thompson, Vicki S.; Barrett, Karen B.; Key, Diane E.

2013-10-15

A method is disclosed for analyzing a biological sample by antibody profiling for identifying forensic samples or for detecting the presence of an analyte. In an illustrative embodiment of the invention, the analyte is a drug, such as marijuana, cocaine (crystalline tropane alkaloid), methamphetamine, methyltestosterone, or mesterolone. The method involves attaching antigens to a surface of a solid support in a preselected pattern to form an array wherein the locations of the antigens are known; contacting the array with the biological sample such that a portion of antibodies in the sample reacts with and binds to antigens in the array, thereby forming immune complexes; washing away antibodies that do not form immune complexes; and detecting the immune complexes, thereby forming an antibody profile. Forensic samples are identified by comparing a sample from an unknown source with a sample from a known source. Further, an assay, such as a test for illegal drug use, can be coupled to a test for identity such that the results of the assay can be positively correlated to a subject's identity.

Rapid classification of biological components

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

Thompson, Vicki S.; Barrett, Karen B.; Key, Diane E.

A method is disclosed for analyzing a biological sample by antibody profiling for identifying forensic samples or for detecting the presence of an analyte. In an illustrative embodiment of the invention, the analyte is a drug, such as marijuana, cocaine, methamphetamine, methyltestosterone, or mesterolone. The method involves attaching antigens to the surface of a solid support in a preselected pattern to form an array wherein the locations of the antigens are known; contacting the array with the biological sample such that a portion of antibodies in the sample reacts with and binds to antigens in the array, thereby forming immunemore » complexes; washing away antibodies that do form immune complexes; and detecting the immune complexes, thereby forming an antibody profile. Forensic samples are identified by comparing a sample from an unknown source with a sample from a known source. Further, an assay, such as a test for illegal drug use, can be coupled to a test for identity such that the results of the assay can be positively correlated to the subject's identity.« less

Application of advanced control techniques to aircraft propulsion systems

NASA Technical Reports Server (NTRS)

Lehtinen, B.

1984-01-01

Two programs are described which involve the application of advanced control techniques to the design of engine control algorithms. Multivariable control theory is used in the F100 MVCS (multivariable control synthesis) program to design controls which coordinate the control inputs for improved engine performance. A systematic method for handling a complex control design task is given. Methods of analytical redundancy are aimed at increasing the control system reliability. The F100 DIA (detection, isolation, and accommodation) program, which investigates the uses of software to replace or augment hardware redundancy for certain critical engine sensor, is described.

Parametrically excited non-linear multidegree-of-freedom systems with repeated natural frequencies

NASA Astrophysics Data System (ADS)

Tezak, E. G.; Nayfeh, A. H.; Mook, D. T.

1982-12-01

A method for analyzing multidegree-of-freedom systems having a repeated natural frequency subjected to a parametric excitation is presented. Attention is given to the ordering of the various terms (linear and non-linear) in the governing equations. The analysis is based on the method of multiple scales. As a numerical example involving a parametric resonance, panel flutter is discussed in detail in order to illustrate the type of results one can expect to obtain with this analysis. Some of the analytical results are verified by a numerical integration of the governing equations.

Study of diatomic molecules. 2: Intensities. [optical emission spectroscopy of ScO

NASA Technical Reports Server (NTRS)

Femenias, J. L.

1978-01-01

The theory of perturbations, giving the diatomic effective Hamiltonian, is used for calculating actual molecular wave functions and intensity factors involved in transitions between states arising from Hund's coupling cases a,b, intermediate a-b, and c tendency. The Herman and Wallis corrections are derived, without any knowledge of the analytical expressions of the wave functions, and generalized to transitions between electronic states with whatever symmetry and multiplicity. A general method for studying perturbed intensities is presented using primarily modern spectroscopic numerical approaches. The method is used in the study of the ScO optical emission spectrum.

Method of controlling a resin curing process. [for fiber reinforced composites

NASA Technical Reports Server (NTRS)

Webster, Charles Neal (Inventor); Scott, Robert O. (Inventor)

1989-01-01

The invention relates to an analytical technique for controlling the curing process of fiber-reinforced composite materials that are formed using thermosetting resins. The technique is the percent gel method and involves development of a time-to-gel equation as a function of temperature. From this equation a rate-of-gel equation is then determined, and a percent gel is calculated which is the product of rate-of-gel times time. Percent gel accounting is used to control the proper pressure application point in an autoclave cure process to achieve desired properties in a production composite part.

Long period perturbations of earth satellite orbits. [Von Zeipel method and zonal harmonics

NASA Technical Reports Server (NTRS)

Wang, K. C.

1979-01-01

All the equations involved in extending the PS phi solution to include the long periodic and second order secular effects of the zonal harmonics are presented. Topics covered include DSphi elements and relations for their conconical transformation into the PS phi elements; the solution algorithm based on the Von Zeipel method; and the elimination of long periodic terms and analytical integration of primed variables. The equations were entered into the ASOP program, checked out, and verified. Comparisons with numerical integrations show the long period theory to be accurate within several meters after 800 revolutions.

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...

The MCNP6 Analytic Criticality Benchmark Suite

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

Brown, Forrest B.

2016-06-16

Analytical benchmarks provide an invaluable tool for verifying computer codes used to simulate neutron transport. Several collections of analytical benchmark problems [1-4] are used routinely in the verification of production Monte Carlo codes such as MCNP® [5,6]. Verification of a computer code is a necessary prerequisite to the more complex validation process. The verification process confirms that a code performs its intended functions correctly. The validation process involves determining the absolute accuracy of code results vs. nature. In typical validations, results are computed for a set of benchmark experiments using a particular methodology (code, cross-section data with uncertainties, and modeling)more » and compared to the measured results from the set of benchmark experiments. The validation process determines bias, bias uncertainty, and possibly additional margins. Verification is generally performed by the code developers, while validation is generally performed by code users for a particular application space. The VERIFICATION_KEFF suite of criticality problems [1,2] was originally a set of 75 criticality problems found in the literature for which exact analytical solutions are available. Even though the spatial and energy detail is necessarily limited in analytical benchmarks, typically to a few regions or energy groups, the exact solutions obtained can be used to verify that the basic algorithms, mathematics, and methods used in complex production codes perform correctly. The present work has focused on revisiting this benchmark suite. A thorough review of the problems resulted in discarding some of them as not suitable for MCNP benchmarking. For the remaining problems, many of them were reformulated to permit execution in either multigroup mode or in the normal continuous-energy mode for MCNP. Execution of the benchmarks in continuous-energy mode provides a significant advance to MCNP verification methods.« less

Evaluation of active sampling strategies for the determination of 1,3-butadiene in air

NASA Astrophysics Data System (ADS)

Vallecillos, Laura; Maceira, Alba; Marcé, Rosa Maria; Borrull, Francesc

2018-03-01

Two analytical methods for determining levels of 1,3-butadiene in urban and industrial atmospheres were evaluated in this study. Both methods are extensively used for determining the concentration of volatile organic compounds in the atmosphere and involve collecting samples by active adsorptive enrichment on solid sorbents. The first method uses activated charcoal as the sorbent and involves liquid desorption with carbon disulfide. The second involves the use of a multi-sorbent bed with two graphitised carbons and a carbon molecular sieve as the sorbent, with thermal desorption. Special attention was paid to the optimization of the sampling procedure through the study of sample volume, the stability of 1,3-butadiene once inside the sampling tube and the humidity effect. In the end, the thermal desorption method showed better repeatability and limits of detection and quantification for 1,3-butadiene than the liquid desorption method, which makes the thermal desorption method more suitable for analysing air samples from both industrial and urban atmospheres. However, sampling must be performed with a pre-tube filled with a drying agent to prevent the loss of the adsorption capacity of the solid adsorbent caused by water vapour. The thermal desorption method has successfully been applied to determine of 1,3-butadiene inside a 1,3-butadiene production plant and at three locations in the vicinity of the same plant.

A Nonlinear Programming Perspective on Sensitivity Calculations for Systems Governed by State Equations

NASA Technical Reports Server (NTRS)

Lewis, Robert Michael

1997-01-01

This paper discusses the calculation of sensitivities. or derivatives, for optimization problems involving systems governed by differential equations and other state relations. The subject is examined from the point of view of nonlinear programming, beginning with the analytical structure of the first and second derivatives associated with such problems and the relation of these derivatives to implicit differentiation and equality constrained optimization. We also outline an error analysis of the analytical formulae and compare the results with similar results for finite-difference estimates of derivatives. We then attend to an investigation of the nature of the adjoint method and the adjoint equations and their relation to directions of steepest descent. We illustrate the points discussed with an optimization problem in which the variables are the coefficients in a differential operator.

Selection of remedial alternatives for mine sites: a multicriteria decision analysis approach.

PubMed

Betrie, Getnet D; Sadiq, Rehan; Morin, Kevin A; Tesfamariam, Solomon

2013-04-15

The selection of remedial alternatives for mine sites is a complex task because it involves multiple criteria and often with conflicting objectives. However, an existing framework used to select remedial alternatives lacks multicriteria decision analysis (MCDA) aids and does not consider uncertainty in the selection of alternatives. The objective of this paper is to improve the existing framework by introducing deterministic and probabilistic MCDA methods. The Preference Ranking Organization Method for Enrichment Evaluation (PROMETHEE) methods have been implemented in this study. The MCDA analysis involves processing inputs to the PROMETHEE methods that are identifying the alternatives, defining the criteria, defining the criteria weights using analytical hierarchical process (AHP), defining the probability distribution of criteria weights, and conducting Monte Carlo Simulation (MCS); running the PROMETHEE methods using these inputs; and conducting a sensitivity analysis. A case study was presented to demonstrate the improved framework at a mine site. The results showed that the improved framework provides a reliable way of selecting remedial alternatives as well as quantifying the impact of different criteria on selecting alternatives. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

Data-Driven Astrochemistry: One Step Further within the Origin of Life Puzzle.

PubMed

Ruf, Alexander; d'Hendecourt, Louis L S; Schmitt-Kopplin, Philippe

2018-06-01

Astrochemistry, meteoritics and chemical analytics represent a manifold scientific field, including various disciplines. In this review, clarifications on astrochemistry, comet chemistry, laboratory astrophysics and meteoritic research with respect to organic and metalorganic chemistry will be given. The seemingly large number of observed astrochemical molecules necessarily requires explanations on molecular complexity and chemical evolution, which will be discussed. Special emphasis should be placed on data-driven analytical methods including ultrahigh-resolving instruments and their interplay with quantum chemical computations. These methods enable remarkable insights into the complex chemical spaces that exist in meteorites and maximize the level of information on the huge astrochemical molecular diversity. In addition, they allow one to study even yet undescribed chemistry as the one involving organomagnesium compounds in meteorites. Both targeted and non-targeted analytical strategies will be explained and may touch upon epistemological problems. In addition, implications of (metal)organic matter toward prebiotic chemistry leading to the emergence of life will be discussed. The precise description of astrochemical organic and metalorganic matter as seeds for life and their interactions within various astrophysical environments may appear essential to further study questions regarding the emergence of life on a most fundamental level that is within the molecular world and its self-organization properties.

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.

Analytical performances of food microbiology laboratories - critical analysis of 7 years of proficiency testing results.

PubMed

Abdel Massih, M; Planchon, V; Polet, M; Dierick, K; Mahillon, J

2016-02-01

Based on the results of 19 food microbiology proficiency testing (PT) schemes, this study aimed to assess the laboratory performances, to highlight the main sources of unsatisfactory analytical results and to suggest areas of improvement. The 2009-2015 results of REQUASUD and IPH PT, involving a total of 48 laboratories, were analysed. On average, the laboratories failed to detect or enumerate foodborne pathogens in 3·0% of the tests. Thanks to a close collaboration with the PT participants, the causes of outliers could be identified in 74% of the cases. The main causes of erroneous PT results were either pre-analytical (handling of the samples, timing of analysis), analytical (unsuitable methods, confusion of samples, errors in colony counting or confirmation) or postanalytical mistakes (calculation and encoding of results). PT schemes are a privileged observation post to highlight analytical problems, which would otherwise remain unnoticed. In this perspective, this comprehensive study of PT results provides insight into the sources of systematic errors encountered during the analyses. This study draws the attention of the laboratories to the main causes of analytical errors and suggests practical solutions to avoid them, in an educational purpose. The observations support the hypothesis that regular participation to PT, when followed by feed-back and appropriate corrective actions, can play a key role in quality improvement and provide more confidence in the laboratory testing results. © 2015 The Society for Applied Microbiology.

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.

Single-analyte to multianalyte fluorescence sensors

NASA Astrophysics Data System (ADS)

Lavigne, John J.; Metzger, Axel; Niikura, Kenichi; Cabell, Larry A.; Savoy, Steven M.; Yoo, J. S.; McDevitt, John T.; Neikirk, Dean P.; Shear, Jason B.; Anslyn, Eric V.

1999-05-01

The rational design of small molecules for the selective complexation of analytes has reached a level of sophistication such that there exists a high degree of prediction. An effective strategy for transforming these hosts into sensors involves covalently attaching a fluorophore to the receptor which displays some fluorescence modulation when analyte is bound. Competition methods, such as those used with antibodies, are also amenable to these synthetic receptors, yet there are few examples. In our laboratories, the use of common dyes in competition assays with small molecules has proven very effective. For example, an assay for citrate in beverages and an assay for the secondary messenger IP3 in cells have been developed. Another approach we have explored focuses on multi-analyte sensor arrays with attempt to mimic the mammalian sense of taste. Our system utilizes polymer resin beads with the desired sensors covalently attached. These functionalized microspheres are then immobilized into micromachined wells on a silicon chip thereby creating our taste buds. Exposure of the resin to analyte causes a change in the transmittance of the bead. This change can be fluorescent or colorimetric. Optical interrogation of the microspheres, by illuminating from one side of the wafer and collecting the signal on the other, results in an image. These data streams are collected using a CCD camera which creates red, green and blue (RGB) patterns that are distinct and reproducible for their environments. Analysis of this data can identify and quantify the analytes present.

Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil

PubMed Central

2013-01-01

Background The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil. Results The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94–106% in atomic absorption and 97–103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6–5.2% in atomic absorption, similar with that of 1.9–6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric methods for 95% confidence interval. Conclusions High-resolution continuum source flame atomic absorption spectrometry can be successfully used for the rapid, multielemental determination of hazardous/priority hazardous metals in soil with similar analytical performances to those in inductively coupled plasma optical emission spectrometry. PMID:23452327

Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil.

PubMed

Frentiu, Tiberiu; Ponta, Michaela; Hategan, Raluca

2013-03-01

The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil. The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94-106% in atomic absorption and 97-103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6-5.2% in atomic absorption, similar with that of 1.9-6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric methods for 95% confidence interval. High-resolution continuum source flame atomic absorption spectrometry can be successfully used for the rapid, multielemental determination of hazardous/priority hazardous metals in soil with similar analytical performances to those in inductively coupled plasma optical emission spectrometry.

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

An Assessment of Operational Energy Capability Improvement Fund (OECIF) Programs 17-S-2544

DTIC Science & Technology

2017-09-19

persistently attack key operational energy problems . OECIF themes are summarized in Table 1, and Appendix A includes more detail on the programs within... problems FY 2014 Analytical methods and tools FY 2015 Improving fuel economy for the current tactical ground fleet FY 2016 Increasing the operational...involve a variety of organizations to solve operational energy problems . In FY 2015, the OECIF program received a one-time $14.1M Congressional plus-up

A HISTORICAL PERSPECTIVE OF NUCLEAR THERMAL HYDRAULICS

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

D’Auria, F; Rohatgi, Upendra S.

The nuclear thermal-hydraulics discipline was developed following the needs for nuclear power plants (NPPs) and, to a more limited extent, research reactors (RR) design and safety. As in all other fields where analytical methods are involved, nuclear thermal-hydraulics took benefit of the development of computers. Thermodynamics, rather than fluid dynamics, is at the basis of the development of nuclear thermal-hydraulics together with the experiments in complex two-phase situations, namely, geometry, high thermal density, and pressure.

Modeling of the Global Water Cycle - Analytical Models

Treesearch

Yongqiang Liu; Roni Avissar

2005-01-01

Both numerical and analytical models of coupled atmosphere and its underlying ground components (land, ocean, ice) are useful tools for modeling the global and regional water cycle. Unlike complex three-dimensional climate models, which need very large computing resources and involve a large number of complicated interactions often difficult to interpret, analytical...

Estimation of Survival Probabilities for Use in Cost-effectiveness Analyses: A Comparison of a Multi-state Modeling Survival Analysis Approach with Partitioned Survival and Markov Decision-Analytic Modeling

PubMed Central

Williams, Claire; Lewsey, James D.; Mackay, Daniel F.; Briggs, Andrew H.

2016-01-01

Modeling of clinical-effectiveness in a cost-effectiveness analysis typically involves some form of partitioned survival or Markov decision-analytic modeling. The health states progression-free, progression and death and the transitions between them are frequently of interest. With partitioned survival, progression is not modeled directly as a state; instead, time in that state is derived from the difference in area between the overall survival and the progression-free survival curves. With Markov decision-analytic modeling, a priori assumptions are often made with regard to the transitions rather than using the individual patient data directly to model them. This article compares a multi-state modeling survival regression approach to these two common methods. As a case study, we use a trial comparing rituximab in combination with fludarabine and cyclophosphamide v. fludarabine and cyclophosphamide alone for the first-line treatment of chronic lymphocytic leukemia. We calculated mean Life Years and QALYs that involved extrapolation of survival outcomes in the trial. We adapted an existing multi-state modeling approach to incorporate parametric distributions for transition hazards, to allow extrapolation. The comparison showed that, due to the different assumptions used in the different approaches, a discrepancy in results was evident. The partitioned survival and Markov decision-analytic modeling deemed the treatment cost-effective with ICERs of just over £16,000 and £13,000, respectively. However, the results with the multi-state modeling were less conclusive, with an ICER of just over £29,000. This work has illustrated that it is imperative to check whether assumptions are realistic, as different model choices can influence clinical and cost-effectiveness results. PMID:27698003

Estimation of Survival Probabilities for Use in Cost-effectiveness Analyses: A Comparison of a Multi-state Modeling Survival Analysis Approach with Partitioned Survival and Markov Decision-Analytic Modeling.

PubMed

Williams, Claire; Lewsey, James D; Mackay, Daniel F; Briggs, Andrew H

2017-05-01

Modeling of clinical-effectiveness in a cost-effectiveness analysis typically involves some form of partitioned survival or Markov decision-analytic modeling. The health states progression-free, progression and death and the transitions between them are frequently of interest. With partitioned survival, progression is not modeled directly as a state; instead, time in that state is derived from the difference in area between the overall survival and the progression-free survival curves. With Markov decision-analytic modeling, a priori assumptions are often made with regard to the transitions rather than using the individual patient data directly to model them. This article compares a multi-state modeling survival regression approach to these two common methods. As a case study, we use a trial comparing rituximab in combination with fludarabine and cyclophosphamide v. fludarabine and cyclophosphamide alone for the first-line treatment of chronic lymphocytic leukemia. We calculated mean Life Years and QALYs that involved extrapolation of survival outcomes in the trial. We adapted an existing multi-state modeling approach to incorporate parametric distributions for transition hazards, to allow extrapolation. The comparison showed that, due to the different assumptions used in the different approaches, a discrepancy in results was evident. The partitioned survival and Markov decision-analytic modeling deemed the treatment cost-effective with ICERs of just over £16,000 and £13,000, respectively. However, the results with the multi-state modeling were less conclusive, with an ICER of just over £29,000. This work has illustrated that it is imperative to check whether assumptions are realistic, as different model choices can influence clinical and cost-effectiveness results.

Comparative Measurement of Microcystins in Diverse Surface ...

EPA Pesticide Factsheets

The measurement of microcystins, cyanotoxins associated with cyanobacterial blooms which are increasingly prevalent in inland waters, is complicated by the diversity of congeners which have been observed in the environment. At present, more than 150 microcystin congeners have been identified, and this poses a significant challenge to analytical methods intended to assess human health risks in surface and drinking water systems. The most widely employed analytical method at present is the ADDA-ELISA technique which is potentially sensitive to all microcystins, but it is primarily intended as a semi-quantitative method, and questions have been raised regarding the potential for cross-reactivity and false positives. LC-MS/MS methods targeting specific congeners, such as US EPA Method 544, are intended for use as a secondary confirmation following a positive ELISA response, but these techniques can target only those congeners for which commercial standards are available. Accordingly, they are not suitable for ascertaining the safety of a given water sample, given the potential for omitting unknown microcystin congeners which might be present.An alternative approach involves oxidative transformation of microcystins to a common product, 2-methyl-3-methoxy-4-phenylbutyric acid, or MMPB. Measuring MMPB by LC-MS/MS can potentially provide a metric for the sum of all microcystin congeners present in a sample, subject to the efficiency and overall yield of conversion. The

Simultaneous determination of brominated and phosphate flame retardants in flame-retarded polyester curtains by a novel extraction method.

PubMed

Miyake, Yuichi; Tokumura, Masahiro; Nakayama, Hayato; Wang, Qi; Amagai, Takashi; Ogo, Sayaka; Kume, Kazunari; Kobayashi, Takeshi; Takasu, Shinji; Ogawa, Kumiko; Kannan, Kurunthachalam

2017-12-01

The use of novel brominated flame retardants (BFRs) and phosphate-based flame retardants (PFRs) has increased as substitutes for hexabromocyclododecane (HBCD) in many consumer products. To facilitate collection of data on chemicals used as flame retardants in textiles and fabrics, we developed an analytical method using liquid chromatography interfaced with tandem mass spectrometry (LC-MS/MS). We compared two extraction methods, one involving ultrasonic extraction (traditional method) using dichloromethane, toluene or acetone and the other encompassing complete dissolution of textile with 25% 1,1,1,3,3,3-hexafluoro-2-propanol/chloroform. The dissolution method extracted up to 204 times more BFRs and PFRs than the traditional ultrasonic extraction. Tris(2,3-dibromopropyl) isocyanurate (TDBP-TAZTO), triphenylphosphine oxide (TPhPO), tris(1,3-dichloro-2-propyl) phosphate (TDCPP), tricresyl phosphate (TCsP), and triphenyl phosphate (TPhP) were found in 40 flame-retarded curtain samples purchased from Japanese market in 2014. TDBP-TAZTO was detected in polyester curtains for the first time. Some of the flame-retarded curtain samples did not contain any of the known target analytes, which suggested the presence of other unknown flame retardants in those fabrics. Copyright © 2017. Published by Elsevier B.V.

Comparative measurement of microcystins in diverse surface ...

EPA Pesticide Factsheets

The measurement of microcystins, cyanotoxins associated with cyanobacterial blooms which are increasingly prevalent in inland waters, is complicated by the diversity of congeners which have been observed in the environment. At present, more than 150 microcystin congeners have been identified, and this poses a significant challenge to analytical methods intended to assess human health risks in surface and drinking water systems. The most widely employed analytical method at present is the ADDA-ELISA technique which is potentially sensitive to all microcystins, but it is primarily intended as a semi-quantitative method, and questions have been raised regarding the potential for cross-reactivity and false positives. LC-MS/MS methods targeting specific congeners, such as US EPA Method 544, are intended for use as a secondary confirmation following a positive ELISA response, but these techniques can target only those congeners for which commercial standards are available. Accordingly, they not suitable for ascertaining the safety of a given water sample, given the potential for omitting unknown microcystin congeners which might be present.An alternative approach involves oxidative transformation of microcystins to a common product, 2-methyl-3-methoxy-4-phenylbutyric acid, or MMPB. Measuring MMPB by LC-MS/MS can potentially provide a metric for the sum of all microcystin congeners present in a sample, subject to the efficiency and overall yield of conversion. The pres

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.

Hydrogen sulfide measurement using sulfide dibimane: critical evaluation with electrospray ion trap mass spectrometry

PubMed Central

Shen, Xinggui; Chakraborty, Sourav; Dugas, Tammy R; Kevil, Christopher G

2015-01-01

Accurate measurement of hydrogen sulfide bioavailability remains a technical challenge due to numerous issues involving sample processing, detection methods used, and actual biochemical products measured. Our group and others have reported that reverse phase HPLC detection of sulfide dibimane (SDB) product from the reaction of H2S/HS− with monobromobimane allows for analytical detection of hydrogen sulfide bioavailability in free and other biochemical forms. However, it remains unclear whether possible interfering contaminants may contribute to HPLC SDB peak readings that may result in inaccurate measurements of bioavailable sulfide. In this study, we critically compared hydrogen sulfide dependent SDB detection using reverse phase HPLC (RP-HPLC) versus quantitative SRM electrospray ionization mass spectrometry (ESI/MS) to obtain greater clarity into the validity of the reverse phase HPLC method for analytical measurement of hydrogen sulfide. Using an LCQ-deca ion-trap mass spectrometer, SDB was identified by ESI/MS positive ion mode, and quantified by selected reaction monitoring (SRM) using hydrocortisone as an internal standard. Collision induced dissociation (CID) parameters were optimized at MS2 level for SDB and hydrocortisone. ESI/MS detection of SDB standard was found to be a log order more sensitive than RP-HPLC with a lower limit of 0.25 nM. Direct comparison of tissue and plasma SDB levels using RP-HPLC and ESI/MS methods revealed comparable sulfide levels in plasma, aorta, heart, lung and brain. Together, these data confirm the use of SDB as valid indicator of H2S bioavailability and highlights differences between analytical detection methods. PMID:24932544

Innovations in coating technology.

PubMed

Behzadi, Sharareh S; Toegel, Stefan; Viernstein, Helmut

2008-01-01

Despite representing one of the oldest pharmaceutical techniques, coating of dosage forms is still frequently used in pharmaceutical manufacturing. The aims of coating range from simply masking the taste or odour of drugs to the sophisticated controlling of site and rate of drug release. The high expectations for different coating technologies have required great efforts regarding the development of reproducible and controllable production processes. Basically, improvements in coating methods have focused on particle movement, spraying systems, and air and energy transport. Thereby, homogeneous distribution of coating material and increased drying efficiency should be accomplished in order to achieve high end product quality. Moreover, given the claim of the FDA to design the end product quality already during the manufacturing process (Quality by Design), the development of analytical methods for the analysis, management and control of coating processes has attracted special attention during recent years. The present review focuses on recent patents claiming improvements in pharmaceutical coating technology and intends to first familiarize the reader with the available procedures and to subsequently explain the application of different analytical tools. Aiming to structure this comprehensive field, coating technologies are primarily divided into pan and fluidized bed coating methods. Regarding pan coating procedures, pans rotating around inclined, horizontal and vertical axes are reviewed separately. On the other hand, fluidized bed technologies are subdivided into those involving fluidized and spouted beds. Then, continuous processing techniques and improvements in spraying systems are discussed in dedicated chapters. Finally, currently used analytical methods for the understanding and management of coating processes are reviewed in detail in the last section of the review.

Shape optimization using a NURBS-based interface-enriched generalized FEM

DOE PAGES

Najafi, Ahmad R.; Safdari, Masoud; Tortorelli, Daniel A.; ...

2016-11-26

This study presents a gradient-based shape optimization over a fixed mesh using a non-uniform rational B-splines-based interface-enriched generalized finite element method, applicable to multi-material structures. In the proposed method, non-uniform rational B-splines are used to parameterize the design geometry precisely and compactly by a small number of design variables. An analytical shape sensitivity analysis is developed to compute derivatives of the objective and constraint functions with respect to the design variables. Subtle but important new terms involve the sensitivity of shape functions and their spatial derivatives. As a result, verification and illustrative problems are solved to demonstrate the precision andmore » capability of the method.« less

Statistical methods for astronomical data with upper limits. I - Univariate distributions

NASA Technical Reports Server (NTRS)

Feigelson, E. D.; Nelson, P. I.

1985-01-01

The statistical treatment of univariate censored data is discussed. A heuristic derivation of the Kaplan-Meier maximum-likelihood estimator from first principles is presented which results in an expression amenable to analytic error analysis. Methods for comparing two or more censored samples are given along with simple computational examples, stressing the fact that most astronomical problems involve upper limits while the standard mathematical methods require lower limits. The application of univariate survival analysis to six data sets in the recent astrophysical literature is described, and various aspects of the use of survival analysis in astronomy, such as the limitations of various two-sample tests and the role of parametric modelling, are discussed.

Site-resolved multiple-quantum filtered correlations and distance measurements by magic-angle spinning NMR: Theory and applications to spins with weak to vanishing quadrupolar couplings

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

Eliav, U., E-mail: amirgo@tau.ac.il, E-mail: eliav@tau.ac.il; Haimovich, A.; Goldbourt, A., E-mail: amirgo@tau.ac.il, E-mail: eliav@tau.ac.il

2016-01-14

We discuss and analyze four magic-angle spinning solid-state NMR methods that can be used to measure internuclear distances and to obtain correlation spectra between a spin I = 1/2 and a half-integer spin S > 1/2 having a small quadrupolar coupling constant. Three of the methods are based on the heteronuclear multiple-quantum and single-quantum correlation experiments, that is, high rank tensors that involve the half spin and the quadrupolar spin are generated. Here, both zero and single-quantum coherence of the half spins are allowed and various coherence orders of the quadrupolar spin are generated, and filtered, via active recoupling ofmore » the dipolar interaction. As a result of generating coherence orders larger than one, the spectral resolution for the quadrupolar nucleus increases linearly with the coherence order. Since the formation of high rank tensors is independent of the existence of a finite quadrupolar interaction, these experiments are also suitable to materials in which there is high symmetry around the quadrupolar spin. A fourth experiment is based on the initial quadrupolar-driven excitation of symmetric high order coherences (up to p = 2S, where S is the spin number) and subsequently generating by the heteronuclear dipolar interaction higher rank (l + 1 or higher) tensors that involve also the half spins. Due to the nature of this technique, it also provides information on the relative orientations of the quadrupolar and dipolar interaction tensors. For the ideal case in which the pulses are sufficiently strong with respect to other interactions, we derive analytical expressions for all experiments as well as for the transferred echo double resonance experiment involving a quadrupolar spin. We show by comparison of the fitting of simulations and the analytical expressions to experimental data that the analytical expressions are sufficiently accurate to provide experimental {sup 7}Li–{sup 13}C distances in a complex of lithium, glycine, and water. Discussion of the regime for which such an approach is valid is given.« less

Laboratory Workhorse: The Analytical Balance.

ERIC Educational Resources Information Center

Clark, Douglas W.

1979-01-01

This report explains the importance of various analytical balances in the water or wastewater laboratory. Stressed is the proper procedure for utilizing the equipment as well as the mechanics involved in its operation. (CS)

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…

Extended method of moments for deterministic analysis of stochastic multistable neurodynamical systems

NASA Astrophysics Data System (ADS)

Deco, Gustavo; Martí, Daniel

2007-03-01

The analysis of transitions in stochastic neurodynamical systems is essential to understand the computational principles that underlie those perceptual and cognitive processes involving multistable phenomena, like decision making and bistable perception. To investigate the role of noise in a multistable neurodynamical system described by coupled differential equations, one usually considers numerical simulations, which are time consuming because of the need for sufficiently many trials to capture the statistics of the influence of the fluctuations on that system. An alternative analytical approach involves the derivation of deterministic differential equations for the moments of the distribution of the activity of the neuronal populations. However, the application of the method of moments is restricted by the assumption that the distribution of the state variables of the system takes on a unimodal Gaussian shape. We extend in this paper the classical moments method to the case of bimodal distribution of the state variables, such that a reduced system of deterministic coupled differential equations can be derived for the desired regime of multistability.

Stakeholder participation in comparative effectiveness research: defining a framework for effective engagement

PubMed Central

Deverka, Patricia A; Lavallee, Danielle C; Desai, Priyanka J; Esmail, Laura C; Ramsey, Scott D; Veenstra, David L; Tunis, Sean R

2012-01-01

Aims Stakeholder engagement is fundamental to comparative effectiveness research (CER), but lacks consistent terminology. This paper aims to define stakeholder engagement and present a conceptual model for involving stakeholders in CER. Materials & methods The definitions and model were developed from a literature search, expert input and experience with the Center for Comparative Effectiveness Research in Cancer Genomics, a proof-of-concept platform for stakeholder involvement in priority setting and CER study design. Results Definitions for stakeholder and stakeholder engagement reflect the target constituencies and their role in CER. The ‘analytic-deliberative’ conceptual model for stakeholder engagement illustrates the inputs, methods and outputs relevant to CER. The model differentiates methods at each stage of the project; depicts the relationship between components; and identifies outcome measures for evaluation of the process. Conclusion While the definitions and model require testing before being broadly adopted, they are an important foundational step and will be useful for investigators, funders and stakeholder groups interested in contributing to CER. PMID:22707880

Stakeholder participation in comparative effectiveness research: defining a framework for effective engagement.

PubMed

Deverka, Patricia A; Lavallee, Danielle C; Desai, Priyanka J; Esmail, Laura C; Ramsey, Scott D; Veenstra, David L; Tunis, Sean R

2012-03-01

AIMS: Stakeholder engagement is fundamental to comparative effectiveness research (CER), but lacks consistent terminology. This paper aims to define stakeholder engagement and present a conceptual model for involving stakeholders in CER. MATERIALS #ENTITYSTARTX00026; METHODS: The definitions and model were developed from a literature search, expert input and experience with the Center for Comparative Effectiveness Research in Cancer Genomics, a proof-of-concept platform for stakeholder involvement in priority setting and CER study design. RESULTS: Definitions for stakeholder and stakeholder engagement reflect the target constituencies and their role in CER. The 'analytic-deliberative' conceptual model for stakeholder engagement illustrates the inputs, methods and outputs relevant to CER. The model differentiates methods at each stage of the project; depicts the relationship between components; and identifies outcome measures for evaluation of the process. CONCLUSION: While the definitions and model require testing before being broadly adopted, they are an important foundational step and will be useful for investigators, funders and stakeholder groups interested in contributing to CER.

Fast quantification of bovine milk proteins employing external cavity-quantum cascade laser spectroscopy.

PubMed

Schwaighofer, Andreas; Kuligowski, Julia; Quintás, Guillermo; Mayer, Helmut K; Lendl, Bernhard

2018-06-30

Analysis of proteins in bovine milk is usually tackled by time-consuming analytical approaches involving wet-chemical, multi-step sample clean-up procedures. The use of external cavity-quantum cascade laser (EC-QCL) based IR spectroscopy was evaluated as an alternative screening tool for direct and simultaneous quantification of individual proteins (i.e. casein and β-lactoglobulin) and total protein content in commercial bovine milk samples. Mid-IR spectra of protein standard mixtures were used for building partial least squares (PLS) regression models. A sample set comprising different milk types (pasteurized; differently processed extended shelf life, ESL; ultra-high temperature, UHT) was analysed and results were compared to reference methods. Concentration values of the QCL-IR spectroscopy approach obtained within several minutes are in good agreement with reference methods involving multiple sample preparation steps. The potential application as a fast screening method for estimating the heat load applied to liquid milk is demonstrated. Copyright © 2018 Elsevier Ltd. All rights reserved.

Development of an analytical method for polycyclic aromatic hydrocarbons in coffee beverages and dark beer using novel high-sensitivity technique of supercritical fluid chromatography/mass spectrometry.

PubMed

Yoshioka, Toshiaki; Nagatomi, Yasushi; Harayama, Koichi; Bamba, Takeshi

2018-07-01

Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic substances that are mainly generated during heating in food; therefore, the European Union (EU) has regulated the amount of benzo[a]pyrene and PAH4 in various types of food. In addition, the Scientific Committee on Food of the EU and the Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives have recommended that 16 PAHs should be monitored. Since coffee beverages and dark beer are roasted during manufacture, monitoring these 16 PAHs is of great importance. On the other hand, supercritical fluid chromatography (SFC) is a separation method that has garnered attention in recent years as a complement for liquid and gas chromatography. Therefore, we developed a rapid high-sensitivity analytical method for the above-mentioned 16 PAHs in coffee beverages and dark beer involving supercritical fluid chromatography/atmospheric pressure chemical ionization-mass spectrometry (SFC/APCI-MS) and simple sample preparation. In this study, we developed a novel analytical technique that increased the sensitivity of MS detection by varying the back-pressure in SFC depending on the elution of PAHs. In addition, analysis of commercially available coffee and dark beer samples in Japan showed that the risk of containing the 16 PAHs may be low. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Automatic-heuristic and executive-analytic processing during reasoning: Chronometric and dual-task considerations.

PubMed

De Neys, Wim

2006-06-01

Human reasoning has been shown to overly rely on intuitive, heuristic processing instead of a more demanding analytic inference process. Four experiments tested the central claim of current dual-process theories that analytic operations involve time-consuming executive processing whereas the heuristic system would operate automatically. Participants solved conjunction fallacy problems and indicative and deontic selection tasks. Experiment 1 established that making correct analytic inferences demanded more processing time than did making heuristic inferences. Experiment 2 showed that burdening the executive resources with an attention-demanding secondary task decreased correct, analytic responding and boosted the rate of conjunction fallacies and indicative matching card selections. Results were replicated in Experiments 3 and 4 with a different secondary-task procedure. Involvement of executive resources for the deontic selection task was less clear. Findings validate basic processing assumptions of the dual-process framework and complete the correlational research programme of K. E. Stanovich and R. F. West (2000).

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.

A new method for designing dual foil electron beam forming systems. I. Introduction, concept of the method

NASA Astrophysics Data System (ADS)

Adrich, Przemysław

2016-05-01

In Part I of this work existing methods and problems in dual foil electron beam forming system design are presented. On this basis, a new method of designing these systems is introduced. The motivation behind this work is to eliminate the shortcomings of the existing design methods and improve overall efficiency of the dual foil design process. The existing methods are based on approximate analytical models applied in an unrealistically simplified geometry. Designing a dual foil system with these methods is a rather labor intensive task as corrections to account for the effects not included in the analytical models have to be calculated separately and accounted for in an iterative procedure. To eliminate these drawbacks, the new design method is based entirely on Monte Carlo modeling in a realistic geometry and using physics models that include all relevant processes. In our approach, an optimal configuration of the dual foil system is found by means of a systematic, automatized scan of the system performance in function of parameters of the foils. The new method, while being computationally intensive, minimizes the involvement of the designer and considerably shortens the overall design time. The results are of high quality as all the relevant physics and geometry details are naturally accounted for. To demonstrate the feasibility of practical implementation of the new method, specialized software tools were developed and applied to solve a real life design problem, as described in Part II of this work.

A study of prediction methods for the high angle-of-attack aerodynamics of straight wings and fighter aircraft

NASA Technical Reports Server (NTRS)

Mcmillan, O. J.; Mendenhall, M. R.; Perkins, S. C., Jr.

1984-01-01

Work is described dealing with two areas which are dominated by the nonlinear effects of vortex flows. The first area concerns the stall/spin characteristics of a general aviation wing with a modified leading edge. The second area concerns the high-angle-of-attack characteristics of high performance military aircraft. For each area, the governing phenomena are described as identified with the aid of existing experimental data. Existing analytical methods are reviewed, and the most promising method for each area used to perform some preliminary calculations. Based on these results, the strengths and weaknesses of the methods are defined, and research programs recommended to improve the methods as a result of better understanding of the flow mechanisms involved.

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.

Non-detonable and non-explosive explosive simulators

DOEpatents

Simpson, R.L.; Pruneda, C.O.

1997-07-15

A simulator which is chemically equivalent to an explosive, but is not detonable or explodable is disclosed. The simulator is a combination of an explosive material with an inert material, either in a matrix or as a coating, where the explosive has a high surface ratio but small volume ratio. The simulator has particular use in the training of explosives detecting dogs, calibrating analytical instruments which are sensitive to either vapor or elemental composition, or other applications where the hazards associated with explosives is undesirable but where chemical and/or elemental equivalence is required. The explosive simulants may be fabricated by different techniques. A first method involves the use of standard slurry coatings to produce a material with a very high binder to explosive ratio without masking the explosive vapor, and a second method involves coating inert substrates with thin layers of explosive. 11 figs.

Protecting privacy of shared epidemiologic data without compromising analysis potential.

PubMed

Cologne, John; Grant, Eric J; Nakashima, Eiji; Chen, Yun; Funamoto, Sachiyo; Katayama, Hiroaki

2012-01-01

Ensuring privacy of research subjects when epidemiologic data are shared with outside collaborators involves masking (modifying) the data, but overmasking can compromise utility (analysis potential). Methods of statistical disclosure control for protecting privacy may be impractical for individual researchers involved in small-scale collaborations. We investigated a simple approach based on measures of disclosure risk and analytical utility that are straightforward for epidemiologic researchers to derive. The method is illustrated using data from the Japanese Atomic-bomb Survivor population. Masking by modest rounding did not adequately enhance security but rounding to remove several digits of relative accuracy effectively reduced the risk of identification without substantially reducing utility. Grouping or adding random noise led to noticeable bias. When sharing epidemiologic data, it is recommended that masking be performed using rounding. Specific treatment should be determined separately in individual situations after consideration of the disclosure risks and analysis needs.

Electrochemical study of ricin at glassy carbon electrode.

PubMed

Ribeiro, Williame F; da Costa, Daniel J E; Lourenço, Anabel S; Lopes, Ilanna C; de Medeiros, Everaldo P; Salazar-Banda, Giancarlo R; do Nascimento, Valberes B; de Araújo, Mário C U

2013-08-21

Ricin, Ricinus communis agglutinin 60 - RCA 60, is a deadly phytotoxic protein which inhibits ribosomes (class II), and there is no known effective antidote in living organisms. Ricin is composed of two polypeptide chains, A and B, linked covalently by a single disulfide bond. The analytical methods for the detection of RCA 60 are commonly laborious, expensive, require skilled labor, and involve sophisticated equipment. Aimed at the development of electroanalytical methods for RCA 60 detection, here we studied the electrochemical oxidation of RCA 60 on a glassy carbon (GC) electrode over a wide pH range, using cyclic voltammetry, differential pulse voltammetry (DPV) and square wave voltammetry (SWV). Two quasi-reversible electrochemical RCA 60 oxidation peaks were identified on the GC electrode by SWV. For values of 2.2 ≤ pH ≤ 10.2, DPV studies revealed that the peak potentials, EP1 and EP2, display a linear dependence with pH and the reaction mechanism involves the transfer of 2H⁺/2e⁻ (peak 1) and 1H⁺/1e⁻ (peak 2). The first and second RCA 60 oxidation steps may correspond to the oxidation of cysteine and tyrosine-tryptophan residues, respectively. The oxidation product of the second RCA 60 oxidation step appears at 7.0 ≤ pH ≤ 11.8. For pH ≥ 10.2, both processes are pH independent, resulting in a pKa of ca. 10.2. A third RCA 60 oxidation peak only appears at acidic pH. RCA 60 samples extracted from different castor seed cultivars showed similar electrochemical behavior, enabling the implementation of an analytical voltammetric method.

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.

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 ...

Multi-criteria clinical decision support: A primer on the use of multiple criteria decision making methods to promote evidence-based, patient-centered healthcare.

PubMed

Dolan, James G

2010-01-01

Current models of healthcare quality recommend that patient management decisions be evidence-based and patient-centered. Evidence-based decisions require a thorough understanding of current information regarding the natural history of disease and the anticipated outcomes of different management options. Patient-centered decisions incorporate patient preferences, values, and unique personal circumstances into the decision making process and actively involve both patients along with health care providers as much as possible. Fundamentally, therefore, evidence-based, patient-centered decisions are multi-dimensional and typically involve multiple decision makers.Advances in the decision sciences have led to the development of a number of multiple criteria decision making methods. These multi-criteria methods are designed to help people make better choices when faced with complex decisions involving several dimensions. They are especially helpful when there is a need to combine "hard data" with subjective preferences, to make trade-offs between desired outcomes, and to involve multiple decision makers. Evidence-based, patient-centered clinical decision making has all of these characteristics. This close match suggests that clinical decision support systems based on multi-criteria decision making techniques have the potential to enable patients and providers to carry out the tasks required to implement evidence-based, patient-centered care effectively and efficiently in clinical settings.The goal of this paper is to give readers a general introduction to the range of multi-criteria methods available and show how they could be used to support clinical decision-making. Methods discussed include the balance sheet, the even swap method, ordinal ranking methods, direct weighting methods, multi-attribute decision analysis, and the analytic hierarchy process (AHP).

Multi-criteria clinical decision support: A primer on the use of multiple criteria decision making methods to promote evidence-based, patient-centered healthcare

PubMed Central

Dolan, James G.

2010-01-01

Current models of healthcare quality recommend that patient management decisions be evidence-based and patient-centered. Evidence-based decisions require a thorough understanding of current information regarding the natural history of disease and the anticipated outcomes of different management options. Patient-centered decisions incorporate patient preferences, values, and unique personal circumstances into the decision making process and actively involve both patients along with health care providers as much as possible. Fundamentally, therefore, evidence-based, patient-centered decisions are multi-dimensional and typically involve multiple decision makers. Advances in the decision sciences have led to the development of a number of multiple criteria decision making methods. These multi-criteria methods are designed to help people make better choices when faced with complex decisions involving several dimensions. They are especially helpful when there is a need to combine “hard data” with subjective preferences, to make trade-offs between desired outcomes, and to involve multiple decision makers. Evidence-based, patient-centered clinical decision making has all of these characteristics. This close match suggests that clinical decision support systems based on multi-criteria decision making techniques have the potential to enable patients and providers to carry out the tasks required to implement evidence-based, patient-centered care effectively and efficiently in clinical settings. The goal of this paper is to give readers a general introduction to the range of multi-criteria methods available and show how they could be used to support clinical decision-making. Methods discussed include the balance sheet, the even swap method, ordinal ranking methods, direct weighting methods, multi-attribute decision analysis, and the analytic hierarchy process (AHP) PMID:21394218

Evaluation of the matrix exponential for use in ground-water-flow and solute-transport simulations; theoretical framework

USGS Publications Warehouse

Umari, A.M.; Gorelick, S.M.

1986-01-01

It is possible to obtain analytic solutions to the groundwater flow and solute transport equations if space variables are discretized but time is left continuous. From these solutions, hydraulic head and concentration fields for any future time can be obtained without ' marching ' through intermediate time steps. This analytical approach involves matrix exponentiation and is referred to as the Matrix Exponential Time Advancement (META) method. Two algorithms are presented for the META method, one for symmetric and the other for non-symmetric exponent matrices. A numerical accuracy indicator, referred to as the matrix condition number, was defined and used to determine the maximum number of significant figures that may be lost in the META method computations. The relative computational and storage requirements of the META method with respect to the time marching method increase with the number of nodes in the discretized problem. The potential greater accuracy of the META method and the associated greater reliability through use of the matrix condition number have to be weighed against this increased relative computational and storage requirements of this approach as the number of nodes becomes large. For a particular number of nodes, the META method may be computationally more efficient than the time-marching method, depending on the size of time steps used in the latter. A numerical example illustrates application of the META method to a sample ground-water-flow problem. (Author 's abstract)

How Qualitative Methods Can be Used to Inform Model Development.

PubMed

Husbands, Samantha; Jowett, Susan; Barton, Pelham; Coast, Joanna

2017-06-01

Decision-analytic models play a key role in informing healthcare resource allocation decisions. However, there are ongoing concerns with the credibility of models. Modelling methods guidance can encourage good practice within model development, but its value is dependent on its ability to address the areas that modellers find most challenging. Further, it is important that modelling methods and related guidance are continually updated in light of any new approaches that could potentially enhance model credibility. The objective of this article was to highlight the ways in which qualitative methods have been used and recommended to inform decision-analytic model development and enhance modelling practices. With reference to the literature, the article discusses two key ways in which qualitative methods can be, and have been, applied. The first approach involves using qualitative methods to understand and inform general and future processes of model development, and the second, using qualitative techniques to directly inform the development of individual models. The literature suggests that qualitative methods can improve the validity and credibility of modelling processes by providing a means to understand existing modelling approaches that identifies where problems are occurring and further guidance is needed. It can also be applied within model development to facilitate the input of experts to structural development. We recommend that current and future model development would benefit from the greater integration of qualitative methods, specifically by studying 'real' modelling processes, and by developing recommendations around how qualitative methods can be adopted within everyday modelling practice.

A continuous latitudinal energy balance model to explore non-uniform climate engineering strategies

NASA Astrophysics Data System (ADS)

Bonetti, F.; McInnes, C. R.

2016-12-01

Current concentrations of atmospheric CO2 exceed measured historical levels in modern times, largely attributed to anthropogenic forcing since the industrial revolution. The required decline in emissions rates has never been achieved leading to recent interest in climate engineering for future risk-mitigation strategies. Climate engineering aims to offset human-driven climate change. It involves techniques developed both to reduce the concentration of CO2 in the atmosphere (Carbon Dioxide Removal (CDR) methods) and to counteract the radiative forcing that it generates (Solar Radiation Management (SRM) methods). In order to investigate effects of SRM technologies for climate engineering, an analytical model describing the main dynamics of the Earth's climate has been developed. The model is a time-dependent Energy Balance Model (EBM) with latitudinal resolution and allows for the evaluation of non-uniform climate engineering strategies. A significant disadvantage of climate engineering techniques involving the management of solar radiation is regional disparities in cooling. This model offers an analytical approach to design multi-objective strategies that counteract climate change on a regional basis: for example, to cool the Artic and restrict undesired impacts at mid-latitudes, or to control the equator-to-pole temperature gradient. Using the Green's function approach the resulting partial differential equation allows for the computation of the surface temperature as a function of time and latitude when a 1% per year increase in the CO2 concentration is considered. After the validation of the model through comparisons with high fidelity numerical models, it will be used to explore strategies for the injection of the aerosol precursors in the stratosphere. In particular, the model involves detailed description of the optical properties of the particles, the wash-out dynamics and the estimation of the radiative cooling they can generate.

A three-time-point method for assessing kinetic parameters of 64Cu-labeled Ramucirumab trapping in VEGFR-2 positive lung tumors.

PubMed

Laffon, Eric; Marthan, Roger

2017-11-01

To describe a three-time-point method for estimating kinetic parameters involved in 64 Cu-labeled Ramucirumab ( 64 Cu-NOTA-RamAb) trapping of VEGFR-2 positive lung tumors. Positron emission tomography (microPET) data of tumor-bearing mice for 64 Cu-NOTA-RamAb trapping in VEGFR-2 positive HCC4006 tumor were used, involving tissue activity measurements acquired at 3, 24 and 48 h post-injection, without and with administration of RamAb blocking dose. A kinetic model provided an analytical formula describing the tissue time-activity-curve, involving 64 Cu-NOTA-RamAb uptake (Ki), release rate constant (k R ) and fraction of free tracer in blood and interstitial volume (F). Fitting analytical formula outcomes on mean microPET data yielded values of the kinetic parameters: Ki = 0.0314/0.0123 gram of blood per hour per gram of tissue, k R  = 0.0387/0.0313 h -1 and F = 0.2075/0.2007 gram of blood per gram of tissue, without/with RamAb blocking dose, respectively (R = 0.99999 for the graph displaying microPET versus theoretical data; P < .01). Three independent kinetic parameters (Ki, k R and F) can be assessed from three data points acquired at early, mid and late imaging, i.e., at 3, 24 and 48 h post-injection, for further characterization of 64 Cu-NOTA-RamAb trapping in VEGFR-2 positive lung tumors. Copyright © 2017 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

Aberrant Gene Expression in Humans

PubMed Central

Yang, Ence; Ji, Guoli; Brinkmeyer-Langford, Candice L.; Cai, James J.

2015-01-01

Gene expression as an intermediate molecular phenotype has been a focus of research interest. In particular, studies of expression quantitative trait loci (eQTL) have offered promise for understanding gene regulation through the discovery of genetic variants that explain variation in gene expression levels. Existing eQTL methods are designed for assessing the effects of common variants, but not rare variants. Here, we address the problem by establishing a novel analytical framework for evaluating the effects of rare or private variants on gene expression. Our method starts from the identification of outlier individuals that show markedly different gene expression from the majority of a population, and then reveals the contributions of private SNPs to the aberrant gene expression in these outliers. Using population-scale mRNA sequencing data, we identify outlier individuals using a multivariate approach. We find that outlier individuals are more readily detected with respect to gene sets that include genes involved in cellular regulation and signal transduction, and less likely to be detected with respect to the gene sets with genes involved in metabolic pathways and other fundamental molecular functions. Analysis of polymorphic data suggests that private SNPs of outlier individuals are enriched in the enhancer and promoter regions of corresponding aberrantly-expressed genes, suggesting a specific regulatory role of private SNPs, while the commonly-occurring regulatory genetic variants (i.e., eQTL SNPs) show little evidence of involvement. Additional data suggest that non-genetic factors may also underlie aberrant gene expression. Taken together, our findings advance a novel viewpoint relevant to situations wherein common eQTLs fail to predict gene expression when heritable, rare inter-individual variation exists. The analytical framework we describe, taking into consideration the reality of differential phenotypic robustness, may be valuable for investigating complex traits and conditions. PMID:25617623

Linear perturbations of a Schwarzschild blackhole by thin disc - convergence

NASA Astrophysics Data System (ADS)

Čížek, P.; Semerák, O.

2012-07-01

In order to find the perturbation of a Schwarzschild space-time due to a rotating thin disc, we try to adjust the method used by [4] in the case of perturbation by a one-dimensional ring. This involves solution of stationary axisymmetric Einstein's equations in terms of spherical-harmonic expansions whose convergence however turned out questionable in numerical examples. Here we show, analytically, that the series are almost everywhere convergent, but in some regions the convergence is not absolute.

Analysis of combustion instability in liquid fuel rocket motors. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Wong, K. W.

1979-01-01

The development of an analytical technique used in the solution of nonlinear velocity-sensitive combustion instability problems is presented. The Galerkin method was used and proved successful. The pressure wave forms exhibit a strong second harmonic distortion and a variety of behaviors are possible depending on the nature of the combustion process and the parametric values involved. A one dimensional model provides insight into the problem by allowing a comparison of Galerkin solutions with more exact finite difference computations.

Fatigue and fracture: Overview

NASA Technical Reports Server (NTRS)

Halford, G. R.

1984-01-01

A brief overview of the status of the fatigue and fracture programs is given. The programs involve the development of appropriate analytic material behavior models for cyclic stress-strain-temperature-time/cyclic crack initiation, and cyclic crack propagation. The underlying thrust of these programs is the development and verification of workable engineering methods for the calculation, in advance of service, of the local cyclic stress-strain response at the critical life governing location in hot section compounds, and the resultant crack initiation and crack growth lifetimes.

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...

Determination of alpidem, an imidazopyridine anxiolytic, and its metabolites by column-switching high-performance liquid chromatography with fluorescence detection.

PubMed

Flaminio, L; Ripamonti, M; Ascalone, V

1994-05-13

Alpidem, 6-chloro-2-(4-chlorophenyl)-N,N-dipropylimidazo[1,2-a]pyridine- 3-acetamide, is an anxiolytic imidazopyridine that undergoes a first-pass elimination after oral administration to humans; it is actively metabolized and three circulating metabolites have been identified in plasma due to N-dealkylation, oxidation or a combination of both processes. For the determination of the unchanged drug and its metabolites in human plasma, a column-switching HPLC method was developed. The method, based on solid-phase extraction (performed on-line), involves the automatic injection of plasma samples (200 microliters) on to a precolumn filled with C18 material, clean-up of the sample with water in order to remove protein and salts and transfer of the analytes to the analytical column (after valve switching) by means of the mobile phase. All the processes were performed in the presence of an internal standard, a compound chemically related to alpidem. During the analytical chromatography, the precolumn was flushed with different solvents and after regeneration with water, it was ready for further injections. The analytical column was a C8 type and the mobile phase was acetonitrile-methanol-phosphate buffer solution (45:15:45, v/v/v) at a flow-rate of 1.5 ml min-1. The column was connected to a fluorimetric detector operating at excitation and emission wavelengths of 255 and 423 nm, respectively. The limits of quantitation of alpidem and three metabolites were 2.5 and 1.5 ng ml-1, respectively, in human plasma.

The development of a change model of "exits" during cognitive analytic therapy for the treatment of depression.

PubMed

Sandhu, Sundeep Kaur; Kellett, Stephen; Hardy, Gillian

2017-11-01

"Exits" in cognitive analytic therapy (CAT) are methods that change unhelpful patterns or roles during the final "revision" phase of the therapy. How exits are conceived and achieved is currently poorly understood. This study focussed on the revision stage to explore and define how change is accomplished in CAT. Qualitative content analysis studied transcripts of sessions 6 and 7 of a protocol delivered 8-session CAT treatment for depression. Eight participants met the study inclusion criteria, and therefore, 16 sessions were analysed. The exit model developed contained 3 distinct (but interacting) phases: (a) developing an observing self via therapist input or client self-reflection, (b) breaking out of old patterns by creating new roles and procedures, and (c) utilisation of a range of methods to support and maintain change. Levels of interrater reliability for the exit categories that formed the model were good. The revision stage of CAT emerged as a complex and dynamic process involving 3 interacting stages. Further research is recommended to understand how exits relate to durability of change and whether change processes differ according to presenting problem. Exit work in cognitive analytic therapy is a dynamic process that requires progression through stages of insight, active change, and consolidation. Development of an "observing self" is an important foundation stone for change, and cognitive analytic therapists need to work within the client's zone of proximal development. A number of aspects appear important in facilitating change, such as attending to the process and feelings generated by change talk. Copyright © 2017 John Wiley & Sons, Ltd.

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.

Multivariate analysis of progressive thermal desorption coupled gas chromatography-mass spectrometry.

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

Van Benthem, Mark Hilary; Mowry, Curtis Dale; Kotula, Paul Gabriel

Thermal decomposition of poly dimethyl siloxane compounds, Sylgard{reg_sign} 184 and 186, were examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a method of producing multiway data using a stepped thermal desorption. The technique involves sequentially heating a sample of the material of interest with subsequent analysis in a commercial GC/MS system. The decomposition chromatograms were analyzed using multivariate analysis tools including principal component analysis (PCA), factor rotation employing the varimax criterion, and multivariate curve resolution. The results of the analysis show seven components related to offgassing of various fractions of siloxanes that varymore » as a function of temperature. Thermal desorption coupled with gas chromatography-mass spectrometry (TD/GC-MS) is a powerful analytical technique for analyzing chemical mixtures. It has great potential in numerous analytic areas including materials analysis, sports medicine, in the detection of designer drugs; and biological research for metabolomics. Data analysis is complicated, far from automated and can result in high false positive or false negative rates. We have demonstrated a step-wise TD/GC-MS technique that removes more volatile compounds from a sample before extracting the less volatile compounds. This creates an additional dimension of separation before the GC column, while simultaneously generating three-way data. Sandia's proven multivariate analysis methods, when applied to these data, have several advantages over current commercial options. It also has demonstrated potential for success in finding and enabling identification of trace compounds. Several challenges remain, however, including understanding the sources of noise in the data, outlier detection, improving the data pretreatment and analysis methods, developing a software tool for ease of use by the chemist, and demonstrating our belief that this multivariate analysis will enable superior differentiation capabilities. In addition, noise and system artifacts challenge the analysis of GC-MS data collected on lower cost equipment, ubiquitous in commercial laboratories. This research has the potential to affect many areas of analytical chemistry including materials analysis, medical testing, and environmental surveillance. It could also provide a method to measure adsorption parameters for chemical interactions on various surfaces by measuring desorption as a function of temperature for mixtures. We have presented results of a novel method for examining offgas products of a common PDMS material. Our method involves utilizing a stepped TD/GC-MS data acquisition scheme that may be almost totally automated, coupled with multivariate analysis schemes. This method of data generation and analysis can be applied to a number of materials aging and thermal degradation studies.« less

LC-MS/MS-based quantification of kynurenine metabolites, tryptophan, monoamines and neopterin in plasma, cerebrospinal fluid and brain.

PubMed

Fuertig, René; Ceci, Angelo; Camus, Sandrine M; Bezard, Erwan; Luippold, Andreas H; Hengerer, Bastian

2016-09-01

The kynurenine (KYN) pathway is implicated in diseases such as cancer, psychiatric, neurodegenerative and autoimmune disorders. Measurement of KYN metabolite levels will help elucidating the involvement of the KYN pathway in the disease pathology and inform drug development. Samples of plasma, cerebrospinal fluid or brain tissue were spiked with deuterated internal standards, processed and analyzed by LC-MS/MS; analytes were chromatographically separated by gradient elution on a C18 reversed phase analytical column without derivatization. We established an LC-MS/MS method to measure 11 molecules, namely tryptophan, KYN, 3-OH-KYN, 3-OH-anthranilic acid, quinolinic acid, picolinic acid, kynurenic acid, xanthurenic acid, serotonin, dopamine and neopterin within 5.5 min, with sufficient sensitivity to quantify these molecules in small sample volumes of plasma, cerebrospinal fluid and brain tissue.

Real-Time XRD Studies of Li-O2 Electrochemical Reaction in Nonaqueous Lithium-Oxygen Battery.

PubMed

Lim, Hyunseob; Yilmaz, Eda; Byon, Hye Ryung

2012-11-01

Understanding of electrochemical process in rechargeable Li-O2 battery has suffered from lack of proper analytical tool, especially related to the identification of chemical species and number of electrons involved in the discharge/recharge process. Here we present a simple and straightforward analytical method for simultaneously attaining chemical and quantified information of Li2O2 (discharge product) and byproducts using in situ XRD measurement. By real-time monitoring of solid-state Li2O2 peak area, the accurate efficiency of Li2O2 formation and the number of electrons can be evaluated during full discharge. Furthermore, by observation of sequential area change of Li2O2 peak during recharge, we found nonlinearity of Li2O2 decomposition rate for the first time in ether-based electrolyte.

Analytical separations of mammalian decomposition products for forensic science: a review.

PubMed

Swann, L M; Forbes, S L; Lewis, S W

2010-12-03

The study of mammalian soft tissue decomposition is an emerging area in forensic science, with a major focus of the research being the use of various chemical and biological methods to study the fate of human remains in the environment. Decomposition of mammalian soft tissue is a postmortem process that, depending on environmental conditions and physiological factors, will proceed until complete disintegration of the tissue. The major stages of decomposition involve complex reactions which result in the chemical breakdown of the body's main constituents; lipids, proteins, and carbohydrates. The first step to understanding this chemistry is identifying the compounds present in decomposition fluids and determining when they are produced. This paper provides an overview of decomposition chemistry and reviews recent advances in this area utilising analytical separation science. Copyright © 2010 Elsevier B.V. All rights reserved.

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.

Optical bandgap of semiconductor nanostructures: Methods for experimental data analysis

NASA Astrophysics Data System (ADS)

Raciti, R.; Bahariqushchi, R.; Summonte, C.; Aydinli, A.; Terrasi, A.; Mirabella, S.

2017-06-01

Determination of the optical bandgap (Eg) in semiconductor nanostructures is a key issue in understanding the extent of quantum confinement effects (QCE) on electronic properties and it usually involves some analytical approximation in experimental data reduction and modeling of the light absorption processes. Here, we compare some of the analytical procedures frequently used to evaluate the optical bandgap from reflectance (R) and transmittance (T) spectra. Ge quantum wells and quantum dots embedded in SiO2 were produced by plasma enhanced chemical vapor deposition, and light absorption was characterized by UV-Vis/NIR spectrophotometry. R&T elaboration to extract the absorption spectra was conducted by two approximated methods (single or double pass approximation, single pass analysis, and double pass analysis, respectively) followed by Eg evaluation through linear fit of Tauc or Cody plots. Direct fitting of R&T spectra through a Tauc-Lorentz oscillator model is used as comparison. Methods and data are discussed also in terms of the light absorption process in the presence of QCE. The reported data show that, despite the approximation, the DPA approach joined with Tauc plot gives reliable results, with clear advantages in terms of computational efforts and understanding of QCE.

Development of solution techniques for nonlinear structural analysis

NASA Technical Reports Server (NTRS)

Vos, R. G.; Andrews, J. S.

1974-01-01

Nonlinear structural solution methods in the current research literature are classified according to order of the solution scheme, and it is shown that the analytical tools for these methods are uniformly derivable by perturbation techniques. A new perturbation formulation is developed for treating an arbitrary nonlinear material, in terms of a finite-difference generated stress-strain expansion. Nonlinear geometric effects are included in an explicit manner by appropriate definition of an applicable strain tensor. A new finite-element pilot computer program PANES (Program for Analysis of Nonlinear Equilibrium and Stability) is presented for treatment of problems involving material and geometric nonlinearities, as well as certain forms on nonconservative loading.

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.

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...

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

PubMed Central

Islas, Gabriela; Hernandez, Prisciliano

2017-01-01

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. PMID:29181027

Analytical Electrochemistry: Methodology and Applications of Dynamic Techniques.

ERIC Educational Resources Information Center

Heineman, William R.; Kissinger, Peter T.

1980-01-01

Reports developments involving the experimental aspects of finite and current analytical electrochemistry including electrode materials (97 cited references), hydrodynamic techniques (56), spectroelectrochemistry (62), stripping voltammetry (70), voltammetric techniques (27), polarographic techniques (59), and miscellany (12). (CS)

Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

PubMed

Srivastava, Alpuna; Pandey, Richa; Verma, Ram K; Gupta, Madan M

2006-01-01

A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanol-water (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 microm, 125 x 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 microg/mL). Detection limits were 10 microg/mL for sennoside B and 35 microg/mL for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 microg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

Development of a Direct Headspace Collection Method from Arabidopsis Seedlings Using HS-SPME-GC-TOF-MS Analysis

PubMed Central

Kusano, Miyako; Iizuka, Yumiko; Kobayashi, Makoto; Fukushima, Atsushi; Saito, Kazuki

2013-01-01

Plants produce various volatile organic compounds (VOCs), which are thought to be a crucial factor in their interactions with harmful insects, plants and animals. Composition of VOCs may differ when plants are grown under different nutrient conditions, i.e., macronutrient-deficient conditions. However, in plants, relationships between macronutrient assimilation and VOC composition remain unclear. In order to identify the kinds of VOCs that can be emitted when plants are grown under various environmental conditions, we established a conventional method for VOC profiling in Arabidopsis thaliana (Arabidopsis) involving headspace-solid-phase microextraction-gas chromatography-time-of-flight-mass spectrometry (HS-SPME-GC-TOF-MS). We grew Arabidopsis seedlings in an HS vial to directly perform HS analysis. To maximize the analytical performance of VOCs, we optimized the extraction method and the analytical conditions of HP-SPME-GC-TOF-MS. Using the optimized method, we conducted VOC profiling of Arabidopsis seedlings, which were grown under two different nutrition conditions, nutrition-rich and nutrition-deficient conditions. The VOC profiles clearly showed a distinct pattern with respect to each condition. This study suggests that HS-SPME-GC-TOF-MS analysis has immense potential to detect changes in the levels of VOCs in not only Arabidopsis, but other plants grown under various environmental conditions. PMID:24957989

Aluminium sensitized spectrofluorimetric determination of fluoroquinolones in milk samples coupled with salting-out assisted liquid-liquid ultrasonic extraction

NASA Astrophysics Data System (ADS)

Xia, Qinghai; Yang, Yaling; Liu, Mousheng

2012-10-01

An aluminium sensitized spectrofluorimetric method coupled with salting-out assisted liquid-liquid ultrasonic extraction for the determination of four widely used fluoroquinolones (FQs) namely norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP) and gatifloxacin (GAT) in bovine raw milk was described. The analytical procedure involves the fluorescence sensitization of aluminium (Al3+) by complexation with FQs, salting-out assisted liquid-liquid ultrasonic extraction (SALLUE), followed by spectrofluorometry. The influence of several parameters on the extraction (the salt species, the amount of salt, pH, temperature and phase volume ratio) was investigated. Under optimized experimental conditions, the detection limits of the method in milk varied from 0.009 μg/mL for NOR to 0.016 μg/mL for GAT (signal-to-noise ratio (S/N) = 3). The relative standard deviations (RSD) values were found to be relatively low (0.54-2.48% for four compounds). The calibration graph was linear from 0.015 to 2.25 μg/mL with coefficient of determinations not less than 0.9974. The methodology developed was applied to the determination of FQs in bovine raw milk samples. The main advantage of this method is simple, accurate and green. The method showed promising applications for analyzing polar analytes especially polar drugs in various sample matrices.

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.

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...

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.

Analytic representations of mK , FK, mη, and Fη in two loop S U (3 ) chiral perturbation theory

NASA Astrophysics Data System (ADS)

Ananthanarayan, B.; Bijnens, Johan; Friot, Samuel; Ghosh, Shayan

2018-06-01

In this work, we consider expressions for the masses and decay constants of the pseudoscalar mesons in S U (3 ) chiral perturbation theory. These involve sunset diagrams and their derivatives evaluated at p2=mP2 (P =π , K , η ). Recalling that there are three mass scales in this theory, mπ, mK and mη, there are instances when the finite part of the sunset diagrams do not admit an expression in terms of elementary functions, and have therefore been evaluated numerically in the past. In a recent publication, an expansion in the external momentum was performed to obtain approximate analytic expressions for mπ and Fπ, the pion mass and decay constant. We provide fully analytic exact expressions for mK and mη, the kaon and eta masses, and FK and Fη, the kaon and eta decay constants. These expressions, calculated using Mellin-Barnes methods, are in the form of double series in terms of two mass ratios. A numerical analysis of the results to evaluate the relative size of contributions coming from loops, chiral logarithms as well as phenomenological low-energy constants is presented. We also present a set of approximate analytic expressions for mK, FK, mη and Fη that facilitate comparisons with lattice results. Finally, we show how exact analytic expressions for mπ and Fπ may be obtained, the latter having been used in conjunction with the results for FK to produce a recently published analytic representation of FK/Fπ.

Metal species involved in long distance metal transport in plants

PubMed Central

Álvarez-Fernández, Ana; Díaz-Benito, Pablo; Abadía, Anunciación; López-Millán, Ana-Flor; Abadía, Javier

2014-01-01

The mechanisms plants use to transport metals from roots to shoots are not completely understood. It has long been proposed that organic molecules participate in metal translocation within the plant. However, until recently the identity of the complexes involved in the long-distance transport of metals could only be inferred by using indirect methods, such as analyzing separately the concentrations of metals and putative ligands and then using in silico chemical speciation software to predict metal species. Molecular biology approaches also have provided a breadth of information about putative metal ligands and metal complexes occurring in plant fluids. The new advances in analytical techniques based on mass spectrometry and the increased use of synchrotron X-ray spectroscopy have allowed for the identification of some metal-ligand species in plant fluids such as the xylem and phloem saps. Also, some proteins present in plant fluids can bind metals and a few studies have explored this possibility. This study reviews the analytical challenges researchers have to face to understand long-distance metal transport in plants as well as the recent advances in the identification of the ligand and metal-ligand complexes in plant fluids. PMID:24723928

A hybrid finite element-transfer matrix model for vibroacoustic systems with flat and homogeneous acoustic treatments.

PubMed

Alimonti, Luca; Atalla, Noureddine; Berry, Alain; Sgard, Franck

2015-02-01

Practical vibroacoustic systems involve passive acoustic treatments consisting of highly dissipative media such as poroelastic materials. The numerical modeling of such systems at low to mid frequencies typically relies on substructuring methodologies based on finite element models. Namely, the master subsystems (i.e., structural and acoustic domains) are described by a finite set of uncoupled modes, whereas condensation procedures are typically preferred for the acoustic treatments. However, although accurate, such methodology is computationally expensive when real life applications are considered. A potential reduction of the computational burden could be obtained by approximating the effect of the acoustic treatment on the master subsystems without introducing physical degrees of freedom. To do that, the treatment has to be assumed homogeneous, flat, and of infinite lateral extent. Under these hypotheses, simple analytical tools like the transfer matrix method can be employed. In this paper, a hybrid finite element-transfer matrix methodology is proposed. The impact of the limiting assumptions inherent within the analytical framework are assessed for the case of plate-cavity systems involving flat and homogeneous acoustic treatments. The results prove that the hybrid model can capture the qualitative behavior of the vibroacoustic system while reducing the computational effort.

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

Implicit motor learning promotes neural efficiency during laparoscopy.

PubMed

Zhu, Frank F; Poolton, Jamie M; Wilson, Mark R; Hu, Yong; Maxwell, Jon P; Masters, Rich S W

2011-09-01

An understanding of differences in expert and novice neural behavior can inform surgical skills training. Outside the surgical domain, electroencephalographic (EEG) coherence analyses have shown that during motor performance, experts display less coactivation between the verbal-analytic and motor planning regions than their less skilled counterparts. Reduced involvement of verbal-analytic processes suggests greater neural efficiency. The authors tested the utility of an implicit motor learning intervention specifically devised to promote neural efficiency by reducing verbal-analytic involvement in laparoscopic performance. In this study, 18 novices practiced a movement pattern on a laparoscopic trainer with either conscious awareness of the movement pattern (explicit motor learning) or suppressed awareness of the movement pattern (implicit motor learning). In a retention test, movement accuracy was compared between the conditions, and coactivation (EEG coherence) was assessed between the motor planning (Fz) region and both the verbal-analytic (T3) and the visuospatial (T4) cortical regions (T3-Fz and T4-Fz, respectively). Movement accuracy in the conditions was not different in a retention test (P = 0.231). Findings showed that the EEG coherence scores for the T3-Fz regions were lower for the implicit learners than for the explicit learners (P = 0.027), but no differences were apparent for the T4-Fz regions (P = 0.882). Implicit motor learning reduced EEG coactivation between verbal-analytic and motor planning regions, suggesting that verbal-analytic processes were less involved in laparoscopic performance. The findings imply that training techniques that discourage nonessential coactivation during motor performance may provide surgeons with more neural resources with which to manage other aspects of surgery.

Validated analytical methodology for the simultaneous determination of a wide range of pesticides in human blood using GC-MS/MS and LC-ESI/MS/MS and its application in two poisoning cases.

PubMed

Luzardo, Octavio P; Almeida-González, Maira; Ruiz-Suárez, Norberto; Zumbado, Manuel; Henríquez-Hernández, Luis A; Meilán, María José; Camacho, María; Boada, Luis D

2015-09-01

Pesticides are frequently responsible for human poisoning and often the information on the involved substance is lacking. The great variety of pesticides that could be responsible for intoxication makes necessary the development of powerful and versatile analytical methodologies, which allows the identification of the unknown toxic substance. Here we developed a methodology for simultaneous identification and quantification in human blood of 109 highly toxic pesticides. The application of this analytical scheme would help in minimizing the cost of this type of chemical identification, maximizing the chances of identifying the pesticide involved. In the methodology that we present here, we use a liquid-liquid extraction, followed by one single purification step, and quantitation of analytes by a combination of liquid and gas chromatography, both coupled to triple quadrupole mass spectrometry, which is operated in the mode of multiple reaction monitoring. The methodology has been fully validated, and its applicability has been demonstrated in two recent cases involving one self-poisoning fatality and one non-fatal homicidal attempt. Copyright © 2015 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.

Analytical Modeling of Groundwater Seepages to St. Lucie Estuary

NASA Astrophysics Data System (ADS)

Lee, J.; Yeh, G.; Hu, G.

2008-12-01

In this paper, six analytical models describing hydraulic interaction of stream-aquifer systems were applied to St Lucie Estuary (SLE) River Estuaries. These are analytical solutions for: (1) flow from a finite aquifer to a canal, (2) flow from an infinite aquifer to a canal, (3) the linearized Laplace system in a seepage surface, (4) wave propagation in the aquifer, (5) potential flow through stratified unconfined aquifers, and (6) flow through stratified confined aquifers. Input data for analytical solutions were obtained from monitoring wells and river stages at seepage-meter sites. Four transects in the study area are available: Club Med, Harbour Ridge, Lutz/MacMillan, and Pendarvis Cove located in the St. Lucie River. The analytical models were first calibrated with seepage meter measurements and then used to estimate of groundwater discharges into St. Lucie River. From this process, analytical relationships between the seepage rate and river stages and/or groundwater tables were established to predict the seasonal and monthly variation in groundwater seepage into SLE. It was found the seepage rate estimations by analytical models agreed well with measured data for some cases but only fair for some other cases. This is not unexpected because analytical solutions have some inherently simplified assumptions, which may be more valid for some cases than the others. From analytical calculations, it is possible to predict approximate seepage rates in the study domain when the assumptions underlying these analytical models are valid. The finite and infinite aquifer models and the linearized Laplace method are good for sites Pendarvis Cove and Lutz/MacMillian, but fair for the other two sites. The wave propagation model gave very good agreement in phase but only fairly agreement in magnitude for all four sites. The stratified unconfined and confined aquifer models gave similarly good agreements with measurements at three sites but poorly at the Club Med site. None of the analytical models presented here can fit the data at this site. To give better estimates at all sites numerical modeling that couple river hydraulics and groundwater flow involving less simplifications of and assumptions for the system may have to be adapted.

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

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.

TDS exposure project: application of the analytic hierarchy process for the prioritization of substances to be analyzed in a total diet study.

PubMed

Papadopoulos, A; Sioen, I; Cubadda, F; Ozer, H; Basegmez, H I Oktay; Turrini, A; Lopez Esteban, M T; Fernandez San Juan, P M; Sokolić-Mihalak, D; Jurkovic, M; De Henauw, S; Aureli, F; Vin, K; Sirot, V

2015-02-01

The objective of this article is to develop a general method based on the analytic hierarchy process (AHP) methodology to rank the substances to be studied in a Total Diet Studies (TDS). This method was tested for different substances and groups of substances (N = 113), for which the TDS approach has been considered relevant. This work was performed by a group of 7 experts from different European countries representing their institutes, which are involved in the TDS EXPOSURE project. The AHP methodology is based on a score system taking into account experts' judgments quantified assigning comparative scores to the different identified issues. Hence, the 10 substances of highest interest in the framework of a TDS are trace elements (methylmercury, cadmium, inorganic arsenic, lead, aluminum, inorganic mercury), dioxins, furans and polychlorinated biphenyls (PCBs), and some additives (sulfites and nitrites). The priority list depends on both the national situation (geographical variations, consumer concern, etc.) and the availability of data. Thus, the list depends on the objectives of the TDS and on reachable analytical performances. Moreover, such a list is highly variable with time and new data (e.g. social context, vulnerable population groups, emerging substances, new toxicological data or health-based guidance values). Copyright © 2014 Elsevier Ltd. All rights reserved.

First-order analytic propagation of satellites in the exponential atmosphere of an oblate planet

NASA Astrophysics Data System (ADS)

Martinusi, Vladimir; Dell'Elce, Lamberto; Kerschen, Gaëtan

2017-04-01

The paper offers the fully analytic solution to the motion of a satellite orbiting under the influence of the two major perturbations, due to the oblateness and the atmospheric drag. The solution is presented in a time-explicit form, and takes into account an exponential distribution of the atmospheric density, an assumption that is reasonably close to reality. The approach involves two essential steps. The first one concerns a new approximate mathematical model that admits a closed-form solution with respect to a set of new variables. The second step is the determination of an infinitesimal contact transformation that allows to navigate between the new and the original variables. This contact transformation is obtained in exact form, and afterwards a Taylor series approximation is proposed in order to make all the computations explicit. The aforementioned transformation accommodates both perturbations, improving the accuracy of the orbit predictions by one order of magnitude with respect to the case when the atmospheric drag is absent from the transformation. Numerical simulations are performed for a low Earth orbit starting at an altitude of 350 km, and they show that the incorporation of drag terms into the contact transformation generates an error reduction by a factor of 7 in the position vector. The proposed method aims at improving the accuracy of analytic orbit propagation and transforming it into a viable alternative to the computationally intensive numerical methods.

Determination of different recreational drugs in sweat by headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME GC/MS): Application to drugged drivers.

PubMed

Gentili, Stefano; Mortali, Claudia; Mastrobattista, Luisa; Berretta, Paolo; Zaami, Simona

2016-09-10

A procedure based on headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) has been developed for the determination of most commonly used drugs of abuse in sweat of drivers stopped during roadside controls. DrugWipe 5A sweat screening device was used to collect sweat by a specific pad rubbed gently over forehead skin surface. The procedure involved an acid hydrolysis, a HS-SPME extraction for drugs of abuse but Δ(9)-tetrahydrocannabinol, which was directly extracted in alkaline medium HS-SPME conditions, a GC separation of analytes by a capillary column and MS detection by electron impact ionisation. The method was linear from the limit of quantification (LOQ) to 50ng drug per pad (r(2)≥0.99), with an intra- and inter-assay precision and accuracy always less than 15% and an analytical recovery between 95.1% and 102.8%, depending on the considered analyte. Using the validated method, sweat from 60 apparently intoxicated drivers were found positive to one or more drugs of abuse, showing sweat patches testing as a viable economic and simple alternative to conventional (blood and/or urine) and non conventional (oral fluid) testing of drugs of abuse in drugged drivers. Copyright © 2016 Elsevier B.V. All rights reserved.

LOVE CANAL MONITORING PROGRAM. VOLUME 1

EPA Science Inventory

This report summarizes the prime contractor activities during the monitoring phase of the Love Canal project. Since GCA Corporation was only responsible for data collection, no analytical results appear in this report. The program involved a multifaceted sampling and analytical e...

A high-accuracy algorithm for solving nonlinear PDEs with high-order spatial derivatives in 1 + 1 dimensions

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

Yao, Jian Hua; Gooding, R.J.

1994-06-01

We propose an algorithm to solve a system of partial differential equations of the type u[sub t](x,t) = F(x, t, u, u[sub x], u[sub xx], u[sub xxx], u[sub xxxx]) in 1 + 1 dimensions using the method of lines with piecewise ninth-order Hermite polynomials, where u and F and N-dimensional vectors. Nonlinear boundary conditions are easily incorporated with this method. We demonstrate the accuracy of this method through comparisons of numerically determine solutions to the analytical ones. Then, we apply this algorithm to a complicated physical system involving nonlinear and nonlocal strain forces coupled to a thermal field. 4 refs.,more » 5 figs., 1 tab.« less

Computational aspects of sensitivity calculations in linear transient structural analysis. Ph.D. Thesis - Virginia Polytechnic Inst. and State Univ.

NASA Technical Reports Server (NTRS)

Greene, William H.

1990-01-01

A study was performed focusing on the calculation of sensitivities of displacements, velocities, accelerations, and stresses in linear, structural, transient response problems. One significant goal of the study was to develop and evaluate sensitivity calculation techniques suitable for large-order finite element analyses. Accordingly, approximation vectors such as vibration mode shapes are used to reduce the dimensionality of the finite element model. Much of the research focused on the accuracy of both response quantities and sensitivities as a function of number of vectors used. Two types of sensitivity calculation techniques were developed and evaluated. The first type of technique is an overall finite difference method where the analysis is repeated for perturbed designs. The second type of technique is termed semi-analytical because it involves direct, analytical differentiation of the equations of motion with finite difference approximation of the coefficient matrices. To be computationally practical in large-order problems, the overall finite difference methods must use the approximation vectors from the original design in the analyses of the perturbed models. In several cases this fixed mode approach resulted in very poor approximations of the stress sensitivities. Almost all of the original modes were required for an accurate sensitivity and for small numbers of modes, the accuracy was extremely poor. To overcome this poor accuracy, two semi-analytical techniques were developed. The first technique accounts for the change in eigenvectors through approximate eigenvector derivatives. The second technique applies the mode acceleration method of transient analysis to the sensitivity calculations. Both result in accurate values of the stress sensitivities with a small number of modes and much lower computational costs than if the vibration modes were recalculated and then used in an overall finite difference method.

Simultaneous determination of nikethamide and lidocaine in human blood and cerebrospinal fluid by high performance liquid chromatography.

PubMed

Chen, Lili; Liao, Linchuan; Zuo, Zhong; Yan, Youyi; Yang, Lin; Fu, Qiang; Chen, Yu; Hou, Junhong

2007-04-11

Nikethamide and lidocaine are often requested to be quantified simultaneously in forensic toxicological analysis. A simple reversed-phase high performance liquid chromatography (RP-HPLC) method has been developed for their simultaneous determination in human blood and cerebrospinal fluid. The method involves simple protein precipitation sample treatment followed by quantification of analytes using HPLC at 263 nm. Analytes were separated on a 5 microm Zorbax Dikema C18 column (150 mm x 4.60 mm, i.d.) with a mobile phase of 22:78 (v/v) mixture of methanol and a diethylamine-acetic acid buffer, pH 4.0. The mean recoveries were between 69.8 and 94.4% for nikethamide and between 78.9 and 97.2% for lidocaine. Limits of detection (LODs) for nikethamide and lidocaine were 0.008 and 0.16 microg/ml in plasma and 0.007 and 0.14 microg/ml in cerebrospinal fluid, respectively. The mean intra-assay and inter-assay coefficients of variation (CVs) for both analytes were less than 9.2 and 10.8%, respectively. The developed method was applied to blood sample analyses in eight forensic cases, where blood concentrations of lidocaine ranged from 0.68 to 34.4 microg/ml and nikethamide ranged from 1.25 to 106.8 microg/ml. In six cases cerebrospinal fluid analysis was requested. The values ranged from 20.3 to 185.6 microg/ml of lidocaine and 8.0 to 72.4 microg/ml of nikethamide. The method is simple and sensitive enough to be used in toxicological analysis for simultaneous determination of nikethamide and lidocaine in blood and cerebrospinal fluid.

Identification and analysis of gastrodin and its five metabolites using ultra fast liquid chromatography electrospray ionization tandem mass spectrometry to investigate influence of multiple-dose and food.

PubMed

Jia, Yuanwei; Shen, Jie; Li, Xin; Xie, Haitang; Wang, Junsong; Luo, Jun; Wang, Kelvin D G; Liu, Qingwang; Kong, Lingyi

2014-09-05

A reliable and highly sensitive ultra performance liquid chromatography electrospray ionization tandem mass spectrometry (UFLC-ESI-MS/MS) analytical method was developed for identification and quantification of gastrodin (GAS) and its metabolites in rat plasma. Five metabolites were identified: p-formylphenyl-β-d-glucopyranoside (M1), p-hydroxybenzonic acid (M2), p-hydroxybenzyl alcohol (M3), p-formaldehydephenyl-β-d-glucopyranoside (M4), p-hydroxybenzaldehyde (M5). The molecular structures of metabolites were proposed based on the characters of their precursor ions, product ions and chromatographic retention time. Four of them were reported firstly in rat plasma. This method involved the addition of bergeninum as the internal standard (IS), UFLC separation, and quantification by MS/MS system using negative electrospray ionization in the multiple reaction monitoring (MRM) mode. The lower limit of quantification of gastrodin and five metabolites were all 1ng/mL. The method was linear in the concentration range of 0.001-10μg/mL. The intra- and inter-day precisions (R.S.D %) were within 15.0% for all analytes. No interference was noted due to endogenous substances. All analytes were stable in rat plasma stored at room temperature and 4°C for at least 4h, -20°C combined with three freeze-thaw cycles for at least 1 month. By this method, the influence of multiple-dose and food on the pharmacokinetics behaviors of GAS and its metabolites were studied for the first time. We hope pharmacokinetic data of present study may inspire rational clinical usage of GAS. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Temperature field for radiative tomato peeling

NASA Astrophysics Data System (ADS)

Cuccurullo, G.; Giordano, L.

2017-01-01

Nowadays peeling of tomatoes is performed by using steam or lye, which are expensive and polluting techniques, thus sustainable alternatives are searched for dry peeling and, among that, radiative heating seems to be a fairly promising method. This paper aims to speed up the prediction of surface temperatures useful for realizing dry-peeling, thus a 1D-analytical model for the unsteady temperature field in a rotating tomato exposed to a radiative heating source is presented. Since only short times are of interest for the problem at hand, the model involves a semi-infinite slab cooled by convective heat transfer while heated by a pulsating heat source. The model being linear, the solution is derived following the Laplace Transform method. A 3D finite element model of the rotating tomato is introduced as well in order to validate the analytical solution. A satisfactory agreement is attained. Therefore, two different ways to predict the onset of the peeling conditions are available which can be of help for proper design of peeling plants. Particular attention is paid to study surface temperature uniformity, that being a critical parameter for realizing an easy tomato peeling.

Mathematical model to estimate risk of calcium-containing renal stones

NASA Technical Reports Server (NTRS)

Pietrzyk, R. A.; Feiveson, A. H.; Whitson, P. A.

1999-01-01

BACKGROUND/AIMS: Astronauts exposed to microgravity during the course of spaceflight undergo physiologic changes that alter the urinary environment so as to increase the risk of renal stone formation. This study was undertaken to identify a simple method with which to evaluate the potential risk of renal stone development during spaceflight. METHOD: We used a large database of urinary risk factors obtained from 323 astronauts before and after spaceflight to generate a mathematical model with which to predict the urinary supersaturation of calcium stone forming salts. RESULT: This model, which involves the fewest possible analytical variables (urinary calcium, citrate, oxalate, phosphorus, and total volume), reliably and accurately predicted the urinary supersaturation of the calcium stone forming salts when compared to results obtained from a group of 6 astronauts who collected urine during flight. CONCLUSIONS: The use of this model will simplify both routine medical monitoring during spaceflight as well as the evaluation of countermeasures designed to minimize renal stone development. This model also can be used for Earth-based applications in which access to analytical resources is limited.

Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

PubMed

Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

2015-12-24

A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). Copyright © 2015 Elsevier B.V. All rights reserved.

Deriving analytic solutions for compact binary inspirals without recourse to adiabatic approximations

NASA Astrophysics Data System (ADS)

Galley, Chad R.; Rothstein, Ira Z.

2017-05-01

We utilize the dynamical renormalization group formalism to calculate the real space trajectory of a compact binary inspiral for long times via a systematic resummation of secularly growing terms. This method generates closed form solutions without orbit averaging, and the accuracy can be systematically improved. The expansion parameter is v5ν Ω (t -t0) where t0 is the initial time, t is the time elapsed, and Ω and v are the angular orbital frequency and initial speed, respectively. ν is the binary's symmetric mass ratio. We demonstrate how to apply the renormalization group method to resum solutions beyond leading order in two ways. First, we calculate the second-order corrections of the leading radiation reaction force, which involves highly nontrivial checks of the formalism (i.e., its renormalizability). Second, we show how to systematically include post-Newtonian corrections to the radiation reaction force. By avoiding orbit averaging, we gain predictive power and eliminate ambiguities in the initial conditions. Finally, we discuss how this methodology can be used to find analytic solutions to the spin equations of motion that are valid over long times.

Rapid classification of biological components

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

Thompson, Vicki S.; Barrett, Karen B.; Key, Diane E.

A method is disclosed for analyzing a biological sample by antibody profiling for identifying forensic samples or for detecting the presence of an analyte. In an illustrative embodiment of the invention, the analyte is a drug, such as marijuana, Cocaine (crystalline tropane alkaloid), methamphetamine, methyltestosterone, or mesterolone. The method involves attaching antigens of the surface of a solid support in a preselected pattern to form an array wherein the locations of the antigens are known; contacting the array with the biological sample such that a portion of antibodies in the sample reacts with and binds to antigens in the array,more » thereby forming immune complexes; washing away antibodies that do not form immune complexes; and detecting the immune complexes, thereby forming an antibody profile. Forensic samples are identified by comparing a sample from an unknown source with a sample from a known source. Further, an assay, such as a test for illegal drug use, can be coupled to a test for identity such that the results of the assay can be positively correlated to a subject's identity.« less

Rapid classification of biological components

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

Thompson, Vicki S.; Barrett, Karen B.; Key, Diane E.

A method is disclosed for analyzing a biological sample by antibody profiling for identifying forensic samples or for detecting the presence of an analyte. In an illustrative embodiment of the invention, the analyte is a drug, such as marijuana, cocaine (crystalline tropane alkaloid), methamphetamine, methyltestosterone, or mesterolone. The method involves attaching antigens to a surface of a solid support in a preselected pattern to form an array wherein the locations of the antigens are known; contacting the array with the biological sample such that a portion of antibodies in the sample reacts with and binds to antigens in the array,more » thereby forming immune complexes; washing away antibodies that do not form immune complexes; and detecting the immune complexes, thereby forming an antibody profile. Forensic samples are identified by comparing a sample from an unknown source with a sample from a known source. Further, an assay, such as a test for illegal drug use, can be coupled to a test for identity such that the results of the assay can be positively correlated to a subject's identity.« less

The application of grounded theory and symbolic interactionism.

PubMed

Jeon, Yun-Hee

2004-09-01

This paper describes the methodological and theoretical context and underpinnings of a study that examined community psychiatric nurses' work with family caregivers of older people with depression. The study used grounded theory research methods, with its theoretical foundations drawn from symbolic interactionism. The aims of the study were to describe and conceptualize the processes involved when community nurses work and interact with family caregivers and to develop an explanatory theory of these processes. This paper begins with an explanation of the rationale for using grounded theory as the method of choice, followed by a discussion of the theoretical underpinnings of the study, including a brief summary of the nature and origins of symbolic interactionism. Key premises of symbolic interactionism regarded as central to the study are outlined and an analytical overview of the grounded theory method is provided. The paper concludes with a commentary on some of the issues and debates in the use of grounded theory in nursing research. The main purpose of this paper is to provide a methodical and critical review of symbolic interactionism and grounded theory that can help readers, particularly those who are intending to use grounded theory, better understand the processes involved in applying this method to their research.

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.