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Sample records for analytical methods validation

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

    Science.gov (United States)

    MacNeil, James D

    2012-08-01

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

  2. Development and Validation of Analytical Method for Losartan ...

    African Journals Online (AJOL)

    Development and Validation of Analytical Method for Losartan-Copper Complex Using UV-Vis Spectrophotometry. ... Tropical Journal of Pharmaceutical Research ... Purpose: To develop a new spectrophotometric method for the analysis of losartan potassium in pharmaceutical formulations by making its complex with ...

  3. Development and validation of analytical methods for dietary supplements

    International Nuclear Information System (INIS)

    Sullivan, Darryl; Crowley, Richard

    2006-01-01

    The expanding use of innovative botanical ingredients in dietary supplements and foods has resulted in a flurry of research aimed at the development and validation of analytical methods for accurate measurement of active ingredients. The pressing need for these methods is being met through an expansive collaborative initiative involving industry, government, and analytical organizations. This effort has resulted in the validation of several important assays as well as important advances in the method engineering procedures which have improved the efficiency of the process. The initiative has also allowed researchers to hurdle many of the barricades that have hindered accurate analysis such as the lack of reference standards and comparative data. As the availability for nutraceutical products continues to increase these methods will provide consumers and regulators with the scientific information needed to assure safety and dependable labeling

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

    Science.gov (United States)

    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…

  5. Oxcarbazepine: validation and application of an analytical method

    Directory of Open Access Journals (Sweden)

    Paula Cristina Rezende Enéas

    2010-06-01

    Full Text Available Oxcarbazepine (OXC is an important anticonvulsant and mood stabilizing drug. A pharmacopoeial monograph for OXC is not yet available and therefore the development and validation of a new analytical method for quantification of this drug is essential. In the present study, a UV spectrophotometric method for the determination of OXC was developed. The various parameters, such as linearity, precision, accuracy and specificity, were studied according to International Conference on Harmonization Guidelines. Batches of 150 mg OXC capsules were prepared and analyzed using the validated UV method. The formulations were also evaluated for parameters including drug-excipient compatibility, flowability, uniformity of weight, disintegration time, assay, uniformity of content and the amount of drug dissolved during the first hour.Oxcarbazepina (OXC é um fármaco anticonvulsivante e estabilizante do humor. O desenvolvimento e validação de método analítico para quantificação da OXC são de fundamental importância devido à ausência de monografias farmacopéicas oficiais para esse fármaco. Nesse trabalho, um método espectrofotométrico UV para determinação da OXC foi desenvolvido. O método proposto foi validado seguindo os parâmetros de linearidade, precisão, exatidão e especificidade de acordo com as normas da Conferência Internacional de Harmonização. Cápsulas de OXC 150 mg foram preparadas e analisadas utilizando-se o método analítico validado. As formulações foram avaliadas com relação à compatibilidade fármaco-excipientes, fluidez, determinação de peso, tempo de desintegração, doseamento, uniformidade de conteúdo e quantidade do fármaco dissolvido após 60 minutos.

  6. Analytical models approximating individual processes: a validation method.

    Science.gov (United States)

    Favier, C; Degallier, N; Menkès, C E

    2010-12-01

    Upscaling population models from fine to coarse resolutions, in space, time and/or level of description, allows the derivation of fast and tractable models based on a thorough knowledge of individual processes. The validity of such approximations is generally tested only on a limited range of parameter sets. A more general validation test, over a range of parameters, is proposed; this would estimate the error induced by the approximation, using the original model's stochastic variability as a reference. This method is illustrated by three examples taken from the field of epidemics transmitted by vectors that bite in a temporally cyclical pattern, that illustrate the use of the method: to estimate if an approximation over- or under-fits the original model; to invalidate an approximation; to rank possible approximations for their qualities. As a result, the application of the validation method to this field emphasizes the need to account for the vectors' biology in epidemic prediction models and to validate these against finer scale models. Copyright © 2010 Elsevier Inc. All rights reserved.

  7. A Generalized Pivotal Quantity Approach to Analytical Method Validation Based on Total Error.

    Science.gov (United States)

    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

  8. Principles of Single-Laboratory Validation of Analytical Methods for Testing the Chemical Composition of Pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Ambrus, A. [Hungarian Food Safety Office, Budapest (Hungary)

    2009-07-15

    Underlying theoretical and practical approaches towards pesticide formulation analysis are discussed, i.e. general principles, performance characteristics, applicability of validation data, verification of method performance, and adaptation of validated methods by other laboratories. The principles of single laboratory validation of analytical methods for testing the chemical composition of pesticides are outlined. Also the theoretical background is described for performing pesticide formulation analysis as outlined in ISO, CIPAC/AOAC and IUPAC guidelines, including methodological characteristics such as specificity, selectivity, linearity, accuracy, trueness, precision and bias. Appendices I–III hereof give practical and elaborated examples on how to use the Horwitz approach and formulae for estimating the target standard deviation towards acceptable analytical repeatability. The estimation of trueness and the establishment of typical within-laboratory reproducibility are treated in greater detail by means of worked-out examples. (author)

  9. Validation of the analytical method for sodium dichloroisocyanurate aimed at drinking water disinfection

    International Nuclear Information System (INIS)

    Martinez Alvarez, Luis Octavio; Alejo Cisneros, Pedro; Garcia Pereira, Reynaldo; Campos Valdez, Doraily

    2014-01-01

    Cuba has developed the first effervescent 3.5 mg sodium dichloroisocyanurate tablets as a non-therapeutic active principle. This ingredient releases certain amount of chlorine when dissolved into a litre of water and it can cause adequate disinfection of drinking water ready to be taken after 30 min. Developing and validating an analytical iodometric method applicable to the quality control of effervescent 3.5 mg sodium dichloroisocyanurate tablets

  10. Validation of analytical method for quality control of B12 Vitamin-10 000 injection

    International Nuclear Information System (INIS)

    Botet Garcia, Martha; Garcia Penna, Caridad Margarita; Troche Concepcion, Yenilen; Cannizares Arencibia, Yanara; Moreno Correoso, Barbara

    2009-01-01

    Analytical method reported by USA Pharmacopeia was validated for quality control of injectable B 1 2 Vitamin (10 000 U) by UV spectrophotometry because this is a simpler and low-cost method allowing quality control of finished product. Calibration curve was graphed at 60 to 140% interval, where it was linear with a correlation coefficient similar to 0, 9999; statistical test for interception and slope was considered non-significant. There was a recovery of 99.7 % in study concentrations interval where the Cochran (G) and Student(t) test were not significant too. Variation coefficient in repetition study was similar to 0.59 % for the 6 assayed replies, whereas in intermediate precision analysis, the Fisher and Student tests were not significant. Analytical method was linear, precise, specific and exact in study concentrations interval

  11. Analytical method validation for quality control and the study of the 50 mg Propylthiouracil stability

    International Nuclear Information System (INIS)

    Valdes Bendoyro, Maria Olga; Garcia Penna, Caridad Margarita; Fernandez, Juan Lugones; Garcia Borges, Lisandra; Martinez Espinosa, Vivian

    2010-01-01

    A high-performance liquid chromatography analytical method was developed and validated for the quality control and stability studies of 50 mg Propylthiouracil tablets. Method is based in active principle separation through a 100 RP-18 RP-18 (5 μm) (250 x 4 mm) Lichrospher chromatography with UV detection to 272 nm, using a mobile phase composed by a ungaseous mixture of a 0.025 M buffer solution-monobasic potassium phosphate to pH= 4,6 ad acetonitrile in a 80:20 ratio with a flux speed of 0,5 mL/min. Analytical method was linear, precise, specific and exact in the study concentrations interval

  12. Determination of proline in honey: comparison between official methods, optimization and validation of the analytical methodology.

    Science.gov (United States)

    Truzzi, Cristina; Annibaldi, Anna; Illuminati, Silvia; Finale, Carolina; Scarponi, Giuseppe

    2014-05-01

    The study compares official spectrophotometric methods for the determination of proline content in honey - those of the International Honey Commission (IHC) and the Association of Official Analytical Chemists (AOAC) - with the original Ough method. Results show that the extra time-consuming treatment stages added by the IHC method with respect to the Ough method are pointless. We demonstrate that the AOACs method proves to be the best in terms of accuracy and time saving. The optimized waiting time for the absorbance recording is set at 35min from the removal of reaction tubes from the boiling bath used in the sample treatment. The optimized method was validated in the matrix: linearity up to 1800mgL(-1), limit of detection 20mgL(-1), limit of quantification 61mgL(-1). The method was applied to 43 unifloral honey samples from the Marche region, Italy. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Analytical techniques and method validation for the measurement of selected semivolatile and nonvolatile organofluorochemicals in air.

    Science.gov (United States)

    Reagen, William K; Lindstrom, Kent R; Thompson, Kathy L; Flaherty, John M

    2004-09-01

    The widespread use of semi- and nonvolatile organofluorochemicals in industrial facilities, concern about their persistence, and relatively recent advancements in liquid chromatography/mass spectrometry (LC/MS) technology have led to the development of new analytical methods to assess potential worker exposure to airborne organofluorochemicals. Techniques were evaluated for the determination of 19 organofluorochemicals and for total fluorine in ambient air samples. Due to the potential biphasic nature of most of these fluorochemicals when airborne, Occupational Safety and Health Administration (OSHA) versatile sampler (OVS) tubes were used to simultaneously trap fluorochemical particulates and vapors from workplace air. Analytical methods were developed for OVS air samples to quantitatively analyze for total fluorine using oxygen bomb combustion/ion selective electrode and for 17 organofluorochemicals using LC/MS and gas chromatography/mass spectrometry (GC/MS). The experimental design for this validation was based on the National Institute of Occupational Safety and Health (NIOSH) Guidelines for Air Sampling and Analytical Method Development and Evaluation, with some revisions of the experimental design. The study design incorporated experiments to determine analytical recovery and stability, sampler capacity, the effect of some environmental parameters on recoveries, storage stability, limits of detection, precision, and accuracy. Fluorochemical mixtures were spiked onto each OVS tube over a range of 0.06-6 microg for each of 12 compounds analyzed by LC/MS and 0.3-30 microg for 5 compounds analyzed by GC/MS. These ranges allowed reliable quantitation at 0.001-0.1 mg/m3 in general for LC/MS analytes and 0.005-0.5 mg/m3 for GC/MS analytes when 60 L of air are sampled. The organofluorochemical exposure guideline (EG) is currently 0.1 mg/m3 for many analytes, with one exception being ammonium perfluorooctanoate (EG is 0.01 mg/m3). Total fluorine results may be used

  14. Validation of analytical methods for the stability studies of naproxen suppositories for infant and adult use

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Garcia Pulpeiro, Oscar

    2011-01-01

    Analytical and validating studies were performed in this paper, with a view to using them in the stability studies of the future formulations of naproxen suppositories for children and adults. The most influential factors in the naproxen stability were determined, that is, the major degradation occurred in acid medium, oxidative medium and by light action. One high-performance liquid chromatography-based method was evaluated, which proved to be adequate to quantify naproxen in suppositories and was selective against degradation products. The quantification limit was 3,480 μg, so it was valid for these studies. Additionally, the parameters specificity for stability, detection and quantification limits were evaluated for the direct semi-aqueous acid-base method, which was formerly validated for the quality control and showed satisfactory results. Nevertheless, the volumetric methods were not regarded as stability indicators; therefore, this method will be used along with the chromatographic methods of choice, that is, thin-layer chromatography and highperformance liquid chromatography, to determine the degradation products

  15. Development and validation of HPLC analytical method for quantitative determination of metronidazole in human plasma

    International Nuclear Information System (INIS)

    Safdar, K.A.; Shyum, S.B.; Usman, S.

    2016-01-01

    The objective of the present study was to develop a simple, rapid and sensitive reversed-phase high performance liquid chromatographic (RP-HPLC) analytical method with UV detection system for the quantitative determination of metronidazole in human plasma. The chromatographic separation was performed by using C18 RP column (250mm X 4.6mm, 5 meu m) as stationary phase and 0.01M potassium dihydrogen phosphate buffered at pH 3.0 and acetonitrile (83:17, v/v) as mobile phase at flow rate of 1.0 ml/min. The UV detection was carried out at 320nm. The method was validated as per the US FDA guideline for bioanalytical method validation and was found to be selective without interferences from mobile phase components, impurities and biological matrix. The method found to be linear over the concentration range of 0.2812 meu g/ml to 18.0 meu g/ml (r2 = 0.9987) with adequate level of accuracy and precision. The samples were found to be stable under various recommended laboratory and storage conditions. Therefore, the method can be used with adequate level of confidence and assurance for bioavailability, bioequivalence and other pharmacokinetic studies of metronidazole in human. (author)

  16. Development and Validation Dissolution Analytical Method of Nimesulide beta-Cyclodextrin 400 mg Tablet

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Carvalho Pereira

    2016-10-01

    Full Text Available The nimesulide (N-(4-nitro-2-phenoxyphenylmethanesulfonamide belongs to the class of non-steroidal anti-inflammatory drugs (NSAIDs and category II of the biopharmaceutical classification, The complexation of nimesulide with b-cyclodextrin is a pharmacological strategy to increase the solubility of the drug The objective of this study was to develop and validate an analytical methodology for dissolving the nimesulide beta-cyclodextrin 400 mg tablet and meets the guidelines of ANVISA for drug registration purposes. Once developed, the dissolution methodology was validated according to the RE of parameters no.  899/2003. In the development of the method it was noted that the duration of the dissolution test was 60 minutes, the volume and the most suitable dissolution medium was 900 mL of aqueous solution of sodium lauryl sulfate 1% (w/ v. It was also noted that rotation of 100 rpm and the paddle apparatus was the most appropriate to evaluate the dissolution of the drug. Spectrophotometric methodology was used to quantify the percentage of dissolved drug. The wavelength was 390 nm using the quantification. The validation of the methodology, system suitability parameters, specificity/selectivity, linearity, precision, accuracy and robustness were satisfactory and proved that the developed dissolution methodology was duly executed. DOI: http://dx.doi.org/10.17807/orbital.v8i5.827

  17. Validation of multivariate classification methods using analytical fingerprints – concept and case study on organic feed for laying hens

    NARCIS (Netherlands)

    Alewijn, Martin; Voet, van der Hilko; Ruth, van Saskia

    2016-01-01

    Multivariate classification methods based on analytical fingerprints have found many applications in the food and feed area, but practical applications are still scarce due to a lack of a generally accepted validation procedure. This paper proposes a new approach for validation of this type of

  18. Development and validation of analytical method for Naftopidil in human plasma by LC–MS/MS

    Directory of Open Access Journals (Sweden)

    Pritam S. Jain

    2015-09-01

    Full Text Available A highly sensitive and simple high-performance liquid chromatographic–tandem mass spectrometric (LC–MS-MS assay is developed and validated for the quantification of Naftopidil in human plasma. Naftopidil is extracted from human plasma by methyl tertiary butyl ether and analyzed using a reversed-phase gradient elution on a discovery C 18 5 μ (50 × 4.6 column. A methanol: 2 mM ammonium formate (90:10 as mobile phase, is used and detection was performed by MS using electrospray ionization in positive mode. Propranolol is used as the internal standard. The lower limits of quantification are 0.495 ng/mL. The calibration curves are linear over the concentration range of 0.495–200.577 ng/mL of plasma for each analyte. This novel LC–MS-MS method shows satisfactory accuracy and precision and is sufficiently sensitive for the performance of pharmacokinetic studies in humans.

  19. VALIDATION OF ANALYTICAL METHODS AND INSTRUMENTATION FOR BERYLLIUM MEASUREMENT: REVIEW AND SUMMARY OF AVAILABLE GUIDES, PROCEDURES, AND PROTOCOLS

    Energy Technology Data Exchange (ETDEWEB)

    Ekechukwu, A.

    2008-12-17

    This document proposes to provide a listing of available sources which can be used to validate analytical methods and/or instrumentation for beryllium determination. A literature review was conducted of available standard methods and publications used for method validation and/or quality control. A comprehensive listing of the articles, papers, and books reviewed is given in Appendix 1. Available validation documents and guides are listed in the appendix; each has a brief description of application and use. In the referenced sources, there are varying approaches to validation and varying descriptions of validation at different stages in method development. This discussion focuses on validation and verification of fully developed methods and instrumentation that have been offered up for use or approval by other laboratories or official consensus bodies such as ASTM International, the International Standards Organization (ISO) and the Association of Official Analytical Chemists (AOAC). This review was conducted as part of a collaborative effort to investigate and improve the state of validation for measuring beryllium in the workplace and the environment. Documents and publications from the United States and Europe are included. Unless otherwise specified, all documents were published in English.

  20. VALIDATION OF ANALYTICAL METHODS AND INSTRUMENTATION FOR BERYLLIUM MEASUREMENT: REVIEW AND SUMMARY OF AVAILABLE GUIDES, PROCEDURES, AND PROTOCOLS

    Energy Technology Data Exchange (ETDEWEB)

    Ekechukwu, A

    2009-05-27

    Method validation is the process of evaluating whether an analytical method is acceptable for its intended purpose. For pharmaceutical methods, guidelines from the United States Pharmacopeia (USP), International Conference on Harmonisation (ICH), and the United States Food and Drug Administration (USFDA) provide a framework for performing such valications. In general, methods for regulatory compliance must include studies on specificity, linearity, accuracy, precision, range, detection limit, quantitation limit, and robustness. Elements of these guidelines are readily adapted to the issue of validation for beryllium sampling and analysis. This document provides a listing of available sources which can be used to validate analytical methods and/or instrumentation for beryllium determination. A literature review was conducted of available standard methods and publications used for method validation and/or quality control. A comprehensive listing of the articles, papers and books reviewed is given in the Appendix. Available validation documents and guides are listed therein; each has a brief description of application and use. In the referenced sources, there are varying approches to validation and varying descriptions of the valication process at different stages in method development. This discussion focuses on valication and verification of fully developed methods and instrumentation that have been offered up for use or approval by other laboratories or official consensus bodies such as ASTM International, the International Standards Organization (ISO) and the Association of Official Analytical Chemists (AOAC). This review was conducted as part of a collaborative effort to investigate and improve the state of validation for measuring beryllium in the workplace and the environment. Documents and publications from the United States and Europe are included. Unless otherwise specified, all referenced documents were published in English.

  1. Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts.

    Science.gov (United States)

    Hollands, Wendy J; Voorspoels, Stefan; Jacobs, Griet; Aaby, Kjersti; Meisland, Ane; Garcia-Villalba, Rocio; Tomas-Barberan, Francisco; Piskula, Mariusz K; Mawson, Deborah; Vovk, Irena; Needs, Paul W; Kroon, Paul A

    2017-04-28

    There is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared two types of flavanol extracts from freeze-dried apples; one was an epicatechin-rich extract containing ∼30% (w/w) monomeric (-)-epicatechin which also contained oligomeric procyanidins (Extract A), the second was an oligomeric procyanidin-rich extract depleted of epicatechin (Extract B). The parameters considered for method optimisation were HPLC columns and conditions, sample heating, mass of extract and dilution volumes. The performance characteristics considered for method validation included standard linearity, method sensitivity, precision and trueness. Eight laboratories participated in the method evaluation. Chromatographic separation of the analytes was best achieved utilizing a Hilic column with a binary mobile phase consisting of acidic acetonitrile and acidic aqueous methanol. The final method showed linearity for epicatechin in the range 5-100μg/mL with a correlation co-efficient >0.999. Intra-day and inter-day precision of the analytes ranged from 2 to 6% and 2 to 13% respectively. Up to dp3, trueness of the method was >95% but decreased with increasing dp. Within laboratory precision showed RSD values <5 and 10% for monomers and oligomers, respectively. Between laboratory precision was 4 and 15% (Extract A) and 7 and 30% (Extract B) for monomers and oligomers, respectively. An analytical method for the separation, identification and quantification of procyanidins in an apple extract was developed, validated and assessed. The results of the inter-laboratory evaluation indicate that the method is reliable and reproducible. Copyright © 2017. Published by Elsevier B.V.

  2. Impurities in biogas - validation of analytical methods for siloxanes; Foeroreningar i biogas - validering av analysmetodik foer siloxaner

    Energy Technology Data Exchange (ETDEWEB)

    Arrhenius, Karine; Magnusson, Bertil; Sahlin, Eskil [SP Technical Research Institute of Sweden, Boraas (Sweden)

    2011-11-15

    Biogas produced from digester or landfill contains impurities which can be harmful for component that will be in contact with the biogas during its utilization. Among these, the siloxanes are often mentioned. During combustion, siloxanes are converted to silicon dioxide which accumulates on the heated surfaces in combustion equipment. Silicon dioxide is a solid compound and will remain in the engine and cause damages. Consequently, it is necessary to develop methods for the accurate determination of these compounds in biogases. In the first part of this report, a method for analysis of siloxanes in biogases was validated. The sampling was performed directly at the plant by drawing a small volume of biogas onto an adsorbent tube under a short period of time. These tubes were subsequently sent to the laboratory for analysis. The purpose of method validation is to demonstrate that the established method is fit for the purpose. This means that the method, as used by the laboratory generating the data, will provide data that meets a set of criteria concerning precision and accuracy. At the end, the uncertainty of the method was calculated. In the second part of this report, the validated method was applied to real samples collected in waste water treatment plants, co-digestion plants and plants digesting other wastes (agriculture waste). Results are presented at the end of this report. As expected, the biogases from waste water treatment plants contained largely higher concentrations of siloxanes than biogases from co-digestion plants and plants digesting agriculture wastes. The concentration of siloxanes in upgraded biogas regardless of which feedstock was digested and which upgrading technique was used was low.

  3. Validation of an analytical method for the determination of the sodium content in foods

    International Nuclear Information System (INIS)

    Valverde Montero, Ericka; Silva Trejos, Paulina

    2012-01-01

    The analytical methodology for quantitative determination of sodium in foods by flame atomic absorption spectrometry was validated. The samples of 0,5 g was realized by microwave oven with 5,0 mL of nitric acid (HNO 3 ) to 65% by mass. The linearity range has been from 0,043 mg/L to 0,70 mg/L with a correlation coefficient equal to 0,998. The detection and quantification limits have reported 0,025 mg/L and 0,043 mg/L, respectively; with 0,805 Lmg -1 of calibration sensitivity and 44 Lmg -1 of analytical sensitivity. The precision was evaluated in terms of repeatability and have obtained a value equal to 2,9% RDS r . The trueness was determined using three NIST ® , certified standards SRM 1846 Infant Formula with a reported value for sodium of (2310 ± 130) mg/kg, SRM 8414 Bovine Muscle Powder with a reported value for sodium of (0,210 ± 0,008)% and SRM 8415 Whole Egg Powder with a reported value for sodium of (0,377 ± 0,034)% by mass. The bias have obtained an average between(-0,010 to 0,009) mg/L. From the list of foods that were selected for the study, for example, whole milk powder, white wheat bread, fresh cheese and mozzarella cheese have submitted highest content in sodium concentrations, ranging from (106 to 452) mg Na /100g. (author) [es

  4. Validation of the Analytical Method for the Determination of Flavonoids in Broccoli

    Directory of Open Access Journals (Sweden)

    Tuszyńska Magdalena

    2014-09-01

    Full Text Available A simple, accurate and selective HPLC method was developed and validated for determination of quercetin and kaempferol, which are the main flavonols in broccoli. The separation was achieved on a reversed-phase C18 column using a mobile phase composed of methanol/water (60/40 and phosphoric acid 0.2% at a flow rate of 1.0 ml min-1. The detection was carried out on a DAD detector at 370 nm. This method was validated according to the requirements for new methods, which include selectivity, linearity, precision, accuracy, limit of detection and limit of quantitation. The current method demonstrates good linearity, with R2 > 0.99. The recovery is within 98.07-102.15% and 97.92-101.83% for quercetin and kaempferol, respectively. The method is selective, in that quercetin and kaempferol are well separated from other compounds of broccoli with good resolution. The low limit of detection and limit of quantitation of quercetin and kaempferol enable the detection and quantitation of these flavonoids in broccoli at low con–centrations.

  5. Analytical Method Development and Validation of Solifenacin in Pharmaceutical Dosage Forms by RP-HPLC

    OpenAIRE

    Shaik, Rihana Parveen; Puttagunta, Srinivasa Babu; Kothapalli Bannoth, Chandrasekar; Challa, Bala Sekhara Reddy

    2014-01-01

    A new, accurate, precise, and robust HPLC method was developed and validated for the determination of solifenacin in tablet dosage form. The chromatographic separation was achieved on an Inertsil ODS 3V C18 (150 mm × 4.6 mm, 5 μm) stationary phase maintained at ambient temperature with a mobile phase combination of monobasic potassium phosphate (pH 3.5) containing 0.1% triethylamine and methanol (gradient mode) at a flow rate of 1.5 mL/min, and the detection was carried out by using UV detect...

  6. Calculations for Adjusting Endogenous Biomarker Levels During Analytical Recovery Assessments for Ligand-Binding Assay Bioanalytical Method Validation.

    Science.gov (United States)

    Marcelletti, John F; Evans, Cindy L; Saxena, Manju; Lopez, Adriana E

    2015-07-01

    It is often necessary to adjust for detectable endogenous biomarker levels in spiked validation samples (VS) and in selectivity determinations during bioanalytical method validation for ligand-binding assays (LBA) with a matrix like normal human serum (NHS). Described herein are case studies of biomarker analyses using multiplex LBA which highlight the challenges associated with such adjustments when calculating percent analytical recovery (%AR). The LBA test methods were the Meso Scale Discovery V-PLEX® proinflammatory and cytokine panels with NHS as test matrix. The NHS matrix blank exhibited varied endogenous content of the 20 individual cytokines before spiking, ranging from undetectable to readily quantifiable. Addition and subtraction methods for adjusting endogenous cytokine levels in %AR calculations are both used in the bioanalytical field. The two methods were compared in %AR calculations following spiking and analysis of VS for cytokines having detectable endogenous levels in NHS. Calculations for %AR obtained by subtracting quantifiable endogenous biomarker concentrations from the respective total analytical VS values yielded reproducible and credible conclusions. The addition method, in contrast, yielded %AR conclusions that were frequently unreliable and discordant with values obtained with the subtraction adjustment method. It is shown that subtraction of assay signal attributable to matrix is a feasible alternative when endogenous biomarkers levels are below the limit of quantitation, but above the limit of detection. These analyses confirm that the subtraction method is preferable over that using addition to adjust for detectable endogenous biomarker levels when calculating %AR for biomarker LBA.

  7. The role of validated analytical methods in JECFA drug assessments and evaluation for recommending MRLs.

    Science.gov (United States)

    Boison, Joe O

    2016-05-01

    The Joint Food and Agriculture Organization and World Health Organization (FAO/WHO) Expert Committee on Food Additives (JECFA) is one of three Codex committees tasked with applying risk analysis and relying on independent scientific advice provided by expert bodies organized by FAO/WHO when developing standards. While not officially part of the Codex Alimentarius Commission structure, JECFA provides independent scientific advice to the Commission and its specialist committees such as the Codex Committee on Residues of Veterinary Drugs in Foods (CCRVDF) in setting maximum residue limits (MRLs) for veterinary drugs. Codex methods of analysis (Types I, II, III, and IV) are defined in the Codex Procedural Manual as are criteria to be used for selecting methods of analysis. However, if a method is to be used under a single laboratory condition to support regulatory work, it must be validated according to an internationally recognized protocol and the use of the method must be embedded in a quality assurance system in compliance with ISO/IEC 17025:2005. This paper examines the attributes of the methods used to generate residue depletion data for drug registration and/or licensing and for supporting regulatory enforcement initiatives that experts consider to be useful and appropriate in their assessment of methods of analysis. Copyright © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis © 2016 John Wiley & Sons, Ltd. © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis © 2016 John Wiley & Sons, Ltd.

  8. "INTRODUCING A FULL VALIDATED ANALYTICAL PROCEDURE AS AN OFFICIAL COMPENDIAL METHOD FOR FENTANYL TRANSDERMAL PATCHES"

    Directory of Open Access Journals (Sweden)

    Amir Mehdizadeh

    2005-04-01

    Full Text Available A simple, sensitive and specific HPLC method and also a simple and fast extraction procedure were developed for quantitative analysis of fentanyl transdermal patches. Chloroform, methanol and ethanol were used as extracting solvents with recovery percent of 92.1, 94.3 and 99.4% respectively. Fentanyl was extracted with ethanol and the eluted fentanyl through the C18 column was monitored by UV detection at 230 nm. The linearity was at the range of 0.5-10 µg/mL with correlation coefficient (r2 of 0.9992. Both intra and inter-day accuracy and precision were within acceptable limits. The detection limit (DL and quantitation limit (QL were 0.15 and 0.5 µg/mL, respectively. Other validation characteristics such as selectivity, robustness and ruggedness were evaluated. Following method validation, a system suitability test (SST including capacity factor (k´, plate number (N, tailing factor (T, and RSD was defined for routine test.

  9. Validation of analytical methods for the quality control of Naproxen suppositories

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Garcia Pulpeiro, Oscar; Hernandez Contreras, Orestes Yuniel

    2011-01-01

    The analysis methods that will be used for the quality control of the future Cuban-made Naproxen suppositories for adults and children were developed for the first time in this paper. One method based on direct ultraviolet spectrophotometry was put forward, which proved to be specific, linear, accurate and precise for the quality control of Naproxen suppositories, taking into account the presence of chromophore groups in their structure. Likewise, the direct semi-aqueous acid-base volumetry method aimed at the quality control of the Naproxen raw material was changed and adapted to the quality control of suppositories. On the basis of the validation process, there was demonstrated the adequate specificity of this method with respect to the formulation components, as well as its linearity, accuracy and precision in 1-3 mg/ml range. The final results were compared and no significant statistical differences among the replicas per each dose were found in both methods; therefore, both may be used in the quality control of Naproxen suppositories

  10. Development and validation of analytical method for the estimation of nateglinide in rabbit plasma

    Directory of Open Access Journals (Sweden)

    Nihar Ranjan Pani

    2012-12-01

    Full Text Available Nateglinide has been widely used in the treatment of type-2 diabetics as an insulin secretogoga. A reliable, rapid, simple and sensitive reversed-phase high performance liquid chromatography (RP-HPLC method was developed and validated for determination of nateglinide in rabbit plasma. The method was developed on Hypersil BDSC-18 column (250 mm×4.6 mm, 5 mm using a mobile phase of 10 mM phosphate buffer (pH 2.5 and acetonitrile (35:65, v/v. The elute was monitored with the UV–vis detector at 210 nm with a flow rate of 1 mL/min. Calibration curve was linear over the concentration range of 25–2000 ng/mL. The retention times of nateglinide and internal standard (gliclazide were 9.608 min and 11.821 min respectively. The developed RP-HPLC method can be successfully applied to the quantitative pharmacokinetic parameters determination of nateglinide in rabbit model. Keywords: HPLC, Nateglinide, Rabbit plasma, Pharmacokinetics

  11. Suspended sediment assessment by combining sound attenuation and backscatter measurements - analytical method and experimental validation

    Science.gov (United States)

    Guerrero, Massimo; Di Federico, Vittorio

    2018-03-01

    The use of acoustic techniques has become common for estimating suspended sediment in water environments. An emitted beam propagates into water producing backscatter and attenuation, which depend on scattering particles concentration and size distribution. Unfortunately, the actual particles size distribution (PSD) may largely affect the accuracy of concentration quantification through the unknown coefficients of backscattering strength, ks2, and normalized attenuation, ζs. This issue was partially solved by applying the multi-frequency approach. Despite this possibility, a relevant scientific and practical question remains regarding the possibility of using acoustic methods to investigate poorly sorted sediment in the spectrum ranging from clay to fine sand. The aim of this study is to investigate the possibility of combining the measurement of sound attenuation and backscatter to determine ζs for the suspended particles and the corresponding concentration. The proposed method is moderately dependent from actual PSD, thus relaxing the need of frequent calibrations to account for changes in ks2 and ζs coefficients. Laboratory tests were conducted under controlled conditions to validate this measurement technique. With respect to existing approaches, the developed method more accurately estimates the concentration of suspended particles ranging from clay to fine sand and, at the same time, gives an indication on their actual PSD.

  12. Analytical Validation of a New Enzymatic and Automatable Method for d-Xylose Measurement in Human Urine Samples

    Directory of Open Access Journals (Sweden)

    Israel Sánchez-Moreno

    2017-01-01

    Full Text Available Hypolactasia, or intestinal lactase deficiency, affects more than half of the world population. Currently, xylose quantification in urine after gaxilose oral administration for the noninvasive diagnosis of hypolactasia is performed with the hand-operated nonautomatable phloroglucinol reaction. This work demonstrates that a new enzymatic xylose quantification method, based on the activity of xylose dehydrogenase from Caulobacter crescentus, represents an excellent alternative to the manual phloroglucinol reaction. The new method is automatable and facilitates the use of the gaxilose test for hypolactasia diagnosis in the clinical practice. The analytical validation of the new technique was performed in three different autoanalyzers, using buffer or urine samples spiked with different xylose concentrations. For the comparison between the phloroglucinol and the enzymatic assays, 224 urine samples of patients to whom the gaxilose test had been prescribed were assayed by both methods. A mean bias of −16.08 mg of xylose was observed when comparing the results obtained by both techniques. After adjusting the cut-off of the enzymatic method to 19.18 mg of xylose, the Kappa coefficient was found to be 0.9531, indicating an excellent level of agreement between both analytical procedures. This new assay represents the first automatable enzymatic technique validated for xylose quantification in urine.

  13. Wetting boundary condition for the color-gradient lattice Boltzmann method: Validation with analytical and experimental data

    Science.gov (United States)

    Akai, Takashi; Bijeljic, Branko; Blunt, Martin J.

    2018-06-01

    In the color gradient lattice Boltzmann model (CG-LBM), a fictitious-density wetting boundary condition has been widely used because of its ease of implementation. However, as we show, this may lead to inaccurate results in some cases. In this paper, a new scheme for the wetting boundary condition is proposed which can handle complicated 3D geometries. The validity of our method for static problems is demonstrated by comparing the simulated results to analytical solutions in 2D and 3D geometries with curved boundaries. Then, capillary rise simulations are performed to study dynamic problems where the three-phase contact line moves. The results are compared to experimental results in the literature (Heshmati and Piri, 2014). If a constant contact angle is assumed, the simulations agree with the analytical solution based on the Lucas-Washburn equation. However, to match the experiments, we need to implement a dynamic contact angle that varies with the flow rate.

  14. Validation of an analytical method for determining halothane in urine as an instrument for evaluating occupational exposure

    International Nuclear Information System (INIS)

    Gonzalez Chamorro, Rita Maria; Jaime Novas, Arelis; Diaz Padron, Heliodora

    2010-01-01

    The occupational exposure to harmful substances may impose the apparition of determined significative changes in the normal physiology of the organism when the adequate security measures are not taken in time in a working place where the risk may be present. Among the chemical risks that may affect the workers' health are the inhalable anesthetic agents. With the objective to take the first steps for the introduction of an epidemiological surveillance system to this personnel, an analytical method for determining this anesthetic in urine was validated with the instrumental conditions created in our laboratory. To carry out this validation the following parameters were taken into account: specificity, lineament, precision, accuracy, detection limit and quantification limit, and the uncertainty of the method was calculated. In the validation procedure it was found that the technique is specific and precise, the detection limit was of 0,118 μg/L, and of the quantification limit of 0,354 μg/L. The global uncertainty was of 0,243, and the expanded of 0,486. The validated method, together with the posterior introduction of the biological exposure limits, will serve as an auxiliary means of diagnosis which will allow us a periodical control of the personnel exposure

  15. Adequacy and validation of an analytical method for the quantification of lead in chamomile tisanes produced in Costa Rica

    International Nuclear Information System (INIS)

    Blanco Barrantes, Jeimy

    2014-01-01

    An analytical methodology is developed and validated to quantify lead in chamomile tisanes. Lead is quantified by utilizing the technique of flame atomic absorption spectroscopy in three brands of chamomile tisanes sold in Costa Rica to determine its safety and quality based on international standards. A method of sample preparation is established through a comparison of different forms of extraction. The acid digestion extraction method has been the procedure utilized, reaching an average recovery percentage of 97,1%, with a standard deviation of 2,3%. The optimization of the chosen analytical procedure and complete validation is performed. The results obtained in the validation of the analytical procedure have shown that the interval where is generated the best calibration curve in terms of the correlation coefficient and the value of the statistically significant intercept equal to zero, have been the comprised between (0,2-3,2) μg/mL (r 2 =0,9996), corresponding to a range between 20% to 320% of the maximum allowed limit. In addition, the procedure has been adequate in terms of accuracy (average recovery percentage 101,1%) and precision under repeatability and intermediate precision (RSD max. 9,3%) and limit of quantification (0,2551 μg/mL). The safety criterion of World Health Organization (WHO) is determined with respect to the concentration of lead in the analyzed products. The 9 analyzed samples of products to prepare chamomile tisanes have stayed without evidencing concentrations of lead above the limit value of 10 μg/g suggested for medicinal herbs by WHO [es

  16. Analytical method for the identification and assay of 12 phthalates in cosmetic products: application of the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques".

    Science.gov (United States)

    Gimeno, Pascal; Maggio, Annie-Françoise; Bousquet, Claudine; Quoirez, Audrey; Civade, Corinne; Bonnet, Pierre-Antoine

    2012-08-31

    Esters of phthalic acid, more commonly named phthalates, may be present in cosmetic products as ingredients or contaminants. Their presence as contaminant can be due to the manufacturing process, to raw materials used or to the migration of phthalates from packaging when plastic (polyvinyl chloride--PVC) is used. 8 phthalates (DBP, DEHP, BBP, DMEP, DnPP, DiPP, DPP, and DiBP), classified H360 or H361, are forbidden in cosmetics according to the European regulation on cosmetics 1223/2009. A GC/MS method was developed for the assay of 12 phthalates in cosmetics, including the 8 phthalates regulated. Analyses are carried out on a GC/MS system with electron impact ionization mode (EI). The separation of phthalates is obtained on a cross-linked 5%-phenyl/95%-dimethylpolysiloxane capillary column 30 m × 0.25 mm (i.d.) × 0.25 mm film thickness using a temperature gradient. Phthalate quantification is performed by external calibration using an internal standard. Validation elements obtained on standard solutions, highlight a satisfactory system conformity (resolution>1.5), a common quantification limit at 0.25 ng injected, an acceptable linearity between 0.5 μg mL⁻¹ and 5.0 μg mL⁻¹ as well as a precision and an accuracy in agreement with in-house specifications. Cosmetic samples ready for analytical injection are analyzed after a dilution in ethanol whereas more complex cosmetic matrices, like milks and creams, are assayed after a liquid/liquid extraction using ter-butyl methyl ether (TBME). Depending on the type of cosmetics analyzed, the common limits of quantification for the 12 phthalates were set at 0.5 or 2.5 μg g⁻¹. All samples were assayed using the analytical approach described in the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques". This analytical protocol is particularly adapted when it is not possible to make reconstituted sample matrices. Copyright © 2012

  17. Validation of an analytical method applicable to study of 1 mg/mL oral Risperidone solution stability

    International Nuclear Information System (INIS)

    Abreu Alvarez, Maikel; Garcia Penna, Caridad Margarita; Martinez Miranda, Lissette

    2010-01-01

    A validated analytical method by high-performance liquid chromatography (HPLC) was applicable to study of 1 mg/mL Risperidone oral solution stability. The above method was linear, accurate, specific and exact. A stability study of the 1 mg/mL Risperidone oral solution was developed determining its expiry date. The shelf life study was conducted for 24 months at room temperature; whereas the accelerated stability study was conducted with product under influence of humidity and temperature; analysis was made during 3 months. Formula fulfilled the quality specifications described in Pharmacopeia. The results of stability according to shelf life after 24 months showed that the product maintains the parameters determining its quality during this time and in accelerated studies there was not significant degradation (p> 0.05) in the product. Under mentioned conditions expiry date was of 2 years

  18. Analytical method development and validation for quantification of uranium by Fourier Transform Infrared Spectroscopy (FTIR) for routine quality control analysis

    International Nuclear Information System (INIS)

    Pereira, Elaine; Silva, Ieda de S.; Gomide, Ricardo G.; Pires, Maria Aparecida F.

    2015-01-01

    This work presents a low cost, simple and new methodology for direct determination uranium in different matrices uranium: organic phase (UO 2 (NO 3 ) 2 .2TBP - uranyl nitrate complex) and aqueous phase (UO 2 (NO 3 ) 2 - NTU - uranyl nitrate), based on Fourier Transform Infrared spectroscopy (FTIR) using KBr pellets technique. The analytical validation is essential to define if a developed methodology is completely adjusted to the objectives that it is destined and is considered one of the main instruments of quality control. The parameters used in the validation process were: selectivity, linearity, limits of detection (LD) and quantitation (LQ), precision (repeatability and intermediate precision), accuracy and robustness. The method for uranium in organic phase (UO 2 (NO 3 ) 2 .2TBP in hexane/embedded in KBr) was linear (r=0.9989) over the range of 1.0 g L -1 a 14.3 g L -1 , LD were 92.1 mg L -1 and LQ 113.1 mg L -1 , precision (RSD < 1.6% and p-value < 0.05), accurate (recovery of 100.1% - 102.9%). The method for uranium aqueous phase (UO 2 (NO 3 )2/embedded in KBr) was linear (r=0.9964) over the range of 5.4 g L -1 a 51.2 g L -1 , LD were 835 mg L -1 and LQ 958 mg L -1 , precision (RSD < 1.0% and p-value < 0.05), accurate (recovery of 99.1% - 102.0%). The FTIR method is robust regarding most of the variables analyzed, as the difference between results obtained under nominal and modified conditions were lower than the critical value for all analytical parameters studied. Some process samples were analyzed in FTIR and compared with gravimetric and x ray fluorescence (XRF) analyses showing similar results in all three methods. The statistical tests (Student-t and Fischer) showed that the techniques are equivalent. (author)

  19. Validation of analytical method to quality control and the stability study of 0.025 % eyedrops Ketotiphen

    International Nuclear Information System (INIS)

    Troche Concepcion, Yenilen; Romero Diaz, Jacqueline Aylema; Garcia Penna, Caridad M

    2010-01-01

    The Ketotiphen eyedrop is prescribed to relief the signs and symptoms of allergic conjunctivitis due to its potent H 1a ntihistaminic effect showing some ability to inhibit the histamine release and other mediators in cases of mastocytosis. The aim of present paper was to develop and validate an analytical method for the high-performance liquid chromatography, to quality control and the stability studies of 0.025 % eyedrop Ketotiphen. Method was based on active principle separation by means of a Lichrosorb RP-18 (5 μm) (250 x 4 mm), with UV detection to 296 nm using a mobile phase including a non-gasified mixture of methanol:buffer-phosphate (75:25; pH 8.5) adding 1 mL of Isopropanol by each 1 000 mL of the previous mixture at a 1.2 mL/min flow velocity. The analytical method was linear, accurate, specific and exact during the study concentrations

  20. Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges

    Directory of Open Access Journals (Sweden)

    Nidal Batrawi

    2017-02-01

    Full Text Available Medroxyprogesterone acetate is widely used in veterinary medicine as intravaginal dosage for the synchronization of breeding cycle in ewes and goats. The main goal of this study was to develop reverse-phase high-performance liquid chromatography method for the quantification of medroxyprogesterone acetate in veterinary vaginal sponges. A single high-performance liquid chromatography/UV isocratic run was used for the analytical assay of the active ingredient medroxyprogesterone. The chromatographic system consisted of a reverse-phase C18 column as the stationary phase and a mixture of 60% acetonitrile and 40% potassium dihydrogen phosphate buffer as the mobile phase; the pH was adjusted to 5.6. The method was validated according to the International Council for Harmonisation (ICH guidelines. Forced degradation studies were also performed to evaluate the stability-indicating properties and specificity of the method. Medroxyprogesterone was eluted at 5.9 minutes. The linearity of the method was confirmed in the range of 0.0576 to 0.1134 mg/mL ( R 2 > 0.999. The limit of quantification was shown to be 3.9 µg/mL. Precision and accuracy ranges were found to be %RSD <0.2 and 98% to 102%, respectively. Medroxyprogesterone capacity factor value of 2.1, tailing factor value of 1.03, and resolution value of 3.9 were obtained in accordance with ICH guidelines. Based on the obtained results, a rapid, precise, accurate, sensitive, and cost-effective analysis procedure was proposed for quantitative determination of medroxyprogesterone in vaginal sponges. This analytical method is the only available method to analyse medroxyprogesterone in veterinary intravaginal dosage form.

  1. Development and Validation of HPLC Analytical Method for Chlorantraniliprole in Bulk and in the Formulation

    Directory of Open Access Journals (Sweden)

    Kapupara Pankaj P.

    2018-03-01

    Full Text Available Background: Chlorantraniliprole is widely used as a pesticide. It is only soluble in dimethyl formamide. However, most of the reported methods used acetonitrile and other solvents.

  2. Validation of an analytical method for the determination in serum of ...

    African Journals Online (AJOL)

    Background: Inter-individual variability in clinical response to psychotropic drugs remains problematic in management of mental illnesses. The patients differ in their ability to absorb, distribute, metabolize and eliminate drugs due to genetic peculiarities, concurrent disease, age, or concomitant medication. Methods: A simple ...

  3. Analytical method development and Validation of Aml odipine Besylate and Nebivolol in their Dosage Form

    OpenAIRE

    Patel Jignesh; Patel Mandev

    2014-01-01

    This work is concerned with application of simple, economical, precise, accurate and reproducible reverse phase high performance liquid chromatographic (RP-HPLC) method for simultaneous estimation of Nebivolol hydrochloride(NBH) and S-Amlodipine besylate (AMB) on thermo Hypersil C18 (Thermo Electron Corporation) (250 x 4.6 mm, 5 μm) using Acetonitrile and Phosphate buffer (pH 2.5 ± 0.1) in ratio of 60:40 as mobile phase. pH of buffer adjusted to 2.5 ± 0.1 with O-phosphoric acid. The flow rate...

  4. A Validated Reverse Phase HPLC Analytical Method for Quantitation of Glycoalkaloids in Solanum lycocarpum and Its Extracts

    Directory of Open Access Journals (Sweden)

    Renata Fabiane Jorge Tiossi

    2012-01-01

    Full Text Available Solanum lycocarpum (Solanaceae is native to the Brazilian Cerrado. Fruits of this species contain the glycoalkaloids solasonine (SN and solamargine (SM, which display antiparasitic and anticancer properties. A method has been developed for the extraction and HPLC-UV analysis of the SN and SM in different parts of S. lycocarpum, mainly comprising ripe and unripe fruits, leaf, and stem. This analytical method was validated and gave good detection response with linearity over a dynamic range of 0.77–1000.00 μg mL−1 and recovery in the range of 80.92–91.71%, allowing a reliable quantitation of the target compounds. Unripe fruits displayed higher concentrations of glycoalkaloids (1.04% ± 0.01 of SN and 0.69% ± 0.00 of SM than the ripe fruits (0.83% ± 0.02 of SN and 0.60% ± 0.01 of SM. Quantitation of glycoalkaloids in the alkaloidic extract gave 45.09% ± 1.14 of SN and 44.37% ± 0.60 of SM, respectively.

  5. Use of reference materials for validating analytical methods. Applied to the determination of As, Co, Na, Hg, Se and Fe using neutron activation analysis

    International Nuclear Information System (INIS)

    Munoz, L; Andonie, O; Kohnenkamp, I

    2000-01-01

    The main purpose of an analytical laboratory is to provide reliable information on the nature and composition of the materials submitted for analysis. This purpose can only be attained if analytical methodologies that have the attributes of accuracy, precision, specificity and sensitivity, among others, are used. The process by which these attributes are evaluated is called validation of the analytical method. The Chilean Nuclear Energy Commission's Neutron Activation Analysis Laboratory is applying a quality guarantee program to ensure the quality of its analytical results, which aims, as well, to attain accreditation for some of its measurements. Validation of the analytical methodologies used is an essential part of applying this program. There are many forms of validation, from comparison with reference techniques to participation in inter-comparison rounds. Certified reference materials were used in this work in order to validate the application of neutron activation analysis in determining As, Co, Na, Hg, Se and Fe in shellfish samples. The use of reference materials was chosen because it is a simple option that easily detects sources of systematic errors. Neutron activation analysis is an instrumental analytical method that does not need chemical treatment and that is based on processes which take place in the nuclei of atoms, making the matrix effects unimportant and different biological reference materials can be used. The following certified reference materials were used for validating the method used: BCR human hair 397, NRCC dogfish muscle DORM-2, NRCC -dogfish liver DOLT-2, NIST - oyster tissue 1566, NIES - mussel 6 and BCR - tuna fish 464. The reference materials were analyzed using the procedure developed for the shellfish samples and the above-mentioned elements were determined. With the results obtained, the parameters of accuracy, precision, detection limit, quantification limit and uncertainty associated with the method were determined for each

  6. Analytical method validation of GC-FID for the simultaneous measurement of hydrocarbons (C2-C4) in their gas mixture

    OpenAIRE

    Oman Zuas; Harry budiman; Muhammad Rizky Mulyana

    2016-01-01

    An accurate gas chromatography coupled to a flame ionization detector (GC-FID) method was validated for the simultaneous analysis of light hydrocarbons (C2-C4) in their gas mixture. The validation parameters were evaluated based on the ISO/IEC 17025 definition including method selectivity, repeatability, accuracy, linearity, limit of detection (LOD), limit of quantitation (LOQ), and ruggedness. Under the optimum analytical conditions, the analysis of gas mixture revealed that each target comp...

  7. Validation of an analytical method for the determination of spiramycin, virginiamycin and tylosin in feeding-stuffs bij thin-layer chromatography and bio-autography

    NARCIS (Netherlands)

    Vincent, U.; Gizzi, G.; Holst, von C.; Jong, de J.; Michard, J.

    2007-01-01

    An inter-laboratory validation was carried out to determine the performance characteristics of an analytical method based on thin-layer chromatography (TLC) coupled to microbiological detection (bio-autography) for screening feed samples for the presence of spiramycin, tylosin and virginiamycin.

  8. Supercritical fluid analytical methods

    International Nuclear Information System (INIS)

    Smith, R.D.; Kalinoski, H.T.; Wright, B.W.; Udseth, H.R.

    1988-01-01

    Supercritical fluids are providing the basis for new and improved methods across a range of analytical technologies. New methods are being developed to allow the detection and measurement of compounds that are incompatible with conventional analytical methodologies. Characterization of process and effluent streams for synfuel plants requires instruments capable of detecting and measuring high-molecular-weight compounds, polar compounds, or other materials that are generally difficult to analyze. The purpose of this program is to develop and apply new supercritical fluid techniques for extraction, separation, and analysis. These new technologies will be applied to previously intractable synfuel process materials and to complex mixtures resulting from their interaction with environmental and biological systems

  9. Development and validation of a multi-analyte method for the regulatory control of carotenoids used as feed additives in fish and poultry feed.

    Science.gov (United States)

    Vincent, Ursula; Serano, Federica; von Holst, Christoph

    2017-08-01

    Carotenoids are used in animal nutrition mainly as sensory additives that favourably affect the colour of fish, birds and food of animal origin. Various analytical methods exist for their quantification in compound feed, reflecting the different physico-chemical characteristics of the carotenoid and the corresponding feed additives. They may be natural products or specific formulations containing the target carotenoids produced by chemical synthesis. In this study a multi-analyte method was developed that can be applied to the determination of all 10 carotenoids currently authorised within the European Union for compound feedingstuffs. The method functions regardless of whether the carotenoids have been added to the compound feed via natural products or specific formulations. It is comprised of three steps: (1) digestion of the feed sample with an enzyme; (2) pressurised liquid extraction; and (3) quantification of the analytes by reversed-phase HPLC coupled to a photodiode array detector in the visible range. The method was single-laboratory validated for poultry and fish feed covering a mass fraction range of the target analyte from 2.5 to 300 mg kg - 1 . The following method performance characteristics were obtained: the recovery rate varied from 82% to 129% and precision expressed as the relative standard deviation of intermediate precision varied from 1.6% to 15%. Based on the acceptable performance obtained in the validation study, the multi-analyte method is considered fit for the intended purpose.

  10. Development and validation of an analytical method for quality control and the stability of the eyedrops 10 % Phenylephrine and the 1 % Tropicamide

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad Margarita; Botet Garcia, Martha; Troche Concepcion, Yenilen

    2011-01-01

    An analytical high-performance liquid chromatography method was developed and validated applicable to quality control and to stability study of 10 % phenylephrine plus eyedrops 1 % tropicamide. To quantify simultaneously both active principles in the finished product, separation was carried out through a Lichrosorb RP-18 (15 μm) (260 x 4 mm) column chromatography, with ultraviolet detection at 253 nm using the mobile phase composed of methanol: distilled water (1:1), with 1.1 g of sodium 1-octasulfanate by litre and pH fitted to 3.0 with phosphoric acid and the quantification of this front to a reference sample using the external standard method. The analytical method developed was linear, precise, specific and accurate in the rank of study concentrations, established for the quality control and stability study of the finished product since there were not analytical methods designed for these aims

  11. Development and validation of an analytical method for the determination of lead isotopic composition using ICP-QMS

    OpenAIRE

    Rodríguez-Salazar, M. T.; Morton Bermea, O.; Hernández-Álvarez, E.; García-Arreola, M. E.; Ortuño-Arzate, M. T.

    2010-01-01

    This work reports a method for the precise and accurate determination of Pb isotope composition in soils and geological matrices by ICP-QMS. Three reference materials (AGV-2, SRM 2709 and JSO-1) were repeatedly measured, using ICP-QMS instruments in order to assess the quality of this analytical procedure. Mass discrimination was evaluated for Pb/Pb with Pb isotope reference material NIST SRM 981, and the correction applied to the above mentioned reference materials to achieve good accuracy o...

  12. Development and validation of a simple high-performance liquid chromatography analytical method for simultaneous determination of phytosterols, cholesterol and squalene in parenteral lipid emulsions.

    Science.gov (United States)

    Novak, Ana; Gutiérrez-Zamora, Mercè; Domenech, Lluís; Suñé-Negre, Josep M; Miñarro, Montserrat; García-Montoya, Encarna; Llop, Josep M; Ticó, Josep R; Pérez-Lozano, Pilar

    2018-02-01

    A simple analytical method for simultaneous determination of phytosterols, cholesterol and squalene in lipid emulsions was developed owing to increased interest in their clinical effects. Method development was based on commonly used stationary (C 18 , C 8 and phenyl) and mobile phases (mixtures of acetonitrile, methanol and water) under isocratic conditions. Differences in stationary phases resulted in peak overlapping or coelution of different peaks. The best separation of all analyzed compounds was achieved on Zorbax Eclipse XDB C 8 (150 × 4.6 mm, 5 μm; Agilent) and ACN-H 2 O-MeOH, 80:19.5:0.5 (v/v/v). In order to achieve a shorter time of analysis, the method was further optimized and gradient separation was established. The optimized analytical method was validated and tested for routine use in lipid emulsion analyses. Copyright © 2017 John Wiley & Sons, Ltd.

  13. Analytical method development and validation of spectrofluorimetric and spectrophotometric determination of some antimicrobial drugs in their pharmaceuticals

    Science.gov (United States)

    Ibrahim, F.; Wahba, M. E. K.; Magdy, G.

    2018-01-01

    In this study, three novel, sensitive, simple and validated spectrophotometric and spectrofluorimetric methods have been proposed for estimation of some important antimicrobial drugs. The first two methods have been proposed for estimation of two important third-generation cephalosporin antibiotics namely, cefixime and cefdinir. Both methods were based on condensation of the primary amino group of the studied drugs with acetyl acetone and formaldehyde in acidic medium. The resulting products were measured by spectrophotometric (Method I) and spectrofluorimetric (Method II) tools. Regarding method I, the absorbance was measured at 315 nm and 403 nm with linearity ranges of 5.0-140.0 and 10.0-100.0 μg/mL for cefixime and cefdinir, respectively. Meanwhile in method II, the produced fluorophore was measured at λem 488 nm or 491 nm after excitation at λex 410 nm with linearity ranges of 0.20-10.0 and 0.20-36.0 μg/mL for cefixime and cefdinir, respectively. On the other hand, method III was devoted to estimate nifuroxazide spectrofluorimetrically depending on formation of highly fluorescent product upon reduction of the studied drug with Zinc powder in acidic medium. Measurement of the fluorescent product was carried out at λem 335 nm following excitation at λex 255 nm with linearity range of 0.05 to 1.6 μg/mL. The developed methods were subjected to detailed validation procedure, moreover they were used for the estimation of the concerned drugs in their pharmaceuticals. It was found that there is a good agreement between the obtained results and those obtained by the reported methods.

  14. Optimization of instrumental neutron activation analysis method by means of 2k experimental design technique aiming the validation of analytical procedures

    International Nuclear Information System (INIS)

    Petroni, Robson; Moreira, Edson G.

    2013-01-01

    In this study optimization of procedures and standardization of Instrumental Neutron Activation Analysis (INAA) methods were carried out for the determination of the elements arsenic, chromium, cobalt, iron, rubidium, scandium, selenium and zinc in biological materials. The aim is to validate the analytical methods for future accreditation at the National Institute of Metrology, Quality and Technology (INMETRO). The 2 k experimental design was applied for evaluation of the individual contribution of selected variables of the analytical procedure in the final mass fraction result. Samples of Mussel Tissue Certified Reference Material and multi-element standards were analyzed considering the following variables: sample decay time, counting time and sample distance to detector. The standard multi-element concentration (comparator standard), mass of the sample and irradiation time were maintained constant in this procedure. By means of the statistical analysis and theoretical and experimental considerations it was determined the optimized experimental conditions for the analytical methods that will be adopted for the validation procedure of INAA methods in the Neutron Activation Analysis Laboratory (LAN) of the Research Reactor Center (CRPq) at the Nuclear and Energy Research Institute (IPEN - CNEN/SP). Optimized conditions were estimated based on the results of z-score tests, main effect and interaction effects. The results obtained with the different experimental configurations were evaluated for accuracy (precision and trueness) for each measurement. (author)

  15. Optimization of instrumental neutron activation analysis method by means of 2{sup k} experimental design technique aiming the validation of analytical procedures

    Energy Technology Data Exchange (ETDEWEB)

    Petroni, Robson; Moreira, Edson G., E-mail: rpetroni@ipen.br, E-mail: emoreira@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    In this study optimization of procedures and standardization of Instrumental Neutron Activation Analysis (INAA) methods were carried out for the determination of the elements arsenic, chromium, cobalt, iron, rubidium, scandium, selenium and zinc in biological materials. The aim is to validate the analytical methods for future accreditation at the National Institute of Metrology, Quality and Technology (INMETRO). The 2{sup k} experimental design was applied for evaluation of the individual contribution of selected variables of the analytical procedure in the final mass fraction result. Samples of Mussel Tissue Certified Reference Material and multi-element standards were analyzed considering the following variables: sample decay time, counting time and sample distance to detector. The standard multi-element concentration (comparator standard), mass of the sample and irradiation time were maintained constant in this procedure. By means of the statistical analysis and theoretical and experimental considerations it was determined the optimized experimental conditions for the analytical methods that will be adopted for the validation procedure of INAA methods in the Neutron Activation Analysis Laboratory (LAN) of the Research Reactor Center (CRPq) at the Nuclear and Energy Research Institute (IPEN - CNEN/SP). Optimized conditions were estimated based on the results of z-score tests, main effect and interaction effects. The results obtained with the different experimental configurations were evaluated for accuracy (precision and trueness) for each measurement. (author)

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

    Directory of Open Access Journals (Sweden)

    Ravi Kumar Konda

    2012-10-01

    Full Text Available 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. Keywords: High performance liquid chromatography, Mass spectrometry, Rasagiline, Liquid–liquid extraction

  17. Volatile composition of Merlot red wine and its contribution to the aroma: optimization and validation of analytical method.

    Science.gov (United States)

    Arcari, Stefany Grützmann; Caliari, Vinicius; Sganzerla, Marla; Godoy, Helena Teixeira

    2017-11-01

    A methodology for the determination of volatile compounds in red wine using headspace solid phase microextraction (HS-SPME) combined with gas chromatography-ion trap/ mass spectrometry (GC-IT/MS) and flame ionization detector (GC -FID) was developed, validated and applied to a sample of Brazilian red wine. The optimization strategy was conducted using the Plackett-Burman design for variable selection and central composite rotational design (CCRD). The response surface methodology showed that the performance of the extraction of the volatile compounds using divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber is improved with no sample dilution, the addition of 30% NaCl, applying an extraction temperature of 56°C and extraction time of 55min. The qualitative method allowed the extraction and identification of 60 volatile compounds in the sample studied, notably the classes of esters, alcohols, and fatty acids. Furthermore, the method was successfully validated for the quantification of 55 volatile compounds of importance in wines and applied to twelve samples of Merlot red wine from South of Brazil. The calculation of the odor activity value (OAV) showed the most important components of the samples aroma. Ethyl isovalerate, ethyl hexanoate, 1-hexanol, octanoic acid and ethyl cinnamate had the greatest contribution to the aroma of the wines analyzed, which is predominantly fruity with the presence of herbal and fatty odors. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Validation of an analytical method for simultaneous high-precision measurements of greenhouse gas emissions from wastewater treatment plants using a gas chromatography-barrier discharge detector system.

    Science.gov (United States)

    Pascale, Raffaella; Caivano, Marianna; Buchicchio, Alessandro; Mancini, Ignazio M; Bianco, Giuliana; Caniani, Donatella

    2017-01-13

    Wastewater treatment plants (WWTPs) emit CO 2 and N 2 O, which may lead to climate change and global warming. Over the last few years, awareness of greenhouse gas (GHG) emissions from WWTPs has increased. Moreover, the development of valid, reliable, and high-throughput analytical methods for simultaneous gas analysis is an essential requirement for environmental applications. In the present study, an analytical method based on a gas chromatograph (GC) equipped with a barrier ionization discharge (BID) detector was developed for the first time. This new method simultaneously analyses CO 2 and N 2 O and has a precision, measured in terms of relative standard of variation RSD%, equal to or less than 6.6% and 5.1%, respectively. The method's detection limits are 5.3ppm v for CO 2 and 62.0ppb v for N 2 O. The method's selectivity, linearity, accuracy, repeatability, intermediate precision, limit of detection and limit of quantification were good at trace concentration levels. After validation, the method was applied to a real case of N 2 O and CO 2 emissions from a WWTP, confirming its suitability as a standard procedure for simultaneous GHG analysis in environmental samples containing CO 2 levels less than 12,000mg/L. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Dried blood spot specimen quality and validation of a new pre-analytical processing method for qualitative HIV-1 PCR, KwaZulu-Natal, South Africa

    Science.gov (United States)

    Parboosing, Raveen; Siyaca, Ntombizandile; Moodley, Pravikrishnen

    2016-01-01

    Background Poor quality dried blood spot (DBS) specimens are usually rejected by virology laboratories, affecting early infant diagnosis of HIV. The practice of combining two incompletely-filled DBS in one specimen preparation tube during pre-analytical specimen processing (i.e., the two-spot method) has been implemented to reduce the number of specimens being rejected for insufficient volume. Objectives This study analysed laboratory data to describe the quality of DBS specimens and the use of the two-spot method over a one-year period, then validated the two-spot method against the standard (one-spot) method. Methods Data on HIV-1 PCR test requests submitted in 2014 to the Department of Virology at Inkosi Albert Luthuli Central Hospital in KwaZulu-Natal province, South Africa were analysed to describe reasons for specimen rejection, as well as results of the two-spot method. The accuracy, lower limit of detection and precision of the two-spot method were assessed. Results Of the 88 481 specimens received, 3.7% were rejected for pre-analytical problems. Of those, 48.9% were rejected as a result of insufficient specimen volume. Two health facilities had significantly more specimen rejections than other facilities. The two-spot method prevented 10 504 specimen rejections. The Pearson correlation coefficient comparing the standard to the two-spot method was 0.997. Conclusions The two-spot method was comparable with the standard method of pre-analytical specimen processing. Two health facilities were identified for targeted retraining on specimen quality. The two-spot method of DBS specimen processing can be used as an adjunct to retraining, to reduce the number of specimens rejected and improve linkage to care. PMID:28879108

  20. Analytical Method Validation and Determination of Pyridoxine, Nicotinamide, and Caffeine in Energy Drinks Using Thin Layer Chromatography-Densitometry

    Directory of Open Access Journals (Sweden)

    Florentinus Dika Octa Riswanto

    2015-03-01

    Full Text Available Food supplement which contains vitamins and stimulants such as caffeine were classified as energy drink. TLC-densitometry method was chosen to determine the pyridoxine, nicotinamide, and caffeine in the energy drink sample. TLC plates of silica gel 60 F254 was used as the stationary phase and methanol : ethyl acetate : ammonia 25% (134:77:10 was used as the mobile phase. The correlation coefficient for each pyridoxine, nicotinamide, and caffeine were 0.9982, 0.9997, and 0.9966, respectively. Detection and quantitation limits of from the three analytes were 4.05 and 13.51 µg/mL; 13.15 and 43.83 µg/mL; 5.43 and 18.11 µg/mL, respectively. The recovery of pyridoxine, nicotinamide, and caffeine were within the required limit range of 95-105%. The percent of RSD were below the limit value of 5.7% for caffeine and nicotinamide and 8% for pyridoxine. The content amount of pyridoxine in the sample 1 and 2 were 33.59 ± 0.981 and 30.29 ± 2.061 µg/mL, respectively. The content amount of nicotinamide in the sample 1 and 2 were 106.53 ± 3.521 and 98.20 ± 3.648 µg/mL, respectively. The content amount of caffeine in the sample 1 and 2 were 249.50 ± 5.080 and 252.80 ± 2.640 µg/mL, respectively. Robustness test results showed that the most optimal method conditions should be applied for the analysis.

  1. Dried blood spot specimen quality and validation of a new pre-analytical processing method for qualitative HIV-1 PCR, KwaZulu-Natal, South Africa.

    Science.gov (United States)

    Govender, Kerusha; Parboosing, Raveen; Siyaca, Ntombizandile; Moodley, Pravikrishnen

    2016-01-01

    Poor quality dried blood spot (DBS) specimens are usually rejected by virology laboratories, affecting early infant diagnosis of HIV. The practice of combining two incompletely-filled DBS in one specimen preparation tube during pre-analytical specimen processing (i.e., the two-spot method) has been implemented to reduce the number of specimens being rejected for insufficient volume. This study analysed laboratory data to describe the quality of DBS specimens and the use of the two-spot method over a one-year period, then validated the two-spot method against the standard (one-spot) method. Data on HIV-1 PCR test requests submitted in 2014 to the Department of Virology at Inkosi Albert Luthuli Central Hospital in KwaZulu-Natal province, South Africa were analysed to describe reasons for specimen rejection, as well as results of the two-spot method. The accuracy, lower limit of detection and precision of the two-spot method were assessed. Of the 88 481 specimens received, 3.7% were rejected for pre-analytical problems. Of those, 48.9% were rejected as a result of insufficient specimen volume. Two health facilities had significantly more specimen rejections than other facilities. The two-spot method prevented 10 504 specimen rejections. The Pearson correlation coefficient comparing the standard to the two-spot method was 0.997. The two-spot method was comparable with the standard method of pre-analytical specimen processing. Two health facilities were identified for targeted retraining on specimen quality. The two-spot method of DBS specimen processing can be used as an adjunct to retraining, to reduce the number of specimens rejected and improve linkage to care.

  2. Analytical method validation of GC-FID for the simultaneous measurement of hydrocarbons (C2-C4 in their gas mixture

    Directory of Open Access Journals (Sweden)

    Oman Zuas

    2016-09-01

    Full Text Available An accurate gas chromatography coupled to a flame ionization detector (GC-FID method was validated for the simultaneous analysis of light hydrocarbons (C2-C4 in their gas mixture. The validation parameters were evaluated based on the ISO/IEC 17025 definition including method selectivity, repeatability, accuracy, linearity, limit of detection (LOD, limit of quantitation (LOQ, and ruggedness. Under the optimum analytical conditions, the analysis of gas mixture revealed that each target component was well-separated with high selectivity property. The method was also found to be precise and accurate. The method linearity was found to be high with good correlation coefficient values (R2 ≥ 0.999 for all target components. It can be concluded that the GC-FID developed method is reliable and suitable for determination of light C2-C4 hydrocarbons (including ethylene, propane, propylene, isobutane, and n-butane in their gas mixture. The validated method has successfully been applied to the estimation of hydrocarbons light C2-C4 hydrocarbons in natural gas samples, showing high performance repeatability with relative standard deviation (RSD less than 1.0% and good selectivity with no interference from other possible components could be observed.

  3. Validation of analytical methods in GMP: the disposable Fast Read 102® device, an alternative practical approach for cell counting

    Directory of Open Access Journals (Sweden)

    Gunetti Monica

    2012-05-01

    Full Text Available Abstract Background The quality and safety of advanced therapy products must be maintained throughout their production and quality control cycle to ensure their final use in patients. We validated the cell count method according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use and European Pharmacopoeia, considering the tests’ accuracy, precision, repeatability, linearity and range. Methods As the cell count is a potency test, we checked accuracy, precision, and linearity, according to ICH Q2. Briefly our experimental approach was first to evaluate the accuracy of Fast Read 102® compared to the Bürker chamber. Once the accuracy of the alternative method was demonstrated, we checked the precision and linearity test only using Fast Read 102®. The data were statistically analyzed by average, standard deviation and coefficient of variation percentages inter and intra operator. Results All the tests performed met the established acceptance criteria of a coefficient of variation of less than ten percent. For the cell count, the precision reached by each operator had a coefficient of variation of less than ten percent (total cells and under five percent (viable cells. The best range of dilution, to obtain a slope line value very similar to 1, was between 1:8 and 1:128. Conclusions Our data demonstrated that the Fast Read 102® count method is accurate, precise and ensures the linearity of the results obtained in a range of cell dilution. Under our standard method procedures, this assay may thus be considered a good quality control method for the cell count as a batch release quality control test. Moreover, the Fast Read 102® chamber is a plastic, disposable device that allows a number of samples to be counted in the same chamber. Last but not least, it overcomes the problem of chamber washing after use and so allows a cell count in a clean environment such as that in a

  4. Validation of an analytical method for the determination of aldehydes and acetone present in the ambient air at the metropolitan area of Costa Rica

    International Nuclear Information System (INIS)

    Rojas Marin, Jose Felix

    2010-01-01

    The analytical method validation has been conducted for the simultaneous determination of 15 carbonyl compounds, the main aldehydes and ketones present in ambient air. The compounds have been captured on cartridges packed with silica gel impregnated with 2.4-dinitrophenylhydrazine (DNPH) at a constant flow of about 1 lmin -1 . Carbonyl compounds present have formed the respective products, which are then eluted with acetonitrile (solid phase extraction). The extracts were analyzed by the technique of high resolution liquid chromatography with ultraviolet detector at a wavelength of 360 nm. The following results were obtained during method validation: linearity from 0.03 mgl -1 to 15 mgl -1 , limits of detection and quantification of 0.02 mgl -1 and 0.06 mgl -1 , the accuracy no significant bias at a confidence level of 95%, accuracy for repeatability and producibility of the analytical method are around 1%. Two sampling campaigns were made in dry and rainy seasons of 2009 for areas of San Jose, Heredia and Belen. The predominant compounds were found to be acetone, acetaldehyde and the formaldehyde was the most abundant in the city of San Jose, others do not have significant amounts, so there is strong correlation between formaldehyde and acetaldehyde suggesting that stem from a common source, possibly vehicle emissions. (author) [es

  5. Sewage-based epidemiology in monitoring the use of new psychoactive substances: Validation and application of an analytical method using LC-MS/MS.

    Science.gov (United States)

    Kinyua, Juliet; Covaci, Adrian; Maho, Walid; McCall, Ann-Kathrin; Neels, Hugo; van Nuijs, Alexander L N

    2015-09-01

    Sewage-based epidemiology (SBE) employs the analysis of sewage to detect and quantify drug use within a community. While SBE has been applied repeatedly for the estimation of classical illicit drugs, only few studies investigated new psychoactive substances (NPS). These compounds mimic effects of illicit drugs by introducing slight modifications to chemical structures of controlled illicit drugs. We describe the optimization, validation, and application of an analytical method using liquid chromatography coupled to positive electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seven NPS in sewage: methoxetamine (MXE), butylone, ethylone, methylone, methiopropamine (MPA), 4-methoxymethamphetamine (PMMA), and 4-methoxyamphetamine (PMA). Sample preparation was performed using solid-phase extraction (SPE) with Oasis MCX cartridges. The LC separation was done with a HILIC (150 x 3 mm, 5 µm) column which ensured good resolution of the analytes with a total run time of 19 min. The lower limit of quantification (LLOQ) was between 0.5 and 5 ng/L for all compounds. The method was validated by evaluating the following parameters: sensitivity, selectivity, linearity, accuracy, precision, recoveries and matrix effects. The method was applied on sewage samples collected from sewage treatment plants in Belgium and Switzerland in which all investigated compounds were detected, except MPA and PMA. Furthermore, a consistent presence of MXE has been observed in most of the sewage samples at levels higher than LLOQ. Copyright © 2015 John Wiley & Sons, Ltd.

  6. Validation of analytical methods in GMP: the disposable Fast Read 102® device, an alternative practical approach for cell counting.

    Science.gov (United States)

    Gunetti, Monica; Castiglia, Sara; Rustichelli, Deborah; Mareschi, Katia; Sanavio, Fiorella; Muraro, Michela; Signorino, Elena; Castello, Laura; Ferrero, Ivana; Fagioli, Franca

    2012-05-31

    The quality and safety of advanced therapy products must be maintained throughout their production and quality control cycle to ensure their final use in patients. We validated the cell count method according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use and European Pharmacopoeia, considering the tests' accuracy, precision, repeatability, linearity and range. As the cell count is a potency test, we checked accuracy, precision, and linearity, according to ICH Q2. Briefly our experimental approach was first to evaluate the accuracy of Fast Read 102® compared to the Bürker chamber. Once the accuracy of the alternative method was demonstrated, we checked the precision and linearity test only using Fast Read 102®. The data were statistically analyzed by average, standard deviation and coefficient of variation percentages inter and intra operator. All the tests performed met the established acceptance criteria of a coefficient of variation of less than ten percent. For the cell count, the precision reached by each operator had a coefficient of variation of less than ten percent (total cells) and under five percent (viable cells). The best range of dilution, to obtain a slope line value very similar to 1, was between 1:8 and 1:128. Our data demonstrated that the Fast Read 102® count method is accurate, precise and ensures the linearity of the results obtained in a range of cell dilution. Under our standard method procedures, this assay may thus be considered a good quality control method for the cell count as a batch release quality control test. Moreover, the Fast Read 102® chamber is a plastic, disposable device that allows a number of samples to be counted in the same chamber. Last but not least, it overcomes the problem of chamber washing after use and so allows a cell count in a clean environment such as that in a Cell Factory. In a good manufacturing practice setting the disposable

  7. Theoretical validation of potential habitability via analytical and boosted tree methods: An optimistic study on recently discovered exoplanets

    Science.gov (United States)

    Saha, S.; Basak, S.; Safonova, M.; Bora, K.; Agrawal, S.; Sarkar, P.; Murthy, J.

    2018-04-01

    Seven Earth-sized planets, known as the TRAPPIST-1 system, was discovered with great fanfare in the last week of February 2017. Three of these planets are in the habitable zone of their star, making them potentially habitable planets (PHPs) a mere 40 light years away. The discovery of the closest potentially habitable planet to us just a year before - Proxima b and a realization that Earth-type planets in circumstellar habitable zones are a common occurrence provides the impetus to the existing pursuit for life outside the Solar System. The search for life has two goals essentially: looking for planets with Earth-like conditions (Earth similarity) and looking for the possibility of life in some form (habitability). An index was recently developed, the Cobb-Douglas Habitability Score (CDHS), based on Cobb-Douglas habitability production function (CD-HPF), which computes the habitability score by using measured and estimated planetary parameters. As an initial set, radius, density, escape velocity and surface temperature of a planet were used. The proposed metric, with exponents accounting for metric elasticity, is endowed with analytical properties that ensure global optima and can be scaled to accommodate a finite number of input parameters. We show here that the model is elastic, and the conditions on elasticity to ensure global maxima can scale as the number of predictor parameters increase. K-NN (K-Nearest Neighbor) classification algorithm, embellished with probabilistic herding and thresholding restriction, utilizes CDHS scores and labels exoplanets into appropriate classes via feature-learning methods yielding granular clusters of habitability. The algorithm works on top of a decision-theoretical model using the power of convex optimization and machine learning. The goal is to characterize the recently discovered exoplanets into an "Earth League" and several other classes based on their CDHS values. A second approach, based on a novel feature-learning and

  8. Analytical method (HPLC, validation used for identification and assay of the pharmaceutical active ingredient, Tylosin tartrate for veterinary use and its finite product Tilodem 50, hydrosoluble powder

    Directory of Open Access Journals (Sweden)

    Maria Neagu

    2010-12-01

    Full Text Available In SC DELOS IMPEX ’96 SRL the quality of the active pharmaceutical ingredient (API for the finite product Tilodem 50 - hydrosoluble powder was acomkplished in the respect of last European Pharmacopoeia.The method for analysis used in this purpose was the compendial method „Tylosin tartrate for veterinary use” in EurPh. in vigour edition and represent a variant developed and validation „in house”.The parameters which was included in the methodology validation for chromatographic method are the followings: Selectivity, Linearity, Linearity range, Detection and Quantification limits, Precision, Repeatability (intra day, Inter-Day Reproductibility, Accuracy, Robustness, Solutions’ stability and System suitability. According to the European Pharmacopoeia, the active pharmaceutical ingredient is consistent, in terms of quality, if it contains Tylosin A - minimum 80% and the amount of Tylosin A, B, C, D, at minimum 95%. Identification and determination of each component separately (Tylosin A, B, C, D is possible by chromatographic separation-HPLC. Validation of analytical methods is presented below.

  9. Validation of an analytical method for the determination of polycyclic aromatic hydrocarbons by high efficiency liquid chromatography in PM10 and PM2,5 particles

    International Nuclear Information System (INIS)

    Herrera Murillo, Jorge; Chaves Villalobos, Maria del Carmen

    2012-01-01

    An analytical method was validated for polycyclic aromatic hydrocarbons in PM10 and PM2,5 particles collected from air by high performance liquid chromatography (HPLC) was validated. The PAHs analyzed in the methodology include: Naphthalene, Acenaphthylene, Fluorene, Acenaphthene, Phenanthrene, Anthracene, fluoranthene, pyrene, Benzo (a)anthracene, Chrysene, Benzo (b)fluoranthene, Benzo (k)fluoranthene, Benzo (a)pyrene, Dibenzo (a, h)anthracene, Benzo (g, h, i)perylene and Indeno (1,2,3-CD)pyrene. For these compounds, the detection limit and quantification limit have been between 0,02 and 0,1 mg/l. An equipment DIONEX, ICS 3000 model is used, that has two in series detectors: one ultraviolet model VWD-1, and fluorescence detector, model RF-2000, separating the different absorption and emission signals for proper identification of individual compounds. For all the compounds analyzed, the recovery factor has found not significantly different from each other and the repeatability and reproducibility has been to be suitable for an analytical method, especially for the lighter PAHs. (author) [es

  10. Validated spectroscopic methods for determination of anti-histaminic drug azelastine in pure form: Analytical application for quality control of its pharmaceutical preparations

    Science.gov (United States)

    El-Masry, Amal A.; Hammouda, Mohammed E. A.; El-Wasseef, Dalia R.; El-Ashry, Saadia M.

    2018-02-01

    Two simple, sensitive, rapid, validated and cost effective spectroscopic methods were established for quantification of antihistaminic drug azelastine (AZL) in bulk powder as well as in pharmaceutical dosage forms. In the first method (A) the absorbance difference between acidic and basic solutions was measured at 228 nm, whereas in the second investigated method (B) the binary complex formed between AZL and Eosin Y in acetate buffer solution (pH 3) was measured at 550 nm. Different criteria that have critical influence on the intensity of absorption were deeply studied and optimized so as to achieve the highest absorption. The proposed methods obeyed Beer's low in the concentration range of (2.0-20.0 μg·mL- 1) and (0.5-15.0 μg·mL- 1) with % recovery ± S.D. of (99.84 ± 0.87), (100.02 ± 0.78) for methods (A) and (B), respectively. Furthermore, the proposed methods were easily applied for quality control of pharmaceutical preparations without any conflict with its co-formulated additives, and the analytical results were compatible with those obtained by the comparison one with no significant difference as insured by student's t-test and the variance ratio F-test. Validation of the proposed methods was performed according the ICH guidelines in terms of linearity, limit of quantification, limit of detection, accuracy, precision and specificity, where the analytical results were persuasive. The absorption spectrum of AZL (16 μg·mL- 1) in 0.1 M HCl. The absorption spectrum of AZL (16 μg·mL- 1) in 0.1 M NaOH. The difference absorption spectrum of AZL (16 μg·mL- 1) in 0.1 M NaOH vs 0.1 M HCl. The absorption spectrum of eosin binary complex with AZL (10 μg·mL- 1).

  11. Life cycle management of analytical methods.

    Science.gov (United States)

    Parr, Maria Kristina; Schmidt, Alexander H

    2018-01-05

    In modern process management, the life cycle concept gains more and more importance. It focusses on the total costs of the process from invest to operation and finally retirement. Also for analytical procedures an increasing interest for this concept exists in the recent years. The life cycle of an analytical method consists of design, development, validation (including instrumental qualification, continuous method performance verification and method transfer) and finally retirement of the method. It appears, that also regulatory bodies have increased their awareness on life cycle management for analytical methods. Thus, the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH), as well as the United States Pharmacopeial Forum discuss the enrollment of new guidelines that include life cycle management of analytical methods. The US Pharmacopeia (USP) Validation and Verification expert panel already proposed a new General Chapter 〈1220〉 "The Analytical Procedure Lifecycle" for integration into USP. Furthermore, also in the non-regulated environment a growing interest on life cycle management is seen. Quality-by-design based method development results in increased method robustness. Thereby a decreased effort is needed for method performance verification, and post-approval changes as well as minimized risk of method related out-of-specification results. This strongly contributes to reduced costs of the method during its life cycle. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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).

  13. DEVELOPMENT AND VALIDATION OF AN HPLC-DAD ANALYTICAL METHOD TO QUANTIFY 5-METHOXYFLAVONES IN METHANOLIC EXTRACTS OF Vochysia divergens POHL CULTURED UNDER STRESS CONDITIONS

    Directory of Open Access Journals (Sweden)

    Letícia Pereira Pimenta

    Full Text Available Vochysia divergens Pohl, known as "Cambara" in Brazil, is an invasive species that is expanding throughout Pantanal in Brazil, to form mono-dominant communities. This expansion is affecting the agricultural areas that support the typical seasonal flood and drought conditions of this biome. This article describes the development and validation of an HPLC-DAD analytical method to quantify 5-methoxyflavones in methanolic extracts of greenhouse-grown V. divergens associated with one of two endophytic fungal species Zopfiella tetraspora (Zt or Melanconiella elegans (Me and later subjected to water stress. The developed method gave good validation parameters and was successfully applied to quantify the flavones 3',5-dimethoxy luteolin-7-O-β-glucopyranoside (1, 5-methoxy luteolin (2, and 3',5-dimethoxy luteolin (3 in the target extracts. Inoculation of the plant with Zt decreased the concentration of flavone 1 in the extract by 2.69-fold as compared to the control. Inoculation of the plant with Zt or Me did not significantly alter the contents of flavones 2 and 3 in the extracts as compared to the control. Therefore, the aerial parts of germinated V. divergens plants inoculated with either Zt or Me responded differently in terms of the production of flavones. These results can cast light on the symbiosis between fungal microorganisms and V. divergens, which most likely influences the response of V. divergens to changes in the availability of water in Pantanal.

  14. Development and validation of a 48-target analytical method for high-throughput monitoring of genetically modified organisms.

    Science.gov (United States)

    Li, Xiaofei; Wu, Yuhua; Li, Jun; Li, Yunjing; Long, Likun; Li, Feiwu; Wu, Gang

    2015-01-05

    The rapid increase in the number of genetically modified (GM) varieties has led to a demand for high-throughput methods to detect genetically modified organisms (GMOs). We describe a new dynamic array-based high throughput method to simultaneously detect 48 targets in 48 samples on a Fludigm system. The test targets included species-specific genes, common screening elements, most of the Chinese-approved GM events, and several unapproved events. The 48 TaqMan assays successfully amplified products from both single-event samples and complex samples with a GMO DNA amount of 0.05 ng, and displayed high specificity. To improve the sensitivity of detection, a preamplification step for 48 pooled targets was added to enrich the amount of template before performing dynamic chip assays. This dynamic chip-based method allowed the synchronous high-throughput detection of multiple targets in multiple samples. Thus, it represents an efficient, qualitative method for GMO multi-detection.

  15. Analytical Validation of Quantitative Real-Time PCR Methods for Quantification of Trypanosoma cruzi DNA in Blood Samples from Chagas Disease Patients.

    Science.gov (United States)

    Ramírez, Juan Carlos; Cura, Carolina Inés; da Cruz Moreira, Otacilio; Lages-Silva, Eliane; Juiz, Natalia; Velázquez, Elsa; Ramírez, Juan David; Alberti, Anahí; Pavia, Paula; Flores-Chávez, María Delmans; Muñoz-Calderón, Arturo; Pérez-Morales, Deyanira; Santalla, José; Marcos da Matta Guedes, Paulo; Peneau, Julie; Marcet, Paula; Padilla, Carlos; Cruz-Robles, David; Valencia, Edward; Crisante, Gladys Elena; Greif, Gonzalo; Zulantay, Inés; Costales, Jaime Alfredo; Alvarez-Martínez, Miriam; Martínez, Norma Edith; Villarroel, Rodrigo; Villarroel, Sandro; Sánchez, Zunilda; Bisio, Margarita; Parrado, Rudy; Maria da Cunha Galvão, Lúcia; Jácome da Câmara, Antonia Cláudia; Espinoza, Bertha; Alarcón de Noya, Belkisyole; Puerta, Concepción; Riarte, Adelina; Diosque, Patricio; Sosa-Estani, Sergio; Guhl, Felipe; Ribeiro, Isabela; Aznar, Christine; Britto, Constança; Yadón, Zaida Estela; Schijman, Alejandro G

    2015-09-01

    An international study was performed by 26 experienced PCR laboratories from 14 countries to assess the performance of duplex quantitative real-time PCR (qPCR) strategies on the basis of TaqMan probes for detection and quantification of parasitic loads in peripheral blood samples from Chagas disease patients. Two methods were studied: Satellite DNA (SatDNA) qPCR and kinetoplastid DNA (kDNA) qPCR. Both methods included an internal amplification control. Reportable range, analytical sensitivity, limits of detection and quantification, and precision were estimated according to international guidelines. In addition, inclusivity and exclusivity were estimated with DNA from stocks representing the different Trypanosoma cruzi discrete typing units and Trypanosoma rangeli and Leishmania spp. Both methods were challenged against 156 blood samples provided by the participant laboratories, including samples from acute and chronic patients with varied clinical findings, infected by oral route or vectorial transmission. kDNA qPCR showed better analytical sensitivity than SatDNA qPCR with limits of detection of 0.23 and 0.70 parasite equivalents/mL, respectively. Analyses of clinical samples revealed a high concordance in terms of sensitivity and parasitic loads determined by both SatDNA and kDNA qPCRs. This effort is a major step toward international validation of qPCR methods for the quantification of T. cruzi DNA in human blood samples, aiming to provide an accurate surrogate biomarker for diagnosis and treatment monitoring for patients with Chagas disease. Copyright © 2015 American Society for Investigative Pathology and the Association for Molecular Pathology. Published by Elsevier Inc. All rights reserved.

  16. The analytic Lanczos method

    International Nuclear Information System (INIS)

    Witte, N.S.

    1998-01-01

    The classical formalism of the Moment Problem has been combined with a cumulant approach and applied to the extensive many-body problem. This has yielded many new exact results for many-body systems in the thermodynamic limit - for the ground state energy, for excited state gaps, and for arbitrary ground state averages. The method applies to any extensive Hamiltonian system, for any phase or symmetry arising in the model, whether on a lattice or in the continuum, and for any dimensionality. The theorems are of a nonperturbative nature with respect to any couplings occuring in the model. (Copyright (1998) World Scientific Publishing Co. Pte. Ltd)

  17. Optimisation and validation of analytical methods for the simultaneous extraction of antioxidants: application to the analysis of tomato sauces.

    Science.gov (United States)

    Motilva, Maria-José; Macià, Alba; Romero, Maria-Paz; Labrador, Agustín; Domínguez, Alba; Peiró, Lluís

    2014-11-15

    In the present study, simultaneous extraction of natural antioxidants (phenols and carotenoids) in complex matrices, such as tomato sauces, is presented. The tomato sauce antioxidant compounds studied were the phenolics hydroxytyrosol, from virgin olive oil, quercetin and its derivatives, from onions, and quercetin-rutinoside as well as the carotenoid, lycopene (cis and trans), from tomatoes. These antioxidant compounds were extracted simultaneously with n-hexane/acetone/ethanol (50/25/25, v/v/v). The phenolics were analysed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS), and lycopene (cis- and trans-forms) was analysed using high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD). After studying the parameters of these methods, they were applied to the analysis of virgin olive oil, fresh onion, tomato concentrate and tomato powder, and commercial five tomato sauces. Subsequently, the results obtained in our laboratory were compared with those from the Gallina Blanca Star Group laboratory. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Consistency of FMEA used in the validation of analytical procedures

    DEFF Research Database (Denmark)

    Oldenhof, M.T.; van Leeuwen, J.F.; Nauta, Maarten

    2011-01-01

    is always carried out under the supervision of an experienced FMEA-facilitator and that the FMEA team has at least two members with competence in the analytical method to be validated. However, the FMEAs of both teams contained valuable information that was not identified by the other team, indicating......In order to explore the consistency of the outcome of a Failure Mode and Effects Analysis (FMEA) in the validation of analytical procedures, an FMEA was carried out by two different teams. The two teams applied two separate FMEAs to a High Performance Liquid Chromatography-Diode Array Detection...

  19. Validation of analytical method to calculate the concentration of conjugated monoclonal antibody; Validacao de metodo analitico para calculo de concentracao de anticorpo monoclonal conjugado

    Energy Technology Data Exchange (ETDEWEB)

    Alcarde, Lais F.; Massicano, Adriana V.F.; Oliveira, Ricardo S.; Araujo, Elaine B. de, E-mail: lais_alcarde@hotmail.com [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    The objective of this study was to develop a quantitative analytical method using high performance liquid chromatography (HPLC) to determine the antibody concentration in conjunction with bifunctional chelator. Assays were performed using a high performance liquid chromatograph, and the following conditions were used: flow rate of 1 mL / min, 15 min run time, 0.2 M sodium phosphate buffer pH 7.0 as the mobile phase and column of molecular exclusion BioSep SEC S-3000 (300 x 7.8 mm, 5 μM - Phenomenex). The calibration curve was obtained with AcM diluted in 0.2 M sodium phosphate buffer pH 7.0 by serial dilution, yielding the concentrations: 400 μg/mL, 200 μg/mL, 100 μg/mL, 50 μg/mL, 25 μg/mL and 12.5 μg/mL. From the calibration curve calculated the equation of the line and with it the concentration of the immunoconjugate. To ensure the validity of the method accuracy and precision studies were conducted. The accuracy test consisted in the evaluation of 3 samples of known concentration, being this test performed with low concentrations (50 μg/mL), medium (100 μg/mL) and high (200 μg/mL). The precision test consisted of 3 consecutive measurements of one sample of known concentration, subject to the conditions set forth above for the other tests. The correlation coefficient of the standard curve was greater than 97%, the accuracy was satisfactory at low concentrations as well as accuracy. The method was validated by showing it for the accurate and precise determination of the concentration of the immunoconjugate. Furthermore, this assay was found to be extremely important, because using the correct mass of the protein, the radiochemical purity of the radioimmunoconjugate was above 95% in all studies.

  20. Validation of Analytical Damping Ratio by Fatigue Stress Limit

    Science.gov (United States)

    Foong, Faruq Muhammad; Chung Ket, Thein; Beng Lee, Ooi; Aziz, Abdul Rashid Abdul

    2018-03-01

    The optimisation process of a vibration energy harvester is usually restricted to experimental approaches due to the lack of an analytical equation to describe the damping of a system. This study derives an analytical equation, which describes the first mode damping ratio of a clamp-free cantilever beam under harmonic base excitation by combining the transverse equation of motion of the beam with the damping-stress equation. This equation, as opposed to other common damping determination methods, is independent of experimental inputs or finite element simulations and can be solved using a simple iterative convergence method. The derived equation was determined to be correct for cases when the maximum bending stress in the beam is below the fatigue limit stress of the beam. However, an increasing trend in the error between the experiment and the analytical results were observed at high stress levels. Hence, the fatigue limit stress was used as a parameter to define the validity of the analytical equation.

  1. Develop and validation of an analytic method for the histamine determination in fish, using chromatography liquidates of high efficiency in reverse phase with ultraviolet detection

    International Nuclear Information System (INIS)

    Valverde Chavarria, J. C.

    1997-01-01

    There were determined and optimized the reaction and conditions analysis, for the derivation of the histamine with the reagent of or-ftalaldehido (OPA), it was proven that it is possible to quantify the one derived formed at 333nm. The good conditions crhomatografics settled down for the determination of the histamine in fish by means of the analytic technique of chromatography it liquidates of high efficiency (HPLC) in reverse phase, using the derivatizacion in precolumn of the histamine with the reagent of OPA, with ultraviolet detection at 333nm. The conditions of the proposed methodology were optimized and the variables of analytic acting were validated, for the analytic quantification of the histamine in the mg g-1 environment. The applicability of the methodology was demonstrated in the histamine determination in samples of fresh fish [es

  2. Analytical methods under emergency conditions

    International Nuclear Information System (INIS)

    Sedlet, J.

    1983-01-01

    This lecture discusses methods for the radiochemical determination of internal contamination of the body under emergency conditions, here defined as a situation in which results on internal radioactive contamination are needed quickly. The purpose of speed is to determine the necessity for medical treatment to increase the natural elimination rate. Analytical methods discussed include whole-body counting, organ counting, wound monitoring, and excreta analysis. 12 references

  3. Waste minimization in analytical methods

    International Nuclear Information System (INIS)

    Green, D.W.; Smith, L.L.; Crain, J.S.; Boparai, A.S.; Kiely, J.T.; Yaeger, J.S. Schilling, J.B.

    1995-01-01

    The US Department of Energy (DOE) will require a large number of waste characterizations over a multi-year period to accomplish the Department's goals in environmental restoration and waste management. Estimates vary, but two million analyses annually are expected. The waste generated by the analytical procedures used for characterizations is a significant source of new DOE waste. Success in reducing the volume of secondary waste and the costs of handling this waste would significantly decrease the overall cost of this DOE program. Selection of appropriate analytical methods depends on the intended use of the resultant data. It is not always necessary to use a high-powered analytical method, typically at higher cost, to obtain data needed to make decisions about waste management. Indeed, for samples taken from some heterogeneous systems, the meaning of high accuracy becomes clouded if the data generated are intended to measure a property of this system. Among the factors to be considered in selecting the analytical method are the lower limit of detection, accuracy, turnaround time, cost, reproducibility (precision), interferences, and simplicity. Occasionally, there must be tradeoffs among these factors to achieve the multiple goals of a characterization program. The purpose of the work described here is to add waste minimization to the list of characteristics to be considered. In this paper the authors present results of modifying analytical methods for waste characterization to reduce both the cost of analysis and volume of secondary wastes. Although tradeoffs may be required to minimize waste while still generating data of acceptable quality for the decision-making process, they have data demonstrating that wastes can be reduced in some cases without sacrificing accuracy or precision

  4. Validation for chromatographic and electrophoretic methods

    OpenAIRE

    Ribani, Marcelo; Bottoli, Carla Beatriz Grespan; Collins, Carol H.; Jardim, Isabel Cristina Sales Fontes; Melo, Lúcio Flávio Costa

    2004-01-01

    The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the dif...

  5. Jet substructure with analytical methods

    Energy Technology Data Exchange (ETDEWEB)

    Dasgupta, Mrinal [University of Manchester, Consortium for Fundamental Physics, School of Physics and Astronomy, Manchester (United Kingdom); Fregoso, Alessandro; Powling, Alexander [University of Manchester, School of Physics and Astronomy, Manchester (United Kingdom); Marzani, Simone [Durham University, Institute for Particle Physics Phenomenology, Durham (United Kingdom)

    2013-11-15

    We consider the mass distribution of QCD jets after the application of jet-substructure methods, specifically the mass-drop tagger, pruning, trimming and their variants. In contrast to most current studies employing Monte Carlo methods, we carry out analytical calculations at the next-to-leading order level, which are sufficient to extract the dominant logarithmic behaviour for each technique, and compare our findings to exact fixed-order results. Our results should ultimately lead to a better understanding of these jet-substructure methods which in turn will influence the development of future substructure tools for LHC phenomenology. (orig.)

  6. Decision analytic methods in RODOS

    International Nuclear Information System (INIS)

    Borzenko, V.; French, S.

    1996-01-01

    In the event of a nuclear accident, RODOS seeks to provide decision support at all levels ranging from the largely descriptive to providing a detailed evaluation of the benefits and disadvantages of various countermeasure strategies and ranking them according to the societal preferences as perceived by the decision makers. To achieve this, it must draw upon several decision analytic methods and bring them together in a coherent manner so that the guidance offered to decision makers is consistent from one stage of an accident to the next. The methods used draw upon multi-attribute value and utility theories

  7. A new colorimetric chemosensors for Cu{sup 2+} and Cd{sup 2+} ions detection: Application in environmental water samples and analytical method validation

    Energy Technology Data Exchange (ETDEWEB)

    Tekuri, Venkatadri; Trivedi, Darshak R., E-mail: darshak_rtrivedi@yahoo.co.in

    2017-06-15

    A new heterocyclic thiophene-2-caboxylic acid hydrazide based chemosensor R1 to R4 were designed, synthesized and characterized by various spectroscopic techniques like FT-IR, UV-Vis, {sup 1}H NMR, {sup 13}C NMR, Mass and SC-XRD. The chemosensor R3 showed a significant color change from colorless to yellow in the presence of Cu{sup 2+} ions and chemosensor R4 showed a significant color change from colorless to yellow in the presence of Cd{sup 2+} ions over the other tested cations such as Cr{sup 3+}, Mn{sup 2+}, Fe{sup 2+}, Fe{sup 3+}, Co{sup 2+}, Ni{sup 2+}, Zn{sup 2+}, Ag{sup 2+}, Al{sup 3+}, Pb{sup 2+}, Hg{sup 2+}, K{sup +}, Ca{sup 2+} and Mg{sup 2+}. The high selective and sensitivity of R3 towards Cu{sup 2+} and R4 towards Cd{sup 2+} ions was confirmed by UV-Vis spectroscopic study. The R3 showed a red shift in the presence of Cu{sup 2+} ions by Δλ{sub max} 67 nm and R4 showed a red shift in the presence of Cd{sup 2+} ions by Δλ{sub max} 105 nm in the absorption spectrum. The binding stoichiometric ratio of the complex between R3 - Cu{sup 2+} and R4 - Cd{sup 2+} ions have been found to be 1:1 using the B-H plot. Under optimized experimental conditions, the R3 and R4 exhibits a dynamic linear absorption response range, from 0 to 50 μM for Cu{sup 2+} ions and 0 to 30 μM for Cd{sup 2+} ions, with the detection limit of 2.8 × 10{sup −6} M for Cu{sup 2+} and 2.0 × 10{sup −7} M for Cd{sup 2+} ions. The proposed analytical method for the quantitative determination of Cu{sup 2+} and Cd{sup 2+} ions was validated and successfully applied for the environmental samples with good precision and accuracy. - Highlights: • Detection of Cu{sup 2+} and Cd{sup 2+} ions has gained significance by virtue of its key role in biological and environmental science. • The R3 and R4 showed instantaneous color change from colorless to yellow in the presence of Cu{sup 2+} and Cd{sup 2+} ions respectively. • The proposed detection methods were validated and

  8. Improvement of the decision efficiency of the accuracy profile by means of a desirability function for analytical methods validation. Application to a diacetyl-monoxime colorimetric assay used for the determination of urea in transdermal iontophoretic extracts.

    Science.gov (United States)

    Rozet, E; Wascotte, V; Lecouturier, N; Préat, V; Dewé, W; Boulanger, B; Hubert, Ph

    2007-05-22

    Validation of analytical methods is a widely used and regulated step for each analytical method. However, the classical approaches to demonstrate the ability to quantify of a method do not necessarily fulfill this objective. For this reason an innovative methodology was recently introduced by using the tolerance interval and accuracy profile, which guarantee that a pre-defined proportion of future measurements obtained with the method will be included within the acceptance limits. Accuracy profile is an effective decision tool to assess the validity of analytical methods. The methodology to build such a profile is detailed here. However, as for any visual tool it has a part of subjectivity. It was then necessary to make the decision process objective in order to quantify the degree of adequacy of an accuracy profile and to allow a thorough comparison between such profiles. To achieve this, we developed a global desirability index based on the three most important validation criteria: the trueness, the precision and the range. The global index allows the classification of the different accuracy profiles obtained according to their respective response functions. A diacetyl-monoxime colorimetric assay for the determination of urea in transdermal iontophoretic extracts was used to illustrate these improvements.

  9. 7 CFR 98.4 - Analytical methods.

    Science.gov (United States)

    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...

  10. 7 CFR 93.4 - Analytical methods.

    Science.gov (United States)

    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...

  11. 7 CFR 94.303 - Analytical methods.

    Science.gov (United States)

    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...

  12. The Validation of an Analytical Method for Sulfentrazone Residue Determination in Soil Using Liquid Chromatography and a Comparison of Chromatographic Sensitivity to Millet as a Bioindicator Species

    Directory of Open Access Journals (Sweden)

    Marcelo Antonio de Oliveira

    2014-07-01

    Full Text Available Commonly used herbicides, such as sulfentrazone, pose the risk of soil contamination due to their persistence, bioaccumulation and toxicity. Phytoremediation by green manure species has been tested using biomarkers, but analytical data are now required to confirm the extraction of sulfentrazone from soil. Thus, the present work was carried out to analyze sulfentrazone residues in soil based on liquid chromatography with a comparison of these values to the sensitivity of the bioindicator Pennisetum glaucum. The soil samples were obtained after cultivation of Crotalaria juncea and Canavalia ensiformis at four seeding densities and with three doses of sulfentrazone. The seedlings were collected into pots, at two different depths, after 75 days of phytoremediator sowing and then were used to determine the herbicide persistence in the soil. A bioassay with P. glaucum was carried out in the same pot. High-performance liquid chromatography (HPLC, using UV-diode array detection (HPLC/UV-DAD, was used to determine the herbicide residues. The HPLC determination was optimized and validated according to the parameters of precision, accuracy, linearity, limit of detection and quantification, robustness and specificity. The bioindicator P. glaucum was more sensitive to sulfentrazone than residue determination by HPLC. Changes in sulfentrazone concentration caused by green manure phytoremediation were accurately identified by the bioindicator. However, a true correlation between the size of the species and the analyte content was not identified.

  13. Analytical methods in rotor dynamics

    CERN Document Server

    Dimarogonas, Andrew D; Chondros, Thomas G

    2013-01-01

    The design and construction of rotating machinery operating at supercritical speeds was, in the 1920s, an event of revolutionary importance for the then new branch of dynamics known as rotor dynamics. In the 1960s, another revolution occurred: In less than a decade, imposed by operational and economic needs, an increase in the power of turbomachinery by one order of magnitude took place. Dynamic analysis of complex rotor forms became a necessity, while the importance of approximate methods for dynamic analysis was stressed. Finally, the emergence of fracture mechanics, as a new branch of applied mechanics, provided analytical tools to investigate crack influence on the dynamic behavior of rotors. The scope of this book is based on all these developments. No topics related to the well-known classical problems are included, rather the book deals exclusively with modern high-power turbomachinery.

  14. 7 CFR 94.103 - Analytical methods.

    Science.gov (United States)

    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...

  15. 7 CFR 94.4 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 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...

  16. A simple validated multi-analyte method for detecting drugs in oral fluid by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

    Science.gov (United States)

    Zheng, Yufang; Sparve, Erik; Bergström, Mats

    2018-06-01

    A UPLC-MS/MS method was developed to identify and quantitate 37 commonly abused drugs in oral fluid. Drugs of interest included amphetamines, benzodiazepines, cocaine, opiates, opioids, phencyclidine and tetrahydrocannabinol. Sample preparation and extraction are simple, and analysis times short. Validation showed satisfactory performance at relevant concentrations. The possibility of contaminated samples as well as the interpretation in relation to well-knows matrices, such as urine, will demand further study. Copyright © 2017 John Wiley & Sons, Ltd.

  17. Analytical methods used at model facility

    International Nuclear Information System (INIS)

    Wing, N.S.

    1984-01-01

    A description of analytical methods used at the model LEU Fuel Fabrication Facility is presented. The methods include gravimetric uranium analysis, isotopic analysis, fluorimetric analysis, and emission spectroscopy

  18. Nuclear analytical methods in the life sciences

    NARCIS (Netherlands)

    de Goeij, J.J.M.

    1994-01-01

    A survey is given of various nuclear analytical methods. The type of analytical information obtainable and advantageous features for application in the life sciences are briefly indicated. These features are: physically different basis of the analytical method, isotopic rather than elemental

  19. Analytical Method Development and Validation for the Simultaneous Estimation of Abacavir and Lamivudine by Reversed-phase High-performance Liquid Chromatography in Bulk and Tablet Dosage Forms.

    Science.gov (United States)

    Raees Ahmad, Sufiyan Ahmad; Patil, Lalit; Mohammed Usman, Mohammed Rageeb; Imran, Mohammad; Akhtar, Rashid

    2018-01-01

    A simple rapid, accurate, precise, and reproducible validated reverse phase high performance liquid chromatography (HPLC) method was developed for the determination of Abacavir (ABAC) and Lamivudine (LAMI) in bulk and tablet dosage forms. The quantification was carried out using Symmetry Premsil C18 (250 mm × 4.6 mm, 5 μm) column run in isocratic way using mobile phase comprising methanol: water (0.05% orthophosphoric acid with pH 3) 83:17 v/v and a detection wavelength of 245 nm and injection volume of 20 μl, with a flow rate of 1 ml/min. In the developed method, the retention times of ABAC and LAMI were found to be 3.5 min and 7.4 min, respectively. The method was validated in terms of linearity, precision, accuracy, limits of detection, limits of quantitation, and robustness in accordance with the International Conference on Harmonization guidelines. The assay of the proposed method was found to be 99% - 101%. The recovery studies were also carried out and mean % recovery was found to be 99% - 101%. The % relative standard deviation from reproducibility was found to be performance liquid chromatography, UV: Ultraviolet, ICH: International Conference on Harmonization, ABAC: Abacavir, LAMI: Lamivudine, HIV: Human immunodeficiency virus, AIDS: Acquired immunodeficiency syndrome, NRTI: Nucleoside reverse transcriptase inhibitors, ARV: Antiretroviral, RSD: Relative standard deviation, RT: Retention time, SD: Standard deviation.

  20. Analytical method development and validation for quantification of uranium in compounds of the nuclear fuel cycle by Fourier Transform Infrared (FTIR) Spectroscopy

    International Nuclear Information System (INIS)

    Pereira, Elaine

    2016-01-01

    This work presents a low cost, simple and new methodology for direct quantification of uranium in compounds of the nuclear fuel cycle, based on Fourier Transform Infrared (FTIR) spectroscopy using KBr pressed discs technique. Uranium in different matrices were used to development and validation: UO 2 (NO 3 )2.2TBP complex (TBP uranyl nitrate complex) in organic phase and uranyl nitrate (UO 2 (NO 3 ) 2 ) in aqueous phase. The parameters used in the validation process were: linearity, selectivity, accuracy, limits of detection (LD) and quantitation (LQ), precision (repeatability and intermediate precision) and robustness. The method for uranium in organic phase (UO 2 (NO 3 )2.2TBP complex in hexane/embedded in KBr) was linear (r = 0.9980) over the range of 0.20% 2.85% U/ KBr disc, LD 0.02% and LQ 0.03%, accurate (recoveries were over 101.0%), robust and precise (RSD < 1.6%). The method for uranium aqueous phase (UO 2 (NO 3 ) 2 /embedded in KBr) was linear (r = 0.9900) over the range of 0.14% 1.29% U/KBr disc, LD 0.01% and LQ 0.02%, accurate (recoveries were over 99.4%), robust and precise (RSD < 1.6%). Some process samples were analyzed in FTIR and compared with gravimetric and X-ray fluorescence (XRF) analyses showing similar results in all three methods. The statistical tests (t-Student and Fischer) showed that the techniques are equivalent. The validated method can be successfully employed for routine quality control analysis for nuclear compounds. (author)

  1. Valid, legally defensible data from your analytical laboratories

    International Nuclear Information System (INIS)

    Gay, D.D.; Allen, V.C.

    1989-01-01

    This paper discusses the definition of valid, legally defensible data. The authors describe the expectations of project managers and what should be gleaned from the laboratory in regard to analytical data

  2. Theoretically Guided Analytical Method Development and Validation for the Estimation of Rifampicin in a Mixture of Isoniazid and Pyrazinamide by UV Spectrophotometer.

    Science.gov (United States)

    Khan, Mohammad F; Rita, Shamima A; Kayser, Md Shahidulla; Islam, Md Shariful; Asad, Sharmeen; Bin Rashid, Ridwan; Bari, Md Abdul; Rahman, Muhammed M; Al Aman, D A Anwar; Setu, Nurul I; Banoo, Rebecca; Rashid, Mohammad A

    2017-01-01

    A simple, rapid, economic, accurate, and precise method for the estimation of rifampicin in a mixture of isoniazid and pyrazinamide by UV spectrophotometeric technique (guided by the theoretical investigation of physicochemical properties) was developed and validated. Theoretical investigations revealed that isoniazid and pyrazinamide both were freely soluble in water and slightly soluble in ethyl acetate whereas rifampicin was practically insoluble in water but freely soluble in ethyl acetate. This indicates that ethyl acetate is an effective solvent for the extraction of rifampicin from a water mixture of isoniazid and pyrazinamide. Computational study indicated that pH range of 6.0-8.0 would favor the extraction of rifampicin. Rifampicin is separated from isoniazid and pyrazinamide at pH 7.4 ± 0.1 by extracting with ethyl acetate. The ethyl acetate was then analyzed at λ max of 344.0 nm. The developed method was validated for linearity, accuracy and precision according to ICH guidelines. The proposed method exhibited good linearity over the concentration range of 2.5-35.0 μg/mL. The intraday and inter-day precision in terms of % RSD ranged from 1.09 to 1.70% and 1.63 to 2.99%, respectively. The accuracy (in terms of recovery) of the method varied from of 96.7 ± 0.9 to 101.1 ± 0.4%. The LOD and LOQ were found to be 0.83 and 2.52 μg/mL, respectively. In addition, the developed method was successfully applied to determine rifampicin combination (isoniazid and pyrazinamide) brands available in Bangladesh.

  3. Maritime Analytics Prototype: Phase 3 Validation

    Science.gov (United States)

    2014-01-01

    different so we need a flexible analysis set hierarchy encoded as directories or groups – like a recipe [C.3.1.4n] Improve the GUI:  Provide more...Problems zooming and panning on the timeline [C.1.2.1c, C.1.2.4e, C.1.3.1c, C.1.1.4c, C.1.1.4b]  Selected the wrong year and then the vessel...Scholtz_VAMetrics_2006.pdf] [21] J. Thomas, and K. Cook , Illuminating the Path, the Research and Development Agenda for Visual analytics: IEEE, 2005. [22

  4. Risk analysis by FMEA as an element of analytical validation.

    Science.gov (United States)

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

    2009-12-05

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

  5. Validación del método analítico para la cuantificación de bacitracina Validation of the analytical method to quantify the bacitracine

    Directory of Open Access Journals (Sweden)

    Carolina Velandia-Castellanos

    2011-06-01

    Full Text Available Se desarrolló y validó un método analítico para la determinación cuantitativa de bacitracina zinc al 15 % y bacitracina metilen disalicilato al 11 %, por el método de cilindro en placa (difusión en agar, con el fin de ser usado en el control de calidad de las materias primas y productos farmacéuticos. Se evaluaron los parámetros de especificidad, selectividad, linealidad del sistema, y del método, exactitud, límite de cuantificación y precisión. Mediante el diseño experimental y la evaluación estadística de los resultados, se demostró que el método analítico es específico, selectivo, lineal, preciso (CVAn analytical method was developed and validated for quantitative determination of 15 % zinc bacitracine and 11 % disalicylate methylene-bacitracine by the plate-cylinder method (agar diffusion to be used in quality control of raw products and pharmaceutical products. Specificity, selectivity, system and method linearity, accuracy, quantification and precision parameters were assessed. By the experimental design and the statistic evaluation of results, it was demonstrated that the analytical method is specific, selective, linear, precise (CV< 5 % and exact (bias < 3 %, Gexp< Gtab< t exp< t tab during the study concentrations. The quantification and detection limit was of 0.02 and 0.005 Ul/mL, respectively. The analytical performance characteristics fulfill the requirement for the proposal analytical implementation.

  6. Reactor Section standard analytical methods. Part 1

    Energy Technology Data Exchange (ETDEWEB)

    Sowden, D.

    1954-07-01

    the Standard Analytical Methods manual was prepared for the purpose of consolidating and standardizing all current analytical methods and procedures used in the Reactor Section for routine chemical analyses. All procedures are established in accordance with accepted practice and the general analytical methods specified by the Engineering Department. These procedures are specifically adapted to the requirements of the water treatment process and related operations. The methods included in this manual are organized alphabetically within the following five sections which correspond to the various phases of the analytical control program in which these analyses are to be used: water analyses, essential material analyses, cotton plug analyses boiler water analyses, and miscellaneous control analyses.

  7. 40 CFR 141.89 - Analytical methods.

    Science.gov (United States)

    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...

  8. 40 CFR 141.704 - Analytical methods.

    Science.gov (United States)

    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...

  9. Consistency of FMEA used in the validation of analytical procedures.

    Science.gov (United States)

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

    2011-02-20

    In order to explore the consistency of the outcome of a Failure Mode and Effects Analysis (FMEA) in the validation of analytical procedures, an FMEA was carried out by two different teams. The two teams applied two separate FMEAs to a High Performance Liquid Chromatography-Diode Array Detection-Mass Spectrometry (HPLC-DAD-MS) analytical procedure used in the quality control of medicines. Each team was free to define their own ranking scales for the probability of severity (S), occurrence (O), and detection (D) of failure modes. We calculated Risk Priority Numbers (RPNs) and we identified the failure modes above the 90th percentile of RPN values as failure modes needing urgent corrective action; failure modes falling between the 75th and 90th percentile of RPN values were identified as failure modes needing necessary corrective action, respectively. Team 1 and Team 2 identified five and six failure modes needing urgent corrective action respectively, with two being commonly identified. Of the failure modes needing necessary corrective actions, about a third were commonly identified by both teams. These results show inconsistency in the outcome of the FMEA. To improve consistency, we recommend that FMEA is always carried out under the supervision of an experienced FMEA-facilitator and that the FMEA team has at least two members with competence in the analytical method to be validated. However, the FMEAs of both teams contained valuable information that was not identified by the other team, indicating that this inconsistency is not always a drawback. Copyright © 2010 Elsevier B.V. All rights reserved.

  10. Determination of Anthracycline Drug Residual in Cleaning Validation Swabs of Stainless-Steel Equipment after Production of Cytostatic Injections Using HPLC Analytical Method

    Directory of Open Access Journals (Sweden)

    Zuzana Slivová

    2015-01-01

    Full Text Available Standard cleaning procedures of production line equipment were verified after manufacture of cytostatic injections containing Anthracycline derivate substance. Residual content of Anthracycline drug substance on stainless-steel equipment surface was determined using swab sampling with a specific HPLC-DAD analysis. The acceptance limit was decided as 200.0 μg/100 cm2. Recovery from the stainless-steel surface was 90.1%. Linearity of the method was observed in the concentration range of 0.155–194 μg/mL when estimated using Zorbax TMS (5 μm, 0.25 m × 4.6 mm ID column at 1.3 mL/min flow rate and 254 nm (DAD 190–600 nm. The mobile phase consisted of lauryl hydrogen sulphate solution (3.7 g/L : methanol : acetonitrile (54 : 16 : 30, v/v/v with pH adjusted to 2.5 using phosphoric acid (85%. The LOD and LOQ for Anthracycline derivate were found to be 0.047 and 0.155 μg/mL, respectively. The method validation confirmed the method provides acceptable degree of selectivity, linearity, accuracy, and precision for the intended purposes.

  11. Analytical Method Development and Validation for the Quantification of Acetone and Isopropyl Alcohol in the Tartaric Acid Base Pellets of Dipyridamole Modified Release Capsules by Using Headspace Gas Chromatographic Technique

    Directory of Open Access Journals (Sweden)

    Sriram Valavala

    2018-01-01

    Full Text Available A simple, sensitive, accurate, robust headspace gas chromatographic method was developed for the quantitative determination of acetone and isopropyl alcohol in tartaric acid-based pellets of dipyridamole modified release capsules. The residual solvents acetone and isopropyl alcohol were used in the manufacturing process of the tartaric acid-based pellets of dipyridamole modified release capsules by considering the solubility of the dipyridamole and excipients in the different manufacturing stages. The method was developed and optimized by using fused silica DB-624 (30 m × 0.32 mm × 1.8 µm column with the flame ionization detector. The method validation was carried out with regard to the guidelines for validation of analytical procedures Q2 demanded by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH. All the validation characteristics were meeting the acceptance criteria. Hence, the developed and validated method can be applied for the intended routine analysis.

  12. Development and validation of new analytical methods for simultaneous estimation of Drotaverine hydrochloride in combination with Omeprazole in a pharmaceutical dosage form

    Directory of Open Access Journals (Sweden)

    Smita Sharma

    2017-02-01

    Full Text Available A rapid and precise method (in accordance with ICH guidelines is developed for the quantitative simultaneous determination of Drotaverine hydrochloride and Omeprazole in a combined pharmaceutical dosage form. Three methods are described for the simultaneous determination of Drotaverine hydrochloride and Omeprazole in a binary mixture. The first method was based on UV-Spectrophotometric determination of two drugs, using Vierordt!s simultaneous equation method. It involves absorbance measurement at 226.8 nm (λmax of Drotaverine hydrochloride and 269.4 nm (λmax of Omeprazole in methanol; linearity was obtained in the range of 5–30 μg ml−1 for both the drugs. The second method was based on HPLC separation of the two drugs using potassium dihydrogen phosphate buffer pH 5.0: Acetonitrile: Triethylamine (60:40:0.5, v/v as a mobile phase. Areas were recorded at 260 nm for both the drugs and retention time was found to be 2.71 min. and 3.87 min for Drotaverine hydrochloride and Omeprazole, respectively at 1.0 mL/min flow rate. The selected chromatographic conditions were found to determine Drotaverine hydrochloride and Omeprazole quantitatively in a combined dosage form without any physical separation. The method has been validated for linearity, accuracy and precision. Linearity was found over the range of 5–30 μg mL−1 for both drugs. The third method was based on HPTLC method for simultaneous quantification of these compounds in pharmaceutical dosage forms. Precoated silica gel 60 F254 plate was used as stationary phase. The separation was carried out using Glacial acetic acid:Cyclohexane:Methanol:(80:15:5 v/v/v as mobile phase. The proposed method was found to be fast, accurate, precise, reproducible and rugged and can be used for a simultaneous analysis of these drugs in combined formulations.

  13. HTGR analytical methods and design verification

    International Nuclear Information System (INIS)

    Neylan, A.J.; Northup, T.E.

    1982-05-01

    Analytical methods for the high-temperature gas-cooled reactor (HTGR) include development, update, verification, documentation, and maintenance of all computer codes for HTGR design and analysis. This paper presents selected nuclear, structural mechanics, seismic, and systems analytical methods related to the HTGR core. This paper also reviews design verification tests in the reactor core, reactor internals, steam generator, and thermal barrier

  14. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS)

    International Nuclear Information System (INIS)

    Guilhen, Sabine Neusatz

    2009-01-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method's performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 +- 11,70)mug.L -1 with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10μg.L -1 . The obtained results fall into a

  15. Analytical method development and validation of simultaneous estimation of rabeprazole, pantoprazole, and itopride by reverse-phase high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Senthamil Selvan Perumal

    2014-12-01

    Full Text Available A simple, selective, rapid, and precise reverse-phase high-performance liquid chromatography (RP-HPLC method for the simultaneous estimation of rabeprazole (RP, pantoprazole (PP, and itopride (IP has been developed. The compounds were well separated on a Phenomenex C18 (Luna column (250 mm × 4.6 mm, dp = 5 μm with C18 guard column (4 mm × 3 mm × 5 μm with a mobile phase consisting of buffer containing 10 mM potassium dihydrogen orthophosphate (adjusted to pH 6.8: acetonitrile (70:30 v/v at a flow rate of 1.0 mL/min and ultraviolet detection at 288 nm. The retention time of RP, PP, and IP were 5.35, 7.92, and 11.16 minutes, respectively. Validation of the proposed method was carried out according to International Conference on Harmonisation (ICH guidelines. Linearity range was obtained for RP, PP, and IP over the concentration range of 2.5–25, 1–30, and 3–35 μg/mL and the r2 values were 0.994, 0.978, and 0.991, respectively. The calculated limit of detection (LOD values were 1, 0.3, and 1 μg/mL and limit of quantitation (LOQ values were 2.5, 1, and 3 μg/mL for RP, PP, and IP correspondingly. Thus, the current study showed that the developed reverse-phase liquid chromatography method is sensitive and selective for the estimation of RP, PP, and IP in combined dosage form.

  16. Analytical method development and validation of simultaneous estimation of rabeprazole, pantoprazole, and itopride by reverse-phase high-performance liquid chromatography.

    Science.gov (United States)

    Perumal, Senthamil Selvan; Ekambaram, Sanmuga Priya; Raja, Samundeswari

    2014-12-01

    A simple, selective, rapid, and precise reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of rabeprazole (RP), pantoprazole (PP), and itopride (IP) has been developed. The compounds were well separated on a Phenomenex C 18 (Luna) column (250 mm × 4.6 mm, dp = 5 μm) with C 18 guard column (4 mm × 3 mm × 5 μm) with a mobile phase consisting of buffer containing 10 mM potassium dihydrogen orthophosphate (adjusted to pH 6.8): acetonitrile (70:30 v/v) at a flow rate of 1.0 mL/min and ultraviolet detection at 288 nm. The retention time of RP, PP, and IP were 5.35, 7.92, and 11.16 minutes, respectively. Validation of the proposed method was carried out according to International Conference on Harmonisation (ICH) guidelines. Linearity range was obtained for RP, PP, and IP over the concentration range of 2.5-25, 1-30, and 3-35 μg/mL and the r 2 values were 0.994, 0.978, and 0.991, respectively. The calculated limit of detection (LOD) values were 1, 0.3, and 1 μg/mL and limit of quantitation (LOQ) values were 2.5, 1, and 3 μg/mL for RP, PP, and IP correspondingly. Thus, the current study showed that the developed reverse-phase liquid chromatography method is sensitive and selective for the estimation of RP, PP, and IP in combined dosage form. Copyright © 2014. Published by Elsevier B.V.

  17. Nuclear analytical methods: Past, present and future

    International Nuclear Information System (INIS)

    Becker, D.A.

    1996-01-01

    The development of nuclear analytical methods as an analytical tool began in 1936 with the publication of the first paper on neutron activation analysis (NAA). This year, 1996, marks the 60th anniversary of that event. This paper attempts to look back at the nuclear analytical methods of the past, to look around and to see where the technology is right now, and finally, to look ahead to try and see where nuclear methods as an analytical technique (or as a group of analytical techniques) will be going in the future. The general areas which the author focuses on are: neutron activation analysis; prompt gamma neutron activation analysis (PGNAA); photon activation analysis (PAA); charged-particle activation analysis (CPAA)

  18. Validation Process Methods

    Energy Technology Data Exchange (ETDEWEB)

    Lewis, John E. [National Renewable Energy Lab. (NREL), Golden, CO (United States); English, Christine M. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Gesick, Joshua C. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Mukkamala, Saikrishna [National Renewable Energy Lab. (NREL), Golden, CO (United States)

    2018-01-04

    This report documents the validation process as applied to projects awarded through Funding Opportunity Announcements (FOAs) within the U.S. Department of Energy Bioenergy Technologies Office (DOE-BETO). It describes the procedures used to protect and verify project data, as well as the systematic framework used to evaluate and track performance metrics throughout the life of the project. This report also describes the procedures used to validate the proposed process design, cost data, analysis methodologies, and supporting documentation provided by the recipients.

  19. 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.

    Science.gov (United States)

    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

  20. Analytical methods of radwaste characterization

    International Nuclear Information System (INIS)

    Garcia, C.M.

    1994-10-01

    In view of the need to carry out more extensive studies on the design of newly proposed methods for the treatment of radioactive wastes collected at PNRI, this study is aimed to provide a guide in the characterization of wastes which is a preparatory step for a well-planned waste processing. (auth.). 8 refs

  1. A New Method to Study Analytic Inequalities

    Directory of Open Access Journals (Sweden)

    Xiao-Ming Zhang

    2010-01-01

    Full Text Available We present a new method to study analytic inequalities involving n variables. Regarding its applications, we proved some well-known inequalities and improved Carleman's inequality.

  2. Development of a validated liquid chromatographic method for quantification of sorafenib tosylate in the presence of stress-induced degradation products and in biological matrix employing analytical quality by design approach.

    Science.gov (United States)

    Sharma, Teenu; Khurana, Rajneet Kaur; Jain, Atul; Katare, O P; Singh, Bhupinder

    2018-05-01

    The current research work envisages an analytical quality by design-enabled development of a simple, rapid, sensitive, specific, robust and cost-effective stability-indicating reversed-phase high-performance liquid chromatographic method for determining stress-induced forced-degradation products of sorafenib tosylate (SFN). An Ishikawa fishbone diagram was constructed to embark upon analytical target profile and critical analytical attributes, i.e. peak area, theoretical plates, retention time and peak tailing. Factor screening using Taguchi orthogonal arrays and quality risk assessment studies carried out using failure mode effect analysis aided the selection of critical method parameters, i.e. mobile phase ratio and flow rate potentially affecting the chosen critical analytical attributes. Systematic optimization using response surface methodology of the chosen critical method parameters was carried out employing a two-factor-three-level-13-run, face-centered cubic design. A method operable design region was earmarked providing optimum method performance using numerical and graphical optimization. The optimum method employed a mobile phase composition consisting of acetonitrile and water (containing orthophosphoric acid, pH 4.1) at 65:35 v/v at a flow rate of 0.8 mL/min with UV detection at 265 nm using a C 18 column. Response surface methodology validation studies confirmed good efficiency and sensitivity of the developed method for analysis of SFN in mobile phase as well as in human plasma matrix. The forced degradation studies were conducted under different recommended stress conditions as per ICH Q1A (R2). Mass spectroscopy studies showed that SFN degrades in strongly acidic, alkaline and oxidative hydrolytic conditions at elevated temperature, while the drug was per se found to be photostable. Oxidative hydrolysis using 30% H 2 O 2 showed maximum degradation with products at retention times of 3.35, 3.65, 4.20 and 5.67 min. The absence of any

  3. Development and validation of a spectroscopic method for the ...

    African Journals Online (AJOL)

    Development and validation of a spectroscopic method for the simultaneous analysis of ... advanced analytical methods such as high pressure liquid ..... equipment. DECLARATIONS ... high-performance liquid chromatography. J Chromatogr.

  4. Method Validation Procedure in Gamma Spectroscopy Laboratory

    International Nuclear Information System (INIS)

    El Samad, O.; Baydoun, R.

    2008-01-01

    The present work describes the methodology followed for the application of ISO 17025 standards in gamma spectroscopy laboratory at the Lebanese Atomic Energy Commission including the management and technical requirements. A set of documents, written procedures and records were prepared to achieve the management part. The technical requirements, internal method validation was applied through the estimation of trueness, repeatability , minimum detectable activity and combined uncertainty, participation in IAEA proficiency tests assure the external method validation, specially that the gamma spectroscopy lab is a member of ALMERA network (Analytical Laboratories for the Measurements of Environmental Radioactivity). Some of these results are presented in this paper. (author)

  5. Validation of a multi-analyte HPLC-DAD method for determination of uric acid, creatinine, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid and 2-methylhippuric acid in human urine.

    Science.gov (United States)

    Remane, Daniela; Grunwald, Soeren; Hoeke, Henrike; Mueller, Andrea; Roeder, Stefan; von Bergen, Martin; Wissenbach, Dirk K

    2015-08-15

    During the last decades exposure sciences and epidemiological studies attracts more attention to unravel the mechanisms for the development of chronic diseases. According to this an existing HPLC-DAD method for determination of creatinine in urine samples was expended for seven analytes and validated. Creatinine, uric acid, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid, and 2-methylhippuric acid were separated by gradient elution (formate buffer/methanol) using an Eclipse Plus C18 Rapid Resolution column (4.6mm×100mm). No interfering signals were detected in mobile phase. After injection of blank urine samples signals for the endogenous compounds but no interferences were detected. All analytes were linear in the selected calibration range and a non weighted calibration model was chosen. Bias, intra-day and inter-day precision for all analytes were below 20% for quality control (QC) low and below 10% for QC medium and high. The limits of quantification in mobile phase were in line with reported reference values but had to be adjusted in urine for homovanillic acid (45mg/L), niacinamide 58.5(mg/L), and indole-3-acetic acid (63mg/L). Comparison of creatinine data obtained by the existing method with those of the developed method showing differences from -120mg/L to +110mg/L with a mean of differences of 29.0mg/L for 50 authentic urine samples. Analyzing 50 authentic urine samples, uric acid, creatinine, hippuric acid, and 2-methylhippuric acid were detected in (nearly) all samples. However, homovanillic acid was detected in 40%, niacinamide in 4% and indole-3-acetic acid was never detected within the selected samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Study of hydroxymethylfurfural and furfural formation in cakes during baking in different ovens, using a validated multiple-stage extraction-based analytical method.

    Science.gov (United States)

    Petisca, Catarina; Henriques, Ana Rita; Pérez-Palacios, Trinidad; Pinho, Olívia; Ferreira, Isabel M P L V O

    2013-12-15

    A procedure for extraction of hydroxymethylfurfural (HMF) and furfural from cakes was validated. Higher yield was achieved by multiple step extraction with water/methanol (70/30) and clarification with Carrez I and II reagents. Oven type and baking time strongly influenced HMF, moisture and volatile profile of model cakes, whereas furfural content was not significantly affected. No correlation was found between these parameters. Baking time influenced moisture and HMF formation in cakes from traditional and microwave ovens but not in steam oven cakes. Significant moisture decrease and HMF increase (3.63, 9.32, and 41.9 mg kg(-1)dw at 20, 40 and 60 min, respectively) were observed during traditional baking. Cakes baked by microwave also presented a significant increase of HMF (up to 16.84 mg kg(-1)dw at 2.5 min). Steam oven cakes possessed the highest moisture content and no significant differences in HMF and furfural. This oven is likely to form low HMF and furfural, maintaining cake moisture and aroma compounds. Copyright © 2013 Elsevier Ltd. All rights reserved.

  7. Mathematical methods for physical and analytical chemistry

    CERN Document Server

    Goodson, David Z

    2011-01-01

    Mathematical Methods for Physical and Analytical Chemistry presents mathematical and statistical methods to students of chemistry at the intermediate, post-calculus level. The content includes a review of general calculus; a review of numerical techniques often omitted from calculus courses, such as cubic splines and Newton's method; a detailed treatment of statistical methods for experimental data analysis; complex numbers; extrapolation; linear algebra; and differential equations. With numerous example problems and helpful anecdotes, this text gives chemistry students the mathematical

  8. Analytical Method for the Validation of Three Polyphenols as a Marker Compound for the Standardization of Solidago virgaurea subsp. gigantea Extracts and Antiadipogenesis of Harvesting Time and Location

    Directory of Open Access Journals (Sweden)

    Seung Hwan Hwang

    2017-01-01

    Full Text Available Protocatechuic acid (PC, chlorogenic acid (CA, and kaempferol-3-O-rutinoside (K-O-R, isolated from the Solidago virgaurea subsp. gigantea (SV extract, were quickly and efficiently separated using HPLC. Our chromatographic method was found to effectively separate PC, CA, and K-O-R at retention times of 5.36, 8.22, and 17.04 min, respectively. Linearity of PC, CA, and K-O-R was found to be in the range of 4.85–485.00, 47.5–1900.00, and 8.50–850.00 μg/ml. Recoveries ranged between 101.32 and 103.30%, 95.82 and 100.25%, and 96.18 and 99.37%, for PC, CA, and K-O-R, respectively. The antiadipogenesis activity of SV extracts collected from five different months and from seven different regions was evaluated using an Oil Red O staining assay in 3T3-L1 cells. Extract from SV collected in April from the Ulleung Island produced over 106.89% inhibition of adipogenesis without cytotoxicity at 50 μg/ml. This extract had a high amount of PC and K-O-R. The developed HPLC method was found to be fast, accurate, precise, and reproducible and could be applied to qualitative and quantitative analysis of three bioactive compounds in SV extracts. The SV extract collected in April from Ulleung Island can be used as a functional food ingredient preventing obesity.

  9. Analytical method for solving radioactive transformations

    International Nuclear Information System (INIS)

    Vudakin, Z.

    1999-01-01

    Analytical method for solving radioactive transformations is presented in this paper. High accuracy series expansion of the depletion function and nonsingular Bateman coefficients are used to overcome numerical difficulties when applying well-known Bateman solution of a simple radioactive decay. Generality and simplicity of the method are found to be useful in evaluating nuclide chains with one hundred or more nuclides in the chain. Method enables evaluation of complete chain, without elimination of short-lives nuclides. It is efficient and accurate

  10. 7 CFR 93.13 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... No. 1, USDA, Agricultural Marketing Service, Science and Technology, 3521 South Agriculture Building... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Standards...

  11. Biodiesel Analytical Methods: August 2002--January 2004

    Energy Technology Data Exchange (ETDEWEB)

    Van Gerpen, J.; Shanks, B.; Pruszko, R.; Clements, D.; Knothe, G.

    2004-07-01

    Biodiesel is an alternative fuel for diesel engines that is receiving great attention worldwide. The material contained in this book is intended to provide the reader with information about biodiesel engines and fuels, analytical methods used to measure fuel properties, and specifications for biodiesel quality control.

  12. Statistically qualified neuro-analytic failure detection method and system

    Science.gov (United States)

    Vilim, Richard B.; Garcia, Humberto E.; Chen, Frederick W.

    2002-03-02

    An apparatus and method for monitoring a process involve development and application of a statistically qualified neuro-analytic (SQNA) model to accurately and reliably identify process change. The development of the SQNA model is accomplished in two stages: deterministic model adaption and stochastic model modification of the deterministic model adaptation. Deterministic model adaption involves formulating an analytic model of the process representing known process characteristics, augmenting the analytic model with a neural network that captures unknown process characteristics, and training the resulting neuro-analytic model by adjusting the neural network weights according to a unique scaled equation error minimization technique. Stochastic model modification involves qualifying any remaining uncertainty in the trained neuro-analytic model by formulating a likelihood function, given an error propagation equation, for computing the probability that the neuro-analytic model generates measured process output. Preferably, the developed SQNA model is validated using known sequential probability ratio tests and applied to the process as an on-line monitoring system. Illustrative of the method and apparatus, the method is applied to a peristaltic pump system.

  13. Desarrollo y validación de los métodos analíticos para el control de calidad del micocilén polvo Development and validation of analytical methods for quality control of Micocilen powder

    Directory of Open Access Journals (Sweden)

    Yania Suárez Pérez

    2011-06-01

    Full Text Available El micocilén es un medicamento que se presenta en forma de polvo. Contiene 2 ingredientes farmacéuticos activos: el ácido undecilénico y el undecilinato de zinc. Por su acción fungistática, se ha convertido en un producto de alta demanda en Cuba, ya que las micosis se favorecen en climas cálidos y húmedos. Se realizó el desarrollo y la validación de 2 métodos analíticos para el control de calidad sobre la base de la cuantificación de cada analito presente en la formulación. Se seleccionaron técnicas volumétricas por neutralización acuosa y complejometría. Los resultados fueron satisfactorios, ya que en ambos casos se obtuvo adecuada especificidad, linealidad, exactitud, precisión y robustez. Los métodos propuestos se compararon con los aplicados anteriormente y se obtuvieron resultados mucho más confiables, según resultados del análisis estadístico aplicado, sin diferencias significativas entre las réplicas de un mismo lote.The undecylenic acid (Micocilen is a drug in powder presentation containing two active pharmaceutical ingredients: undecylenic acid and zinc undecylenate. By its fungistatic action becames a first line product in Cuba because of mycoses are typical of wet and warm climates. Development and validation of two analytical methods for the quality control on the base of the quantification of each symbol present in the formula. Volumetric techniques were selected by aqueous neutralization and complexometric. Results were satisfactory since in both cases an appropriate specificity, linearity, accuracy, precision and robustness were obtained. Methods proposed were compared to those previously applied obtaining more reliable results, according to results of analytical analysis applied, without significant differences among replica of a same batch.

  14. Prioritizing pesticide compounds for analytical methods development

    Science.gov (United States)

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

    2012-01-01

    The U.S. Geological Survey (USGS) has a periodic need to re-evaluate pesticide compounds in terms of priorities for inclusion in monitoring and studies and, thus, must also assess the current analytical capabilities for pesticide detection. To meet this need, a strategy has been developed to prioritize pesticides and degradates for analytical methods development. Screening procedures were developed to separately prioritize pesticide compounds in water and sediment. The procedures evaluate pesticide compounds in existing USGS analytical methods for water and sediment and compounds for which recent agricultural-use information was available. Measured occurrence (detection frequency and concentrations) in water and sediment, predicted concentrations in water and predicted likelihood of occurrence in sediment, potential toxicity to aquatic life or humans, and priorities of other agencies or organizations, regulatory or otherwise, were considered. Several existing strategies for prioritizing chemicals for various purposes were reviewed, including those that identify and prioritize persistent, bioaccumulative, and toxic compounds, and those that determine candidates for future regulation of drinking-water contaminants. The systematic procedures developed and used in this study rely on concepts common to many previously established strategies. The evaluation of pesticide compounds resulted in the classification of compounds into three groups: Tier 1 for high priority compounds, Tier 2 for moderate priority compounds, and Tier 3 for low priority compounds. For water, a total of 247 pesticide compounds were classified as Tier 1 and, thus, are high priority for inclusion in analytical methods for monitoring and studies. Of these, about three-quarters are included in some USGS analytical method; however, many of these compounds are included on research methods that are expensive and for which there are few data on environmental samples. The remaining quarter of Tier 1

  15. Analytical detection methods for irradiated foods

    International Nuclear Information System (INIS)

    1991-03-01

    The present publication is a review of scientific literature on the analytical identification of foods treated with ionizing radiation and the quantitative determination of absorbed dose of radiation. Because of the extremely low level of chemical changes resulting from irradiation or because of the lack of specificity to irradiation of any chemical changes, a few methods of quantitative determination of absorbed dose have shown promise until now. On the other hand, the present review has identified several possible methods, which could be used, following further research and testing, for the identification of irradiated foods. An IAEA Co-ordinated Research Programme on Analytical Detection Methods for Irradiation Treatment of Food ('ADMIT'), established in 1990, is currently investigating many of the methods cited in the present document. Refs and tab

  16. Workshop on Analytical Methods in Statistics

    CERN Document Server

    Jurečková, Jana; Maciak, Matúš; Pešta, Michal

    2017-01-01

    This volume collects authoritative contributions on analytical methods and mathematical statistics. The methods presented include resampling techniques; the minimization of divergence; estimation theory and regression, eventually under shape or other constraints or long memory; and iterative approximations when the optimal solution is difficult to achieve. It also investigates probability distributions with respect to their stability, heavy-tailness, Fisher information and other aspects, both asymptotically and non-asymptotically. The book not only presents the latest mathematical and statistical methods and their extensions, but also offers solutions to real-world problems including option pricing. The selected, peer-reviewed contributions were originally presented at the workshop on Analytical Methods in Statistics, AMISTAT 2015, held in Prague, Czech Republic, November 10-13, 2015.

  17. Quantifying the measurement uncertainty of results from environmental analytical methods.

    Science.gov (United States)

    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.

  18. Systems and Methods for Composable Analytics

    Science.gov (United States)

    2014-04-29

    simplistic module that performs a mathematical operation on two numbers. The most important method is the Execute() method. This will get called when it is...addition, an input control is also specified in the example below. In this example, the mathematical operator can only be chosen from a preconfigured...approaches. Some of the industries that could benefit from Composable Analytics include pharmaceuticals, health care, insurance, actuaries , and

  19. Modeling Run Test Validity: A Meta-Analytic Approach

    National Research Council Canada - National Science Library

    Vickers, Ross

    2002-01-01

    .... This study utilized data from 166 samples (N = 5,757) to test the general hypothesis that differences in testing methods could account for the cross-situational variation in validity. Only runs >2 km...

  20. Risk analysis of analytical validations by probabilistic modification of FMEA

    DEFF Research Database (Denmark)

    Barends, D.M.; Oldenhof, M.T.; Vredenbregt, M.J.

    2012-01-01

    Risk analysis is a valuable addition to validation of an analytical chemistry process, enabling not only detecting technical risks, but also risks related to human failures. Failure Mode and Effect Analysis (FMEA) can be applied, using a categorical risk scoring of the occurrence, detection...... and severity of failure modes, and calculating the Risk Priority Number (RPN) to select failure modes for correction. We propose a probabilistic modification of FMEA, replacing the categorical scoring of occurrence and detection by their estimated relative frequency and maintaining the categorical scoring...... of severity. In an example, the results of traditional FMEA of a Near Infrared (NIR) analytical procedure used for the screening of suspected counterfeited tablets are re-interpretated by this probabilistic modification of FMEA. Using this probabilistic modification of FMEA, the frequency of occurrence...

  1. LATUX: An Iterative Workflow for Designing, Validating, and Deploying Learning Analytics Visualizations

    Science.gov (United States)

    Martinez-Maldonado, Roberto; Pardo, Abelardo; Mirriahi, Negin; Yacef, Kalina; Kay, Judy; Clayphan, Andrew

    2015-01-01

    Designing, validating, and deploying learning analytics tools for instructors or students is a challenge that requires techniques and methods from different disciplines, such as software engineering, human-computer interaction, computer graphics, educational design, and psychology. Whilst each has established its own design methodologies, we now…

  2. Application of Multi-Analyte Methods for Pesticide Formulations

    Energy Technology Data Exchange (ETDEWEB)

    Lantos, J.; Virtics, I. [Plant Protection & Soil Conservation Service of Szabolcs-Szatmár-Bereg County, Nyíregyháza (Hungary)

    2009-07-15

    The application of multi-analyte methods for pesticide formulations by GC analysis is discussed. HPLC was used to determine active ingredients. HPLC elution sequences were related to individual n-octanol/water partition coefficients. Real laboratory data are presented and evaluated with regard to validation requirements. The retention time data of pesticides on different HPLC columns under gradient and isocratic conditions are compared to illustrate the applicability of the methodologies. (author)

  3. Nuclear analytical methods for platinum group elements

    International Nuclear Information System (INIS)

    2005-04-01

    Platinum group elements (PGE) are of special interest for analytical research due to their economic importance like chemical peculiarities as catalysts, medical applications as anticancer drugs, and possible environmental detrimental impact as exhaust from automobile catalyzers. Natural levels of PGE are so low in concentration that most of the current analytical techniques approach their limit of detection capacity. In addition, Ru, Rh, Pd, Re, Os, Ir, and Pt analyses still constitute a challenge in accuracy and precision of quantification in natural matrices. Nuclear analytical techniques, such as neutron activation analysis, X ray fluorescence, or proton-induced X ray emission (PIXE), which are generally considered as reference methods for many analytical problems, are useful as well. However, due to methodological restrictions, they can, in most cases, only be applied after pre-concentration and under special irradiation conditions. This report was prepared following a coordinated research project and a consultants meeting addressing the subject from different viewpoints. The experts involved suggested to discuss the issue according to the (1) application, hence, the concentration levels encountered, and (2) method applied for analysis. Each of the different fields of application needs special consideration for sample preparation, PGE pre-concentration, and determination. Additionally, each analytical method requires special attention regarding the sensitivity and sample type. Quality assurance/quality control aspects are considered towards the end of the report. It is intended to provide the reader of this publication with state-of-the-art information on the various aspects of PGE analysis and to advise which technique might be most suitable for a particular analytical problem related to platinum group elements. In particular, many case studies described in detail from the authors' laboratory experience might help to decide which way to go. As in many cases

  4. Secondary waste minimization in analytical methods

    International Nuclear Information System (INIS)

    Green, D.W.; Smith, L.L.; Crain, J.S.; Boparai, A.S.; Kiely, J.T.; Yaeger, J.S.; Schilling, J.B.

    1995-01-01

    The characterization phase of site remediation is an important and costly part of the process. Because toxic solvents and other hazardous materials are used in common analytical methods, characterization is also a source of new waste, including mixed waste. Alternative analytical methods can reduce the volume or form of hazardous waste produced either in the sample preparation step or in the measurement step. The authors are examining alternative methods in the areas of inorganic, radiological, and organic analysis. For determining inorganic constituents, alternative methods were studied for sample introduction into inductively coupled plasma spectrometers. Figures of merit for the alternative methods, as well as their associated waste volumes, were compared with the conventional approaches. In the radiological area, the authors are comparing conventional methods for gross α/β measurements of soil samples to an alternative method that uses high-pressure microwave dissolution. For determination of organic constituents, microwave-assisted extraction was studied for RCRA regulated semivolatile organics in a variety of solid matrices, including spiked samples in blank soil; polynuclear aromatic hydrocarbons in soils, sludges, and sediments; and semivolatile organics in soil. Extraction efficiencies were determined under varying conditions of time, temperature, microwave power, moisture content, and extraction solvent. Solvent usage was cut from the 300 mL used in conventional extraction methods to about 30 mL. Extraction results varied from one matrix to another. In most cases, the microwave-assisted extraction technique was as efficient as the more common Soxhlet or sonication extraction techniques

  5. Risk analysis of analytical validations by probabilistic modification of FMEA.

    Science.gov (United States)

    Barends, D M; Oldenhof, M T; Vredenbregt, M J; Nauta, M J

    2012-05-01

    Risk analysis is a valuable addition to validation of an analytical chemistry process, enabling not only detecting technical risks, but also risks related to human failures. Failure Mode and Effect Analysis (FMEA) can be applied, using a categorical risk scoring of the occurrence, detection and severity of failure modes, and calculating the Risk Priority Number (RPN) to select failure modes for correction. We propose a probabilistic modification of FMEA, replacing the categorical scoring of occurrence and detection by their estimated relative frequency and maintaining the categorical scoring of severity. In an example, the results of traditional FMEA of a Near Infrared (NIR) analytical procedure used for the screening of suspected counterfeited tablets are re-interpretated by this probabilistic modification of FMEA. Using this probabilistic modification of FMEA, the frequency of occurrence of undetected failure mode(s) can be estimated quantitatively, for each individual failure mode, for a set of failure modes, and the full analytical procedure. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Comparison of nuclear analytical methods with competitive methods

    International Nuclear Information System (INIS)

    1987-10-01

    The use of nuclear analytical techniques, especially neutron activation analysis, already have a 50 year old history. Today several sensitive and accurate, non-nuclear trace element analytical techniques are available and new methods are continuously developed. The IAEA is supporting the development of nuclear analytical laboratories in its Member States. In order to be able to advise the developing countries which methods to use in different applications, it is important to know the present status and development trends of nuclear analytical methods, what are their benefits, drawbacks and recommended fields of application, compared with other, non-nuclear techniques. In order to get an answer to these questions the IAEA convened this Advisory Group Meeting. This volume is the outcome of the presentations and discussions of the meeting. A separate abstract was prepared for each of the 21 papers. Refs, figs, tabs

  7. Preliminary Assessment of ATR-C Capabilities to Provide Integral Benchmark Data for Key Structural/Matrix Materials that May be Used for Nuclear Data Testing and Analytical Methods Validation

    Energy Technology Data Exchange (ETDEWEB)

    John D. Bess

    2009-03-01

    The purpose of this research is to provide a fundamental computational investigation into the possible integration of experimental activities with the Advanced Test Reactor Critical (ATR-C) facility with the development of benchmark experiments. Criticality benchmarks performed in the ATR-C could provide integral data for key matrix and structural materials used in nuclear systems. Results would then be utilized in the improvement of nuclear data libraries and as a means for analytical methods validation. It is proposed that experiments consisting of well-characterized quantities of materials be placed in the Northwest flux trap position of the ATR-C. The reactivity worth of the material could be determined and computationally analyzed through comprehensive benchmark activities including uncertainty analyses. Experiments were modeled in the available benchmark model of the ATR using MCNP5 with the ENDF/B-VII.0 cross section library. A single bar (9.5 cm long, 0.5 cm wide, and 121.92 cm high) of each material could provide sufficient reactivity difference in the core geometry for computational modeling and analysis. However, to provide increased opportunity for the validation of computational models, additional bars of material placed in the flux trap would increase the effective reactivity up to a limit of 1$ insertion. For simplicity in assembly manufacture, approximately four bars of material could provide a means for additional experimental benchmark configurations, except in the case of strong neutron absorbers and many materials providing positive reactivity. Future tasks include the cost analysis and development of the experimental assemblies, including means for the characterization of the neutron flux and spectral indices. Oscillation techniques may also serve to provide additional means for experimentation and validation of computational methods and acquisition of integral data for improving neutron cross sections. Further assessment of oscillation

  8. Preliminary Assessment of ATR-C Capabilities to Provide Integral Benchmark Data for Key Structural/Matrix Materials that May be Used for Nuclear Data Testing and Analytical Methods Validation

    Energy Technology Data Exchange (ETDEWEB)

    John D. Bess

    2009-07-01

    The purpose of this document is to identify some suggested types of experiments that can be performed in the Advanced Test Reactor Critical (ATR-C) facility. A fundamental computational investigation is provided to demonstrate possible integration of experimental activities in the ATR-C with the development of benchmark experiments. Criticality benchmarks performed in the ATR-C could provide integral data for key matrix and structural materials used in nuclear systems. Results would then be utilized in the improvement of nuclear data libraries and as a means for analytical methods validation. It is proposed that experiments consisting of well-characterized quantities of materials be placed in the Northwest flux trap position of the ATR-C. The reactivity worth of the material could be determined and computationally analyzed through comprehensive benchmark activities including uncertainty analyses. Experiments were modeled in the available benchmark model of the ATR using MCNP5 with the ENDF/B-VII.0 cross section library. A single bar (9.5 cm long, 0.5 cm wide, and 121.92 cm high) of each material could provide sufficient reactivity difference in the core geometry for computational modeling and analysis. However, to provide increased opportunity for the validation of computational models, additional bars of material placed in the flux trap would increase the effective reactivity up to a limit of 1$ insertion. For simplicity in assembly manufacture, approximately four bars of material could provide a means for additional experimental benchmark configurations, except in the case of strong neutron absorbers and many materials providing positive reactivity. Future tasks include the cost analysis and development of the experimental assemblies, including means for the characterization of the neutron flux and spectral indices. Oscillation techniques may also serve to provide additional means for experimentation and validation of computational methods and acquisition of

  9. Directory of Analytical Methods, Department 1820

    International Nuclear Information System (INIS)

    Whan, R.E.

    1986-01-01

    The Materials Characterization Department performs chemical, physical, and thermophysical analyses in support of programs throughout the Laboratories. The department has a wide variety of techniques and instruments staffed by experienced personnel available for these analyses, and we strive to maintain near state-of-the-art technology by continued updates. We have prepared this Directory of Analytical Methods in order to acquaint you with our capabilities and to help you identify personnel who can assist with your analytical needs. The descriptions of the various capabilities are requester-oriented and have been limited in length and detail. Emphasis has been placed on applications and limitations with notations of estimated analysis time and alternative or related techniques. A short, simplified discussion of underlying principles is also presented along with references if more detail is desired. The contents of this document have been organized in the order: bulky analysis, microanalysis, surface analysis, optical and thermal property measurements

  10. Modern methods in analytical acoustics lecture notes

    CERN Document Server

    Crighton, D G; Williams, J E Ffowcs; Heckl, M; Leppington, F G

    1992-01-01

    Modern Methods in Analytical Acoustics considers topics fundamental to the understanding of noise, vibration and fluid mechanisms. The series of lectures on which this material is based began by some twenty five years ago and has been developed and expanded ever since. Acknowledged experts in the field have given this course many times in Europe and the USA. Although the scope of the course has widened considerably, the primary aim of teaching analytical techniques of acoustics alongside specific areas of wave motion and unsteady fluid mechanisms remains. The distinguished authors of this volume are drawn from Departments of Acoustics, Engineering of Applied Mathematics in Berlin, Cambridge and London. Their intention is to reach a wider audience of all those concerned with acoustic analysis than has been able to attend the course.

  11. Big data analytics methods and applications

    CERN Document Server

    Rao, BLS; Rao, SB

    2016-01-01

    This book has a collection of articles written by Big Data experts to describe some of the cutting-edge methods and applications from their respective areas of interest, and provides the reader with a detailed overview of the field of Big Data Analytics as it is practiced today. The chapters cover technical aspects of key areas that generate and use Big Data such as management and finance; medicine and healthcare; genome, cytome and microbiome; graphs and networks; Internet of Things; Big Data standards; bench-marking of systems; and others. In addition to different applications, key algorithmic approaches such as graph partitioning, clustering and finite mixture modelling of high-dimensional data are also covered. The varied collection of themes in this volume introduces the reader to the richness of the emerging field of Big Data Analytics.

  12. Method validation in pharmaceutical analysis: from theory to practical optimization

    Directory of Open Access Journals (Sweden)

    Jaqueline Kaleian Eserian

    2015-01-01

    Full Text Available The validation of analytical methods is required to obtain high-quality data. For the pharmaceutical industry, method validation is crucial to ensure the product quality as regards both therapeutic efficacy and patient safety. The most critical step in validating a method is to establish a protocol containing well-defined procedures and criteria. A well planned and organized protocol, such as the one proposed in this paper, results in a rapid and concise method validation procedure for quantitative high performance liquid chromatography (HPLC analysis.   Type: Commentary

  13. Analytical chromatography. Methods, instrumentation and applications

    International Nuclear Information System (INIS)

    Yashin, Ya I; Yashin, A Ya

    2006-01-01

    The state-of-the-art and the prospects in the development of main methods of analytical chromatography, viz., gas, high performance liquid and ion chromatographic techniques, are characterised. Achievements of the past 10-15 years in the theory and general methodology of chromatography and also in the development of new sorbents, columns and chromatographic instruments are outlined. The use of chromatography in the environmental control, biology, medicine, pharmaceutics, and also for monitoring the quality of foodstuffs and products of chemical, petrochemical and gas industries, etc. is considered.

  14. The Emergence of the Analytical Method

    DEFF Research Database (Denmark)

    Plum, Maja

    2012-01-01

    accountability, visibility and documentation. It is argued that pedagogy is generated as a sequential and unit-specified way of working on the production of ‘the learning child’, forming a time- and material-optimising approach. Hereby, the nursery teacher, as a daily scientific researcher, comes to serve...... the nation by an ongoing observational intervention, producing the learning foundation for the entrepreneurial citizen, and thus the nation as a knowledge society in a globalised world. This is what this article terms the emergence of the analytical method....

  15. Analytical N beam position monitor method

    Directory of Open Access Journals (Sweden)

    A. Wegscheider

    2017-11-01

    Full Text Available Measurement and correction of focusing errors is of great importance for performance and machine protection of circular accelerators. Furthermore LHC needs to provide equal luminosities to the experiments ATLAS and CMS. High demands are also set on the speed of the optics commissioning, as the foreseen operation with β^{*}-leveling on luminosity will require many operational optics. A fast measurement of the β-function around a storage ring is usually done by using the measured phase advance between three consecutive beam position monitors (BPMs. A recent extension of this established technique, called the N-BPM method, was successfully applied for optics measurements at CERN, ALBA, and ESRF. We present here an improved algorithm that uses analytical calculations for both random and systematic errors and takes into account the presence of quadrupole, sextupole, and BPM misalignments, in addition to quadrupolar field errors. This new scheme, called the analytical N-BPM method, is much faster, further improves the measurement accuracy, and is applicable to very pushed beam optics where the existing numerical N-BPM method tends to fail.

  16. Analytical N beam position monitor method

    Science.gov (United States)

    Wegscheider, A.; Langner, A.; Tomás, R.; Franchi, A.

    2017-11-01

    Measurement and correction of focusing errors is of great importance for performance and machine protection of circular accelerators. Furthermore LHC needs to provide equal luminosities to the experiments ATLAS and CMS. High demands are also set on the speed of the optics commissioning, as the foreseen operation with β*-leveling on luminosity will require many operational optics. A fast measurement of the β -function around a storage ring is usually done by using the measured phase advance between three consecutive beam position monitors (BPMs). A recent extension of this established technique, called the N-BPM method, was successfully applied for optics measurements at CERN, ALBA, and ESRF. We present here an improved algorithm that uses analytical calculations for both random and systematic errors and takes into account the presence of quadrupole, sextupole, and BPM misalignments, in addition to quadrupolar field errors. This new scheme, called the analytical N-BPM method, is much faster, further improves the measurement accuracy, and is applicable to very pushed beam optics where the existing numerical N-BPM method tends to fail.

  17. Analytical thermal model validation for Cassini radioisotope thermoelectric generator

    International Nuclear Information System (INIS)

    Lin, E.I.

    1997-01-01

    The Saturn-bound Cassini spacecraft is designed to rely, without precedent, on the waste heat from its three radioisotope thermoelectric generators (RTGs) to warm the propulsion module subsystem, and the RTG end dome temperature is a key determining factor of the amount of waste heat delivered. A previously validated SINDA thermal model of the RTG was the sole guide to understanding its complex thermal behavior, but displayed large discrepancies against some initial thermal development test data. A careful revalidation effort led to significant modifications and adjustments of the model, which result in a doubling of the radiative heat transfer from the heat source support assemblies to the end domes and bring up the end dome and flange temperature predictions to within 2 C of the pertinent test data. The increased inboard end dome temperature has a considerable impact on thermal control of the spacecraft central body. The validation process offers an example of physically-driven analytical model calibration with test data from not only an electrical simulator but also a nuclear-fueled flight unit, and has established the end dome temperatures of a flight RTG where no in-flight or ground-test data existed before

  18. A validated analytical method to study the long-term stability of natural and synthetic glucocorticoids in livestock urine using ultra-high performance liquid chromatography coupled to Orbitrap-high resolution mass spectrometry.

    Science.gov (United States)

    De Clercq, Nathalie; Julie, Vanden Bussche; Croubels, Siska; Delahaut, Philippe; Vanhaecke, Lynn

    2013-08-02

    Due to their growth-promoting effects, the use of synthetic glucocorticoids is strictly regulated in the European Union (Council Directive 2003/74/EC). In the frame of the national control plans, which should ensure the absence of residues in food products of animal origin, in recent years, a higher frequency of prednisolone positive bovine urines has been observed. This has raised questions with respect to the stability of natural corticoids in the respective urine samples and their potential to be transformed into synthetic analogs. In this study, a ultra high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) methodology was developed to examine the stability of glucocorticoids in bovine urine under various storage conditions (up to 20 weeks) and to define suitable conditions for sample handling and storage, using an Orbitrap Exactive™. To this end, an extraction procedure was optimized using a Plackett-Burman experimental design to determine the key conditions for optimal extraction of glucocorticoids from urine. Next, the analytical method was successfully validated according to the guidelines of CD 2002/657/EC. Decision limits and detection capabilities for prednisolone, prednisone and methylprednisolone ranged, respectively, from 0.1 to 0.5μgL(-1) and from 0.3 to 0.8μgL(-1). For the natural glucocorticoids limits of detection and limits of quantification for dihydrocortisone, cortisol and cortisone ranged, respectively, from 0.1 to 0.2μgL(-1) and from 0.3 to 0.8μgL(-1). The stability study demonstrated that filter-sterilization of urine, storage at -80°C, and acidic conditions (pH 3) were optimal for preservation of glucocorticoids in urine and able to significantly limit degradation up to 20 weeks. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Model-Based Method for Sensor Validation

    Science.gov (United States)

    Vatan, Farrokh

    2012-01-01

    Fault detection, diagnosis, and prognosis are essential tasks in the operation of autonomous spacecraft, instruments, and in situ platforms. One of NASA s key mission requirements is robust state estimation. Sensing, using a wide range of sensors and sensor fusion approaches, plays a central role in robust state estimation, and there is a need to diagnose sensor failure as well as component failure. Sensor validation can be considered to be part of the larger effort of improving reliability and safety. The standard methods for solving the sensor validation problem are based on probabilistic analysis of the system, from which the method based on Bayesian networks is most popular. Therefore, these methods can only predict the most probable faulty sensors, which are subject to the initial probabilities defined for the failures. The method developed in this work is based on a model-based approach and provides the faulty sensors (if any), which can be logically inferred from the model of the system and the sensor readings (observations). The method is also more suitable for the systems when it is hard, or even impossible, to find the probability functions of the system. The method starts by a new mathematical description of the problem and develops a very efficient and systematic algorithm for its solution. The method builds on the concepts of analytical redundant relations (ARRs).

  20. The analytic nodal method in cylindrical geometry

    International Nuclear Information System (INIS)

    Prinsloo, Rian H.; Tomasevic, Djordje I.

    2008-01-01

    Nodal diffusion methods have been used extensively in nuclear reactor calculations, specifically for their performance advantage, but also for their superior accuracy. More specifically, the Analytic Nodal Method (ANM), utilising the transverse integration principle, has been applied to numerous reactor problems with much success. In this work, a nodal diffusion method is developed for cylindrical geometry. Application of this method to three-dimensional (3D) cylindrical geometry has never been satisfactorily addressed and we propose a solution which entails the use of conformal mapping. A set of 1D-equations with an adjusted, geometrically dependent, inhomogeneous source, is obtained. This work describes the development of the method and associated test code, as well as its application to realistic reactor problems. Numerical results are given for the PBMR-400 MW benchmark problem, as well as for a 'cylindrisized' version of the well-known 3D LWR IAEA benchmark. Results highlight the improved accuracy and performance over finite-difference core solutions and investigate the applicability of nodal methods to 3D PBMR type problems. Results indicate that cylindrical nodal methods definitely have a place within PBMR applications, yielding performance advantage factors of 10 and 20 for 2D and 3D calculations, respectively, and advantage factors of the order of 1000 in the case of the LWR problem

  1. Radiochemical methods. Analytical chemistry by open learning

    Energy Technology Data Exchange (ETDEWEB)

    Geary, W.J.; James, A.M. (ed.)

    1986-01-01

    This book presents the analytical uses of radioactive isotopes within the context of radiochemistry as a whole. It is designed for scientists with relatively little background knowledge of the subject. Thus the initial emphasis is on developing the basic concepts of radioactive decay, particularly as they affect the potential usage of radioisotopes. Discussion of the properties of various types of radiation, and of factors such as half-life, is related to practical considerations such as counting and preparation methods, and handling/disposal problems. Practical aspects are then considered in more detail, and the various radioanalytical methods are outlined with particular reference to their applicability. The approach is 'user friendly' and the use of self assessment questions allows the reader to test his/her understanding of individual sections easily. For those who wish to develop their knowledge further, a reading list is provided.

  2. Numerical methods: Analytical benchmarking in transport theory

    International Nuclear Information System (INIS)

    Ganapol, B.D.

    1988-01-01

    Numerical methods applied to reactor technology have reached a high degree of maturity. Certainly one- and two-dimensional neutron transport calculations have become routine, with several programs available on personal computer and the most widely used programs adapted to workstation and minicomputer computational environments. With the introduction of massive parallelism and as experience with multitasking increases, even more improvement in the development of transport algorithms can be expected. Benchmarking an algorithm is usually not a very pleasant experience for the code developer. Proper algorithmic verification by benchmarking involves the following considerations: (1) conservation of particles, (2) confirmation of intuitive physical behavior, and (3) reproduction of analytical benchmark results. By using today's computational advantages, new basic numerical methods have been developed that allow a wider class of benchmark problems to be considered

  3. Detection of food irradiation - two analytical methods

    International Nuclear Information System (INIS)

    1994-01-01

    This publication summarizes the activities of Nordic countries in the field of detection of irradiated food. The National Food Agency of Denmark has coordinated the project. The two analytical methods investigated were: the gas-chromatographic determination of the hydrocarbon/lipid ratio in irradiated chicken meat, and a bioassay based on microelectrophoresis of DNA from single cells. Also a method for determination of o-tyrosine in the irradiated and non-irradiated chicken meat has been tested. The first method based on radiolytical changes in fatty acids, contained in chicken meat, has been tested and compared in the four Nordic countries. Four major hydrocarbons (C16:2, C16:3, C17:1 and C17:2) have been determined and reasonable agreement was observed between the dose level and hydrocarbons concentration. Results of a bioassay, where strand breaks of DNA are demonstrated by microelectrophoresis of single cells, prove a correlation between the dose levels and the pattern of DNA fragments migration. The hydrocarbon method can be applied to detect other irradiated, fat-containing foods, while the DNA method can be used for some animal and some vegetable foods as well.Both methods allow to determine the fact of food irradiation beyond any doubt, thus making them suitable for food control analysis. The detailed determination protocols are given. (EG)

  4. Validation of the method for investigation of radiopharmaceuticals for in vitro use

    International Nuclear Information System (INIS)

    Vranjes, S; Jovanovic, M.; Orlic, M.; Lazic, E. . E-mail address of corresponding author: sanjav@vin.bg.ac.yu

    2005-01-01

    The aim of this study was to validate analytical method for determination of total radioactivity and radioactive concentration of 125 I-triiodotironin, radiopharmaceutical for in vitro use. Analytical parameters: selectivity, accuracy, linearity and range of this method were determined. Values obtained for all parameters are reasonable for analytical methods, therefore this method could be used for farther investigation. (author)

  5. Analytical method for Buddleja colorants in foods.

    Science.gov (United States)

    Aoki, H; Kuze, N; Ichi, T; Koda, T

    2001-04-01

    Buddleja yellow colorant derived from Buddleja officinalis Maxim. has recently been approved for use as a new kind of natural colorant for food additives in China. In order to distinguish Buddleja yellow colorant from other yellow colorants, two known phenylpropanoid glycosides, acteoside (= verbascoside) and poliumoside, were isolated from the colorant as marker substances for Buddleja yellow colorant. Poliumoside has not been detected in B. officinalis Maxim. previously. These phenylpropanoid glycosides were not detected in the fruits of Gardenia jasminoides Ellis or in the stamens of the flowers of Crocus sativus L., which also contain crocetin derivatives as coloring components, using a photodiode array and mass chromatograms. Thus, an analytical HPLC method was developed to distinguish foods that have been colored with yellow colorants containing crocetin derivatives, using phenylpropanoid glycosides as markers.

  6. Analytical method for high resolution liquid chromatography for quality control French Macaw

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad M; Torres Amaro, Leonid; Menendez Castillo, Rosa; Sanchez, Esther; Martinez Espinosa, Vivian; Gonzalez, Maria Lidia; Rodriguez, Carlos

    2007-01-01

    Was developed and validated an analytical method for high resolution liquid chromatography applicable to quality control of drugs dry French Macaw (Senna alata L. Roxb.) With ultraviolet detection at 340 nm. The method for high resolution liquid chromatography used to quantify the sennosides A and B, main components, was validated and proved to be specific, linear, precise and accurate. (Author)

  7. Validation of an advanced analytical procedure applied to the measurement of environmental radioactivity.

    Science.gov (United States)

    Thanh, Tran Thien; Vuong, Le Quang; Ho, Phan Long; Chuong, Huynh Dinh; Nguyen, Vo Hoang; Tao, Chau Van

    2018-04-01

    In this work, an advanced analytical procedure was applied to calculate radioactivity in spiked water samples in a close geometry gamma spectroscopy. It included MCNP-CP code in order to calculate the coincidence summing correction factor (CSF). The CSF results were validated by a deterministic method using ETNA code for both p-type HPGe detectors. It showed that a good agreement for both codes. Finally, the validity of the developed procedure was confirmed by a proficiency test to calculate the activities of various radionuclides. The results of the radioactivity measurement with both detectors using the advanced analytical procedure were received the ''Accepted'' statuses following the proficiency test. Copyright © 2018 Elsevier Ltd. All rights reserved.

  8. Microgenetic Learning Analytics Methods: Workshop Report

    Science.gov (United States)

    Aghababyan, Ani; Martin, Taylor; Janisiewicz, Philip; Close, Kevin

    2016-01-01

    Learning analytics is an emerging discipline and, as such, benefits from new tools and methodological approaches. This work reviews and summarizes our workshop on microgenetic data analysis techniques using R, held at the second annual Learning Analytics Summer Institute in Cambridge, Massachusetts, on 30 June 2014. Specifically, this paper…

  9. Validación de un método analítico empleando cromatografía líquida de alta eficiencia para la determinación de ibuprofeno en medios biorrelevantes Validation of an analytical method by liquid chromatography for determination of ibuprofen in biorelevant media

    Directory of Open Access Journals (Sweden)

    Sandra M. Gómez

    2010-01-01

    Full Text Available An analytical method by liquid chromatography has been proposed and validated to study the apparent solubility of ibuprofen in biorelevant dissolution media. The main properties of the studied media were pH values of 5.0 and 6.5 and the presence or absence of some natural surfactant agents. The parameters evaluated were specificity, linearity, precision, accuracy, and detection and quantification limits, as well as the drug stability under the analysis conditions. The developed method was useful to determine the apparent solubility of this drug as a function of temperature and surfactants concentration to demonstrate the validity of the Biopharmaceutics Classification System.

  10. Hanford environmental analytical methods: Methods as of March 1990

    International Nuclear Information System (INIS)

    Goheen, S.C.; McCulloch, M.; Daniel, J.L.

    1993-05-01

    This paper from the analytical laboratories at Hanford describes the method used to measure pH of single-shell tank core samples. Sludge or solid samples are mixed with deionized water. The pH electrode used combines both a sensor and reference electrode in one unit. The meter amplifies the input signal from the electrode and displays the pH visually

  11. Analytical Method to Estimate the Complex Permittivity of Oil Samples

    Directory of Open Access Journals (Sweden)

    Lijuan Su

    2018-03-01

    Full Text Available In this paper, an analytical method to estimate the complex dielectric constant of liquids is presented. The method is based on the measurement of the transmission coefficient in an embedded microstrip line loaded with a complementary split ring resonator (CSRR, which is etched in the ground plane. From this response, the dielectric constant and loss tangent of the liquid under test (LUT can be extracted, provided that the CSRR is surrounded by such LUT, and the liquid level extends beyond the region where the electromagnetic fields generated by the CSRR are present. For that purpose, a liquid container acting as a pool is added to the structure. The main advantage of this method, which is validated from the measurement of the complex dielectric constant of olive and castor oil, is that reference samples for calibration are not required.

  12. The validation of the analytical method (HPLC, use for identification and assay of the pharmaceutical active ingredient, colistine sulphate and the finished product Colidem 50 – hydrosoluble powder, in SC DELOS impex ‘96 SRL

    Directory of Open Access Journals (Sweden)

    Maria Neagu,

    2011-06-01

    Full Text Available In SC DELOS IMPEX ’96 SRL the quality of the active pharmaceutical ingredient (API for the finished product Colidem 50 - hydrosoluble powder is make according to European Pharmacopoeia, curent edition. The method for analysis use in this purpose is the compendial method „Colistine sulphate” in E.P. in current edition and represent a optimized variant, developed and validated „in house”.The parameters which was included in the methodology validation for chromatographic method are the follow: Selectivity/Specificity, Linearity, Range of Linearity, Limit of Detection and Limit of Quantification, Precision (Repeatability - intra day, inter-Day Reproducibility, Accuracy, Robustness, Stability Solutions and System Suitability.

  13. Evaluation and analytical validation of a handheld digital refractometer for urine specific gravity measurement

    Directory of Open Access Journals (Sweden)

    Sara P. Wyness

    2016-08-01

    Full Text Available Objectives: Refractometers are commonly used to determine urine specific gravity (SG in the assessment of hydration status and urine specimen validity testing. Few comprehensive performance evaluations are available demonstrating refractometer capability from a clinical laboratory perspective. The objective of this study was therefore to conduct an analytical validation of a handheld digital refractometer used for human urine SG testing. Design and methods: A MISCO Palm Abbe™ refractometer was used for all experiments, including device familiarization, carryover, precision, accuracy, linearity, analytical sensitivity, evaluation of potential substances which contribute to SG (i.e. “interference”, and reference interval evaluation. A manual refractometer, urine osmometer, and a solute score (sum of urine chloride, creatinine, glucose, potassium, sodium, total protein, and urea nitrogen; all in mg/dL were used as comparative methods for accuracy assessment. Results: Significant carryover was not observed. A wash step was still included as good laboratory practice. Low imprecision (%CV, <0.01 was demonstrated using low and high QC material. Accuracy studies showed strong correlation to manual refractometry. Linear correlation was also demonstrated between SG, osmolality, and solute score. Linearity of Palm Abbe performance was verified with observed error of ≤0.1%. Increases in SG were observed with increasing concentrations of albumin, creatinine, glucose, hemoglobin, sodium chloride, and urea. Transference of a previously published urine SG reference interval of 1.0020–1.0300 was validated. Conclusions: The Palm Abbe digital refractometer was a fast, simple, and accurate way to measure urine SG. Analytical validity was confirmed by the present experiments. Keywords: Specific gravity, Osmolality, Digital refractometry, Hydration, Sports medicine, Urine drug testing, Urine adulteration

  14. Analytical validation of Gentian NGAL particle-enhanced enhanced turbidimetric immunoassay (PETIA

    Directory of Open Access Journals (Sweden)

    Gian Luca Salvagno

    2017-08-01

    Full Text Available Objectives: This study was designed to validate the analytical performance of the new Gentian particle-enhanced enhanced turbidimetric immunoassay (PETIA for measuring neutrophil gelatinase-associated lipocalin (NGAL in serum samples. Design and methods: Analytical validation of the Gentian NGAL assay was carried out on a Roche Cobas c501 and was based on assessment of limit of blank (LOB, limit of detection (LOD, functional sensitivity, imprecision, linearity and concordance with the BioPorto NGAL test. Results: The LOB and LOD of Gentian NGAL were found to be 3.8 ng/mL and 6.3 ng/mL, respectively. An analytical coefficient of variation (CV of 20% corresponded to a NGAL value of 10 ng/mL. The intra-assay and inter-assay imprecision (CV was between 0.4 and 5.2% and 0.6 and 7.1% and the total imprecision (CV was 3.7%. The linearity was optimal at NGAL concentrations between 37 and 1420 ng/mL (r=1.00; p<0.001. An excellent correlation was observed between values measured with Gentian NGAL and BioPorto NGAL in 74 routine serum samples (r=0.993. The mean percentage bias of the Gentian assay versus the Bioporto assay was +3.1% (95% CI, +1.6% to +4.5%. Conclusions: These results show that Gentian NGAL may be a viable option to other commercial immunoassays for both routine and urgent assessment of serum NGAL. Keywords: Neutrophil gelatinase-associated lipocalin, NGAL, Analytical validation, Acute kidney injury

  15. Method for effective usage of Google Analytics tools

    Directory of Open Access Journals (Sweden)

    Ирина Николаевна Егорова

    2016-01-01

    Full Text Available Modern Google Analytics tools have been investigated against effective attraction channels for users and bottlenecks detection. Conducted investigation allowed to suggest modern method for effective usage of Google Analytics tools. The method is based on main traffic indicators analysis, as well as deep analysis of goals and their consecutive tweaking. Method allows to increase website conversion and might be useful for SEO and Web analytics specialists

  16. Nonlinear ordinary differential equations analytical approximation and numerical methods

    CERN Document Server

    Hermann, Martin

    2016-01-01

    The book discusses the solutions to nonlinear ordinary differential equations (ODEs) using analytical and numerical approximation methods. Recently, analytical approximation methods have been largely used in solving linear and nonlinear lower-order ODEs. It also discusses using these methods to solve some strong nonlinear ODEs. There are two chapters devoted to solving nonlinear ODEs using numerical methods, as in practice high-dimensional systems of nonlinear ODEs that cannot be solved by analytical approximate methods are common. Moreover, it studies analytical and numerical techniques for the treatment of parameter-depending ODEs. The book explains various methods for solving nonlinear-oscillator and structural-system problems, including the energy balance method, harmonic balance method, amplitude frequency formulation, variational iteration method, homotopy perturbation method, iteration perturbation method, homotopy analysis method, simple and multiple shooting method, and the nonlinear stabilized march...

  17. 40 CFR 141.25 - Analytical methods for radioactivity.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 22 2010-07-01 2010-07-01 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...

  18. Validation of an analytical method for nitrous oxide (N2O) laughing gas by headspace gas chromatography coupled to mass spectrometry (HS-GC-MS): forensic application to a lethal intoxication.

    Science.gov (United States)

    Giuliani, N; Beyer, J; Augsburger, M; Varlet, V

    2015-03-01

    Drug abuse is a widespread problem affecting both teenagers and adults. Nitrous oxide is becoming increasingly popular as an inhalation drug, causing harmful neurological and hematological effects. Some gas chromatography-mass spectrometry (GC-MS) methods for nitrous oxide measurement have been previously described. The main drawbacks of these methods include a lack of sensitivity for forensic applications; including an inability to quantitatively determine the concentration of gas present. The following study provides a validated method using HS-GC-MS which incorporates hydrogen sulfide as a suitable internal standard allowing the quantification of nitrous oxide. Upon analysis, sample and internal standard have similar retention times and are eluted quickly from the molecular sieve 5Å PLOT capillary column and the Porabond Q column therefore providing rapid data collection whilst preserving well defined peaks. After validation, the method has been applied to a real case of N2O intoxication indicating concentrations in a mono-intoxication. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Analytical validation of a new point-of-care assay for serum amyloid A in horses.

    Science.gov (United States)

    Schwartz, D; Pusterla, N; Jacobsen, S; Christopher, M M

    2018-01-17

    Serum amyloid A (SAA) is a major acute phase protein in horses. A new point-of-care (POC) test for SAA (Stablelab) is available, but studies evaluating its analytical accuracy are lacking. To evaluate the analytical performance of the SAA POC test by 1) determining linearity and precision, 2) comparing results in whole blood with those in serum or plasma, and 3) comparing POC results with those obtained using a previously validated turbidimetric immunoassay (TIA). Assay validation. Analytical validation of the POC test was done in accordance with American Society of Veterinary Clinical Pathology guidelines using residual equine serum/plasma and whole blood samples from the Clinical Pathology Laboratory at the University of California-Davis. A TIA was used as the reference method. We also evaluated the effect of haematocrit (HCT). The POC test was linear for SAA concentrations of up to at least 1000 μg/mL (r = 0.991). Intra-assay CVs were 13, 18 and 15% at high (782 μg/mL), intermediate (116 μg/mL) and low (64 μg/mL) concentrations. Inter-assay (inter-batch) CVs were 45, 14 and 15% at high (1372 μg/mL), intermediate (140 μg/mL) and low (56 μg/mL) concentrations. SAA results in whole blood were significantly lower than those in serum/plasma (P = 0.0002), but were positively correlated (r = 0.908) and not affected by HCT (P = 0.261); proportional negative bias was observed in samples with SAA>500 μg/mL. The difference between methods exceeded the 95% confidence interval of the combined imprecision of both methods (15%). Analytical validation could not be performed in whole blood, the sample most likely to be used stall side. The POC test has acceptable accuracy and precision in equine serum/plasma with SAA concentrations of up to at least 1000 μg/mL. Low inter-batch precision at high concentrations may affect serial measurements, and the use of the same test batch and sample type (serum/plasma or whole blood) is recommended. Comparison of results between the

  20. Analytical methods for heat transfer and fluid flow problems

    CERN Document Server

    Weigand, Bernhard

    2015-01-01

    This book describes useful analytical methods by applying them to real-world problems rather than solving the usual over-simplified classroom problems. The book demonstrates the applicability of analytical methods even for complex problems and guides the reader to a more intuitive understanding of approaches and solutions. Although the solution of Partial Differential Equations by numerical methods is the standard practice in industries, analytical methods are still important for the critical assessment of results derived from advanced computer simulations and the improvement of the underlying numerical techniques. Literature devoted to analytical methods, however, often focuses on theoretical and mathematical aspects and is therefore useless to most engineers. Analytical Methods for Heat Transfer and Fluid Flow Problems addresses engineers and engineering students. The second edition has been updated, the chapters on non-linear problems and on axial heat conduction problems were extended. And worked out exam...

  1. Recent developments in analytical detection methods for radiation processed foods

    International Nuclear Information System (INIS)

    Wu Jilan

    1993-01-01

    A short summary of the programmes of 'ADMIT' (FAO/IAEA) and the developments in analytical detection methods for radiation processed foods has been given. It is suggested that for promoting the commercialization of radiation processed foods and controlling its quality, one must pay more attention to the study of analytical detection methods of irradiated food

  2. On the validity and practical applicability of derivative analyticity relations

    International Nuclear Information System (INIS)

    Kolar, P.; Fischer, J.

    1983-09-01

    We examine derivative analyticity relations (DAR), which were originally proposed by Bronzan as an alternative to dispersion relations and in which the dispersion integral is replaced by a tangent series of derivatives. We characterize the class of functions satisfying DAR, and show that outside this class the dispersion integral represents a Borel-like sum of tangent series. We point out difficulties connected with the application of DAR. (author)

  3. Approximate Analytic and Numerical Solutions to Lane-Emden Equation via Fuzzy Modeling Method

    Directory of Open Access Journals (Sweden)

    De-Gang Wang

    2012-01-01

    Full Text Available A novel algorithm, called variable weight fuzzy marginal linearization (VWFML method, is proposed. This method can supply approximate analytic and numerical solutions to Lane-Emden equations. And it is easy to be implemented and extended for solving other nonlinear differential equations. Numerical examples are included to demonstrate the validity and applicability of the developed technique.

  4. Analytical methods for predicting contaminant transport

    International Nuclear Information System (INIS)

    Pigford, T.H.

    1989-09-01

    This paper summarizes some of the previous and recent work at the University of California on analytical solutions for predicting contaminate transport in porous and fractured geologic media. Emphasis is given here to the theories for predicting near-field transport, needed to derive the time-dependent source term for predicting far-field transport and overall repository performance. New theories summarized include solubility-limited release rate with flow backfill in rock, near-field transport of radioactive decay chains, interactive transport of colloid and solute, transport of carbon-14 as carbon dioxide in unsaturated rock, and flow of gases out of and a waste container through cracks and penetrations. 28 refs., 4 figs

  5. Valid analytical performance specifications for combined analytical bias and imprecision for the use of common reference intervals.

    Science.gov (United States)

    Hyltoft Petersen, Per; Lund, Flemming; Fraser, Callum G; Sandberg, Sverre; Sölétormos, György

    2018-01-01

    Background Many clinical decisions are based on comparison of patient results with reference intervals. Therefore, an estimation of the analytical performance specifications for the quality that would be required to allow sharing common reference intervals is needed. The International Federation of Clinical Chemistry (IFCC) recommended a minimum of 120 reference individuals to establish reference intervals. This number implies a certain level of quality, which could then be used for defining analytical performance specifications as the maximum combination of analytical bias and imprecision required for sharing common reference intervals, the aim of this investigation. Methods Two methods were investigated for defining the maximum combination of analytical bias and imprecision that would give the same quality of common reference intervals as the IFCC recommendation. Method 1 is based on a formula for the combination of analytical bias and imprecision and Method 2 is based on the Microsoft Excel formula NORMINV including the fractional probability of reference individuals outside each limit and the Gaussian variables of mean and standard deviation. The combinations of normalized bias and imprecision are illustrated for both methods. The formulae are identical for Gaussian and log-Gaussian distributions. Results Method 2 gives the correct results with a constant percentage of 4.4% for all combinations of bias and imprecision. Conclusion The Microsoft Excel formula NORMINV is useful for the estimation of analytical performance specifications for both Gaussian and log-Gaussian distributions of reference intervals.

  6. Some analytical methods for explosives: Part 2

    Energy Technology Data Exchange (ETDEWEB)

    Selig, W.

    1965-12-08

    This report is the second compilation of methods for analyzing explosives. All the methods were developed for routine performance by techniques, and an attempt has therefore been made to keep them as simple as possible. Methods are presented for analyzing plastic-bonded explosives based on sym-cyclomethylenetetra-nitramine (HMX), based on viton in addition to HMX, and based on pentraerythritol tetranitrate (PETN).

  7. Validation of NAA Method for Urban Particulate Matter

    International Nuclear Information System (INIS)

    Woro Yatu Niken Syahfitri; Muhayatun; Diah Dwiana Lestiani; Natalia Adventini

    2009-01-01

    Nuclear analytical techniques have been applied in many countries for determination of environmental pollutant. Method of NAA (neutron activation analysis) representing one of nuclear analytical technique of that has low detection limits, high specificity, high precision, and accuracy for large majority of naturally occurring elements, and ability of non-destructive and simultaneous determination of multi-elemental, and can handle small sample size (< 1 mg). To ensure quality and reliability of the method, validation are needed to be done. A standard reference material, SRM NIST 1648 Urban Particulate Matter, has been used to validate NAA method. Accuracy and precision test were used as validation parameters. Particulate matter were validated for 18 elements: Ti, I, V, Br, Mn, Na, K, Cl, Cu, Al, As, Fe, Co, Zn, Ag, La, Cr, and Sm,. The result showed that the percent relative standard deviation of the measured elemental concentrations are found to be within ranged from 2 to 14,8% for most of the elements analyzed whereas Hor rat value in range 0,3-1,3. Accuracy test results showed that relative bias ranged from -11,1 to 3,6%. Based on validation results, it can be stated that NAA method is reliable for characterization particulate matter and other similar matrix samples to support air quality monitoring. (author)

  8. Analytical method for solving radioactive transformations

    International Nuclear Information System (INIS)

    Vukadin, Z.

    1999-01-01

    The exact method of solving radioactive transformations is presented. Nonsingular Bateman coefficients, which can be computed using recurrence formulas, greatly reduce computational time and eliminate singularities that often arise in problems involving nuclide transmutations. Depletion function power series expansion enables high accuracy of the performed calculations, specially in a case of a decay constants with closely spaced values. Generality and simplicity of the method make the method useful for many practical applications. (author)

  9. Determination of aluminum by four analytical methods

    International Nuclear Information System (INIS)

    Hanson, T.J.; Smetana, K.M.

    1975-11-01

    Four procedures have been developed for determining the aluminum concentration in basic matrices. Atomic Absorption Spectroscopy (AAS) was the routine method of analysis. Citrate was required to complex the aluminum and eliminate matrix effects. AAS was the least accurate of the four methods studied and was adversely affected by high aluminum concentrations. The Fluoride Electrode Method was the most accurate and precise of the four methods. A Gran's Plot determination was used to determine the end point and average standard recovery was 100% +- 2%. The Thermometric Titration Method was the fastest method for determining aluminum and could also determine hydroxide concentration at the same time. Standard recoveries were 100% +- 5%. The pH Electrode Method also measures aluminum and hydroxide content simultaneously, but is less accurate and more time consuming that the thermal titration. Samples were analyzed using all four methods and results were compared to determine the strengths and weaknesses of each. On the basis of these comparisons, conclusions were drawn concerning the application of each method to our laboratory needs

  10. Application of system reliability analytical method, GO-FLOW

    International Nuclear Information System (INIS)

    Matsuoka, Takeshi; Fukuto, Junji; Mitomo, Nobuo; Miyazaki, Keiko; Matsukura, Hiroshi; Kobayashi, Michiyuki

    1999-01-01

    The Ship Research Institute proceed a developmental study on GO-FLOW method with various advancing functionalities for the system reliability analysis method occupying main parts of PSA (Probabilistic Safety Assessment). Here was attempted to intend to upgrade functionality of the GO-FLOW method, to develop an analytical function integrated with dynamic behavior analytical function, physical behavior and probable subject transfer, and to prepare a main accident sequence picking-out function. In 1997 fiscal year, in dynamic event-tree analytical system, an analytical function was developed by adding dependency between headings. In simulation analytical function of the accident sequence, main accident sequence of MRX for improved ship propulsion reactor became possible to be covered perfectly. And, input data for analysis was prepared with a function capable easily to set by an analysis operator. (G.K.)

  11. Extension of the analytic nodal method to four energy groups

    International Nuclear Information System (INIS)

    Parsons, D.K.; Nigg, D.W.

    1985-01-01

    The Analytic Nodal Method is one of several recently-developed coarse mesh numerical methods for efficiently and accurately solving the multidimensional static and transient neutron diffusion equations. This summary describes a mathematically rigorous extension of the Analytic Nodal Method to the frequently more physically realistic four-group case. A few general theoretical considerations are discussed, followed by some calculated results for a typical steady-state two-dimensional PWR quarter core application. 8 refs

  12. Intercalibration of analytical methods on marine environmental samples

    International Nuclear Information System (INIS)

    1988-06-01

    The pollution of the seas by various chemical substances constitutes nowadays one of the principal concerns of mankind. The International Atomic Energy Agency has organized in past years several intercomparison exercises in the framework of its Analytical Quality Control Service. The present intercomparison had a double aim: first, to give laboratories participating in this intercomparison an opportunity for checking their analytical performance. Secondly, to produce on the basis of the results of this intercomparison a reference material made of fish tissue which would be accurately certified with respect to many trace elements. Such a material could be used by analytical chemists to check the validity of new analytical procedures. In total, 53 laboratories from 29 countries reported results (585 laboratory means for 48 elements). 5 refs, 52 tabs

  13. Analytical methods applied to water pollution

    International Nuclear Information System (INIS)

    Baudin, G.

    1977-01-01

    A comparison of different methods applied to water analysis is given. The discussion is limited to the problems presented by inorganic elements, accessible to nuclear activation analysis methods. The following methods were compared: activation analysis: with gamma-ray spectrometry, atomic absorption spectrometry, fluorimetry, emission spectrometry, colorimetry or spectrophotometry, X-ray fluorescence, mass spectrometry, voltametry, polarography or other electrochemical methods, activation analysis-beta measurements. Drinking-water, irrigation waters, sea waters, industrial wastes and very pure waters are the subjects of the investigations. The comparative evaluation is made on the basis of storage of samples, in situ analysis, treatment and concentration, specificity and interference, monoelement or multielement analysis, analysis time and accuracy. The significance of the neutron analysis is shown. (T.G.)

  14. Measuring Students' Writing Ability on a Computer-Analytic Developmental Scale: An Exploratory Validity Study

    Science.gov (United States)

    Burdick, Hal; Swartz, Carl W.; Stenner, A. Jackson; Fitzgerald, Jill; Burdick, Don; Hanlon, Sean T.

    2013-01-01

    The purpose of the study was to explore the validity of a novel computer-analytic developmental scale, the Writing Ability Developmental Scale. On the whole, collective results supported the validity of the scale. It was sensitive to writing ability differences across grades and sensitive to within-grade variability as compared to human-rated…

  15. Analytical method for establishing indentation rolling resistance

    Directory of Open Access Journals (Sweden)

    Gładysiewicz Lech

    2018-01-01

    Full Text Available Belt conveyors are highly reliable machines able to work in special operating conditions. Harsh environment, long distance of transporting and great mass of transported martials are cause of high energy usage. That is why research in the field of belt conveyor transportation nowadays focuses on reducing the power consumption without lowering their efficiency. In this paper, previous methods for testing rolling resistance are described, and new method designed by authors was presented. New method of testing rolling resistance is quite simple and inexpensive. Moreover it allows to conduct the experimental tests of the impact of different parameters on the value of indentation rolling resistance such as core design, cover thickness, ambient temperature, idler travel frequency, or load value as well. Finally results of tests of relationship between rolling resistance and idler travel frequency and between rolling resistance and idler travel speed was presented.

  16. Analytical method for establishing indentation rolling resistance

    Science.gov (United States)

    Gładysiewicz, Lech; Konieczna, Martyna

    2018-01-01

    Belt conveyors are highly reliable machines able to work in special operating conditions. Harsh environment, long distance of transporting and great mass of transported martials are cause of high energy usage. That is why research in the field of belt conveyor transportation nowadays focuses on reducing the power consumption without lowering their efficiency. In this paper, previous methods for testing rolling resistance are described, and new method designed by authors was presented. New method of testing rolling resistance is quite simple and inexpensive. Moreover it allows to conduct the experimental tests of the impact of different parameters on the value of indentation rolling resistance such as core design, cover thickness, ambient temperature, idler travel frequency, or load value as well. Finally results of tests of relationship between rolling resistance and idler travel frequency and between rolling resistance and idler travel speed was presented.

  17. Analytical methods for the determination of tungsten

    International Nuclear Information System (INIS)

    Topping, J.J.

    1978-01-01

    Methods developed and employed in the recent literature (1969 to 1975) for the detection and determination of tungsten in a wide variety of matrices are reviewed. This paper is a supplement to the books, monographs and review papers which deal with the earlier literature. (author)

  18. Surveillance of emerging drugs of abuse in Hong Kong: validation of an analytical tool.

    Science.gov (United States)

    Tang, Magdalene H Y; Ching, C K; Tse, M L; Ng, Carol; Lee, Caroline; Chong, Y K; Wong, Watson; Mak, Tony W L

    2015-04-01

    To validate a locally developed chromatography-based method to monitor emerging drugs of abuse whilst performing regular drug testing in abusers. Cross-sectional study. Eleven regional hospitals, seven social service units, and a tertiary level clinical toxicology laboratory in Hong Kong. A total of 972 drug abusers and high-risk individuals were recruited from acute, rehabilitation, and high-risk settings between 1 November 2011 and 31 July 2013. A subset of the participants was of South Asian ethnicity. In total, 2000 urine or hair specimens were collected. Proof of concept that surveillance of emerging drugs of abuse can be performed whilst conducting routine drug of abuse testing in patients. The method was successfully applied to 2000 samples with three emerging drugs of abuse detected in five samples: PMMA (paramethoxymethamphetamine), TFMPP [1-(3-trifluoromethylphenyl)piperazine], and methcathinone. The method also detected conventional drugs of abuse, with codeine, methadone, heroin, methamphetamine, and ketamine being the most frequently detected drugs. Other findings included the observation that South Asians had significantly higher rates of using opiates such as heroin, methadone, and codeine; and that ketamine and cocaine had significantly higher detection rates in acute subjects compared with the rehabilitation population. This locally developed analytical method is a valid tool for simultaneous surveillance of emerging drugs of abuse and routine drug monitoring of patients at minimal additional cost and effort. Continued, proactive surveillance and early identification of emerging drugs will facilitate prompt clinical, social, and legislative management.

  19. An analytic parton shower. Algorithms, implementation and validation

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, Sebastian

    2012-06-15

    The realistic simulation of particle collisions is an indispensable tool to interpret the data measured at high-energy colliders, for example the now running Large Hadron Collider at CERN. These collisions at these colliders are usually simulated in the form of exclusive events. This thesis focuses on the perturbative QCD part involved in the simulation of these events, particularly parton showers and the consistent combination of parton showers and matrix elements. We present an existing parton shower algorithm for emissions off final state partons along with some major improvements. Moreover, we present a new parton shower algorithm for emissions off incoming partons. The aim of these particular algorithms, called analytic parton shower algorithms, is to be able to calculate the probabilities for branchings and for whole events after the event has been generated. This allows a reweighting procedure to be applied after the events have been simulated. We show a detailed description of the algorithms, their implementation and the interfaces to the event generator WHIZARD. Moreover we discuss the implementation of a MLM-type matching procedure and an interface to the shower and hadronization routines from PYTHIA. Finally, we compare several predictions by our implementation to experimental measurements at LEP, Tevatron and LHC, as well as to predictions obtained using PYTHIA. (orig.)

  20. An analytic parton shower. Algorithms, implementation and validation

    International Nuclear Information System (INIS)

    Schmidt, Sebastian

    2012-06-01

    The realistic simulation of particle collisions is an indispensable tool to interpret the data measured at high-energy colliders, for example the now running Large Hadron Collider at CERN. These collisions at these colliders are usually simulated in the form of exclusive events. This thesis focuses on the perturbative QCD part involved in the simulation of these events, particularly parton showers and the consistent combination of parton showers and matrix elements. We present an existing parton shower algorithm for emissions off final state partons along with some major improvements. Moreover, we present a new parton shower algorithm for emissions off incoming partons. The aim of these particular algorithms, called analytic parton shower algorithms, is to be able to calculate the probabilities for branchings and for whole events after the event has been generated. This allows a reweighting procedure to be applied after the events have been simulated. We show a detailed description of the algorithms, their implementation and the interfaces to the event generator WHIZARD. Moreover we discuss the implementation of a MLM-type matching procedure and an interface to the shower and hadronization routines from PYTHIA. Finally, we compare several predictions by our implementation to experimental measurements at LEP, Tevatron and LHC, as well as to predictions obtained using PYTHIA. (orig.)

  1. Pyrrolizidine alkaloids in honey: comparison of analytical methods

    NARCIS (Netherlands)

    Kempf, M.; Wittig, M.; Reinhard, A.; Ohe, von der K.; Blacquière, T.; Raezke, K.P.; Michel, R.; Schreier, P.; Beuerle, T.

    2011-01-01

    Pyrrolizidine alkaloids (PAs) are a structurally diverse group of toxicologically relevant secondary plant metabolites. Currently, two analytical methods are used to determine PA content in honey. To achieve reasonably high sensitivity and selectivity, mass spectrometry detection is demanded. One

  2. Analytical chemistry methods for boron carbide absorber material. [Standard

    Energy Technology Data Exchange (ETDEWEB)

    DELVIN WL

    1977-07-01

    This standard provides analytical chemistry methods for the analysis of boron carbide powder and pellets for the following: total C and B, B isotopic composition, soluble C and B, fluoride, chloride, metallic impurities, gas content, water, nitrogen, and oxygen. (DLC)

  3. Robustness study in SSNTD method validation: indoor radon quality

    International Nuclear Information System (INIS)

    Dias, D.C.S.; Silva, N.C.; Bonifácio, R.L.

    2017-01-01

    Quality control practices are indispensable to organizations aiming to reach analytical excellence. Method validation is an essential component to quality systems in laboratories, serving as a powerful tool for standardization and reliability of outcomes. This paper presents a study of robustness conducted over a SSNTD technique validation process, with the goal of developing indoor radon measurements at the highest level of quality. This quality parameter indicates how well a technique is able to provide reliable results in face of unexpected variations along the measurement. In this robustness study, based on the Youden method, 7 analytical conditions pertaining to different phases of the SSNTD technique (with focus on detector etching) were selected. Based on the ideal values for each condition as reference, extreme levels regarded as high and low were prescribed to each condition. A partial factorial design of 8 unique etching procedures was defined, where each presented their own set of high and low condition values. The Youden test provided 8 indoor radon concentration results, which allowed percentage estimations that indicate the potential influence of each analytical condition on the SSNTD technique. As expected, detector etching factors such as etching solution concentration, temperature and immersion time were identified as the most critical parameters to the technique. Detector etching is a critical step in the SSNTD method – one that must be carefully designed during validation and meticulously controlled throughout the entire process. (author)

  4. Robustness study in SSNTD method validation: indoor radon quality

    Energy Technology Data Exchange (ETDEWEB)

    Dias, D.C.S.; Silva, N.C.; Bonifácio, R.L., E-mail: danilacdias@gmail.com [Comissao Nacional de Energia Nuclear (LAPOC/CNEN), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2017-07-01

    Quality control practices are indispensable to organizations aiming to reach analytical excellence. Method validation is an essential component to quality systems in laboratories, serving as a powerful tool for standardization and reliability of outcomes. This paper presents a study of robustness conducted over a SSNTD technique validation process, with the goal of developing indoor radon measurements at the highest level of quality. This quality parameter indicates how well a technique is able to provide reliable results in face of unexpected variations along the measurement. In this robustness study, based on the Youden method, 7 analytical conditions pertaining to different phases of the SSNTD technique (with focus on detector etching) were selected. Based on the ideal values for each condition as reference, extreme levels regarded as high and low were prescribed to each condition. A partial factorial design of 8 unique etching procedures was defined, where each presented their own set of high and low condition values. The Youden test provided 8 indoor radon concentration results, which allowed percentage estimations that indicate the potential influence of each analytical condition on the SSNTD technique. As expected, detector etching factors such as etching solution concentration, temperature and immersion time were identified as the most critical parameters to the technique. Detector etching is a critical step in the SSNTD method – one that must be carefully designed during validation and meticulously controlled throughout the entire process. (author)

  5. NUMERICAL AND ANALYTIC METHODS OF ESTIMATION BRIDGES’ CONSTRUCTIONS

    Directory of Open Access Journals (Sweden)

    Y. Y. Luchko

    2010-03-01

    Full Text Available In this article the numerical and analytical methods of calculation of the stressed-and-strained state of bridge constructions are considered. The task on increasing of reliability and accuracy of the numerical method and its solution by means of calculations in two bases are formulated. The analytical solution of the differential equation of deformation of a ferro-concrete plate under the action of local loads is also obtained.

  6. Validación de métodos analíticos para el control de calidad de naproxeno supositorios Validation of analytical methods for the quality control of Naproxen suppositories

    Directory of Open Access Journals (Sweden)

    Yaslenis Rodríguez Hernández

    2011-09-01

    Full Text Available En el presente trabajo se desarrollaron por primera vez, los métodos de análisis que serán utilizados para el control de calidad de las futuras formulaciones de supositorios de naproxeno, para uso infantil y adulto de producción nacional. Se propuso un método por espectrofotometría ultravioleta directa, el cual resultó específico, lineal, exacto y preciso para su aplicación en el control de calidad del naproxeno en supositorios, teniendo en cuenta la presencia de grupos cromóforos en su estructura. Se modificó el método por volumetría ácido-base semiacuosa directa reportado para control de calidad de la materia prima de naproxeno y se adaptó al control de calidad en los supositorios. A partir del proceso de validación realizado, se demostró la adecuada especificidad frente a los componentes de la formulación, así como su linealidad, exactitud y precisión en el rango de 1 a 3 mg/mL. Se compararon los resultados obtenidos por ambos métodos sin detectar diferencias estadísticamente significativas entre las réplicas analizadas por cada dosis, por lo que cualquiera de ellos pueden aplicarse al control de calidad de los supositorios.The analysis methods that will be used for the quality control of the future Cuban-made Naproxen suppositories for adults and children were developed for the first time in this paper. One method based on direct ultraviolet spectrophotometry was put forward, which proved to be specific, linear, accurate and precise for the quality control of Naproxen suppositories, taking into account the presence of chromophore groups in their structure. Likewise, the direct semi-aqueous acid-base volumetry method aimed at the quality control of the Naproxen raw material was changed and adapted to the quality control of suppositories. On the basis of the validation process, there was demonstrated the adequate specificity of this method with respect to the formulation components, as well as its linearity, accuracy and

  7. Analytical techniques for instrument design - matrix methods

    International Nuclear Information System (INIS)

    Robinson, R.A.

    1997-01-01

    We take the traditional Cooper-Nathans approach, as has been applied for many years for steady-state triple-axis spectrometers, and consider its generalisation to other inelastic scattering spectrometers. This involves a number of simple manipulations of exponentials of quadratic forms. In particular, we discuss a toolbox of matrix manipulations that can be performed on the 6- dimensional Cooper-Nathans matrix: diagonalisation (Moller-Nielsen method), coordinate changes e.g. from (Δk I ,Δk F to ΔE, ΔQ ampersand 2 dummy variables), integration of one or more variables (e.g. over such dummy variables), integration subject to linear constraints (e.g. Bragg's Law for analysers), inversion to give the variance-covariance matrix, and so on. We show how these tools can be combined to solve a number of important problems, within the narrow-band limit and the gaussian approximation. We will argue that a generalised program that can handle multiple different spectrometers could (and should) be written in parallel to the Monte-Carlo packages that are becoming available. We will also discuss the complementarity between detailed Monte-Carlo calculations and the approach presented here. In particular, Monte-Carlo methods traditionally simulate the real experiment as performed in practice, given a model scattering law, while the Cooper-Nathans method asks the inverse question: given that a neutron turns up in a particular spectrometer configuration (e.g. angle and time of flight), what is the probability distribution of possible scattering events at the sample? The Monte-Carlo approach could be applied in the same spirit to this question

  8. Surface analytical methods in nuclear technology

    International Nuclear Information System (INIS)

    Baumgaertner, F.

    1985-06-01

    Application of SEM-EDX, AES, XPS are exemplarily demonstrated for highly radioactive materials with ionizing dose rates of about 1 Sv near the surface. The samples studied are aerosols from the high level waste vitrification process, postprecipitation in a pretreated fuel solution and emulsifying sludge from a solvent extraction process. The results of the chemical composition differentiated down to microscopic level reveal much more information about the history of a sample than those available from the integral macro-methods analysing. Elucidication of chemical composition and body structure in micrometer level may give insight into the origin and generation processes of samples under investigation. (orig.)

  9. Analytical techniques for instrument design - Matrix methods

    International Nuclear Information System (INIS)

    Robinson, R.A.

    1997-01-01

    The authors take the traditional Cooper-Nathans approach, as has been applied for many years for steady-state triple-axis spectrometers, and consider its generalization to other inelastic scattering spectrometers. This involves a number of simple manipulations of exponentials of quadratic forms. In particular, they discuss a toolbox of matrix manipulations that can be performed on the 6-dimensional Cooper-Nathans matrix. They show how these tools can be combined to solve a number of important problems, within the narrow-band limit and the gaussian approximation. They will argue that a generalized program that can handle multiple different spectrometers could (and should) be written in parallel to the Monte-Carlo packages that are becoming available. They also discuss the complementarity between detailed Monte-Carlo calculations and the approach presented here. In particular, Monte-Carlo methods traditionally simulate the real experiment as performed in practice, given a model scattering law, while the Cooper-Nathans method asks the inverse question: given that a neutron turns up in a particular spectrometer configuration (e.g. angle and time of flight), what is the probability distribution of possible scattering events at the sample? The Monte-Carlo approach could be applied in the same spirit to this question

  10. An analytic solution for numerical modeling validation in electromagnetics: the resistive sphere

    Science.gov (United States)

    Swidinsky, Andrei; Liu, Lifei

    2017-11-01

    We derive the electromagnetic response of a resistive sphere to an electric dipole source buried in a conductive whole space. The solution consists of an infinite series of spherical Bessel functions and associated Legendre polynomials, and follows the well-studied problem of a conductive sphere buried in a resistive whole space in the presence of a magnetic dipole. Our result is particularly useful for controlled-source electromagnetic problems using a grounded electric dipole transmitter and can be used to check numerical methods of calculating the response of resistive targets (such as finite difference, finite volume, finite element and integral equation). While we elect to focus on the resistive sphere in our examples, the expressions in this paper are completely general and allow for arbitrary source frequency, sphere radius, transmitter position, receiver position and sphere/host conductivity contrast so that conductive target responses can also be checked. Commonly used mesh validation techniques consist of comparisons against other numerical codes, but such solutions may not always be reliable or readily available. Alternatively, the response of simple 1-D models can be tested against well-known whole space, half-space and layered earth solutions, but such an approach is inadequate for validating models with curved surfaces. We demonstrate that our theoretical results can be used as a complementary validation tool by comparing analytic electric fields to those calculated through a finite-element analysis; the software implementation of this infinite series solution is made available for direct and immediate application.

  11. Manual of selected physico-chemical analytical methods. IV

    International Nuclear Information System (INIS)

    Beran, M.; Klosova, E.; Krtil, J.; Sus, F.; Kuvik, V.; Vrbova, L.; Hamplova, M.; Lengyel, J.; Kelnar, L.; Zakouril, K.

    1990-11-01

    The Central Testing Laboratory of the Nuclear Research Institute at Rez has for a decade been participating in the development of analytical procedures and has been providing analyses of samples of different types and origin. The analytical procedures developed have been published in special journals and a number of them in the Manuals of analytical methods, in three parts. The 4th part of the Manual contains selected physico-chemical methods developed or modified by the Laboratory in the years 1986-1990 within the project ''Development of physico-chemical analytical methods''. In most cases, techniques are involved for non-nuclear applications. Some can find wider applications, especially in analyses of environmental samples. Others have been developed for specific cases of sample analyses or require special instrumentation (mass spectrometer), which partly restricts their applicability by other institutions. (author)

  12. Validation of ultraviolet method to determine serum phosphorus level

    International Nuclear Information System (INIS)

    Garcia Borges, Lisandra; Perez Prieto, Teresa Maria; Valdes Diez, Lilliam

    2009-01-01

    Validation of a spectrophotometry method applicable in clinic labs was proposed to analytical assessment of serum phosphates using a kit UV-phosphorus of domestic production from 'Carlos J. Finlay' Biologics Production Enterprise (Havana, Cuba). Analysis method was based on phosphorus reaction to ammonium molybdenum to acid pH to creating a measurable complex to 340 nm. Specificity and precision were measured considering the method strength, linearity, accuracy and sensitivity. Analytical method was linear up to 4,8 mmol/L, precise (CV 30 .999) during clinical interest concentration interval where there were not interferences by matrix. Detection limit values were of 0.037 mmol/L and of quantification of 0.13 mmol/L both were satisfactory for product use

  13. Methods and applications of analytical perturbation theory

    International Nuclear Information System (INIS)

    Kirchgraber, U.; Stiefel, E.

    1978-01-01

    This monograph on perturbation theory is based on various courses and lectures held by the authors at the ETH, Zurich and at the University of Texas, Austin. Its principal intention is to inform application-minded mathematicians, physicists and engineers about recent developments in this field. The reader is not assumed to have mathematical knowledge beyond what is presented in standard courses on analysis and linear algebra. Chapter I treats the transformations of systems of differential equations and the integration of perturbed systems in a formal way. These tools are applied in Chapter II to celestial mechanics and to the theory of tops and gyroscopic motion. Chapter III is devoted to the discussion of Hamiltonian systems of differential equations and exposes the algebraic aspects of perturbation theory showing also the necessary modifications of the theory in case of singularities. The last chapter gives the mathematical justification for the methods developed in the previous chapters and investigates important questions such as error estimations for the solutions and asymptotic stability. Each chapter ends with useful comments and an extensive reference to the original literature. (HJ) [de

  14. Chapter 12. Sampling and analytical methods

    International Nuclear Information System (INIS)

    Busenberg, E.; Plummer, L.N.; Cook, P.G.; Solomon, D.K.; Han, L.F.; Groening, M.; Oster, H.

    2006-01-01

    When water samples are taken for the analysis of CFCs, regardless of the sampling method used, contamination of samples by contact with atmospheric air (with its 'high' CFC concentrations) is a major concern. This is because groundwaters usually have lower CFC concentrations than those waters which have been exposed to the modern air. Some groundwaters might not contain CFCs and, therefore, are most sensitive to trace contamination by atmospheric air. Thus, extreme precautions are needed to obtain uncontaminated samples when groundwaters, particularly those with older ages, are sampled. It is recommended at the start of any CFC investigation that samples from a CFC-free source be collected and analysed, as a check upon the sampling equipment and methodology. The CFC-free source might be a deep monitoring well or, alternatively, CFC-free water could be carefully prepared in the laboratory. It is especially important that all tubing, pumps and connection that will be used in the sampling campaign be checked in this manner

  15. Analytic Methods Used in Quality Control in a Compounding Pharmacy.

    Science.gov (United States)

    Allen, Loyd V

    2017-01-01

    Analytical testing will no doubt become a more important part of pharmaceutical compounding as the public and regulatory agencies demand increasing documentation of the quality of compounded preparations. Compounding pharmacists must decide what types of testing and what amount of testing to include in their quality-control programs, and whether testing should be done in-house or outsourced. Like pharmaceutical compounding, analytical testing should be performed only by those who are appropriately trained and qualified. This article discusses the analytical methods that are used in quality control in a compounding pharmacy. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

  16. Analytical method for optimization of maintenance policy based on available system failure data

    International Nuclear Information System (INIS)

    Coria, V.H.; Maximov, S.; Rivas-Dávalos, F.; Melchor, C.L.; Guardado, J.L.

    2015-01-01

    An analytical optimization method for preventive maintenance (PM) policy with minimal repair at failure, periodic maintenance, and replacement is proposed for systems with historical failure time data influenced by a current PM policy. The method includes a new imperfect PM model based on Weibull distribution and incorporates the current maintenance interval T 0 and the optimal maintenance interval T to be found. The Weibull parameters are analytically estimated using maximum likelihood estimation. Based on this model, the optimal number of PM and the optimal maintenance interval for minimizing the expected cost over an infinite time horizon are also analytically determined. A number of examples are presented involving different failure time data and current maintenance intervals to analyze how the proposed analytical optimization method for periodic PM policy performances in response to changes in the distribution of the failure data and the current maintenance interval. - Highlights: • An analytical optimization method for preventive maintenance (PM) policy is proposed. • A new imperfect PM model is developed. • The Weibull parameters are analytically estimated using maximum likelihood. • The optimal maintenance interval and number of PM are also analytically determined. • The model is validated by several numerical examples

  17. The Method of Manufactured Universes for validating uncertainty quantification methods

    KAUST Repository

    Stripling, H.F.; Adams, M.L.; McClarren, R.G.; Mallick, B.K.

    2011-01-01

    The Method of Manufactured Universes is presented as a validation framework for uncertainty quantification (UQ) methodologies and as a tool for exploring the effects of statistical and modeling assumptions embedded in these methods. The framework

  18. ASTM Validates Air Pollution Test Methods

    Science.gov (United States)

    Chemical and Engineering News, 1973

    1973-01-01

    The American Society for Testing and Materials (ASTM) has validated six basic methods for measuring pollutants in ambient air as the first part of its Project Threshold. Aim of the project is to establish nationwide consistency in measuring pollutants; determining precision, accuracy and reproducibility of 35 standard measuring methods. (BL)

  19. Validated modified Lycopodium spore method development for ...

    African Journals Online (AJOL)

    Validated modified lycopodium spore method has been developed for simple and rapid quantification of herbal powdered drugs. Lycopodium spore method was performed on ingredients of Shatavaryadi churna, an ayurvedic formulation used as immunomodulator, galactagogue, aphrodisiac and rejuvenator. Estimation of ...

  20. New Analytical Method for the Determination of Metronidazole in ...

    African Journals Online (AJOL)

    New Analytical Method for the Determination of Metronidazole in Human Plasma: Application to Bioequivalence Study. ... Methods: Metronidazole was extracted from human plasma through one step of ... http://dx.doi.org/10.4314/tjpr.v11i5.14.

  1. Pyrrolizidine alkaloids in honey: comparison of analytical methods.

    Science.gov (United States)

    Kempf, M; Wittig, M; Reinhard, A; von der Ohe, K; Blacquière, T; Raezke, K-P; Michel, R; Schreier, P; Beuerle, T

    2011-03-01

    Pyrrolizidine alkaloids (PAs) are a structurally diverse group of toxicologically relevant secondary plant metabolites. Currently, two analytical methods are used to determine PA content in honey. To achieve reasonably high sensitivity and selectivity, mass spectrometry detection is demanded. One method is an HPLC-ESI-MS-MS approach, the other a sum parameter method utilising HRGC-EI-MS operated in the selected ion monitoring mode (SIM). To date, no fully validated or standardised method exists to measure the PA content in honey. To establish an LC-MS method, several hundred standard pollen analysis results of raw honey were analysed. Possible PA plants were identified and typical commercially available marker PA-N-oxides (PANOs). Three distinct honey sets were analysed with both methods. Set A consisted of pure Echium honey (61-80% Echium pollen). Echium is an attractive bee plant. It is quite common in all temperate zones worldwide and is one of the major reasons for PA contamination in honey. Although only echimidine/echimidine-N-oxide were available as reference for the LC-MS target approach, the results for both analytical techniques matched very well (n = 8; PA content ranging from 311 to 520 µg kg(-1)). The second batch (B) consisted of a set of randomly picked raw honeys, mostly originating from Eupatorium spp. (0-15%), another common PA plant, usually characterised by the occurrence of lycopsamine-type PA. Again, the results showed good consistency in terms of PA-positive samples and quantification results (n = 8; ranging from 0 to 625 µg kg(-1) retronecine equivalents). The last set (C) was obtained by consciously placing beehives in areas with a high abundance of Jacobaea vulgaris (ragwort) from the Veluwe region (the Netherlands). J. vulgaris increasingly invades countrysides in Central Europe, especially areas with reduced farming or sites with natural restorations. Honey from two seasons (2007 and 2008) was sampled. While only trace amounts of

  2. An Investigation to Manufacturing Analytical Services Composition using the Analytical Target Cascading Method.

    Science.gov (United States)

    Tien, Kai-Wen; Kulvatunyou, Boonserm; Jung, Kiwook; Prabhu, Vittaldas

    2017-01-01

    As cloud computing is increasingly adopted, the trend is to offer software functions as modular services and compose them into larger, more meaningful ones. The trend is attractive to analytical problems in the manufacturing system design and performance improvement domain because 1) finding a global optimization for the system is a complex problem; and 2) sub-problems are typically compartmentalized by the organizational structure. However, solving sub-problems by independent services can result in a sub-optimal solution at the system level. This paper investigates the technique called Analytical Target Cascading (ATC) to coordinate the optimization of loosely-coupled sub-problems, each may be modularly formulated by differing departments and be solved by modular analytical services. The result demonstrates that ATC is a promising method in that it offers system-level optimal solutions that can scale up by exploiting distributed and modular executions while allowing easier management of the problem formulation.

  3. Analytical validation of a novel multiplex test for detection of advanced adenoma and colorectal cancer in symptomatic patients.

    Science.gov (United States)

    Dillon, Roslyn; Croner, Lisa J; Bucci, John; Kairs, Stefanie N; You, Jia; Beasley, Sharon; Blimline, Mark; Carino, Rochele B; Chan, Vicky C; Cuevas, Danissa; Diggs, Jeff; Jennings, Megan; Levy, Jacob; Mina, Ginger; Yee, Alvin; Wilcox, Bruce

    2018-05-30

    Early detection of colorectal cancer (CRC) is key to reducing associated mortality. Despite the importance of early detection, approximately 40% of individuals in the United States between the ages of 50-75 have never been screened for CRC. The low compliance with colonoscopy and fecal-based screening may be addressed with a non-invasive alternative such as a blood-based test. We describe here the analytical validation of a multiplexed blood-based assay that measures the plasma concentrations of 15 proteins to assess advanced adenoma (AA) and CRC risk in symptomatic patients. The test was developed on an electrochemiluminescent immunoassay platform employing four multi-marker panels, to be implemented in the clinic as a laboratory developed test (LDT). Under the Clinical Laboratory Improvement Amendments (CLIA) and College of American Pathologists (CAP) regulations, a United States-based clinical laboratory utilizing an LDT must establish performance characteristics relating to analytical validity prior to releasing patient test results. This report describes a series of studies demonstrating the precision, accuracy, analytical sensitivity, and analytical specificity for each of the 15 assays, as required by CLIA/CAP. In addition, the report describes studies characterizing each of the assays' dynamic range, parallelism, tolerance to common interfering substances, spike recovery, and stability to sample freeze-thaw cycles. Upon completion of the analytical characterization, a clinical accuracy study was performed to evaluate concordance of AA and CRC classifier model calls using the analytical method intended for use in the clinic. Of 434 symptomatic patient samples tested, the percent agreement with original CRC and AA calls was 87% and 92% respectively. All studies followed CLSI guidelines and met the regulatory requirements for implementation of a new LDT. The results provide the analytical evidence to support the implementation of the novel multi-marker test as

  4. Rigid inclusions-Comparison between analytical and numerical methods

    International Nuclear Information System (INIS)

    Gomez Perez, R.; Melentijevic, S.

    2014-01-01

    This paper compares different analytical methods for analysis of rigid inclusions with finite element modeling. First of all, the load transfer in the distribution layer is analyzed for its different thicknesses and different inclusion grids to define the range between results obtained by analytical and numerical methods. The interaction between the soft soil and the inclusion in the estimation of settlements is studied as well. Considering different stiffness of the soft soil, settlements obtained analytical and numerically are compared. The influence of the soft soil modulus of elasticity on the neutral point depth was also performed by finite elements. This depth has a great importance for the definition of the total length of rigid inclusion. (Author)

  5. SPANDOM - source projection analytic nodal discrete ordinates method

    International Nuclear Information System (INIS)

    Kim, Tae Hyeong; Cho, Nam Zin

    1994-01-01

    We describe a new discrete ordinates nodal method for the two-dimensional transport equation. We solve the discrete ordinates equation analytically after the source term is projected and represented in polynomials. The method is applied to two fast reactor benchmark problems and compared with the TWOHEX code. The results indicate that the present method accurately predicts not only multiplication factor but also flux distribution

  6. Development of Analytical Method for Detection of Some ...

    African Journals Online (AJOL)

    All rights reserved. ... 3Centre for Water Research and Analysis (ALIR), Faculty of Science and Technology, Universiti Kebangsaan (UKM), ... Purpose: To develop and validate a simple method using solid – phase extraction along with liquid.

  7. A Table Lookup Method for Exact Analytical Solutions of Nonlinear Fractional Partial Differential Equations

    Directory of Open Access Journals (Sweden)

    Ji Juan-Juan

    2017-01-01

    Full Text Available A table lookup method for solving nonlinear fractional partial differential equations (fPDEs is proposed in this paper. Looking up the corresponding tables, we can quickly obtain the exact analytical solutions of fPDEs by using this method. To illustrate the validity of the method, we apply it to construct the exact analytical solutions of four nonlinear fPDEs, namely, the time fractional simplified MCH equation, the space-time fractional combined KdV-mKdV equation, the (2+1-dimensional time fractional Zoomeron equation, and the space-time fractional ZKBBM equation. As a result, many new types of exact analytical solutions are obtained including triangular periodic solution, hyperbolic function solution, singular solution, multiple solitary wave solution, and Jacobi elliptic function solution.

  8. Simplified Analytical Methods to Analyze Lock Gates Submitted to Ship Collisions and Earthquakes

    Directory of Open Access Journals (Sweden)

    Buldgen Loic

    2015-09-01

    Full Text Available This paper presents two simplified analytical methods to analyze lock gates submitted to two different accidental loads. The case of an impact involving a vessel is first investigated. In this situation, the resistance of the struck gate is evaluated by assuming a local and a global deforming mode. The super-element method is used in the first case, while an equivalent beam model is simultaneously introduced to capture the overall bending motion of the structure. The second accidental load considered in this paper is the seismic action, for which an analytical method is presented to evaluate the total hydrodynamic pressure applied on a lock gate during an earthquake, due account being taken of the fluid-structure interaction. For each of these two actions, numerical validations are presented and the analytical results are compared to finite-element solutions.

  9. Validación del método analítico para el control de la calidad y estudio de estabilidad de propiltiouracilo 50 mg Analytical method validation for quality control and the study of the 50 mg Propylthiouracil stability

    Directory of Open Access Journals (Sweden)

    María Olga Valdés Bendoyro

    2010-03-01

    Full Text Available Se desarrolló y validó un método analítico por cromatografía líquida de alta resolución, para el control de la calidad y los estudios de estabilidad del propiltiouracilo 50 mg, tabletas. El método se basó en la separación del principio activo a través una columna cromatográfica Lichrospher 100 RP-18 RP-18 (5 µm (250 x 4 mm, con detección ultravioleta a 272 nm, para lo cual se empleó una fase móvil compuesta por una mezcla desgasificada de solución amortiguadora fosfato de potasio monobásico 0,025 M a pH= 4,6, y acetonitrilo en una proporción de 80:20, con una velocidad de flujo de 0,5 mL/min. El método analítico resultó lineal, preciso, específico y exacto en el intervalo de concentraciones estudiadas.A high-performance liquid chromatography analytical method was developed and validated for the quality control and stability studies of 50 mg Propylthiouracil tablets. Method is based in active principle separation through a 100 RP-18 RP-18 (5 µm (250 x 4 mm Lichrospher chromatography with UV detection to 272 nm, using a mobile phase composed by a ungaseous mixture of a 0.025 M buffer solution-monobasic potassium phosphate to pH= 4,6 ad acetonitrile in a 80:20 ratio with a flux speed of 0,5 mL/min. Analytical method was linear, precise, specific and exact in the study concentrations interval.

  10. Valid analytical performance specifications for combined analytical bias and imprecision for the use of common reference intervals

    DEFF Research Database (Denmark)

    Hyltoft Petersen, Per; Lund, Flemming; Fraser, Callum G

    2018-01-01

    for the combination of analytical bias and imprecision and Method 2 is based on the Microsoft Excel formula NORMINV including the fractional probability of reference individuals outside each limit and the Gaussian variables of mean and standard deviation. The combinations of normalized bias and imprecision...... are illustrated for both methods. The formulae are identical for Gaussian and log-Gaussian distributions. Results Method 2 gives the correct results with a constant percentage of 4.4% for all combinations of bias and imprecision. Conclusion The Microsoft Excel formula NORMINV is useful for the estimation...

  11. Approximate analytical methods for solving ordinary differential equations

    CERN Document Server

    Radhika, TSL; Rani, T Raja

    2015-01-01

    Approximate Analytical Methods for Solving Ordinary Differential Equations (ODEs) is the first book to present all of the available approximate methods for solving ODEs, eliminating the need to wade through multiple books and articles. It covers both well-established techniques and recently developed procedures, including the classical series solution method, diverse perturbation methods, pioneering asymptotic methods, and the latest homotopy methods.The book is suitable not only for mathematicians and engineers but also for biologists, physicists, and economists. It gives a complete descripti

  12. Analytical Evaluation of Beam Deformation Problem Using Approximate Methods

    DEFF Research Database (Denmark)

    Barari, Amin; Kimiaeifar, A.; Domairry, G.

    2010-01-01

    The beam deformation equation has very wide applications in structural engineering. As a differential equation, it has its own problem concerning existence, uniqueness and methods of solutions. Often, original forms of governing differential equations used in engineering problems are simplified......, and this process produces noise in the obtained answers. This paper deals with the solution of second order of differential equation governing beam deformation using four analytical approximate methods, namely the Perturbation, Homotopy Perturbation Method (HPM), Homotopy Analysis Method (HAM) and Variational...... Iteration Method (VIM). The comparisons of the results reveal that these methods are very effective, convenient and quite accurate for systems of non-linear differential equation....

  13. Analytic continuation of quantum Monte Carlo data. Stochastic sampling method

    Energy Technology Data Exchange (ETDEWEB)

    Ghanem, Khaldoon; Koch, Erik [Institute for Advanced Simulation, Forschungszentrum Juelich, 52425 Juelich (Germany)

    2016-07-01

    We apply Bayesian inference to the analytic continuation of quantum Monte Carlo (QMC) data from the imaginary axis to the real axis. Demanding a proper functional Bayesian formulation of any analytic continuation method leads naturally to the stochastic sampling method (StochS) as the Bayesian method with the simplest prior, while it excludes the maximum entropy method and Tikhonov regularization. We present a new efficient algorithm for performing StochS that reduces computational times by orders of magnitude in comparison to earlier StochS methods. We apply the new algorithm to a wide variety of typical test cases: spectral functions and susceptibilities from DMFT and lattice QMC calculations. Results show that StochS performs well and is able to resolve sharp features in the spectrum.

  14. Dependability validation by means of fault injection: method, implementation, application

    International Nuclear Information System (INIS)

    Arlat, Jean

    1990-01-01

    This dissertation presents theoretical and practical results concerning the use of fault injection as a means for testing fault tolerance in the framework of the experimental dependability validation of computer systems. The dissertation first presents the state-of-the-art of published work on fault injection, encompassing both hardware (fault simulation, physical fault Injection) and software (mutation testing) issues. Next, the major attributes of fault injection (faults and their activation, experimental readouts and measures, are characterized taking into account: i) the abstraction levels used to represent the system during the various phases of its development (analytical, empirical and physical models), and Il) the validation objectives (verification and evaluation). An evaluation method is subsequently proposed that combines the analytical modeling approaches (Monte Carlo Simulations, closed-form expressions. Markov chains) used for the representation of the fault occurrence process and the experimental fault Injection approaches (fault Simulation and physical injection); characterizing the error processing and fault treatment provided by the fault tolerance mechanisms. An experimental tool - MESSALINE - is then defined and presented. This tool enables physical faults to be Injected In an hardware and software prototype of the system to be validated. Finally, the application of MESSALINE for testing two fault-tolerant systems possessing very dissimilar features and the utilization of the experimental results obtained - both as design feedbacks and for dependability measures evaluation - are used to illustrate the relevance of the method. (author) [fr

  15. Moving beyond Traditional Methods of Survey Validation

    Science.gov (United States)

    Maul, Andrew

    2017-01-01

    In his focus article, "Rethinking Traditional Methods of Survey Validation," published in this issue of "Measurement: Interdisciplinary Research and Perspectives," Andrew Maul wrote that it is commonly believed that self-report, survey-based instruments can be used to measure a wide range of psychological attributes, such as…

  16. Literature Review on Processing and Analytical Methods for ...

    Science.gov (United States)

    Report The purpose of this report was to survey the open literature to determine the current state of the science regarding the processing and analytical methods currently available for recovery of F. tularensis from water and soil matrices, and to determine what gaps remain in the collective knowledge concerning F. tularensis identification from environmental samples.

  17. 40 CFR 425.03 - Sulfide analytical methods and applicability.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 29 2010-07-01 2010-07-01 false Sulfide analytical methods and applicability. 425.03 Section 425.03 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS LEATHER TANNING AND FINISHING POINT SOURCE CATEGORY General Provisions...

  18. THE QuEChERS ANALYTICAL METHOD COMBINED WITH LOW ...

    African Journals Online (AJOL)

    The method has also been applied to different cereal samples and satisfactory average recoveries ... Analysis of multiclass pesticide residues in foods is a challenging task because of the ... compounds set by regulatory bodies. ..... analytes were used to evaluate the influences of the selected factors on performance of the.

  19. Frontier in nanoscale flows fractional calculus and analytical methods

    CERN Document Server

    Lewis, Roland; Liu, Hong-yan

    2014-01-01

    This ebook covers the basic properties of nanoscale flows, and various analytical and numerical methods for nanoscale flows and environmental flows. This ebook is a good reference not only for audience of the journal, but also for various communities in mathematics, nanotechnology and environmental science.

  20. Advances in the Analytical Methods for Determining the Antioxidant ...

    African Journals Online (AJOL)

    Advances in the Analytical Methods for Determining the Antioxidant Properties of Honey: A Review. M Moniruzzaman, MI Khalil, SA Sulaiman, SH Gan. Abstract. Free radicals and reactive oxygen species (ROS) have been implicated in contributing to the processes of aging and disease. In an effort to combat free radical ...

  1. An Analytical Method for the Abel Inversion of Asymmetrical Gaussian Profiles

    International Nuclear Information System (INIS)

    Xu Guosheng; Wan Baonian

    2007-01-01

    An analytical algorithm for fast calculation of the Abel inversion for density profile measurement in tokamak is developed. Based upon the assumptions that the particle source is negligibly small in the plasma core region, density profiles can be approximated by an asymmetrical Gaussian distribution controlled only by one parameter V 0 /D and V 0 /D is constant along the radial direction, the analytical algorithm is presented and examined against a testing profile. The validity is confirmed by benchmark with the standard Abel inversion method and the theoretical profile. The scope of application as well as the error analysis is also discussed in detail

  2. A GPU code for analytic continuation through a sampling method

    Directory of Open Access Journals (Sweden)

    Johan Nordström

    2016-01-01

    Full Text Available We here present a code for performing analytic continuation of fermionic Green’s functions and self-energies as well as bosonic susceptibilities on a graphics processing unit (GPU. The code is based on the sampling method introduced by Mishchenko et al. (2000, and is written for the widely used CUDA platform from NVidia. Detailed scaling tests are presented, for two different GPUs, in order to highlight the advantages of this code with respect to standard CPU computations. Finally, as an example of possible applications, we provide the analytic continuation of model Gaussian functions, as well as more realistic test cases from many-body physics.

  3. Prediction of polymer flooding performance using an analytical method

    International Nuclear Information System (INIS)

    Tan Czek Hoong; Mariyamni Awang; Foo Kok Wai

    2001-01-01

    The study investigated the applicability of an analytical method developed by El-Khatib in polymer flooding. Results from a simulator UTCHEM and experiments were compared with the El-Khatib prediction method. In general, by assuming a constant viscosity polymer injection, the method gave much higher recovery values than the simulation runs and the experiments. A modification of the method gave better correlation, albeit only oil production. Investigation is continuing on modifying the method so that a better overall fit can be obtained for polymer flooding. (Author)

  4. Use of scientometrics to assess nuclear and other analytical methods

    International Nuclear Information System (INIS)

    Lyon, W.S.

    1986-01-01

    Scientometrics involves the use of quantitative methods to investigate science viewed as an information process. Scientometric studies can be useful in ascertaining which methods have been most employed for various analytical determinations as well as for predicting which methods will continue to be used in the immediate future and which appear to be losing favor with the analytical community. Published papers in the technical literature are the primary source materials for scientometric studies; statistical methods and computer techniques are the tools. Recent studies have included growth and trends in prompt nuclear analysis impact of research published in a technical journal, and institutional and national representation, speakers and topics at several IAEA conferences, at modern trends in activation analysis conferences, and at other non-nuclear oriented conferences. Attempts have also been made to predict future growth of various topics and techniques. 13 refs., 4 figs., 17 tabs

  5. An analytic data analysis method for oscillatory slug tests.

    Science.gov (United States)

    Chen, Chia-Shyun

    2006-01-01

    An analytical data analysis method is developed for slug tests in partially penetrating wells in confined or unconfined aquifers of high hydraulic conductivity. As adapted from the van der Kamp method, the determination of the hydraulic conductivity is based on the occurrence times and the displacements of the extreme points measured from the oscillatory data and their theoretical counterparts available in the literature. This method is applied to two sets of slug test response data presented by Butler et al.: one set shows slow damping with seven discernable extremities, and the other shows rapid damping with three extreme points. The estimates of the hydraulic conductivity obtained by the analytic method are in good agreement with those determined by an available curve-matching technique.

  6. Use of scientometrics to assess nuclear and other analytical methods

    Energy Technology Data Exchange (ETDEWEB)

    Lyon, W.S.

    1986-01-01

    Scientometrics involves the use of quantitative methods to investigate science viewed as an information process. Scientometric studies can be useful in ascertaining which methods have been most employed for various analytical determinations as well as for predicting which methods will continue to be used in the immediate future and which appear to be losing favor with the analytical community. Published papers in the technical literature are the primary source materials for scientometric studies; statistical methods and computer techniques are the tools. Recent studies have included growth and trends in prompt nuclear analysis impact of research published in a technical journal, and institutional and national representation, speakers and topics at several IAEA conferences, at modern trends in activation analysis conferences, and at other non-nuclear oriented conferences. Attempts have also been made to predict future growth of various topics and techniques. 13 refs., 4 figs., 17 tabs.

  7. An analytical optimization method for electric propulsion orbit transfer vehicles

    International Nuclear Information System (INIS)

    Oleson, S.R.

    1993-01-01

    Due to electric propulsion's inherent propellant mass savings over chemical propulsion, electric propulsion orbit transfer vehicles (EPOTVs) are a highly efficient mode of orbit transfer. When selecting an electric propulsion device (ion, MPD, or arcjet) and propellant for a particular mission, it is preferable to use quick, analytical system optimization methods instead of time intensive numerical integration methods. It is also of interest to determine each thruster's optimal operating characteristics for a specific mission. Analytical expressions are derived which determine the optimal specific impulse (Isp) for each type of electric thruster to maximize payload fraction for a desired thrusting time. These expressions take into account the variation of thruster efficiency with specific impulse. Verification of the method is made with representative electric propulsion values on a LEO-to-GEO mission. Application of the method to specific missions is discussed

  8. Analytical Validation of Accelerator Mass Spectrometry for Pharmaceutical Development: the Measurement of Carbon-14 Isotope Ratio

    International Nuclear Information System (INIS)

    Keck, B.D.; Ognibene, T.; Vogel, J.S.

    2010-01-01

    Accelerator mass spectrometry (AMS) is an isotope based measurement technology that utilizes carbon-14 labeled compounds in the pharmaceutical development process to measure compounds at very low concentrations, empowers microdosing as an investigational tool, and extends the utility of 14 C labeled compounds to dramatically lower levels. It is a form of isotope ratio mass spectrometry that can provide either measurements of total compound equivalents or, when coupled to separation technology such as chromatography, quantitation of specific compounds. The properties of AMS as a measurement technique are investigated here, and the parameters of method validation are shown. AMS, independent of any separation technique to which it may be coupled, is shown to be accurate, linear, precise, and robust. As the sensitivity and universality of AMS is constantly being explored and expanded, this work underpins many areas of pharmaceutical development including drug metabolism as well as absorption, distribution and excretion of pharmaceutical compounds as a fundamental step in drug development. The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of 14 C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the 14 C label), stable across samples storage conditions for at least one year, linear over 4 orders of magnitude with an analytical range from one tenth Modern to at least 2000 Modern (instrument specific). Further, accuracy was excellent between 1 and 3 percent while precision expressed as coefficient of variation is between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of carbon-14 (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with 14 C corresponds to 30 fg equivalents. AMS

  9. Analytical Validation of Accelerator Mass Spectrometry for Pharmaceutical Development: the Measurement of Carbon-14 Isotope Ratio.

    Energy Technology Data Exchange (ETDEWEB)

    Keck, B D; Ognibene, T; Vogel, J S

    2010-02-05

    Accelerator mass spectrometry (AMS) is an isotope based measurement technology that utilizes carbon-14 labeled compounds in the pharmaceutical development process to measure compounds at very low concentrations, empowers microdosing as an investigational tool, and extends the utility of {sup 14}C labeled compounds to dramatically lower levels. It is a form of isotope ratio mass spectrometry that can provide either measurements of total compound equivalents or, when coupled to separation technology such as chromatography, quantitation of specific compounds. The properties of AMS as a measurement technique are investigated here, and the parameters of method validation are shown. AMS, independent of any separation technique to which it may be coupled, is shown to be accurate, linear, precise, and robust. As the sensitivity and universality of AMS is constantly being explored and expanded, this work underpins many areas of pharmaceutical development including drug metabolism as well as absorption, distribution and excretion of pharmaceutical compounds as a fundamental step in drug development. The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of {sup 14}C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the {sup 14}C label), stable across samples storage conditions for at least one year, linear over 4 orders of magnitude with an analytical range from one tenth Modern to at least 2000 Modern (instrument specific). Further, accuracy was excellent between 1 and 3 percent while precision expressed as coefficient of variation is between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of carbon-14 (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with {sup 14}C corresponds to 30 fg

  10. Long-Term Prediction of Satellite Orbit Using Analytical Method

    Directory of Open Access Journals (Sweden)

    Jae-Cheol Yoon

    1997-12-01

    Full Text Available A long-term prediction algorithm of geostationary orbit was developed using the analytical method. The perturbation force models include geopotential upto fifth order and degree and luni-solar gravitation, and solar radiation pressure. All of the perturbation effects were analyzed by secular variations, short-period variations, and long-period variations for equinoctial elements such as the semi-major axis, eccentricity vector, inclination vector, and mean longitude of the satellite. Result of the analytical orbit propagator was compared with that of the cowell orbit propagator for the KOREASAT. The comparison indicated that the analytical solution could predict the semi-major axis with an accuarcy of better than ~35meters over a period of 3 month.

  11. Methods of analytical check for highly pure tungsten

    International Nuclear Information System (INIS)

    Miklin, D.G.; Karpov, Yu.A.; Orlova, V.A.

    1993-01-01

    The review is devoted to the methods of high-purity tungsten analysis. Current trends in the development of this branch of analytical chemistry are considered. Application of both instrument mass-spectrometry analysis and optico-spectral, activation methods and mass-spectrometry ones with inductively-bound plasma in combination with preliminary isolation of the basis and impurity concentration is expected to be the most actual

  12. Validation of the Rotation Ratios Method

    International Nuclear Information System (INIS)

    Foss, O.A.; Klaksvik, J.; Benum, P.; Anda, S.

    2007-01-01

    Background: The rotation ratios method describes rotations between pairs of sequential pelvic radiographs. The method seems promising but has not been validated. Purpose: To validate the accuracy of the rotation ratios method. Material and Methods: Known pelvic rotations between 165 radiographs obtained from five skeletal pelvises in an experimental material were compared with the corresponding calculated rotations to describe the accuracy of the method. The results from a clinical material of 262 pelvic radiographs from 46 patients defined the ranges of rotational differences compared. Repeated analyses, both on the experimental and the clinical material, were performed using the selected reference points to describe the robustness and the repeatability of the method. Results: The reference points were easy to identify and barely influenced by pelvic rotations. The mean differences between calculated and real pelvic rotations were 0.0 deg (SD 0.6) for vertical rotations and 0.1 deg (SD 0.7) for transversal rotations in the experimental material. The intra- and interobserver repeatability of the method was good. Conclusion: The accuracy of the method was reasonably high, and the method may prove to be clinically useful

  13. Hanford environmental analytical methods (methods as of March 1990)

    International Nuclear Information System (INIS)

    Goheen, S.D.; McCulloch, M.; Daniel, J.L.

    1993-05-01

    Information is provided on the techniques employed towards the chemical analysis of volatile, semi-volatile matter, pesticides and PCB's at the Hanford Reservation. Sample preparation methods are included

  14. Development and validation of an analytical method for the separation and determination of major bioactive curcuminoids in Curcuma longa rhizomes and herbal products using non-aqueous capillary electrophoresis.

    Science.gov (United States)

    Anubala, S; Sekar, R; Nagaiah, K

    2014-06-01

    A simple, fast and efficient non-aqueous capillary electrophoresis method (NACE) was developed for the simultaneous determination of three major bioactive curcuminoids (CMNs) in Curcuma longa rhizomes and its herbal products. Good separation, resolution and reproducibility were achieved with the background electrolyte (BGE) consisting a mixture of 15.0 mM sodium tetraborate and 7.4 mM sodium hydroxide (NaOH) in 2:10:15 (v/v/v) of water, 1-propanol, and methanol. The influences of background electrolyte, sodium hydroxide, water, sodium dodecyl sulfate and hydroxylpropyl-β-cyclodextrin on separations were investigated. The separation was carried out in a fused-silica capillary tube with reverse polarity. Hydrodynamic injection of 25mbar for 12s was used for injecting samples and a voltage of 28 kV was applied for separation. The ultrasonication method was used for the extraction of CMNs from the turmeric herbal products and the extract was filtered and directly injected without any further treatments. The limits of detection and quantification were less than 5.0 and 14.6 µg/ml respectively for all CMNs. The percentage recoveries for CMNs were >97.2% (%RSD, <2.62). The results obtained by the method were compared with existing spectrophotometric and HPLC methods. The related compounds in the extract did not interfere in the determination of CMNs. The proposed NACE method is better than existing chromatographic and electrophoretic methods in terms of simple electrophoretic medium, fast analysis and good resolution. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Nuclear and nuclear related analytical methods applied in environmental research

    International Nuclear Information System (INIS)

    Popescu, Ion V.; Gheboianu, Anca; Bancuta, Iulian; Cimpoca, G. V; Stihi, Claudia; Radulescu, Cristiana; Oros Calin; Frontasyeva, Marina; Petre, Marian; Dulama, Ioana; Vlaicu, G.

    2010-01-01

    Nuclear Analytical Methods can be used for research activities on environmental studies like water quality assessment, pesticide residues, global climatic change (transboundary), pollution and remediation. Heavy metal pollution is a problem associated with areas of intensive industrial activity. In this work the moss bio monitoring technique was employed to study the atmospheric deposition in Dambovita County Romania. Also, there were used complementary nuclear and atomic analytical methods: Neutron Activation Analysis (NAA), Atomic Absorption Spectrometry (AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). These high sensitivity analysis methods were used to determine the chemical composition of some samples of mosses placed in different areas with different pollution industrial sources. The concentrations of Cr, Fe, Mn, Ni and Zn were determined. The concentration of Fe from the same samples was determined using all these methods and we obtained a very good agreement, in statistical limits, which demonstrate the capability of these analytical methods to be applied on a large spectrum of environmental samples with the same results. (authors)

  16. Analytical methods for determination of mycotoxins: a review.

    Science.gov (United States)

    Turner, Nicholas W; Subrahmanyam, Sreenath; Piletsky, Sergey A

    2009-01-26

    Mycotoxins are small (MW approximately 700), toxic chemical products formed as secondary metabolites by a few fungal species that readily colonise crops and contaminate them with toxins in the field or after harvest. Ochratoxins and Aflatoxins are mycotoxins of major significance and hence there has been significant research on broad range of analytical and detection techniques that could be useful and practical. Due to the variety of structures of these toxins, it is impossible to use one standard technique for analysis and/or detection. Practical requirements for high-sensitivity analysis and the need for a specialist laboratory setting create challenges for routine analysis. Several existing analytical techniques, which offer flexible and broad-based methods of analysis and in some cases detection, have been discussed in this manuscript. There are a number of methods used, of which many are lab-based, but to our knowledge there seems to be no single technique that stands out above the rest, although analytical liquid chromatography, commonly linked with mass spectroscopy is likely to be popular. This review manuscript discusses (a) sample pre-treatment methods such as liquid-liquid extraction (LLE), supercritical fluid extraction (SFE), solid phase extraction (SPE), (b) separation methods such as (TLC), high performance liquid chromatography (HPLC), gas chromatography (GC), and capillary electrophoresis (CE) and (c) others such as ELISA. Further currents trends, advantages and disadvantages and future prospects of these methods have been discussed.

  17. FORECASTING PILE SETTLEMENT ON CLAYSTONE USING NUMERICAL AND ANALYTICAL METHODS

    Directory of Open Access Journals (Sweden)

    Ponomarev Andrey Budimirovich

    2016-06-01

    Full Text Available In the article the problem of designing pile foundations on claystones is reviewed. The purpose of this paper is comparative analysis of the analytical and numerical methods for forecasting the settlement of piles on claystones. The following tasks were solved during the study: 1 The existing researches of pile settlement are analyzed; 2 The characteristics of experimental studies and the parameters for numerical modeling are presented, methods of field research of single piles’ operation are described; 3 Calculation of single pile settlement is performed using numerical methods in the software package Plaxis 2D and analytical method according to the requirements SP 24.13330.2011; 4 Experimental data is compared with the results of analytical and numerical calculations; 5 Basing on these results recommendations for forecasting pile settlement on claystone are presented. Much attention is paid to the calculation of pile settlement considering the impacted areas in ground space beside pile and the comparison with the results of field experiments. Basing on the obtained results, for the prediction of settlement of single pile on claystone the authors recommend using the analytical method considered in SP 24.13330.2011 with account for the impacted areas in ground space beside driven pile. In the case of forecasting the settlement of single pile on claystone by numerical methods in Plaxis 2D the authors recommend using the Hardening Soil model considering the impacted areas in ground space beside the driven pile. The analyses of the results and calculations are presented for examination and verification; therefore it is necessary to continue the research work of deep foundation at another experimental sites to improve the reliability of the calculation of pile foundation settlement. The work is of great interest for geotechnical engineers engaged in research, design and construction of pile foundations.

  18. Analytical validation of an ultraviolet-visible procedure for determining lutein concentration and application to lutein-loaded nanoparticles.

    Science.gov (United States)

    Silva, Jéssica Thaís do Prado; Silva, Anderson Clayton da; Geiss, Julia Maria Tonin; de Araújo, Pedro Henrique Hermes; Becker, Daniela; Bracht, Lívia; Leimann, Fernanda Vitória; Bona, Evandro; Guerra, Gustavo Petri; Gonçalves, Odinei Hess

    2017-09-01

    Lutein is a carotenoid presenting known anti-inflammatory and antioxidant properties. Lutein-rich diets have been associated with neurological improvement as well as reduction of the risk of vision loss due to Age-Related Macular Degeneration (AMD). Micro and nanoencapsulation have demonstrated to be effective techniques in protecting lutein against degradation and also in improving its bioavailability. However, actual lutein concentration inside the capsules and encapsulation efficiency are key parameters that must be precisely known when designing in vitro and in vivo tests. In this work an analytical procedure was validated for the determination of the actual lutein content in zein nanoparticles using ultraviolet-visible spectroscopy. Method validation followed the International Conference on Harmonisation (ICH) guidelines which evaluate linearity, detection limit, quantification limit, accuracy and precision. The validated methodology was applied to characterize lutein-loaded nanoparticles. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Modification and validation of an analytical source model for external beam radiotherapy Monte Carlo dose calculations

    Energy Technology Data Exchange (ETDEWEB)

    Davidson, Scott E., E-mail: sedavids@utmb.edu [Radiation Oncology, The University of Texas Medical Branch, Galveston, Texas 77555 (United States); Cui, Jing [Radiation Oncology, University of Southern California, Los Angeles, California 90033 (United States); Kry, Stephen; Ibbott, Geoffrey S.; Followill, David S. [Department of Radiation Physics, The University of Texas MD Anderson Cancer Center, Houston, Texas 77030 (United States); Deasy, Joseph O. [Department of Medical Physics, Memorial Sloan Kettering Cancer Center, New York, New York 10065 (United States); Vicic, Milos [Department of Applied Physics, University of Belgrade, Belgrade 11000 (Serbia); White, R. Allen [Bioinformatics and Computational Biology, The University of Texas MD Anderson Cancer Center, Houston, Texas 77030 (United States)

    2016-08-15

    Purpose: A dose calculation tool, which combines the accuracy of the dose planning method (DPM) Monte Carlo code and the versatility of a practical analytical multisource model, which was previously reported has been improved and validated for the Varian 6 and 10 MV linear accelerators (linacs). The calculation tool can be used to calculate doses in advanced clinical application studies. One shortcoming of current clinical trials that report dose from patient plans is the lack of a standardized dose calculation methodology. Because commercial treatment planning systems (TPSs) have their own dose calculation algorithms and the clinical trial participant who uses these systems is responsible for commissioning the beam model, variation exists in the reported calculated dose distributions. Today’s modern linac is manufactured to tight specifications so that variability within a linac model is quite low. The expectation is that a single dose calculation tool for a specific linac model can be used to accurately recalculate dose from patient plans that have been submitted to the clinical trial community from any institution. The calculation tool would provide for a more meaningful outcome analysis. Methods: The analytical source model was described by a primary point source, a secondary extra-focal source, and a contaminant electron source. Off-axis energy softening and fluence effects were also included. The additions of hyperbolic functions have been incorporated into the model to correct for the changes in output and in electron contamination with field size. A multileaf collimator (MLC) model is included to facilitate phantom and patient dose calculations. An offset to the MLC leaf positions was used to correct for the rudimentary assumed primary point source. Results: Dose calculations of the depth dose and profiles for field sizes 4 × 4 to 40 × 40 cm agree with measurement within 2% of the maximum dose or 2 mm distance to agreement (DTA) for 95% of the data

  20. Ethical leadership: meta-analytic evidence of criterion-related and incremental validity.

    Science.gov (United States)

    Ng, Thomas W H; Feldman, Daniel C

    2015-05-01

    This study examines the criterion-related and incremental validity of ethical leadership (EL) with meta-analytic data. Across 101 samples published over the last 15 years (N = 29,620), we observed that EL demonstrated acceptable criterion-related validity with variables that tap followers' job attitudes, job performance, and evaluations of their leaders. Further, followers' trust in the leader mediated the relationships of EL with job attitudes and performance. In terms of incremental validity, we found that EL significantly, albeit weakly in some cases, predicted task performance, citizenship behavior, and counterproductive work behavior-even after controlling for the effects of such variables as transformational leadership, use of contingent rewards, management by exception, interactional fairness, and destructive leadership. The article concludes with a discussion of ways to strengthen the incremental validity of EL. (PsycINFO Database Record (c) 2015 APA, all rights reserved).

  1. Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

    Directory of Open Access Journals (Sweden)

    Eloy Yordad Companioni Damas

    2009-01-01

    Full Text Available This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(apyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

  2. Spacecraft early design validation using formal methods

    International Nuclear Information System (INIS)

    Bozzano, Marco; Cimatti, Alessandro; Katoen, Joost-Pieter; Katsaros, Panagiotis; Mokos, Konstantinos; Nguyen, Viet Yen; Noll, Thomas; Postma, Bart; Roveri, Marco

    2014-01-01

    The size and complexity of software in spacecraft is increasing exponentially, and this trend complicates its validation within the context of the overall spacecraft system. Current validation methods are labor-intensive as they rely on manual analysis, review and inspection. For future space missions, we developed – with challenging requirements from the European space industry – a novel modeling language and toolset for a (semi-)automated validation approach. Our modeling language is a dialect of AADL and enables engineers to express the system, the software, and their reliability aspects. The COMPASS toolset utilizes state-of-the-art model checking techniques, both qualitative and probabilistic, for the analysis of requirements related to functional correctness, safety, dependability and performance. Several pilot projects have been performed by industry, with two of them having focused on the system-level of a satellite platform in development. Our efforts resulted in a significant advancement of validating spacecraft designs from several perspectives, using a single integrated system model. The associated technology readiness level increased from level 1 (basic concepts and ideas) to early level 4 (laboratory-tested)

  3. An analytical method for neutron thermalization calculations in heterogenous reactors

    Energy Technology Data Exchange (ETDEWEB)

    Pop-Jordanov, J [Boris Kidric Institute of Nuclear Sciences, Vinca, Belgrade (Yugoslavia)

    1965-07-01

    It is well known that the use of the diffusion approximation for stumethods are rather laborious and require the use of large digital computers. In this paper, the use of the diffusion approximation in absorbing media has been avoided, but the treatment remained analytical, thus simplifying practical calculations.

  4. Methods for the calculation of uncertainty in analytical chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Sohn, S. C.; Park, Y. J.; Park, K. K.; Jee, K. Y.; Joe, K. S.; Kim, W. H

    2000-07-01

    This report describes the statistical rules for evaluating and expressing uncertainty in analytical chemistry. The procedures for the evaluation of uncertainty in chemical analysis are illustrated by worked examples. This report, in particular, gives guidance on how uncertainty can be estimated from various chemical analyses. This report can be also used for planning the experiments which will provide the information required to obtain an estimate of uncertainty for the method.

  5. An analytical method for neutron thermalization calculations in heterogenous reactors

    International Nuclear Information System (INIS)

    Pop-Jordanov, J.

    1965-01-01

    It is well known that the use of the diffusion approximation for studying neutron thermalization in heterogeneous reactors may result in considerable errors. On the other hand, more exact numerical methods are rather laborious and require the use of large digital computers. In this paper, the use of the diffusion approximation in absorbing media has been avoided, but the treatment remained analytical, thus simplifying practical calculations

  6. Analytical method comparisons for the accurate determination of PCBs in sediments

    Energy Technology Data Exchange (ETDEWEB)

    Numata, M.; Yarita, T.; Aoyagi, Y.; Yamazaki, M.; Takatsu, A. [National Metrology Institute of Japan, Tsukuba (Japan)

    2004-09-15

    National Metrology Institute of Japan in National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has been developing several matrix reference materials, for example, sediments, water and biological tissues, for the determinations of heavy metals and organometallic compounds. The matrix compositions of those certified reference materials (CRMs) are similar to compositions of actual samples, and those are useful for validating analytical procedures. ''Primary methods of measurements'' are essential to obtain accurate and SI-traceable certified values in the reference materials, because the methods have the highest quality of measurement. However, inappropriate analytical operations, such as incomplete extraction of analytes or crosscontamination during analytical procedures, will cause error of analytical results, even if one of the primary methods, isotope-dilution, is utilized. To avoid possible procedural bias for the certification of reference materials, we employ more than two analytical methods which have been optimized beforehand. Because the accurate determination of trace POPs in the environment is important to evaluate their risk, reliable CRMs are required by environmental chemists. Therefore, we have also been preparing matrix CRMs for the determination of POPs. To establish accurate analytical procedures for the certification of POPs, extraction is one of the critical steps as described above. In general, conventional extraction techniques for the determination of POPs, such as Soxhlet extraction (SOX) and saponification (SAP), have been characterized well, and introduced as official methods for environmental analysis. On the other hand, emerging techniques, such as microwave-assisted extraction (MAE), pressurized fluid extraction (PFE) and supercritical fluid extraction (SFE), give higher recovery yields of analytes with relatively short extraction time and small amount of solvent, by reasons of the high

  7. Analytical Methods for Biomass Characterization during Pretreatment and Bioconversion

    Energy Technology Data Exchange (ETDEWEB)

    Pu, Yunqiao [ORNL; Meng, Xianzhi [University of Tennessee, Knoxville (UTK); Yoo, Chang Geun; Li, Mi; Ragauskas, Arthur J [ORNL

    2016-01-01

    Lignocellulosic biomass has been introduced as a promising resource for alternative fuels and chemicals because of its abundance and complement for petroleum resources. Biomass is a complex biopolymer and its compositional and structural characteristics largely vary depending on its species as well as growth environments. Because of complexity and variety of biomass, understanding its physicochemical characteristics is a key for effective biomass utilization. Characterization of biomass does not only provide critical information of biomass during pretreatment and bioconversion, but also give valuable insights on how to utilize the biomass. For better understanding biomass characteristics, good grasp and proper selection of analytical methods are necessary. This chapter introduces existing analytical approaches that are widely employed for biomass characterization during biomass pretreatment and conversion process. Diverse analytical methods using Fourier transform infrared (FTIR) spectroscopy, gel permeation chromatography (GPC), and nuclear magnetic resonance (NMR) spectroscopy for biomass characterization are reviewed. In addition, biomass accessibility methods by analyzing surface properties of biomass are also summarized in this chapter.

  8. Validation of pestice multi residue analysis method on cucumber

    International Nuclear Information System (INIS)

    2011-01-01

    In this study we aimed to validate the method of multi pesticide residue analysis on cucumber. Before real sample injection, system suitability test was performed in gas chromatography (GC). For this purpose, a sensitive pesticide mixture was used for GC-NPD and estimated the performance parameters such as number of effective theoretical plates, resolution factor, asymmetry, tailing and selectivity. It was detected that the system was suitable for calibration and sample injection. Samples were fortified at the level of 0.02, 0.2, 0.8 and 1 mg/kg with mixture of dichlorvos, malathion and chloropyrifos pesticides. In the fortification step 1 4C-carbaryl was also added on homogenized analytical portions to make use of 1 4C labelled pesticides for the determining extraction efficiency. Then the basic analytical process, such as ethyl acetate extraction, filtration, evaporation and cleanup, were performed. The GPC calibration using 1 4C- carbaryl and fortification mixture (dichlorvos, malathion and chloropyrifos) showed that pesticide fraction come through the column between the 8-23 ml fractions. The recovery of 1 4C-carbaryl after the extraction and cleanup step were 92.63-111.73 % and 74.83-102.22 %, respectively. The stability of pesticides during analysis is an important factor. In this study, stability test was performed including matrix effect. Our calculation and t test results showed that above mentioned pesticides were not stabile during sample processing in our laboratory conditions and it was found that sample comminution with dry ice may improve stability. In the other part of the study, 1 4C-chloropyrifos was used to determine homogeneity of analytical portions taken from laboratory samples. Use of 1 4C labelled pesticides allows us for quick quantification analyte, even with out clean-up. The analytical results show that after sample processing with waring blender, analytical portions were homogenous. Sample processing uncertainty depending on quantity of

  9. EPA's analytical methods for water: The next generation

    International Nuclear Information System (INIS)

    Hites, R.A.; Budde, W.L.

    1991-01-01

    By the late 1970s, it had become clear to EPA that organic compounds were polluting many of the nation's waters. By 1977, as a result of a lawsuit by several environmentally concerned plaintiffs, EPA had focused on a list of 114 'priority' organic pollutants. Its long-term goal was the regulation of specific compounds that were found to pose significant environmental problems, a daunting task. Tens of thousands of samples needed to be measured by hundreds of different laboratories. Clearly, there were concerns about the comparability of data among laboratories. The result was a series of laboratory-based analytical 'methods.' These EPA methods are detailed, step-by-step directions (recipes) that describe everything the analyst needs to know to complete a satisfactory analysis. During the 1970s the first set of methods was developed; this was the '600 series' for the analysis of organic compounds in wastewater. In 1979 and the 1980s, a set of '500 series' methods, focusing on drinking water, was developed. By now, many of the 500 and 600 series methods are in widespread use, and it is clear that there are considerably overlaps among the methods in terms of both procedures and analytes. Indiana University was asked by EPA to consider the question, 'Is it possible to revise or eliminate some of the 500 and 600 series methods and effect a savings of time and money?' This and related questions were studied and recommendations were developed

  10. On the nonlinear dynamics of trolling-mode AFM: Analytical solution using multiple time scales method

    Science.gov (United States)

    Sajjadi, Mohammadreza; Pishkenari, Hossein Nejat; Vossoughi, Gholamreza

    2018-06-01

    Trolling mode atomic force microscopy (TR-AFM) has resolved many imaging problems by a considerable reduction of the liquid-resonator interaction forces in liquid environments. The present study develops a nonlinear model of the meniscus force exerted to the nanoneedle of TR-AFM and presents an analytical solution to the distributed-parameter model of TR-AFM resonator utilizing multiple time scales (MTS) method. Based on the developed analytical solution, the frequency-response curves of the resonator operation in air and liquid (for different penetration length of the nanoneedle) are obtained. The closed-form analytical solution and the frequency-response curves are validated by the comparison with both the finite element solution of the main partial differential equations and the experimental observations. The effect of excitation angle of the resonator on horizontal oscillation of the probe tip and the effect of different parameters on the frequency-response of the system are investigated.

  11. A Process Analytical Technology (PAT) approach to control a new API manufacturing process: development, validation and implementation.

    Science.gov (United States)

    Schaefer, Cédric; Clicq, David; Lecomte, Clémence; Merschaert, Alain; Norrant, Edith; Fotiadu, Frédéric

    2014-03-01

    Pharmaceutical companies are progressively adopting and introducing Process Analytical Technology (PAT) and Quality-by-Design (QbD) concepts promoted by the regulatory agencies, aiming the building of the quality directly into the product by combining thorough scientific understanding and quality risk management. An analytical method based on near infrared (NIR) spectroscopy was developed as a PAT tool to control on-line an API (active pharmaceutical ingredient) manufacturing crystallization step during which the API and residual solvent contents need to be precisely determined to reach the predefined seeding point. An original methodology based on the QbD principles was designed to conduct the development and validation of the NIR method and to ensure that it is fitted for its intended use. On this basis, Partial least squares (PLS) models were developed and optimized using chemometrics methods. The method was fully validated according to the ICH Q2(R1) guideline and using the accuracy profile approach. The dosing ranges were evaluated to 9.0-12.0% w/w for the API and 0.18-1.50% w/w for the residual methanol. As by nature the variability of the sampling method and the reference method are included in the variability obtained for the NIR method during the validation phase, a real-time process monitoring exercise was performed to prove its fit for purpose. The implementation of this in-process control (IPC) method on the industrial plant from the launch of the new API synthesis process will enable automatic control of the final crystallization step in order to ensure a predefined quality level of the API. In addition, several valuable benefits are expected including reduction of the process time, suppression of a rather difficult sampling and tedious off-line analyses. © 2013 Published by Elsevier B.V.

  12. A long-term validation of the modernised DC-ARC-OES solid-sample method.

    Science.gov (United States)

    Flórián, K; Hassler, J; Förster, O

    2001-12-01

    The validation procedure based on ISO 17025 standard has been used to study and illustrate both the longterm stability of the calibration process of the DC-ARC solid sample spectrometric method and the main validation criteria of the method. In the calculation of the validation characteristics depending on the linearity(calibration), also the fulfilment of predetermining criteria such as normality and homoscedasticity was checked. In order to decide whether there are any trends in the time-variation of the analytical signal or not, also the Neumann test of trend was applied and evaluated. Finally, a comparison with similar validation data of the ETV-ICP-OES method was carried out.

  13. Multiplier ideal sheaves and analytic methods in algebraic geometry

    International Nuclear Information System (INIS)

    Demailly, J.-P.

    2001-01-01

    Our main purpose here is to describe a few analytic tools which are useful to study questions such as linear series and vanishing theorems for algebraic vector bundles. One of the early successes of analytic methods in this context is Kodaira's use of the Bochner technique in relation with the theory of harmonic forms, during the decade 1950-60.The idea is to represent cohomology classes by harmonic forms and to prove vanishing theorems by means of suitable a priori curvature estimates. We pursue the study of L2 estimates, in relation with the Nullstellenstatz and with the extension problem. We show how subadditivity can be used to derive an approximation theorem for (almost) plurisubharmonic functions: any such function can be approximated by a sequence of (almost) plurisubharmonic functions which are smooth outside an analytic set, and which define the same multiplier ideal sheaves. From this, we derive a generalized version of the hard Lefschetz theorem for cohomology with values in a pseudo-effective line bundle; namely, the Lefschetz map is surjective when the cohomology groups are twisted by the relevant multiplier ideal sheaves. These notes are essentially written with the idea of serving as an analytic tool- box for algebraic geometers. Although efficient algebraic techniques exist, our feeling is that the analytic techniques are very flexible and offer a large variety of guidelines for more algebraic questions (including applications to number theory which are not discussed here). We made a special effort to use as little prerequisites and to be as self-contained as possible; hence the rather long preliminary sections dealing with basic facts of complex differential geometry

  14. Multiplier ideal sheaves and analytic methods in algebraic geometry

    Energy Technology Data Exchange (ETDEWEB)

    Demailly, J -P [Universite de Grenoble I, Institut Fourier, Saint-Martin d' Heres (France)

    2001-12-15

    Our main purpose here is to describe a few analytic tools which are useful to study questions such as linear series and vanishing theorems for algebraic vector bundles. One of the early successes of analytic methods in this context is Kodaira's use of the Bochner technique in relation with the theory of harmonic forms, during the decade 1950-60.The idea is to represent cohomology classes by harmonic forms and to prove vanishing theorems by means of suitable a priori curvature estimates. We pursue the study of L2 estimates, in relation with the Nullstellenstatz and with the extension problem. We show how subadditivity can be used to derive an approximation theorem for (almost) plurisubharmonic functions: any such function can be approximated by a sequence of (almost) plurisubharmonic functions which are smooth outside an analytic set, and which define the same multiplier ideal sheaves. From this, we derive a generalized version of the hard Lefschetz theorem for cohomology with values in a pseudo-effective line bundle; namely, the Lefschetz map is surjective when the cohomology groups are twisted by the relevant multiplier ideal sheaves. These notes are essentially written with the idea of serving as an analytic tool- box for algebraic geometers. Although efficient algebraic techniques exist, our feeling is that the analytic techniques are very flexible and offer a large variety of guidelines for more algebraic questions (including applications to number theory which are not discussed here). We made a special effort to use as little prerequisites and to be as self-contained as possible; hence the rather long preliminary sections dealing with basic facts of complex differential geometry.

  15. Analytical methods for determination of terbinafine hydrochloride in pharmaceuticals and biological materials

    Directory of Open Access Journals (Sweden)

    Basavaiah Kanakapura

    2016-06-01

    Full Text Available Terbinafine is a new powerful antifungal agent indicated for both oral and topical treatment of mycosessince. It is highly effective in the treatment of determatomycoses. The chemical and pharmaceutical analysis of the drug requires effective analytical methods for quality control and pharmacodynamic and pharmacokinetic studies. Ever since it was introduced as an effective antifungal agent, many methods have been developed and validated for its assay in pharmaceuticals and biological materials. This article reviews the various methods reported during the last 25 years.

  16. Analytic function expansion nodal method for nuclear reactor core design

    International Nuclear Information System (INIS)

    Noh, Hae Man

    1995-02-01

    In most advanced nodal methods the transverse integration is commonly used to reduce the multi-dimensional diffusion equation into equivalent one- dimensional diffusion equations when derving the nodal coupling equations. But the use of the transverse integration results in some limitations. The first limitation is that the transverse leakage term which appears in the transverse integration procedure must be appropriately approximated. The second limitation is that the one-dimensional flux shapes in each spatial direction resulted from the nodal calculation are not accurate enough to be directly used in reconstructing the pinwise flux distributions. Finally the transverse leakage defined for a non-rectangular node such as a hexagonal node or a triangular node is too complicated to be easily handled and may contain non-physical singular terms of step-function and delta-function types. In this thesis, the Analytic Function Expansion Nodal (AFEN) method and its two variations : the Polynomial Expansion Nodal (PEN) method and the hybrid of the AFEN and PEN methods, have been developed to overcome the limitations of the transverse integration procedure. All of the methods solve the multidimensional diffusion equation without the transverse integration. The AFEN method which we believe is the major contribution of this study to the reactor core analysis expands the homogeneous flux distributions within a node in non-separable analytic basis functions satisfying the neutron diffusion equations at any point of the node and expresses the coefficients of the flux expansion in terms of the nodal unknowns which comprise a node-average flux, node-interface fluxes, and corner-point fluxes. Then, the nodal coupling equations composed of the neutron balance equations, the interface current continuity equations, and the corner-point leakage balance equations are solved iteratively to determine all the nodal unknowns. Since the AFEN method does not use the transverse integration in

  17. Validation of the quality control methods for active ingredients of Fungirex cream

    International Nuclear Information System (INIS)

    Perez Navarro, Maikel; Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania

    2014-01-01

    Fungirex cream is a two-drug product, that is, undecylenic acid and zinc undecylenate over a suitable basis. Since this is a product not documented in the official monographs of the pharmacopoeia, simple analytical methods were suggested for quantitation of analytes of interest in the cream, which are useful for release of newly prepared cream batches. To validate two volumetric methods for the quality control of active ingredients in Fungirex cream

  18. Modelling of packet traffic with matrix analytic methods

    DEFF Research Database (Denmark)

    Andersen, Allan T.

    1995-01-01

    BISDN network. The heuristic formula did not seem to yield substantially better results than already available approximations. Finally, some results for the finite capacity BMAP/G/1 queue have been obtained. The steady state probability vector of the embedded chain is found by a direct method where...... process. A heuristic formula for the tail behaviour of a single server queue fed by a superposition of renewal processes has been evaluated. The evaluation was performed by applying Matrix Analytic methods. The heuristic formula has applications in the Call Admission Control (CAC) procedure of the future...

  19. Benchmark Comparison of Cloud Analytics Methods Applied to Earth Observations

    Science.gov (United States)

    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.

  20. Benchmark Comparison of Cloud Analytics Methods Applied to Earth Observations

    Science.gov (United States)

    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.

  1. Simplified Analytical Method for Optimized Initial Shape Analysis of Self-Anchored Suspension Bridges and Its Verification

    Directory of Open Access Journals (Sweden)

    Myung-Rag Jung

    2015-01-01

    Full Text Available A simplified analytical method providing accurate unstrained lengths of all structural elements is proposed to find the optimized initial state of self-anchored suspension bridges under dead loads. For this, equilibrium equations of the main girder and the main cable system are derived and solved by evaluating the self-weights of cable members using unstrained cable lengths and iteratively updating both the horizontal tension component and the vertical profile of the main cable. Furthermore, to demonstrate the validity of the simplified analytical method, the unstrained element length method (ULM is applied to suspension bridge models based on the unstressed lengths of both cable and frame members calculated from the analytical method. Through numerical examples, it is demonstrated that the proposed analytical method can indeed provide an optimized initial solution by showing that both the simplified method and the nonlinear FE procedure lead to practically identical initial configurations with only localized small bending moment distributions.

  2. Development and Validation of Analytical Method for Losartan ...

    African Journals Online (AJOL)

    HP

    determination of losartan potassium concentration in pharmaceutical formulations in the visible region. ... This metal triggers a series of electron transfer reactions as a cofactor in a number of critical ... potassium with 50 ml of distilled water and.

  3. Validación de método analítico para el control de la calidad de vitamina B12 10 000 inyección Validation of analytical method for quality control of B12 Vitamin-10 000 injection

    Directory of Open Access Journals (Sweden)

    Martha Botet García

    2009-12-01

    Full Text Available Se validó el método analítico reportado en la Farmacopea de los Estados Unidos, para el control de la calidad de vitamina B12 10 000 U (cianocobalamina inyectable, por espectrofotometría ultravioleta, por ser este un método más sencillo, económico y que permite controlar la calidad del producto terminado. La curva de calibración se realizó en el intervalo de 60 al 140 %, donde fue lineal con un coeficiente de correlación igual a 0,9999; la prueba estadística para el intercepto y la pendiente se consideró no significativa. Se obtuvo un recobrado del 99,97 % en el intervalo de concentraciones estudiado, y las pruebas de Cochran (G y Student (t resultaron no significativas. El coeficiente de variación en el estudio de la repetibilidad fue igual a 0,59 % para las 6 réplicas ensayadas, mientras que en los análisis de la precisión intermedia las pruebas de Fischer y Student no significativas. El método analítico resultó lineal, preciso, específico y exacto en el intervalo de concentraciones estudiadas.Analytical method reported by USA Pharmacopeia was validated for quality control of injectable B12 Vitamin (10 000 U by UV spectrophotometry because this is a simpler and low-cost method allowing quality control of finished product. Calibration curve was graphed at 60 to 140 % interval, where it was linear with a correlation coefficient similar to 0, 9999; statistical test for interception and slope was considered non-significant. There was a recovery of 99.7 % in study concentrations interval where the Cochran (G and Student(t test were not significant too. Variation coefficient in repetition study was similar to 0.59 % for the 6 assayed replies, whereas in intermediate precision analysis, the Fisher and Student tests were not significant. Analytical method was linear, precise, specific and exact in study concentrations interval.

  4. Validación del método analítico para el control de la calidad y estudio de estabilidad de ketotifeno colirio 0,025 % Validation of analytical method to quality control and the stability study of 0.025 % eyedrops Ketotiphen

    Directory of Open Access Journals (Sweden)

    Yenilen Troche Concepción

    2010-09-01

    Full Text Available El colirio de ketotifeno se indica para aliviar los signos y síntomas de las conjuntivitis alérgicas, por ser este un potente antihistamínico H1 que muestra cierta capacidad para inhibir la liberación de histamina y otros mediadores en mastocitos. En este trabajo se desarrolló y validó un método analítico por cromatografía líquida de alta resolución, para el control de la calidad y los estudios de estabilidad del ketotifeno colirio 0,025 %. El método se basó en la separación del principio activo a través una columna cromatográfica Lichrosorb RP-18 (5 µm (250 x 4 mm, con detección ultravioleta a 296 nm, para lo cual se empleó una fase móvil compuesta por una mezcla desgasificada de metanol:buffer fosfato (75:25; pH 8,5 y se le añadió 1 mL de isopropanol por cada 1 000 mL de la mezcla anterior, con una velocidad de flujo de 1,2 mL/min. El método analítico resultó lineal, preciso, específico y exacto en el intervalo de concentraciones estudiadas.The Ketotiphen eyedrop is prescribed to relief the signs and symptoms of allergic conjunctivitis due to its potent H1 antihistaminic effect showing some ability to inhibit the histamine release and other mediators in cases of mastocytosis. The aim of present paper was to develop and validate an analytical method for the high-performance liquid chromatography, to quality control and the stability studies of 0.025 % eyedrop Ketotiphen. Method was based on active principle separation by means of a Lichrosorb RP-18 (5 µm (250 x 4 mm, with UV detection to 296 nm using a mobile phase including a non-gasified mixture of methanol:buffer-phosphate (75:25; pH 8.5 adding 1 mL of Isopropanol by each 1 000 mL of the previous mixture at a 1.2 mL/min flow velocity. The analytical method was linear, accurate, specific and exact during the study concentrations.

  5. Analytical Methods for Mycotoxin Detection in Southeast Asian Nations (ASEAN).

    Science.gov (United States)

    Lim, Chee Wei; Chung, Gerald; Chan, Sheot Harn

    2017-10-03

    Aflatoxins B 1 (AFB 1 ) and B₂ (AFB₂) and G 1 and G₂ remain the top mycotoxins routinely analyzed and monitored by Association of Southeast Asian Nations (ASEAN) national laboratories primarily for food safety regulation in the major food commodities, nuts and spices. LC tandem fluorescence detection (LC–fluorescence) represents a current mainstream analytical method, with a progressive migration to a primary method by LC tandem MS (MS/MS) for the next half decade. Annual proficiency testing (PT) is conducted by ASEAN Food Reference Laboratories (AFRLs) for mycotoxin testing as part of capability building in national laboratories, with the scope of PT materials spanning from naturally mycotoxin-contaminated spices and nuts in the early 2010s to the recent contamination of corn flour in 2017 for total aflatoxin assay development. The merits of the mainstream LC–fluorescence method are witnessed by a significant improvement ( P < 0.05) in PT z -score passing rates (≤2) from 11.8 to 79.2% for AFB 1 , 23.5 to 83.3% for AFB₂, and 23.5 to 79.2% for total aflatoxins in the last 5 years. This paper discusses the journey of ASEAN national laboratories in analytical testing through AFRLs, and the progressive collective adoption of a multimycotoxin LC-MS/MS method aided by an isotopic dilution assay as a future primary method for safer food commodities.

  6. A preliminary investigation of PSA validation methods

    Energy Technology Data Exchange (ETDEWEB)

    Unwin, S D [Science Applications International Corp., (United States)

    1995-09-01

    This document has been prepared to support the initial phase of the Atomic Energy Control Board`s program to review and evaluate Probabilistic Safety Assessment (PSA) studies conducted by nuclear generating station designers and licensees. The document provides (1) a review of current and prospective applications of PSA technology in the Canadian nuclear power industry; (2) an assessment of existing practices and techniques for the review or risk and hazard identification studies in the international nuclear power sector and other technological sectors; and (3) proposed analytical framework in which to develop systematic techniques for the scrutiny and evaluation of a PSA model. These frameworks are based on consideration of the mathematical structure of a PSA model and are intended to facilitate the development of methods to evaluate a model relative to intended end-uses. (author). 34 refs., 10 tabs., 3 figs.

  7. A preliminary investigation of PSA validation methods

    International Nuclear Information System (INIS)

    Unwin, S.D.

    1995-09-01

    This document has been prepared to support the initial phase of the Atomic Energy Control Board's program to review and evaluate Probabilistic Safety Assessment (PSA) studies conducted by nuclear generating station designers and licensees. The document provides (1) a review of current and prospective applications of PSA technology in the Canadian nuclear power industry; (2) an assessment of existing practices and techniques for the review or risk and hazard identification studies in the international nuclear power sector and other technological sectors; and (3) proposed analytical framework in which to develop systematic techniques for the scrutiny and evaluation of a PSA model. These frameworks are based on consideration of the mathematical structure of a PSA model and are intended to facilitate the development of methods to evaluate a model relative to intended end-uses. (author). 34 refs., 10 tabs., 3 figs

  8. SU-E-T-479: Development and Validation of Analytical Models Predicting Secondary Neutron Radiation in Proton Therapy Applications

    International Nuclear Information System (INIS)

    Farah, J; Bonfrate, A; Donadille, L; Martinetti, F; Trompier, F; Clairand, I; De Olivera, A; Delacroix, S; Herault, J; Piau, S; Vabre, I

    2014-01-01

    Purpose: Test and validation of analytical models predicting leakage neutron exposure in passively scattered proton therapy. Methods: Taking inspiration from the literature, this work attempts to build an analytical model predicting neutron ambient dose equivalents, H*(10), within the local 75 MeV ocular proton therapy facility. MC simulations were first used to model H*(10) in the beam axis plane while considering a closed final collimator and pristine Bragg peak delivery. Next, MC-based analytical model was tested against simulation results and experimental measurements. The model was also expended in the vertical direction to enable a full 3D mapping of H*(10) inside the treatment room. Finally, the work focused on upgrading the literature model to clinically relevant configurations considering modulated beams, open collimators, patient-induced neutron fluctuations, etc. Results: The MC-based analytical model efficiently reproduced simulated H*(10) values with a maximum difference below 10%. In addition, it succeeded in predicting measured H*(10) values with differences <40%. The highest differences were registered at the closest and farthest positions from isocenter where the analytical model failed to faithfully reproduce the high neutron fluence and energy variations. The differences remains however acceptable taking into account the high measurement/simulation uncertainties and the end use of this model, i.e. radiation protection. Moreover, the model was successfully (differences < 20% on simulations and < 45% on measurements) extended to predict neutrons in the vertical direction with respect to the beam line as patients are in the upright seated position during ocular treatments. Accounting for the impact of beam modulation, collimation and the present of a patient in the beam path is far more challenging and conversion coefficients are currently being defined to predict stray neutrons in clinically representative treatment configurations. Conclusion

  9. An interactive website for analytical method comparison and bias estimation.

    Science.gov (United States)

    Bahar, Burak; Tuncel, Ayse F; Holmes, Earle W; Holmes, Daniel T

    2017-12-01

    Regulatory standards mandate laboratories to perform studies to ensure accuracy and reliability of their test results. Method comparison and bias estimation are important components of these studies. We developed an interactive website for evaluating the relative performance of two analytical methods using R programming language tools. The website can be accessed at https://bahar.shinyapps.io/method_compare/. The site has an easy-to-use interface that allows both copy-pasting and manual entry of data. It also allows selection of a regression model and creation of regression and difference plots. Available regression models include Ordinary Least Squares, Weighted-Ordinary Least Squares, Deming, Weighted-Deming, Passing-Bablok and Passing-Bablok for large datasets. The server processes the data and generates downloadable reports in PDF or HTML format. Our website provides clinical laboratories a practical way to assess the relative performance of two analytical methods. Copyright © 2017 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  10. A nonlinear analytic function expansion nodal method for transient calculations

    Energy Technology Data Exchange (ETDEWEB)

    Joo, Han Gyn; Park, Sang Yoon; Cho, Byung Oh; Zee, Sung Quun [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

    1998-12-31

    The nonlinear analytic function expansion nodal (AFEN) method is applied to the solution of the time-dependent neutron diffusion equation. Since the AFEN method requires both the particular solution and the homogeneous solution to the transient fixed source problem, the derivation of the solution method is focused on finding the particular solution efficiently. To avoid complicated particular solutions, the source distribution is approximated by quadratic polynomials and the transient source is constructed such that the error due to the quadratic approximation is minimized, In addition, this paper presents a new two-node solution scheme that is derived by imposing the constraint of current continuity at the interface corner points. The method is verified through a series of application to the NEACRP PWR rod ejection benchmark problems. 6 refs., 2 figs., 1 tab. (Author)

  11. Analytical methods for toxic gases from thermal degradation of polymers

    Science.gov (United States)

    Hsu, M.-T. S.

    1977-01-01

    Toxic gases evolved from the thermal oxidative degradation of synthetic or natural polymers in small laboratory chambers or in large scale fire tests are measured by several different analytical methods. Gas detector tubes are used for fast on-site detection of suspect toxic gases. The infrared spectroscopic method is an excellent qualitative and quantitative analysis for some toxic gases. Permanent gases such as carbon monoxide, carbon dioxide, methane and ethylene, can be quantitatively determined by gas chromatography. Highly toxic and corrosive gases such as nitrogen oxides, hydrogen cyanide, hydrogen fluoride, hydrogen chloride and sulfur dioxide should be passed into a scrubbing solution for subsequent analysis by either specific ion electrodes or spectrophotometric methods. Low-concentration toxic organic vapors can be concentrated in a cold trap and then analyzed by gas chromatography and mass spectrometry. The limitations of different methods are discussed.

  12. A nonlinear analytic function expansion nodal method for transient calculations

    Energy Technology Data Exchange (ETDEWEB)

    Joo, Han Gyn; Park, Sang Yoon; Cho, Byung Oh; Zee, Sung Quun [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

    1999-12-31

    The nonlinear analytic function expansion nodal (AFEN) method is applied to the solution of the time-dependent neutron diffusion equation. Since the AFEN method requires both the particular solution and the homogeneous solution to the transient fixed source problem, the derivation of the solution method is focused on finding the particular solution efficiently. To avoid complicated particular solutions, the source distribution is approximated by quadratic polynomials and the transient source is constructed such that the error due to the quadratic approximation is minimized, In addition, this paper presents a new two-node solution scheme that is derived by imposing the constraint of current continuity at the interface corner points. The method is verified through a series of application to the NEACRP PWR rod ejection benchmark problems. 6 refs., 2 figs., 1 tab. (Author)

  13. Reducing waste generation and radiation exposure by analytical method modification

    International Nuclear Information System (INIS)

    Ekechukwu, A.A.

    1996-01-01

    The primary goal of an analytical support laboratory has traditionally been to provide accurate data in a timely and cost effective fashion. Added to this goal is now the need to provide the same high quality data while generating as little waste as possible. At the Savannah River Technology Center (SRTC), we have modified and reengineered several methods to decrease generated waste and hence reduce radiation exposure. These method changes involved improving detection limits (which decreased the amount of sample required for analysis), decreasing reaction and analysis time, decreasing the size of experimental set-ups, recycling spent solvent and reagents, and replacing some methods. These changes had the additional benefits of reducing employee radiation exposure and exposure to hazardous chemicals. In all cases, the precision, accuracy, and detection limits were equal to or better than the replaced method. Most of the changes required little or no expenditure of funds. This paper describes these changes and discusses some of their applications

  14. Validation of Multilevel Constructs: Validation Methods and Empirical Findings for the EDI

    Science.gov (United States)

    Forer, Barry; Zumbo, Bruno D.

    2011-01-01

    The purposes of this paper are to highlight the foundations of multilevel construct validation, describe two methodological approaches and associated analytic techniques, and then apply these approaches and techniques to the multilevel construct validation of a widely-used school readiness measure called the Early Development Instrument (EDI;…

  15. The fitness for purpose of analytical methods applied to fluorimetric uranium determination in water matrix

    International Nuclear Information System (INIS)

    Grinman, Ana; Giustina, Daniel; Mondini, Julia; Diodat, Jorge

    2008-01-01

    Full text: This paper describes the steps which should be followed by a laboratory in order to validate the fluorimetric method for natural uranium in water matrix. The validation of an analytical method is a necessary requirement prior accreditation under Standard norm ISO/IEC 17025, of a non normalized method. Different analytical techniques differ in a sort of variables to be validated. Depending on the chemical process, measurement technique, matrix type, data fitting and measurement efficiency, a laboratory must set up experiments to verify reliability of data, through the application of several statistical tests and by participating in Quality Programs (QP) organized by reference laboratories such as the National Institute of Standards and Technology (NIST), National Physics Laboratory (NPL), or Environmental Measurements Laboratory (EML). However, the participation in QP not only involves international reference laboratories, but also, the national ones which are able to prove proficiency to the Argentinean Accreditation Board. The parameters that the ARN laboratory had to validate in the fluorimetric method to fit in accordance with Eurachem guide and IUPAC definitions, are: Detection Limit, Quantification Limit, Precision, Intra laboratory Precision, Reproducibility Limit, Repeatability Limit, Linear Range and Robustness. Assays to fit the above parameters were designed on the bases of statistics requirements, and a detailed data treatment is presented together with the respective tests in order to show the parameters validated. As a final conclusion, the uranium determination by fluorimetry is a reliable method for direct measurement to meet radioprotection requirements in water matrix, within its linear range which is fixed every time a calibration is carried out at the beginning of the analysis. The detection limit ( depending on blank standard deviation and slope) varies between 3 ug U and 5 ug U which yields minimum detectable concentrations (MDC) of

  16. Simultaneous determination of renal function biomarkers in urine using a validated paper-based microfluidic analytical device.

    Science.gov (United States)

    Rossini, Eduardo Luiz; Milani, Maria Izabel; Carrilho, Emanuel; Pezza, Leonardo; Pezza, Helena Redigolo

    2018-01-02

    In this paper, we describe a validated paper-based microfluidic analytical device for the simultaneous quantification of two important biomarkers of renal function in urine. This paper platform provides an inexpensive, simple, and easy to use colorimetric method for the quantification of creatinine (CRN) and uric acid (UA) in urine samples. The microfluidic paper-based analytical device (μPAD) consists of a main channel with three identical arms, each containing a circular testing zone and a circular uptake zone. Creatinine detection is based on the Jaffé reaction, in which CRN reacts with picrate to form an orange-red product. Uric acid quantification is based on the reduction of Fe 3+ to Fe 2+ by UA, which is detected in a colorimetric reaction using 1,10-phenanthroline. Under optimum conditions, obtained through chemometrics, the concentrations of the analytes showed good linear correlations with the effective intensities, and the method presented satisfactory repeatability. The limits of detection and the linear ranges, respectively, were 15.7 mg L -1 and 50-600 mg L -1 for CRN and 16.5 mg L -1 and 50-500 mg L -1 for UA. There were no statistically significant differences between the results obtained using the μPAD and a chromatographic comparative method (Student's t-test at 95% confidence level). Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Validación del método analítico para el control de la calidad y estudio de estabilidad de fenilefrina 10 % colirio Validation of an analytical method for quality control and stability study of 10 % Phenylephrine eyedrops

    Directory of Open Access Journals (Sweden)

    Raiza Monteagudo Licea

    2010-12-01

    Full Text Available La fenilefrina se emplea como midriático en exámenes de ojos y otros procedimientos oftálmicos. Se utiliza como vasoconstrictor con anestésicos locales. En este trabajo se validó un método analítico por cromatografía líquida de alta resolución para el control de la calidad y los estudios de estabilidad de la fenilefrina 10 % colirio. El método se basó en la separación del principio activo a través una columna cromatográfica Lichrosorb RP-18 (5 µm (250 x 4 mm, con detección ultravioleta a 280 nm, para lo cual se empleó una fase móvil compuesta por una mezcla desgasificada de metanol:agua destilada (1:1, con 1,1 g de 1-octanosulfonato de sodio por litro ajustado a pH 3,0 con ácido fosfórico, con una velocidad de flujo de 1,0 mL/min. El método analítico resultó lineal, preciso, específico y exacto en el intervalo de concentraciones estudiadas.Phenylephrine is used like mydiatric in eye examinations and other ophthalmic procedures. It is used as vasoconstrictor with local anesthetic agents. In present paper a high ressolution liquid chromatography analytical method was validated to quality control and stability studies of 10 % Phenylephrine (eyedrops. Mathod was based in separation of active principle through a Lichrosorb RO-18 (5 µm (250 x 4 mm chromatography column with UV detection at 280 nm using a mobile phase composed by a non-gasified mixture of methanol distilled water (1:1 with 1.1 g of 1-sodium octane-sulphonate by liter adjusted to pH 3,0 with phosphoric acid at a flow speed of 1.0 mL/min. Analytical method was linear, accuracy, specific and exact in the interval of study concentrations.

  18. Testing and Validation of the Dynamic Inertia Measurement Method

    Science.gov (United States)

    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.

  19. Analytical method for thermal stress analysis of plasma facing materials

    Science.gov (United States)

    You, J. H.; Bolt, H.

    2001-10-01

    The thermo-mechanical response of plasma facing materials (PFMs) to heat loads from the fusion plasma is one of the crucial issues in fusion technology. In this work, a fully analytical description of the thermal stress distribution in armour tiles of plasma facing components is presented which is expected to occur under typical high heat flux (HHF) loads. The method of stress superposition is applied considering the temperature gradient and thermal expansion mismatch. Several combinations of PFMs and heat sink metals are analysed and compared. In the framework of the present theoretical model, plastic flow and the effect of residual stress can be quantitatively assessed. Possible failure features are discussed.

  20. Analytical method for thermal stress analysis of plasma facing materials

    International Nuclear Information System (INIS)

    You, J.H.; Bolt, H.

    2001-01-01

    The thermo-mechanical response of plasma facing materials (PFMs) to heat loads from the fusion plasma is one of the crucial issues in fusion technology. In this work, a fully analytical description of the thermal stress distribution in armour tiles of plasma facing components is presented which is expected to occur under typical high heat flux (HHF) loads. The method of stress superposition is applied considering the temperature gradient and thermal expansion mismatch. Several combinations of PFMs and heat sink metals are analysed and compared. In the framework of the present theoretical model, plastic flow and the effect of residual stress can be quantitatively assessed. Possible failure features are discussed

  1. Higher geometry an introduction to advanced methods in analytic geometry

    CERN Document Server

    Woods, Frederick S

    2005-01-01

    For students of mathematics with a sound background in analytic geometry and some knowledge of determinants, this volume has long been among the best available expositions of advanced work on projective and algebraic geometry. Developed from Professor Woods' lectures at the Massachusetts Institute of Technology, it bridges the gap between intermediate studies in the field and highly specialized works.With exceptional thoroughness, it presents the most important general concepts and methods of advanced algebraic geometry (as distinguished from differential geometry). It offers a thorough study

  2. Diffusion weighted MRI by spatiotemporal encoding: Analytical description and in vivo validations

    Science.gov (United States)

    Solomon, Eddy; Shemesh, Noam; Frydman, Lucio

    2013-07-01

    Diffusion-weighted (DW) MRI is a powerful modality for studying microstructure in normal and pathological tissues. The accuracy derived from DW MRI depends on the acquisition of quality images, and on a precise assessment of the b-values involved. Conventional DW MRI tends to be of limited use in regions suffering from large magnetic field or chemical shift heterogeneities, which severely distort the MR images. In this study we propose novel sequences based on SPatio-temporal ENcoding (SPEN), which overcome such shortcomings owing to SPEN's inherent robustness to offsets. SPEN, however, relies on the simultaneous application of gradients and radiofrequency-swept pulses, which may impart different diffusion weightings along the spatial axes. These will be further complicated in DW measurements by the diffusion-sensitizing gradients, and will in general lead to complex, spatially-dependent b-values. This study presents a formalism for analyzing these diffusion-weighted SPEN (dSPEN) data, which takes into account the concomitant effects of adiabatic pulses, of the imaging as well as diffusion gradients, and of the cross-terms between them. These analytical b-values derivations are subject to experimental validations in phantom systems and ex vivo spinal cords. Excellent agreement is found between the theoretical predictions and these dSPEN experiments. The ensuing methodology is then demonstrated by in vivo mapping of diffusion in human breast - organs where conventional k-space DW acquisition methods are challenged by both field and chemical shift heterogeneities. These studies demonstrate the increased robustness of dSPEN vis-à-vis comparable DW echo planar imaging, and demonstrate the value of this new methodology for medium- or high-field diffusion measurements in heterogeneous systems.

  3. Method of sections in analytical calculations of pneumatic tires

    Science.gov (United States)

    Tarasov, V. N.; Boyarkina, I. V.

    2018-01-01

    Analytical calculations in the pneumatic tire theory are more preferable in comparison with experimental methods. The method of section of a pneumatic tire shell allows to obtain equations of intensities of internal forces in carcass elements and bead rings. Analytical dependencies of intensity of distributed forces have been obtained in tire equator points, on side walls (poles) and pneumatic tire bead rings. Along with planes in the capacity of secant surfaces cylindrical surfaces are used for the first time together with secant planes. The tire capacity equation has been obtained using the method of section, by means of which a contact body is cut off from the tire carcass along the contact perimeter by the surface which is normal to the bearing surface. It has been established that the Laplace equation for the solution of tasks of this class of pneumatic tires contains two unknown values that requires the generation of additional equations. The developed computational schemes of pneumatic tire sections and new equations allow to accelerate the pneumatic tire structure improvement process during engineering.

  4. Performance of analytical methods for tomographic gamma scanning

    International Nuclear Information System (INIS)

    Prettyman, T.H.; Mercer, D.J.

    1997-01-01

    The use of gamma-ray computerized tomography for nondestructive assay of radioactive materials has led to the development of specialized analytical methods. Over the past few years, Los Alamos has developed and implemented a computer code, called ARC-TGS, for the analysis of data obtained by tomographic gamma scanning (TGS). ARC-TGS reduces TGS transmission and emission tomographic data, providing the user with images of the sample contents, the activity or mass of selected radionuclides, and an estimate of the uncertainty in the measured quantities. The results provided by ARC-TGS can be corrected for self-attenuation when the isotope of interest emits more than one gamma-ray. In addition, ARC-TGS provides information needed to estimate TGS quantification limits and to estimate the scan time needed to screen for small amounts of radioactivity. In this report, an overview of the analytical methods used by ARC-TGS is presented along with an assessment of the performance of these methods for TGS

  5. Space Suit Joint Torque Measurement Method Validation

    Science.gov (United States)

    Valish, Dana; Eversley, Karina

    2012-01-01

    In 2009 and early 2010, a test method was developed and performed to quantify the torque required to manipulate joints in several existing operational and prototype space suits. This was done in an effort to develop joint torque requirements appropriate for a new Constellation Program space suit system. The same test method was levied on the Constellation space suit contractors to verify that their suit design met the requirements. However, because the original test was set up and conducted by a single test operator there was some question as to whether this method was repeatable enough to be considered a standard verification method for Constellation or other future development programs. In order to validate the method itself, a representative subset of the previous test was repeated, using the same information that would be available to space suit contractors, but set up and conducted by someone not familiar with the previous test. The resultant data was compared using graphical and statistical analysis; the results indicated a significant variance in values reported for a subset of the re-tested joints. Potential variables that could have affected the data were identified and a third round of testing was conducted in an attempt to eliminate and/or quantify the effects of these variables. The results of the third test effort will be used to determine whether or not the proposed joint torque methodology can be applied to future space suit development contracts.

  6. Analytical method of spectra calculations in the Bargmann representation

    International Nuclear Information System (INIS)

    Maciejewski, Andrzej J.; Przybylska, Maria; Stachowiak, Tomasz

    2014-01-01

    We formulate a universal method for solving an arbitrary quantum system which, in the Bargmann representation, is described by a system of linear equations with one independent variable, such as one- and multi-photon Rabi models, or N level systems interacting with a single mode of the electromagnetic field and their various generalizations. We explain three types of conditions that determine the spectrum and show their usage for two deformations of the Rabi model. We prove that the spectra of both models are just zeros of transcendental functions, which in one case are given explicitly in terms of confluent Heun functions. - Highlights: • Analytical method of spectrum determination in Bargmann representation is proposed. • Three types of conditions determining spectrum are identified. • Method to two generalizations of the Rabi system is applied

  7. Analytical method for the isotopic characterization of soils

    International Nuclear Information System (INIS)

    Sibello Hernandez, Rita; Cozzella, Maria Letizia; Mariani, Mario

    2014-01-01

    The aim of this work was to develop an analytical method in order to determine the isotopic composition of different elements in soil samples and to determine the existence of contamination. The method used in the digestion of the samples was the EPA 3050B, and some metal concentration were determined including uranium and thorium. For elements with even lower concentrations such as plutonium and radium a treatment after mineralization by EPA, was necessary. The measurement technique used was mass spectrometry with quadrupole and plasma induced associated (ICP-MS). Results of the analysis performed in two laboratories showed a good correspondence. This method allowed to perform the isotopic characterization of studied soils and results showed that the studied soils do not present any local pollution and that the presence of plutonium-239, is due to global failure

  8. Decentral gene expression analysis: analytical validation of the Endopredict genomic multianalyte breast cancer prognosis test

    Directory of Open Access Journals (Sweden)

    Kronenwett Ralf

    2012-10-01

    Full Text Available Abstract Background EndoPredict (EP is a clinically validated multianalyte gene expression test to predict distant metastasis in ER-positive, HER2-negative breast cancer treated with endocrine therapy alone. The test is based on the combined analysis of 12 genes in formalin-fixed, paraffin-embedded (FFPE tissue by reverse transcription-quantitative real-time PCR (RT-qPCR. Recently, it was shown that EP is feasible for reliable decentralized assessment of gene expression. The aim of this study was the analytical validation of the performance characteristics of the assay and its verification in a molecular-pathological routine laboratory. Methods Gene expression values to calculate the EP score were assayed by one-step RT-qPCR using RNA from FFPE tumor tissue. Limit of blank, limit of detection, linear range, and PCR efficiency were assessed for each of the 12 PCR assays using serial samples dilutions. Different breast cancer samples were used to evaluate RNA input range, precision and inter-laboratory variability. Results PCR assays were linear up to Cq values between 35.1 and 37.2. Amplification efficiencies ranged from 75% to 101%. The RNA input range without considerable change of the EP score was between 0.16 and 18.5 ng/μl. Analysis of precision (variation of day, day time, instrument, operator, reagent lots resulted in a total noise (standard deviation of 0.16 EP score units on a scale from 0 to 15. The major part of the total noise (SD 0.14 was caused by the replicate-to-replicate noise of the PCR assays (repeatability and was not associated with different operating conditions (reproducibility. Performance characteristics established in the manufacturer’s laboratory were verified in a routine molecular pathology laboratory. Comparison of 10 tumor samples analyzed in two different laboratories showed a Pearson coefficient of 0.995 and a mean deviation of 0.15 score units. Conclusions The EP test showed reproducible performance

  9. Vertical equilibrium with sub-scale analytical methods for geological CO2 sequestration

    KAUST Repository

    Gasda, S. E.; Nordbotten, J. M.; Celia, M. A.

    2009-01-01

    equilibrium with sub-scale analytical method (VESA) combines the flexibility of a numerical method, allowing for heterogeneous and geologically complex systems, with the efficiency and accuracy of an analytical method, thereby eliminating expensive grid

  10. Comparison of validation methods for forming simulations

    Science.gov (United States)

    Schug, Alexander; Kapphan, Gabriel; Bardl, Georg; Hinterhölzl, Roland; Drechsler, Klaus

    2018-05-01

    The forming simulation of fibre reinforced thermoplastics could reduce the development time and improve the forming results. But to take advantage of the full potential of the simulations it has to be ensured that the predictions for material behaviour are correct. For that reason, a thorough validation of the material model has to be conducted after characterising the material. Relevant aspects for the validation of the simulation are for example the outer contour, the occurrence of defects and the fibre paths. To measure these features various methods are available. Most relevant and also most difficult to measure are the emerging fibre orientations. For that reason, the focus of this study was on measuring this feature. The aim was to give an overview of the properties of different measuring systems and select the most promising systems for a comparison survey. Selected were an optical, an eddy current and a computer-assisted tomography system with the focus on measuring the fibre orientations. Different formed 3D parts made of unidirectional glass fibre and carbon fibre reinforced thermoplastics were measured. Advantages and disadvantages of the tested systems were revealed. Optical measurement systems are easy to use, but are limited to the surface plies. With an eddy current system also lower plies can be measured, but it is only suitable for carbon fibres. Using a computer-assisted tomography system all plies can be measured, but the system is limited to small parts and challenging to evaluate.

  11. Heat Conduction Analysis Using Semi Analytical Finite Element Method

    International Nuclear Information System (INIS)

    Wargadipura, A. H. S.

    1997-01-01

    Heat conduction problems are very often found in science and engineering fields. It is of accrual importance to determine quantitative descriptions of this important physical phenomena. This paper discusses the development and application of a numerical formulation and computation that can be used to analyze heat conduction problems. The mathematical equation which governs the physical behaviour of heat conduction is in the form of second order partial differential equations. The numerical resolution used in this paper is performed using the finite element method and Fourier series, which is known as semi-analytical finite element methods. The numerical solution results in simultaneous algebraic equations which is solved using the Gauss elimination methodology. The computer implementation is carried out using FORTRAN language. In the final part of the paper, a heat conduction problem in a rectangular plate domain with isothermal boundary conditions in its edge is solved to show the application of the computer program developed and also a comparison with analytical solution is discussed to assess the accuracy of the numerical solution obtained

  12. Analytic moment method calculations of the drift wave spectrum

    International Nuclear Information System (INIS)

    Thayer, D.R.; Molvig, K.

    1985-11-01

    A derivation and approximate solution of renormalized mode coupling equations describing the turbulent drift wave spectrum is presented. Arguments are given which indicate that a weak turbulence formulation of the spectrum equations fails for a system with negative dissipation. The inadequacy of the weak turbulence theory is circumvented by utilizing a renormalized formation. An analytic moment method is developed to approximate the solution of the nonlinear spectrum integral equations. The solution method employs trial functions to reduce the integral equations to algebraic equations in basic parameters describing the spectrum. An approximate solution of the spectrum equations is first obtained for a mode dissipation with known solution, and second for an electron dissipation in the NSA

  13. Introduction to Analytical Methods for Internal Combustion Engine Cam Mechanisms

    CERN Document Server

    Williams, J J

    2013-01-01

    Modern design methods of Automotive Cam Design require the computation of a range of parameters. This book provides a logical sequence of steps for the derivation of the relevant equations from first principles, for the more widely used cam mechanisms. Although originally derived for use in high performance engines, this work is equally applicable to the design of mass produced automotive and other internal combustion engines.   Introduction to Analytical Methods for Internal Combustion Engine Cam Mechanisms provides the equations necessary for the design of cam lift curves with an associated smooth acceleration curve. The equations are derived for the kinematics and kinetics of all the mechanisms considered, together with those for cam curvature and oil entrainment velocity. This permits the cam shape, all loads, and contact stresses to be evaluated, and the relevant tribology to be assessed. The effects of asymmetry on the manufacture of cams for finger follower and offset translating curved followers is ...

  14. Analytical methods manual for the Mineral Resource Surveys Program, U.S. Geological Survey

    Science.gov (United States)

    Arbogast, Belinda F.

    1996-01-01

    The analytical methods validated by the Mineral Resource Surveys Program, Geologic Division, is the subject of this manual. This edition replaces the methods portion of Open-File Report 90-668 published in 1990. Newer methods may be used which have been approved by the quality assurance (QA) project and are on file with the QA coordinator.This manual is intended primarily for use by laboratory scientists; this manual can also assist laboratory users to evaluate the data they receive. The analytical methods are written in a step by step approach so that they may be used as a training tool and provide detailed documentation of the procedures for quality assurance. A "Catalog of Services" is available for customer (submitter) use with brief listings of:the element(s)/species determined,method of determination,reference to cite,contact person,summary of the technique,and analyte concentration range.For a copy please contact the Branch office at (303) 236-1800 or fax (303) 236-3200.

  15. An analytical method for computing atomic contact areas in biomolecules.

    Science.gov (United States)

    Mach, Paul; Koehl, Patrice

    2013-01-15

    We propose a new analytical method for detecting and computing contacts between atoms in biomolecules. It is based on the alpha shape theory and proceeds in three steps. First, we compute the weighted Delaunay triangulation of the union of spheres representing the molecule. In the second step, the Delaunay complex is filtered to derive the dual complex. Finally, contacts between spheres are collected. In this approach, two atoms i and j are defined to be in contact if their centers are connected by an edge in the dual complex. The contact areas between atom i and its neighbors are computed based on the caps formed by these neighbors on the surface of i; the total area of all these caps is partitioned according to their spherical Laguerre Voronoi diagram on the surface of i. This method is analytical and its implementation in a new program BallContact is fast and robust. We have used BallContact to study contacts in a database of 1551 high resolution protein structures. We show that with this new definition of atomic contacts, we generate realistic representations of the environments of atoms and residues within a protein. In particular, we establish the importance of nonpolar contact areas that complement the information represented by the accessible surface areas. This new method bears similarity to the tessellation methods used to quantify atomic volumes and contacts, with the advantage that it does not require the presence of explicit solvent molecules if the surface of the protein is to be considered. © 2012 Wiley Periodicals, Inc. Copyright © 2012 Wiley Periodicals, Inc.

  16. Softcopy quality ruler method: implementation and validation

    Science.gov (United States)

    Jin, Elaine W.; Keelan, Brian W.; Chen, Junqing; Phillips, Jonathan B.; Chen, Ying

    2009-01-01

    A softcopy quality ruler method was implemented for the International Imaging Industry Association (I3A) Camera Phone Image Quality (CPIQ) Initiative. This work extends ISO 20462 Part 3 by virtue of creating reference digital images of known subjective image quality, complimenting the hardcopy Standard Reference Stimuli (SRS). The softcopy ruler method was developed using images from a Canon EOS 1Ds Mark II D-SLR digital still camera (DSC) and a Kodak P880 point-and-shoot DSC. Images were viewed on an Apple 30in Cinema Display at a viewing distance of 34 inches. Ruler images were made for 16 scenes. Thirty ruler images were generated for each scene, representing ISO 20462 Standard Quality Scale (SQS) values of approximately 2 to 31 at an increment of one just noticeable difference (JND) by adjusting the system modulation transfer function (MTF). A Matlab GUI was developed to display the ruler and test images side-by-side with a user-adjustable ruler level controlled by a slider. A validation study was performed at Kodak, Vista Point Technology, and Aptina Imaging in which all three companies set up a similar viewing lab to run the softcopy ruler method. The results show that the three sets of data are in reasonable agreement with each other, with the differences within the range expected from observer variability. Compared to previous implementations of the quality ruler, the slider-based user interface allows approximately 2x faster assessments with 21.6% better precision.

  17. GenoSets: visual analytic methods for comparative genomics.

    Directory of Open Access Journals (Sweden)

    Aurora A Cain

    Full Text Available Many important questions in biology are, fundamentally, comparative, and this extends to our analysis of a growing number of sequenced genomes. Existing genomic analysis tools are often organized around literal views of genomes as linear strings. Even when information is highly condensed, these views grow cumbersome as larger numbers of genomes are added. Data aggregation and summarization methods from the field of visual analytics can provide abstracted comparative views, suitable for sifting large multi-genome datasets to identify critical similarities and differences. We introduce a software system for visual analysis of comparative genomics data. The system automates the process of data integration, and provides the analysis platform to identify and explore features of interest within these large datasets. GenoSets borrows techniques from business intelligence and visual analytics to provide a rich interface of interactive visualizations supported by a multi-dimensional data warehouse. In GenoSets, visual analytic approaches are used to enable querying based on orthology, functional assignment, and taxonomic or user-defined groupings of genomes. GenoSets links this information together with coordinated, interactive visualizations for both detailed and high-level categorical analysis of summarized data. GenoSets has been designed to simplify the exploration of multiple genome datasets and to facilitate reasoning about genomic comparisons. Case examples are included showing the use of this system in the analysis of 12 Brucella genomes. GenoSets software and the case study dataset are freely available at http://genosets.uncc.edu. We demonstrate that the integration of genomic data using a coordinated multiple view approach can simplify the exploration of large comparative genomic data sets, and facilitate reasoning about comparisons and features of interest.

  18. Validated analytical modeling of diesel engine regulated exhaust CO emission rate

    Directory of Open Access Journals (Sweden)

    Waleed F Faris

    2016-06-01

    Full Text Available Albeit vehicle analytical models are often favorable for explainable mathematical trends, no analytical model has been developed of the regulated diesel exhaust CO emission rate for trucks yet. This research unprecedentedly develops and validates for trucks a model of the steady speed regulated diesel exhaust CO emission rate analytically. It has been found that the steady speed–based CO exhaust emission rate is based on (1 CO2 dissociation, (2 the water–gas shift reaction, and (3 the incomplete combustion of hydrocarbon. It has been found as well that the steady speed–based CO exhaust emission rate based on CO2 dissociation is considerably less than the rate that is based on the water–gas shift reaction. It has also been found that the steady speed–based CO exhaust emission rate based on the water–gas shift reaction is the dominant source of CO exhaust emission. The study shows that the average percentage of deviation of the steady speed–based simulated results from the corresponding field data is 1.7% for all freeway cycles with 99% coefficient of determination at the confidence level of 95%. This deviation of the simulated results from field data outperforms its counterpart of widely recognized models such as the comprehensive modal emissions model and VT-Micro for all freeway cycles.

  19. Analytical validation of an ultra low-cost mobile phone microplate reader for infectious disease testing.

    Science.gov (United States)

    Wang, Li-Ju; Naudé, Nicole; Demissie, Misganaw; Crivaro, Anne; Kamoun, Malek; Wang, Ping; Li, Lei

    2018-07-01

    Most mobile health (mHealth) diagnostic devices for laboratory tests only analyze one sample at a time, which is not suitable for large volume serology testing, especially in low-resource settings with shortage of health professionals. In this study, we developed an ultra-low-cost clinically-accurate mobile phone microplate reader (mReader), and clinically validated this optical device for 12 infectious disease tests. The mReader optically reads 96 samples on a microplate at one time. 771 de-identified patient samples were tested for 12 serology assays for bacterial/viral infections. The mReader and the clinical instrument blindly read and analyzed all tests in parallel. The analytical accuracy and the diagnostic performance of the mReader were evaluated across the clinical reportable categories by comparison with clinical laboratorial testing results. The mReader exhibited 97.59-99.90% analytical accuracy and envision the mReader can benefit underserved areas/populations and low-resource settings in rural clinics/hospitals at a low cost (~$50 USD) with clinical-level analytical quality. It has the potential to improve health access, speed up healthcare delivery, and reduce health disparities and education disparities by providing access to a low-cost spectrophotometer. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. USING ANALYTIC HIERARCHY PROCESS (AHP METHOD IN RURAL DEVELOPMENT

    Directory of Open Access Journals (Sweden)

    Tülay Cengiz

    2003-04-01

    Full Text Available Rural development is a body of economical and social policies towards improving living conditions in rural areas through enabling rural population to utilize economical, social, cultural and technological blessing of city life in place, without migrating. As it is understood from this description, rural development is a very broad concept. Therefore, in development efforts problem should be stated clearly, analyzed and many criterias should be evaluated by experts. Analytic Hierarchy Process (AHP method can be utilized at there stages of development efforts. AHP methods is one of multi-criteria decision method. After degrading a problem in smaller pieces, relative importance and level of importance of two compared elements are determined. It allows evaluation of quality and quantity factors. At the same time, it permits utilization of ideas of many experts and use them in decision process. Because mentioned features of AHP method, it could be used in rural development works. In this article, cultural factors, one of the important components of rural development is often ignored in many studies, were evaluated as an example. As a result of these applications and evaluations, it is concluded that AHP method could be helpful in rural development efforts.

  1. No Impact of the Analytical Method Used for Determining Cystatin C on Estimating Glomerular Filtration Rate in Children.

    Science.gov (United States)

    Alberer, Martin; Hoefele, Julia; Benz, Marcus R; Bökenkamp, Arend; Weber, Lutz T

    2017-01-01

    Measurement of inulin clearance is considered to be the gold standard for determining kidney function in children, but this method is time consuming and expensive. The glomerular filtration rate (GFR) is on the other hand easier to calculate by using various creatinine- and/or cystatin C (Cys C)-based formulas. However, for the determination of serum creatinine (Scr) and Cys C, different and non-interchangeable analytical methods exist. Given the fact that different analytical methods for the determination of creatinine and Cys C were used in order to validate existing GFR formulas, clinicians should be aware of the type used in their local laboratory. In this study, we compared GFR results calculated on the basis of different GFR formulas and either used Scr and Cys C values as determined by the analytical method originally employed for validation or values obtained by an alternative analytical method to evaluate any possible effects on the performance. Cys C values determined by means of an immunoturbidimetric assay were used for calculating the GFR using equations in which this analytical method had originally been used for validation. Additionally, these same values were then used in other GFR formulas that had originally been validated using a nephelometric immunoassay for determining Cys C. The effect of using either the compatible or the possibly incompatible analytical method for determining Cys C in the calculation of GFR was assessed in comparison with the GFR measured by creatinine clearance (CrCl). Unexpectedly, using GFR equations that employed Cys C values derived from a possibly incompatible analytical method did not result in a significant difference concerning the classification of patients as having normal or reduced GFR compared to the classification obtained on the basis of CrCl. Sensitivity and specificity were adequate. On the other hand, formulas using Cys C values derived from a compatible analytical method partly showed insufficient

  2. Determination of mycotoxins in foods: current state of analytical methods and limitations.

    Science.gov (United States)

    Köppen, Robert; Koch, Matthias; Siegel, David; Merkel, Stefan; Maul, Ronald; Nehls, Irene

    2010-05-01

    Mycotoxins are natural contaminants produced by a range of fungal species. Their common occurrence in food and feed poses a threat to the health of humans and animals. This threat is caused either by the direct contamination of agricultural commodities or by a "carry-over" of mycotoxins and their metabolites into animal tissues, milk, and eggs after feeding of contaminated hay or corn. As a consequence of their diverse chemical structures and varying physical properties, mycotoxins exhibit a wide range of biological effects. Individual mycotoxins can be genotoxic, mutagenic, carcinogenic, teratogenic, and oestrogenic. To protect consumer health and to reduce economic losses, surveillance and control of mycotoxins in food and feed has become a major objective for producers, regulatory authorities and researchers worldwide. However, the variety of chemical structures makes it impossible to use one single technique for mycotoxin analysis. Hence, a vast number of analytical methods has been developed and validated. The heterogeneity of food matrices combined with the demand for a fast, simultaneous and accurate determination of multiple mycotoxins creates enormous challenges for routine analysis. The most crucial issues will be discussed in this review. These are (1) the collection of representative samples, (2) the performance of classical and emerging analytical methods based on chromatographic or immunochemical techniques, (3) the validation of official methods for enforcement, and (4) the limitations and future prospects of the current methods.

  3. A Semi-Analytical Method for the PDFs of A Ship Rolling in Random Oblique Waves

    Science.gov (United States)

    Liu, Li-qin; Liu, Ya-liu; Xu, Wan-hai; Li, Yan; Tang, You-gang

    2018-03-01

    The PDFs (probability density functions) and probability of a ship rolling under the random parametric and forced excitations were studied by a semi-analytical method. The rolling motion equation of the ship in random oblique waves was established. The righting arm obtained by the numerical simulation was approximately fitted by an analytical function. The irregular waves were decomposed into two Gauss stationary random processes, and the CARMA (2, 1) model was used to fit the spectral density function of parametric and forced excitations. The stochastic energy envelope averaging method was used to solve the PDFs and the probability. The validity of the semi-analytical method was verified by the Monte Carlo method. The C11 ship was taken as an example, and the influences of the system parameters on the PDFs and probability were analyzed. The results show that the probability of ship rolling is affected by the characteristic wave height, wave length, and the heading angle. In order to provide proper advice for the ship's manoeuvring, the parametric excitations should be considered appropriately when the ship navigates in the oblique seas.

  4. Improvement of spatial discretization error on the semi-analytic nodal method using the scattered source subtraction method

    International Nuclear Information System (INIS)

    Yamamoto, Akio; Tatsumi, Masahiro

    2006-01-01

    In this paper, the scattered source subtraction (SSS) method is newly proposed to improve the spatial discretization error of the semi-analytic nodal method with the flat-source approximation. In the SSS method, the scattered source is subtracted from both side of the diffusion or the transport equation to make spatial variation of the source term to be small. The same neutron balance equation is still used in the SSS method. Since the SSS method just modifies coefficients of node coupling equations (those used in evaluation for the response of partial currents), its implementation is easy. Validity of the present method is verified through test calculations that are carried out in PWR multi-assemblies configurations. The calculation results show that the SSS method can significantly improve the spatial discretization error. Since the SSS method does not have any negative impact on execution time, convergence behavior and memory requirement, it will be useful to reduce the spatial discretization error of the semi-analytic nodal method with the flat-source approximation. (author)

  5. An Analytical Method of Auxiliary Sources Solution for Plane Wave Scattering by Impedance Cylinders

    DEFF Research Database (Denmark)

    Larsen, Niels Vesterdal; Breinbjerg, Olav

    2004-01-01

    Analytical Method of Auxiliary Sources solutions for plane wave scattering by circular impedance cylinders are derived by transformation of the exact eigenfunction series solutions employing the Hankel function wave transformation. The analytical Method of Auxiliary Sources solution thus obtained...

  6. An analytically based numerical method for computing view factors in real urban environments

    Science.gov (United States)

    Lee, Doo-Il; Woo, Ju-Wan; Lee, Sang-Hyun

    2018-01-01

    A view factor is an important morphological parameter used in parameterizing in-canyon radiative energy exchange process as well as in characterizing local climate over urban environments. For realistic representation of the in-canyon radiative processes, a complete set of view factors at the horizontal and vertical surfaces of urban facets is required. Various analytical and numerical methods have been suggested to determine the view factors for urban environments, but most of the methods provide only sky-view factor at the ground level of a specific location or assume simplified morphology of complex urban environments. In this study, a numerical method that can determine the sky-view factors ( ψ ga and ψ wa ) and wall-view factors ( ψ gw and ψ ww ) at the horizontal and vertical surfaces is presented for application to real urban morphology, which are derived from an analytical formulation of the view factor between two blackbody surfaces of arbitrary geometry. The established numerical method is validated against the analytical sky-view factor estimation for ideal street canyon geometries, showing a consolidate confidence in accuracy with errors of less than 0.2 %. Using a three-dimensional building database, the numerical method is also demonstrated to be applicable in determining the sky-view factors at the horizontal (roofs and roads) and vertical (walls) surfaces in real urban environments. The results suggest that the analytically based numerical method can be used for the radiative process parameterization of urban numerical models as well as for the characterization of local urban climate.

  7. Analytical methods and problems for the diamides type of extractants

    International Nuclear Information System (INIS)

    Cuillerdier, C.; Nigond, L.; Musikas, C.; Vitart, H.; Hoel, P.

    1989-01-01

    Diamides of carboxylic acids and especially malonamides are able to extract alpha emitters (including trivalent ions such as Am and Cm) contained in the wastes solutions of the nuclear industry. As they are completely incinerable and easy to purify, they could be an alternative to the mixture CMPO-TBP which is used in the TRUEX process. A large oxyalkyl radical enhances the distribution coefficients of americium in nitric acid sufficiently to permit the decontamination of wastes solutions in a classical mixers-settlers battery. Now researches are pursued with the aim of optimizing the formula of extractant, the influence of the structure of the extractant on its basicity and stability under radiolysis and hydrolysis is investigated. Analytical methods (potentiometry and NMR of C 13 ) have been developed for solvent titration and to evaluate the percentage of degradation and to identify some of the degradation products

  8. Analytical methods used in plutonium purification cycles by trilaurylamine

    International Nuclear Information System (INIS)

    Perez, J.J.

    1965-01-01

    The utilisation of trilaurylamine as a solvent extractant for the purification of plutonium has entailed to perfect a set of analytical methods which involves, various techniques. The organic impurities of the solvent can be titrated by gas-liquid chromatography. The titration of the main degradation product, the di-laurylamine, can be accomplished also by spectro-colorimetry. Potentiometry is used for the analysis of the different salts of amine-nitrate-sulfate-bisulfate as also the extracted nitric acid. The determination of the nitrate in aqueous phase is carried out by constant current potentiometry. The range of application, the accuracy and the procedure of these analysis are related in the present report. (author) [fr

  9. Nuclear analytical methods for trace element studies in calcified tissues

    International Nuclear Information System (INIS)

    Chaudhry, M.A.; Chaudhry, M.N.

    2001-01-01

    Full text: Various nuclear analytical methods have been developed and applied to determine the elemental composition of calcified tissues (teeth and bones). Fluorine was determined by prompt gamma activation analysis through the 19 F(p,ag) 16 O reaction. Carbon was measured by activation analysis with He-3 ions, and the technique of Proton-Induced X-ray Emission (PIXE) was applied to simultaneously determine Ca, P, and trace elements in well-documented teeth. Dental hard tissues, enamel, dentine, cement, and their junctions, as well as different parts of the same tissue, were examined separately. Furthermore, using a Proton Microprobe, we measured the surface distribution of F and other elements on and around carious lesions on the enamel. The depth profiles of F, and other elements, were also measured right up to the amelodentin junction

  10. Laser induced uranium fluorescence as an analytical method

    International Nuclear Information System (INIS)

    Krutman, I.

    1985-01-01

    A laser induced fluorescence system was developed to measure uranium trace level amounts in aqueous solution with reliable and simple materials and electronics. A nitrogen pulsed laser was built with the storage energy capacitor directly coupled to laser tube electrodes as a transmission line device. This laser operated at 3Hz repetition rate with peak intensity around 21 Kw and temporal width of 4.5 x 10 -9 s. A sample compartment made of rigid PVC and a photomultiplier housing of aluminium were constructed and assembled forming a single integrated device. As a result of this prototype system we made several analytical measurements with U dissolved in nitric acid to obtain a calibration curve. We obtained a straight line from a plot of U concentration versus fluorescence intensity fitted by a least square method that produced a regression coefficient of 0.994. The lower limit of U determination was 30 ppb -+ 3.5%. (Author) [pt

  11. Precision profiles and analytic reliability of radioimmunologic methods

    International Nuclear Information System (INIS)

    Yaneva, Z.; Popova, Yu.

    1991-01-01

    The aim of the present study is to investigate and compare some methods for creation of 'precision profiles' (PP) and to clarify their possibilities for determining the analytical reliability of RIA. Only methods without complicated mathematical calculations has been used. The reproducibility in serums with a concentration of the determinable hormone in the whole range of the calibration curve has been studied. The radioimmunoassay has been performed with TSH-RIA set (ex East Germany), and comparative evaluations - with commercial sets of HOECHST (Germany) and AMERSHAM (GB). Three methods for obtaining the relationship concentration (IU/l) -reproducibility (C.V.,%) are used and a comparison is made of their corresponding profiles: preliminary rough profile, Rodbard-PP and Ekins-PP. It is concluded that the creation of a precision profile is obligatory and the method of its construction does not influence the relationship's course. PP allows to determine concentration range giving stable results which improves the efficiency of the analitical work. 16 refs., 4 figs

  12. The Method of Manufactured Universes for validating uncertainty quantification methods

    KAUST Repository

    Stripling, H.F.

    2011-09-01

    The Method of Manufactured Universes is presented as a validation framework for uncertainty quantification (UQ) methodologies and as a tool for exploring the effects of statistical and modeling assumptions embedded in these methods. The framework calls for a manufactured reality from which experimental data are created (possibly with experimental error), an imperfect model (with uncertain inputs) from which simulation results are created (possibly with numerical error), the application of a system for quantifying uncertainties in model predictions, and an assessment of how accurately those uncertainties are quantified. The application presented in this paper manufactures a particle-transport universe, models it using diffusion theory with uncertain material parameters, and applies both Gaussian process and Bayesian MARS algorithms to make quantitative predictions about new experiments within the manufactured reality. The results of this preliminary study indicate that, even in a simple problem, the improper application of a specific UQ method or unrealized effects of a modeling assumption may produce inaccurate predictions. We conclude that the validation framework presented in this paper is a powerful and flexible tool for the investigation and understanding of UQ methodologies. © 2011 Elsevier Ltd. All rights reserved.

  13. Short-Term Predictive Validity of Cluster Analytic and Dimensional Classification of Child Behavioral Adjustment in School

    Science.gov (United States)

    Kim, Sangwon; Kamphaus, Randy W.; Baker, Jean A.

    2006-01-01

    A constructive debate over the classification of child psychopathology can be stimulated by investigating the validity of different classification approaches. We examined and compared the short-term predictive validity of cluster analytic and dimensional classifications of child behavioral adjustment in school using the Behavior Assessment System…

  14. Toward a Unified Validation Framework in Mixed Methods Research

    Science.gov (United States)

    Dellinger, Amy B.; Leech, Nancy L.

    2007-01-01

    The primary purpose of this article is to further discussions of validity in mixed methods research by introducing a validation framework to guide thinking about validity in this area. To justify the use of this framework, the authors discuss traditional terminology and validity criteria for quantitative and qualitative research, as well as…

  15. Ecological Vulnerability Assessment Based on Fuzzy Analytical Method and Analytic Hierarchy Process in Yellow River Delta.

    Science.gov (United States)

    Wu, Chunsheng; Liu, Gaohuan; Huang, Chong; Liu, Qingsheng; Guan, Xudong

    2018-04-25

    The Yellow River Delta (YRD), located in Yellow River estuary, is characterized by rich ecological system types, and provides habitats or migration stations for wild birds, all of which makes the delta an ecological barrier or ecotone for inland areas. Nevertheless, the abundant natural resources of YRD have brought huge challenges to the area, and frequent human activities and natural disasters have damaged the ecological systems seriously, and certain ecological functions have been threatened. Therefore, it is necessary to determine the status of the ecological environment based on scientific methods, which can provide scientifically robust data for the managers or stakeholders to adopt timely ecological protection measures. The aim of this study was to obtain the spatial distribution of the ecological vulnerability (EV) in YRD based on 21 indicators selected from underwater status, soil condition, land use, landform, vegetation cover, meteorological conditions, ocean influence, and social economy. In addition, the fuzzy analytic hierarchy process (FAHP) method was used to obtain the weights of the selected indicators, and a fuzzy logic model was constructed to obtain the result. The result showed that the spatial distribution of the EV grades was regular, while the fuzzy membership of EV decreased gradually from the coastline to inland area, especially around the river crossing, where it had the lowest EV. Along the coastline, the dikes had an obviously protective effect for the inner area, while the EV was higher in the area where no dikes were built. This result also showed that the soil condition and groundwater status were highly related to the EV spatially, with the correlation coefficients −0.55 and −0.74 respectively, and human activities had exerted considerable pressure on the ecological environment.

  16. An analytic solution of projectile motion with the quadratic resistance law using the homotopy analysis method

    International Nuclear Information System (INIS)

    Yabushita, Kazuki; Yamashita, Mariko; Tsuboi, Kazuhiro

    2007-01-01

    We consider the problem of two-dimensional projectile motion in which the resistance acting on an object moving in air is proportional to the square of the velocity of the object (quadratic resistance law). It is well known that the quadratic resistance law is valid in the range of the Reynolds number: 1 x 10 3 ∼ 2 x 10 5 (for instance, a sphere) for practical situations, such as throwing a ball. It has been considered that the equations of motion of this case are unsolvable for a general projectile angle, although some solutions have been obtained for a small projectile angle using perturbation techniques. To obtain a general analytic solution, we apply Liao's homotopy analysis method to this problem. The homotopy analysis method, which is different from a perturbation technique, can be applied to a problem which does not include small parameters. We apply the homotopy analysis method for not only governing differential equations, but also an algebraic equation of a velocity vector to extend the radius of convergence. Ultimately, we obtain the analytic solution to this problem and investigate the validation of the solution

  17. CT hepatic perfusion measurement: Comparison of three analytic methods

    International Nuclear Information System (INIS)

    Kanda, Tomonori; Yoshikawa, Takeshi; Ohno, Yoshiharu; Kanata, Naoki; Koyama, Hisanobu; Takenaka, Daisuke; Sugimura, Kazuro

    2012-01-01

    Objectives: To compare the efficacy of three analytic methods, maximum slope (MS), dual-input single-compartment model (CM) and deconvolution (DC), for CT measurements of hepatic perfusion and assess the effects of extra-hepatic systemic factors. Materials and methods: Eighty-eight patients who were suspected of having metastatic liver tumors underwent hepatic CT perfusion. The scans were performed at the hepatic hilum 7–77 s after administration of contrast material. Hepatic arterial and portal perfusions (HAP and HPP, ml/min/100 ml) and arterial perfusion fraction (APF, %) were calculated with the three methods, followed by correlation assessment. Partial correlation analysis was used to assess the effects on hepatic perfusion values by various factors such as age, sex, risk of cardiovascular diseases, arrival time of contrast material at abdominal aorta, transit time from abdominal aorta to hepatic parenchyma, and liver dysfunction. Results: Mean HAP of MS was significantly higher than DC. HPP of CM was significantly higher than MS and CM, and HPP of MS was significantly higher than DC. There was no significant difference in APF. HAP and APF showed significant and moderate correlations among the methods. HPP showed significant and moderate correlations between CM and DC, and poor correlation between MS and CM or DC. All methods showed weak correlations between HAP or APF and age or sex. Finally, MS showed weak correlations between HAP or HPP and arrival time or cardiovascular risks. Conclusions: Hepatic perfusion values arrived at with the three methods are not interchangeable. CM and DC are less susceptible to extra-hepatic systemic factors

  18. Validación de métodos analíticos para los estudios de estabilidad del naproxeno en supositorios para uso infantil y adulto Validation of analytical methods for the stability studies of naproxen suppositories for infant and adult use

    Directory of Open Access Journals (Sweden)

    Yaslenis Rodríguez Hernández

    2011-12-01

    Full Text Available En el presente trabajo se realizaron los estudios analíticos y de validación para su aplicación en los estudios de estabilidad de las futuras formulaciones de supositorios de naproxeno para uso infantil y adulto. Se determinaron los factores que más influyeron en la estabilidad del naproxeno; la mayor degradación ocurrió en el medio ácido, oxidante y por acción de la luz. Se evaluó un método por cromatografía líquida de alta resolución, el cual mostró adecuado desempeño para cuantificar naproxeno en supositorios y fue selectivo frente a los productos de degradación. Se obtuvo un límite de cuantificación de 3,480 µg, por lo que fue válido para la realización de dichos estudios. Adicionalmente, se evaluaron los parámetros especificidad para estabilidad, límites de detección y de cuantificación para el método por volumetría ácido-base semiacuosa directa validado anteriormente para control de calidad, lo cual mostró resultados satisfactorios. No obstante, los métodos volumétricos no se consideran indicadores de estabilidad, por lo que este método será utilizado conjuntamente con los métodos cromatográficos de elección para determinar productos de degradación: cromatografía de capa delgada y cromatografía líquida de alta resolución.Analytical and validating studies were performed in this paper, with a view to using them in the stability studies of the future formulations of naproxen suppositories for children and adults. The most influential factors in the naproxen stability were determined, that is, the major degradation occurred in acid medium, oxidative medium and by light action. One high-performance liquid chromatography-based method was evaluated, which proved to be adequate to quantify naproxen in suppositories and was selective against degradation products. The quantification limit was 3,480 µg, so it was valid for these studies. Additionally, the parameters specificity for stability, detection and

  19. Analytical methods associated with the recovery of uranium

    International Nuclear Information System (INIS)

    Dixon, K.

    1983-01-01

    This report summarizes various approaches made to the analysis of materials arising from the processing of Karoo deposits for uranium. These materials include head and residue samples, aqueous solutions and organic solvents and, finally, the precipitated cakes of the elements recovered, i.e. uranium, molybdenum, and arsenic. Analysis was required for these elements and also vanadium, carbon, sulphur, and carbonate in the head and residue samples. The concentration of uranium, molybdenum, and arsenic, other than in the precipitated cakes, ranges from 1 to 2000μg/g, and that of carbon, sulphur, and carbonate from 0,1 to 5 per cent. The analysis of cakes necessitates the determination of silver, arsenic, iron, copper, calcium, magnesium, manganese, molybdenum, lead, tin, titanium, and vanadium within the range 1 to 1000μg/g, and of sodium and silica within the range 10 to 20 000μg/g. The methods used include combustion methods for carbon, sulphur, and carbonate, and atomic-absorption, X-ray-fluorescence, and emission methods for the other analytes. The accuracy of the analysis is within 10 per cent

  20. SU-E-J-145: Validation of An Analytical Model for in Vivo Range Verification Using GATE Monte Carlo Simulation in Proton Therapy

    International Nuclear Information System (INIS)

    Lee, C; Lin, H; Chao, T; Hsiao, I; Chuang, K

    2015-01-01

    Purpose: Predicted PET images on the basis of analytical filtering approach for proton range verification has been successful developed and validated using FLUKA Monte Carlo (MC) codes and phantom measurements. The purpose of the study is to validate the effectiveness of analytical filtering model for proton range verification on GATE/GEANT4 Monte Carlo simulation codes. Methods: In this study, we performed two experiments for validation of predicted β+-isotope by the analytical model with GATE/GEANT4 simulations. The first experiments to evaluate the accuracy of predicting β+-yields as a function of irradiated proton energies. In second experiment, we simulate homogeneous phantoms of different materials irradiated by a mono-energetic pencil-like proton beam. The results of filtered β+-yields distributions by the analytical model is compared with those of MC simulated β+-yields in proximal and distal fall-off ranges. Results: The results investigate the distribution between filtered β+-yields and MC simulated β+-yields distribution in different conditions. First, we found that the analytical filtering can be applied over the whole range of the therapeutic energies. Second, the range difference between filtered β+-yields and MC simulated β+-yields at the distal fall-off region are within 1.5mm for all materials used. The findings validated the usefulness of analytical filtering model on range verification of proton therapy on GATE Monte Carlo simulations. In addition, there is a larger discrepancy between filtered prediction and MC simulated β+-yields using GATE code, especially in proximal region. This discrepancy might Result from the absence of wellestablished theoretical models for predicting the nuclear interactions. Conclusion: Despite the fact that large discrepancies of the distributions between MC-simulated and predicted β+-yields were observed, the study prove the effectiveness of analytical filtering model for proton range verification using

  1. FDIR Strategy Validation with the B Method

    Science.gov (United States)

    Sabatier, D.; Dellandrea, B.; Chemouil, D.

    2008-08-01

    In a formation flying satellite system, the FDIR strategy (Failure Detection, Isolation and Recovery) is paramount. When a failure occurs, satellites should be able to take appropriate reconfiguration actions to obtain the best possible results given the failure, ranging from avoiding satellite-to-satellite collision to continuing the mission without disturbance if possible. To achieve this goal, each satellite in the formation has an implemented FDIR strategy that governs how it detects failures (from tests or by deduction) and how it reacts (reconfiguration using redundant equipments, avoidance manoeuvres, etc.). The goal is to protect the satellites first and the mission as much as possible. In a project initiated by the CNES, ClearSy experiments the B Method to validate the FDIR strategies developed by Thales Alenia Space, of the inter satellite positioning and communication devices that will be used for the SIMBOL-X (2 satellite configuration) and the PEGASE (3 satellite configuration) missions and potentially for other missions afterward. These radio frequency metrology sensor devices provide satellite positioning and inter satellite communication in formation flying. This article presents the results of this experience.

  2. Validation of the ultraviolet spectrophotometry method for the quality control of ciprofloxacin chlorhydrate in Ciprecu tablets

    International Nuclear Information System (INIS)

    Perez Navarro, Maikel; Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania

    2014-01-01

    Quinolones are a group of antimicrobials of high clinical significance. Ciprofloxacin hydrochloride monohydrate is a second-generation antibacterial fluoroquinolone for treatment of several infections and is marketed as eye drops, injections, capsule and tablets. To develop and to validate an ultraviolet spectrophotometric analytical method to be used in the quality control of ciprofloxacin hydrochloride monohydrate in newly manufactured Ciprecu tablets

  3. Groundwater Seepage Estimation into Amirkabir Tunnel Using Analytical Methods and DEM and SGR Method

    OpenAIRE

    Hadi Farhadian; Homayoon Katibeh

    2015-01-01

    In this paper, groundwater seepage into Amirkabir tunnel has been estimated using analytical and numerical methods for 14 different sections of the tunnel. Site Groundwater Rating (SGR) method also has been performed for qualitative and quantitative classification of the tunnel sections. The obtained results of above mentioned methods were compared together. The study shows reasonable accordance with results of the all methods unless for two sections of tunnel. In these t...

  4. Analytical resource assessment method for continuous (unconventional) oil and gas accumulations - The "ACCESS" Method

    Science.gov (United States)

    Crovelli, Robert A.; revised by Charpentier, Ronald R.

    2012-01-01

    The U.S. Geological Survey (USGS) periodically assesses petroleum resources of areas within the United States and the world. The purpose of this report is to explain the development of an analytic probabilistic method and spreadsheet software system called Analytic Cell-Based Continuous Energy Spreadsheet System (ACCESS). The ACCESS method is based upon mathematical equations derived from probability theory. The ACCESS spreadsheet can be used to calculate estimates of the undeveloped oil, gas, and NGL (natural gas liquids) resources in a continuous-type assessment unit. An assessment unit is a mappable volume of rock in a total petroleum system. In this report, the geologic assessment model is defined first, the analytic probabilistic method is described second, and the spreadsheet ACCESS is described third. In this revised version of Open-File Report 00-044 , the text has been updated to reflect modifications that were made to the ACCESS program. Two versions of the program are added as appendixes.

  5. A Multi-Projector Calibration Method for Virtual Reality Simulators with Analytically Defined Screens

    Directory of Open Access Journals (Sweden)

    Cristina Portalés

    2017-06-01

    Full Text Available The geometric calibration of projectors is a demanding task, particularly for the industry of virtual reality simulators. Different methods have been developed during the last decades to retrieve the intrinsic and extrinsic parameters of projectors, most of them being based on planar homographies and some requiring an extended calibration process. The aim of our research work is to design a fast and user-friendly method to provide multi-projector calibration on analytically defined screens, where a sample is shown for a virtual reality Formula 1 simulator that has a cylindrical screen. The proposed method results from the combination of surveying, photogrammetry and image processing approaches, and has been designed by considering the spatial restrictions of virtual reality simulators. The method has been validated from a mathematical point of view, and the complete system—which is currently installed in a shopping mall in Spain—has been tested by different users.

  6. Application of analytical target cascading method in multidisciplinary design optimization of ship conceptual design

    Directory of Open Access Journals (Sweden)

    WANG Jian

    2017-10-01

    Full Text Available [Objectives] Ship conceptual design requires the coordination of many different disciplines for comprehensive optimization, which presents a complicated system design problem affecting several fields of technology. However, the development of overall ship design is relatively slow compared with other subjects. [Methods] The decomposition and coordination strategy of ship design is presented, and the analytical target cascading (ATC method is applied to the multidisciplinary design optimization of the conceptual design phase of ships on this basis. A tank ship example covering the 5 disciplines of buoyancy and stability, rapidity, maneuverability, capacity and economy is established to illustrate the analysis process in the present study. [Results] The results demonstrate the stability, convergence and validity of the ATC method in dealing with the complex coupling effect occurring in ship conceptual design.[Conclusions] The proposed method provides an effective basis for optimization of ship conceptual design.

  7. Modern analytic methods applied to the art and archaeology

    International Nuclear Information System (INIS)

    Tenorio C, M. D.; Longoria G, L. C.

    2010-01-01

    The interaction of diverse areas as the analytic chemistry, the history of the art and the archaeology has allowed the development of a variety of techniques used in archaeology, in conservation and restoration. These methods have been used to date objects, to determine the origin of the old materials and to reconstruct their use and to identify the degradation processes that affect the integrity of the art works. The objective of this chapter is to offer a general vision on the researches that have been realized in the Instituto Nacional de Investigaciones Nucleares (ININ) in the field of cultural goods. A series of researches carried out in collaboration with national investigators and of the foreigner is described shortly, as well as with the great support of degree students and master in archaeology of the National School of Anthropology and History, since one of the goals that have is to diffuse the knowledge of the existence of these techniques among the young archaeologists, so that they have a wider vision of what they could use in an in mediate future and they can check hypothesis with scientific methods. (Author)

  8. Analytic-numerical method of determining the freezing front location

    Directory of Open Access Journals (Sweden)

    R. Grzymkowski

    2011-07-01

    Full Text Available Mathematical modeling of thermal processes combined with the reversible phase transitions of type: solid phase – liquid phase leads to formulation of the parabolic boundary problems with the moving boundary. Solution of such defined problem requires, most often, to use sophisticated numerical techniques and far advanced mathematical tools. Excellent illustration of the complexity of considered problems, as well as of the variety of approaches used for finding their solutions, gives the papers [1-4]. In the current paper, the authors present the, especially attractive from the engineer point of view, analytic-numerical method for finding the approximate solution of selected class of problems which can be reduced to the one-phase solidification problem of a plate with the unknown a priori, varying in time boundary of the region in which the solution is sought. Proposed method is based on the known formalism of initial expansion of the sought function describing the temperature field into the power series, some coefficients of which are determined with the aid of boundary conditions, and on the approximation of the function defining the location of freezing front with the broken line, parameters of which are numerically determined.

  9. Analytical method for determining the channel-temperature distribution

    International Nuclear Information System (INIS)

    Kurbatov, I.M.

    1992-01-01

    The distribution of the predicted temperature over the volume or cross section of the active zone is important for thermal calculations of reactors taking into account random deviations. This requires a laborious calculation which includes the following steps: separation of the nominal temperature field, within the temperature range, into intervals, in each of which the temperature is set equal to its average value in the interval; determination of the number of channels whose temperature falls within each interval; construction of the channel-temperature distribution in each interval in accordance with the weighted error function; and summation of the number of channels with the same temperature over all intervals. This procedure can be greatly simplified with the help of methods which eliminate numerous variant calculations when the nominal temperature field is open-quotes refinedclose quotes up to the optimal field according to different criteria. In the present paper a universal analytical method is proposed for determining, by changing the coefficients in the channel-temperature distribution function, the form of this function that reflects all conditions of operation of the elements in the active zone. The problem is solved for the temperature of the coolant at the outlet from the reactor channels

  10. Measurement of company effectiveness using analytic network process method

    Directory of Open Access Journals (Sweden)

    Goran Janjić

    2017-07-01

    Full Text Available The sustainable development of an organisation is monitored through the organisation’s performance, which beforehand incorporates all stakeholders’ requirements in its strategy. The strategic management concept enables organisations to monitor and evaluate their effectiveness along with efficiency by monitoring of the implementation of set strategic goals. In the process of monitoring and measuring effectiveness, an organisation can use multiple-criteria decision-making methods as help. This study uses the method of analytic network process (ANP to define the weight factors of the mutual influences of all the important elements of an organisation’s strategy. The calculation of an organisation’s effectiveness is based on the weight factors and the degree of fulfilment of the goal values of the strategic map measures. New business conditions influence the changes in the importance of certain elements of an organisation’s business in relation to competitive advantage on the market, and on the market, increasing emphasis is given to non-material resources in the process of selection of the organisation’s most important measures.

  11. Measurement of company effectiveness using analytic network process method

    Science.gov (United States)

    Goran, Janjić; Zorana, Tanasić; Borut, Kosec

    2017-07-01

    The sustainable development of an organisation is monitored through the organisation's performance, which beforehand incorporates all stakeholders' requirements in its strategy. The strategic management concept enables organisations to monitor and evaluate their effectiveness along with efficiency by monitoring of the implementation of set strategic goals. In the process of monitoring and measuring effectiveness, an organisation can use multiple-criteria decision-making methods as help. This study uses the method of analytic network process (ANP) to define the weight factors of the mutual influences of all the important elements of an organisation's strategy. The calculation of an organisation's effectiveness is based on the weight factors and the degree of fulfilment of the goal values of the strategic map measures. New business conditions influence the changes in the importance of certain elements of an organisation's business in relation to competitive advantage on the market, and on the market, increasing emphasis is given to non-material resources in the process of selection of the organisation's most important measures.

  12. Analytical methods for study of transmission line lightning protection

    International Nuclear Information System (INIS)

    Pettersson, Per.

    1993-04-01

    Transmission line lightning performance is studied by analytical methods. The elements of shielding failure flashovers and back-flashovers are analysed as functions of incidence, response and insulation. Closed-form approximate expressions are sought to enhance understanding of the phenomena. Probabilistic and wave propagation aspects are particularly studied. The electrogeometric model of lightning attraction to structures is used in combination with the log-normal probability distribution of lightning to ground currents. The log-normality is found to be retained for the currents collected by mast-type as well as line-type structures, but with a change of scale. For both types, exceedingly simple formulas for the number of hits are derived. Simple closed-form expressions for the line outage rates from back- flashovers and shielding failure flashovers are derived in a uniform way as functions of the critical currents. The expressions involve the standardized normal distribution function. System response is analysed by use of Laplace transforms in combination with text-book transmission-line theory. Inversion into time domain is accomplished by an approximate asymptotic method producing closed-form results. The back-flashover problem is analysed in particular. Approximate, image type expressions are derived for shunt admittance of wires above, on and under ground for analyses of fast transients. The derivation parallels that for series impedance, now well-known. 3 refs, 5 figs

  13. Dosimetric validation of the anisotropic analytical algorithm for photon dose calculation: fundamental characterization in water

    International Nuclear Information System (INIS)

    Fogliata, Antonella; Nicolini, Giorgia; Vanetti, Eugenio; Clivio, Alessandro; Cozzi, Luca

    2006-01-01

    In July 2005 a new algorithm was released by Varian Medical Systems for the Eclipse planning system and installed in our institute. It is the anisotropic analytical algorithm (AAA) for photon dose calculations, a convolution/superposition model for the first time implemented in a Varian planning system. It was therefore necessary to perform validation studies at different levels with a wide investigation approach. To validate the basic performances of the AAA, a detailed analysis of data computed by the AAA configuration algorithm was carried out and data were compared against measurements. To better appraise the performance of AAA and the capability of its configuration to tailor machine-specific characteristics, data obtained from the pencil beam convolution (PBC) algorithm implemented in Eclipse were also added in the comparison. Since the purpose of the paper is to address the basic performances of the AAA and of its configuration procedures, only data relative to measurements in water will be reported. Validation was carried out for three beams: 6 MV and 15 MV from a Clinac 2100C/D and 6 MV from a Clinac 6EX. Generally AAA calculations reproduced very well measured data, and small deviations were observed, on average, for all the quantities investigated for open and wedged fields. In particular, percentage depth-dose curves showed on average differences between calculation and measurement smaller than 1% or 1 mm, and computed profiles in the flattened region matched measurements with deviations smaller than 1% for all beams, field sizes, depths and wedges. Percentage differences in output factors were observed as small as 1% on average (with a range smaller than ±2%) for all conditions. Additional tests were carried out for enhanced dynamic wedges with results comparable to previous results. The basic dosimetric validation of the AAA was therefore considered satisfactory

  14. Analytical validation and reference intervals for freezing point depression osmometer measurements of urine osmolality in dogs.

    Science.gov (United States)

    Guerrero, Samantha; Pastor, Josep; Tvarijonaviciute, Asta; Cerón, José Joaquín; Balestra, Graziano; Caldin, Marco

    2017-11-01

    Urine osmolality (UOsm) is considered the most accurate measure of urine concentration and is used to assess body fluid homeostasis and renal function. We performed analytical validation of freezing point depression measurement of canine UOsm, to establish reference intervals (RIs) and to determine the effect of age, sex, and reproductive status on UOsm in dogs. Clinically healthy dogs ( n = 1,991) were retrospectively selected and stratified in groups by age (young [0-12 mo], adults [13-84 mo], and seniors [>84 mo]), sex (females and males), and reproductive status (intact and neutered). RIs were calculated for each age group. Intra- and inter-assay coefficients of variation were dogs, and 366-2,178 mOsm/kg in seniors. Senior dogs had a significantly lower UOsm than young and adult dogs ( p dogs ( p dogs.

  15. Analytical Performance Modeling and Validation of Intel’s Xeon Phi Architecture

    Energy Technology Data Exchange (ETDEWEB)

    Chunduri, Sudheer; Balaprakash, Prasanna; Morozov, Vitali; Vishwanath, Venkatram; Kumaran, Kalyan

    2017-01-01

    Modeling the performance of scientific applications on emerging hardware plays a central role in achieving extreme-scale computing goals. Analytical models that capture the interaction between applications and hardware characteristics are attractive because even a reasonably accurate model can be useful for performance tuning before the hardware is made available. In this paper, we develop a hardware model for Intel’s second-generation Xeon Phi architecture code-named Knights Landing (KNL) for the SKOPE framework. We validate the KNL hardware model by projecting the performance of mini-benchmarks and application kernels. The results show that our KNL model can project the performance with prediction errors of 10% to 20%. The hardware model also provides informative recommendations for code transformations and tuning.

  16. Development of analytical methods for iodine speciation in fresh water

    International Nuclear Information System (INIS)

    Takaku, Yuichi; Ohtsuka, Yoshihito; Hisamatsu, Shun'ichi

    2007-01-01

    Analytical methods for physicochemical speciation of iodine in fresh water samples were developed to elucidate its behavior in the environment. The methods combined inductively coupled plasma mass spectrometry (ICP-MS) with size exclusion high performance liquid chromatography (SEC) or capillary electrophoresis (CE). Freshwater samples were collected from Lake Towada and rivers surrounding the lake. After filtration through a 0.45 μm pore size membrane filter, iodine in the water samples was pre-concentrated with an ultra-filtration filter which had a cut-off size of 10 kDa. The fraction with molecular size over 10 kDa was concentrated to 100 times in the original water, and then introduced into the SEC-ICP-MS. Molecular size chromatograms of all river and lake water samples showed two peaks for iodine concentrations: 40 kDa and 20 kDa. The method for separately determining two valence states of inorganic iodine, I - and IO 3 - , was also developed using the CE-ICP-MS system and it was successfully applied to the fresh water samples. Analysis results of surface water samples in Lake Towada and rivers surrounding the lake indicated that the chemical form of inorganic iodine in all samples was IO 3 - . Additional lake water samples were collected from Lake O-ike-higashi in the Juni-ko area at Shirakami-Sanchi, which is a UNESCO natural world heritage. The lake has a strong thermocline during all seasons; its bottom layer is in a highly reductive state. Depth profiles of I - and IO 3 - clearly showed that I - was not detected in the surface layer, but it was predominant in the bottom layer, and vice versa for IO 3 - . As this separation method is rapid and sensitive, it will be widely used in the future. (author)

  17. Migração de β-caprolactama de embalagens contendo poliamida 6 para simulante ácido acético 3% e validação do método analítico β-Caprolactam migration from polyamide 6 packaging into 3% acetic acid food simulant and validation of the analytical method

    Directory of Open Access Journals (Sweden)

    Juliana Silva Félix

    2007-08-01

    Full Text Available Este trabalho teve como objetivo desenvolver e validar método analítico para determinar ε-caprolactama no simulante de alimentos solução de ácido acético 3% e estudar sua migração de embalagens contendo poliamida 6 para o simulante em contato. Foi empregada a cromatografia gasosa usando ε-caprolactama como padrão analítico e 2-azociclononanona como padrão interno. A linearidade esteve entre 1,60 e 640,00 µg de ε-caprolactama.mL-1 de simulante, com coeficiente de correlação 0,9999. Os limites de detecção e de quantificação do método foram 0,24 e 1,60 ng, respectivamente. A precisão do método revelou valores de coeficiente de variação menores que 4,3% e a avaliação da exatidão mostrou recuperação de 100 a 106%. O método demonstrou ser eficaz para quantificar ε-caprolactama no simulante, apresentando ampla linearidade, boa precisão e exatidão. No ensaio de migração, embalagens contendo poliamida 6 foram colocadas em tubos de vidro com 10 mL do simulante, que foram hermeticamente fechados e acondicionados a 40 ± 1 °C durante 10 dias. O ensaio de migração foi realizado por imersão total. A quantidade de ε-caprolactama migrada variou de 7,8 a 10,5 e de 6,9 a 7,6 mg.kg-1 de simulante para as embalagens destinadas aos produtos cárneos e queijos, respectivamente. Todas as embalagens atenderam às exigências da Legislação Brasileira para migração de ε-caprolactama.The aim of this work was to develop and validate an analytical method to determine ε-caprolactam in 3% acetic acid solution and to study its migration from polyamide 6 into food simulant. Gas chromatography was used with ε-caprolactam as an analytical standard and 2-azacyclononanone as an internal standard. The linearity was obtained by the concentration range of 1.60 to 640.00 µg.mL-1, with a correlation coefficient of 0.9999. Detection and quantification limits of the method were 0.24 ng and 1.60 ng, respectively. Relative standard

  18. A Validated Analytical Model for Availability Prediction of IPTV Services in VANETs

    Directory of Open Access Journals (Sweden)

    Bernd E. Wolfinger

    2014-12-01

    Full Text Available In vehicular ad hoc networks (VANETs, besides the original applications typically related to traffic safety, we nowadays can observe an increasing trend toward infotainment applications, such as IPTV services. Quality of experience (QoE, as observed by the end users of IPTV, is highly important to guarantee adequate user acceptance for the service. In IPTV, QoE is mainly determined by the availability of TV channels for the users. This paper presents an efficient and rather generally applicable analytical model that allows one to predict the blocking probability of TV channels, both for channel-switching-induced, as well as for handover-induced blocking events. We present the successful validation of the model by means of simulation, and we introduce a new measure for QoE. Numerous case studies illustrate how the analytical model and our new QoE measure can be applied successfully for the dimensioning of IPTV systems, taking into account the QoE requirements of the IPTV service users in strongly diverse traffic scenarios.

  19. Analytical one parameter method for PID motion controller settings

    NARCIS (Netherlands)

    van Dijk, Johannes; Aarts, Ronald G.K.M.

    2012-01-01

    In this paper analytical expressions for PID-controllers settings for electromechanical motion systems are presented. It will be shown that by an adequate frequency domain oriented parametrization, the parameters of a PID-controller are analytically dependent on one variable only, the cross-over

  20. Analytical Validation of a Portable Mass Spectrometer Featuring Interchangeable, Ambient Ionization Sources for High Throughput Forensic Evidence Screening.

    Science.gov (United States)

    Lawton, Zachary E; Traub, Angelica; Fatigante, William L; Mancias, Jose; O'Leary, Adam E; Hall, Seth E; Wieland, Jamie R; Oberacher, Herbert; Gizzi, Michael C; Mulligan, Christopher C

    2017-06-01

    Forensic evidentiary backlogs are indicative of the growing need for cost-effective, high-throughput instrumental methods. One such emerging technology that shows high promise in meeting this demand while also allowing on-site forensic investigation is portable mass spectrometric (MS) instrumentation, particularly that which enables the coupling to ambient ionization techniques. While the benefits of rapid, on-site screening of contraband can be anticipated, the inherent legal implications of field-collected data necessitates that the analytical performance of technology employed be commensurate with accepted techniques. To this end, comprehensive analytical validation studies are required before broad incorporation by forensic practitioners can be considered, and are the focus of this work. Pertinent performance characteristics such as throughput, selectivity, accuracy/precision, method robustness, and ruggedness have been investigated. Reliability in the form of false positive/negative response rates is also assessed, examining the effect of variables such as user training and experience level. To provide flexibility toward broad chemical evidence analysis, a suite of rapidly-interchangeable ion sources has been developed and characterized through the analysis of common illicit chemicals and emerging threats like substituted phenethylamines. Graphical Abstract ᅟ.

  1. Analytical Validation of a Portable Mass Spectrometer Featuring Interchangeable, Ambient Ionization Sources for High Throughput Forensic Evidence Screening

    Science.gov (United States)

    Lawton, Zachary E.; Traub, Angelica; Fatigante, William L.; Mancias, Jose; O'Leary, Adam E.; Hall, Seth E.; Wieland, Jamie R.; Oberacher, Herbert; Gizzi, Michael C.; Mulligan, Christopher C.

    2017-06-01

    Forensic evidentiary backlogs are indicative of the growing need for cost-effective, high-throughput instrumental methods. One such emerging technology that shows high promise in meeting this demand while also allowing on-site forensic investigation is portable mass spectrometric (MS) instrumentation, particularly that which enables the coupling to ambient ionization techniques. While the benefits of rapid, on-site screening of contraband can be anticipated, the inherent legal implications of field-collected data necessitates that the analytical performance of technology employed be commensurate with accepted techniques. To this end, comprehensive analytical validation studies are required before broad incorporation by forensic practitioners can be considered, and are the focus of this work. Pertinent performance characteristics such as throughput, selectivity, accuracy/precision, method robustness, and ruggedness have been investigated. Reliability in the form of false positive/negative response rates is also assessed, examining the effect of variables such as user training and experience level. To provide flexibility toward broad chemical evidence analysis, a suite of rapidly-interchangeable ion sources has been developed and characterized through the analysis of common illicit chemicals and emerging threats like substituted phenethylamines. [Figure not available: see fulltext.

  2. Propulsion and launching analysis of variable-mass rockets by analytical methods

    OpenAIRE

    D.D. Ganji; M. Gorji; M. Hatami; A. Hasanpour; N. Khademzadeh

    2013-01-01

    In this study, applications of some analytical methods on nonlinear equation of the launching of a rocket with variable mass are investigated. Differential transformation method (DTM), homotopy perturbation method (HPM) and least square method (LSM) were applied and their results are compared with numerical solution. An excellent agreement with analytical methods and numerical ones is observed in the results and this reveals that analytical methods are effective and convenient. Also a paramet...

  3. The analytic regularization ζ function method and the cut-off method in Casimir effect

    International Nuclear Information System (INIS)

    Svaiter, N.F.; Svaiter, B.F.

    1990-01-01

    The zero point energy associated to a hermitian massless scalar field in the presence of perfectly reflecting plates in a three dimensional flat space-time is discussed. A new technique to unify two different methods - the ζ function and a variant of the cut-off method - used to obtain the so called Casimir energy is presented, and the proof of the analytic equivalence between both methods is given. (author)

  4. Development and Validation of a Dissolution Test Method for ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a dissolution test method for dissolution release of artemether and lumefantrine from tablets. Methods: A single dissolution method for evaluating the in vitro release of artemether and lumefantrine from tablets was developed and validated. The method comprised of a dissolution medium of ...

  5. Desenvolvimento e validação de método analítico para nistatina creme vaginal por cromatografia líquida de alta eficiência Development and validation of an analytical method for Nystatin vaginal cream by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Zênia Maria Maciel Lavra

    2008-12-01

    1.0 mL/minute and wavelength of 305 nm. The validated method showed to be accurate, precise, robust, linear and specific, in addition to being fast and practical, able to be used for analytic dosing of nystatin vaginal cream.

  6. Validación del método analítico para el control de la calidad y el estudio de estabilidad del neolimpilen Validation of the analytical method for the quality control and the stability study of neolimpilem

    Directory of Open Access Journals (Sweden)

    Caridad M García Peña

    2004-08-01

    significativas. El método resultó específico, lineal, preciso y exacto.The analytical method developed for the quality control and for the stability study in the quantification of hydroxypropylmethylcellulose and sodium laurisulfate was validated by spectrophotometry with ultraviolet detection at 635 and 650 nm, respectively. Besides, the analytical results of the stability study conducted in the solution for cleaning and conservating rigid contact lens (neolimpilen are presented. Three batches packed in two different flasks were used to carry out the study by accelerated stability and shelf life in order to prove the phsyical and chemical stability of the solution at room temperature for 24 months. In the validation of hydroxypropylmethylcellulose, teh calibration curve in the range from 0.06 to 0.l8 mg/mL showed a lineal behavior with a correlation coefficient equal to 0.99581. The statistical test for the interval and the slope was not significant. A recovery of 99.8 % was obtained in the studied concentration range and Cochran (G and Student's (t tests were not indicative. The variation coefficient in the repeatabililty was 0.9 % for 10 tested replicas,. whereas Fischer and Student's tests were not significant in the reproducibility. The method proved to be specific, lineal, precise and exact. In the validation of sodium laurisulfate the calibration curve in the range 1.44 -3.0 mg/mL behaved in a lineal way with a correlation coefficient equal to 0.99036. The statistical test for the interval and the slope was not signficant. A recovery of 99.9% was attained in the studied concentration range and Cochran (G and Student's (t tests were not significant. The method proved to be specific, lineal, precise and exact.

  7. Analytical methods for waste minimisation in the convenience food industry.

    Science.gov (United States)

    Darlington, R; Staikos, T; Rahimifard, S

    2009-04-01

    Waste creation in some sectors of the food industry is substantial, and while much of the used material is non-hazardous and biodegradable, it is often poorly dealt with and simply sent to landfill mixed with other types of waste. In this context, overproduction wastes were found in a number of cases to account for 20-40% of the material wastes generated by convenience food manufacturers (such as ready-meals and sandwiches), often simply just to meet the challenging demands placed on the manufacturer due to the short order reaction time provided by the supermarkets. Identifying specific classes of waste helps to minimise their creation, through consideration of what the materials constitute and why they were generated. This paper aims to provide means by which food industry wastes can be identified, and demonstrate these mechanisms through a practical example. The research reported in this paper investigated the various categories of waste and generated three analytical methods for the support of waste minimisation activities by food manufacturers. The waste classifications and analyses are intended to complement existing waste minimisation approaches and are described through consideration of a case study convenience food manufacturer that realised significant financial savings through waste measurement, analysis and reduction.

  8. NIOSH Manual of Analytical Methods (third edition). Fourth supplement

    Energy Technology Data Exchange (ETDEWEB)

    1990-08-15

    The NIOSH Manual of Analytical Methods, 3rd edition, was updated for the following chemicals: allyl-glycidyl-ether, 2-aminopyridine, aspartame, bromine, chlorine, n-butylamine, n-butyl-glycidyl-ether, carbon-dioxide, carbon-monoxide, chlorinated-camphene, chloroacetaldehyde, p-chlorophenol, crotonaldehyde, 1,1-dimethylhydrazine, dinitro-o-cresol, ethyl-acetate, ethyl-formate, ethylenimine, sodium-fluoride, hydrogen-fluoride, cryolite, sodium-hexafluoroaluminate, formic-acid, hexachlorobutadiene, hydrogen-cyanide, hydrogen-sulfide, isopropyl-acetate, isopropyl-ether, isopropyl-glycidyl-ether, lead, lead-oxide, maleic-anhydride, methyl-acetate, methyl-acrylate, methyl-tert-butyl ether, methyl-cellosolve-acetate, methylcyclohexanol, 4,4'-methylenedianiline, monomethylaniline, monomethylhydrazine, nitric-oxide, p-nitroaniline, phenyl-ether, phenyl-ether-biphenyl mixture, phenyl-glycidyl-ether, phenylhydrazine, phosphine, ronnel, sulfuryl-fluoride, talc, tributyl-phosphate, 1,1,2-trichloro-1,2,2-trifluoroethane, trimellitic-anhydride, triorthocresyl-phosphate, triphenyl-phosphate, and vinyl-acetate.

  9. An analytical method for optimal design of MR valve structures

    International Nuclear Information System (INIS)

    Nguyen, Q H; Choi, S B; Lee, Y S; Han, M S

    2009-01-01

    This paper proposes an analytical methodology for the optimal design of a magnetorheological (MR) valve structure. The MR valve structure is constrained in a specific volume and the optimization problem identifies geometric dimensions of the valve structure that maximize the yield stress pressure drop of a MR valve or the yield stress damping force of a MR damper. In this paper, the single-coil and two-coil annular MR valve structures are considered. After describing the schematic configuration and operating principle of a typical MR valve and damper, a quasi-static model is derived based on the Bingham model of a MR fluid. The magnetic circuit of the valve and damper is then analyzed by applying Kirchoff's law and the magnetic flux conservation rule. Based on quasi-static modeling and magnetic circuit analysis, the optimization problem of the MR valve and damper is built. In order to reduce the computation load, the optimization problem is simplified and a procedure to obtain the optimal solution of the simplified optimization problem is presented. The optimal solution of the simplified optimization problem of the MR valve structure constrained in a specific volume is then obtained and compared with the solution of the original optimization problem and the optimal solution obtained from the finite element method

  10. AN ANALYTICAL METHOD FOR CHEMICAL SPECIATION OF SELENIUM IN SOIL

    Directory of Open Access Journals (Sweden)

    Constantin Luca

    2010-10-01

    Full Text Available Selenium is an essential microelement, sometimes redoubtable, through its beneficial role - risk depending on its concentration in the food chain, at low dose is an important nutrient in the life of humans and animals, contrary at high doses, it becomes toxic. Selenium may be find itself in the environment (soil, sediment, water in many forms (oxidized, reduced, organometallic which determine their mobility and toxicity. Determination of chemical speciation (identification of different chemical forms provides much more complete information for a better understanding of the behavior and the potential impact on the environment. In this work we present the results of methodological research on the extraction of sequential forms of selenium in the soil and the coupling of analytical methods capable of identifying very small amounts of selenium in soils An efficient scheme of sequential extractions forms of selenium (SES consisting in atomic absorption spectrometry coupled with hydride generation (HGAAS has been developed into five experimental steps, detailed in the paper. This operational scheme has been applied to the analysis of chemical speciation in the following areas: the Bărăgan Plain and Central Dobrogea of Romania.

  11. Validating and Determining the Weight of Items Used for Evaluating Clinical Governance Implementation Based on Analytic Hierarchy Process Model

    Directory of Open Access Journals (Sweden)

    Elaheh Hooshmand

    2015-10-01

    Full Text Available Background The purpose of implementing a system such as Clinical Governance (CG is to integrate, establish and globalize distinct policies in order to improve quality through increasing professional knowledge and the accountability of healthcare professional toward providing clinical excellence. Since CG is related to change, and change requires money and time, CG implementation has to be focused on priority areas that are in more dire need of change. The purpose of the present study was to validate and determine the significance of items used for evaluating CG implementation. Methods The present study was descriptive-quantitative in method and design. Items used for evaluating CG implementation were first validated by the Delphi method and then compared with one another and ranked based on the Analytical Hierarchy Process (AHP model. Results The items that were validated for evaluating CG implementation in Iran include performance evaluation, training and development, personnel motivation, clinical audit, clinical effectiveness, risk management, resource allocation, policies and strategies, external audit, information system management, research and development, CG structure, implementation prerequisites, the management of patients’ non-medical needs, complaints and patients’ participation in the treatment process. The most important items based on their degree of significance were training and development, performance evaluation, and risk management. The least important items included the management of patients’ non-medical needs, patients’ participation in the treatment process and research and development. Conclusion The fundamental requirements of CG implementation included having an effective policy at national level, avoiding perfectionism, using the expertise and potentials of the entire country and the coordination of this model with other models of quality improvement such as accreditation and patient safety.

  12. Estimating Fuel Cycle Externalities: Analytical Methods and Issues, Report 2

    Energy Technology Data Exchange (ETDEWEB)

    Barnthouse, L.W.; Cada, G.F.; Cheng, M.-D.; Easterly, C.E.; Kroodsma, R.L.; Lee, R.; Shriner, D.S.; Tolbert, V.R.; Turner, R.S.

    1994-07-01

    of complex issues that also have not been fully addressed. This document contains two types of papers that seek to fill part of this void. Some of the papers describe analytical methods that can be applied to one of the five steps of the damage function approach. The other papers discuss some of the complex issues that arise in trying to estimate externalities. This report, the second in a series of eight reports, is part of a joint study by the U.S. Department of Energy (DOE) and the Commission of the European Communities (EC)* on the externalities of fuel cycles. Most of the papers in this report were originally written as working papers during the initial phases of this study. The papers provide descriptions of the (non-radiological) atmospheric dispersion modeling that the study uses; reviews much of the relevant literature on ecological and health effects, and on the economic valuation of those impacts; contains several papers on some of the more complex and contentious issues in estimating externalities; and describes a method for depicting the quality of scientific information that a study uses. The analytical methods and issues that this report discusses generally pertain to more than one of the fuel cycles, though not necessarily to all of them. The report is divided into six parts, each one focusing on a different subject area.

  13. Fuel Cycle Externalities: Analytical Methods and Issues, Report 2

    International Nuclear Information System (INIS)

    Barnthouse, L.W.; Cada, G.F.; Cheng, M.-D.; Easterly, C.E.; Kroodsma, R.L.; Lee, R.; Shriner, D.S.; Tolbert, V.R.; Turner, R.S.

    1994-01-01

    that also have not been fully addressed. This document contains two types of papers that seek to fill part of this void. Some of the papers describe analytical methods that can be applied to one of the five steps of the damage function approach. The other papers discuss some of the complex issues that arise in trying to estimate externalities. This report, the second in a series of eight reports, is part of a joint study by the U.S. Department of Energy (DOE) and the Commission of the European Communities (EC)* on the externalities of fuel cycles. Most of the papers in this report were originally written as working papers during the initial phases of this study. The papers provide descriptions of the (non-radiological) atmospheric dispersion modeling that the study uses; reviews much of the relevant literature on ecological and health effects, and on the economic valuation of those impacts; contains several papers on some of the more complex and contentious issues in estimating externalities; and describes a method for depicting the quality of scientific information that a study uses. The analytical methods and issues that this report discusses generally pertain to more than one of the fuel cycles, though not necessarily to all of them. The report is divided into six parts, each one focusing on a different subject area

  14. Method validation for chemical composition determination by electron microprobe with wavelength dispersive spectrometer

    Science.gov (United States)

    Herrera-Basurto, R.; Mercader-Trejo, F.; Muñoz-Madrigal, N.; Juárez-García, J. M.; Rodriguez-López, A.; Manzano-Ramírez, A.

    2016-07-01

    The main goal of method validation is to demonstrate that the method is suitable for its intended purpose. One of the advantages of analytical method validation is translated into a level of confidence about the measurement results reported to satisfy a specific objective. Elemental composition determination by wavelength dispersive spectrometer (WDS) microanalysis has been used over extremely wide areas, mainly in the field of materials science, impurity determinations in geological, biological and food samples. However, little information is reported about the validation of the applied methods. Herein, results of the in-house method validation for elemental composition determination by WDS are shown. SRM 482, a binary alloy Cu-Au of different compositions, was used during the validation protocol following the recommendations for method validation proposed by Eurachem. This paper can be taken as a reference for the evaluation of the validation parameters more frequently requested to get the accreditation under the requirements of the ISO/IEC 17025 standard: selectivity, limit of detection, linear interval, sensitivity, precision, trueness and uncertainty. A model for uncertainty estimation was proposed including systematic and random errors. In addition, parameters evaluated during the validation process were also considered as part of the uncertainty model.

  15. Evaluation of FTIR-based analytical methods for the analysis of simulated wastes

    International Nuclear Information System (INIS)

    Rebagay, T.V.; Cash, R.J.; Dodd, D.A.; Lockrem, L.L.; Meacham, J.E.; Winkelman, W.D.

    1994-01-01

    Three FTIR-based analytical methods that have potential to characterize simulated waste tank materials have been evaluated. These include: (1) fiber optics, (2) modular transfer optic using light guides equipped with non-contact sampling peripherals, and (3) photoacoustic spectroscopy. Pertinent instrumentation and experimental procedures for each method are described. The results show that the near-infrared (NIR) region of the infrared spectrum is the region of choice for the measurement of moisture in waste simulants. Differentiation of the NIR spectrum, as a preprocessing steps, will improve the analytical result. Preliminary data indicate that prominent combination bands of water and the first overtone band of the ferrocyanide stretching vibration may be utilized to measure water and ferrocyanide species simultaneously. Both near-infrared and mid-infrared spectra must be collected, however, to measure ferrocyanide species unambiguously and accurately. For ease of sample handling and the potential for field or waste tank deployment, the FTIR-Fiber Optic method is preferred over the other two methods. Modular transfer optic using light guides and photoacoustic spectroscopy may be used as backup systems and for the validation of the fiber optic data

  16. An analytical method for the calculation of static characteristics of linear step motors for control rod drives in nuclear reactors

    International Nuclear Information System (INIS)

    Khan, S.H.; Ivanov, A.A.

    1995-01-01

    An analytical method for calculating static characteristics of linear dc step motors (LSM) is described. These multiphase passive-armature motors are now being developed for control rod drives (CRD) in large nuclear reactors. The static characteristics of such LSM is defined by the variation of electromagnetic force with armature displacement and it determines motor performance in its standing and dynamic modes of operation. The proposed analytical technique for calculating this characteristic is based on the permeance analysis method applied to phase magnetic circuits of LSM. Reluctances of various parts of phase magnetic circuit is calculated analytically by assuming probable flux paths and by taking into account complex nature of magnetic field distribution in it. For given armature positions stator and armature iron saturations are taken into account by an efficient iterative algorithm which gives fast convergence. The method is validated by comparing theoretical results with experimental ones which shows satisfactory agreement for small stator currents and weak iron saturation

  17. Studies on analytical method and nondestructive measuring method on the sensitization of austenitic stainless steels

    International Nuclear Information System (INIS)

    Onimura, Kichiro; Arioka, Koji; Horai, Manabu; Noguchi, Shigeru.

    1982-03-01

    Austenitic stainless steels are widely used as structural materials for the machine and equipment of various kinds of plants, such as thermal power, nuclear power, and chemical plants. The machines and equipment using this kind of material, however, have the possibility of suffering corrosion damage while in service, and these damages are considered to be largely due to the sensitization of the material in sometimes. So, it is necessary to develop an analytical method for grasping the sensitization of the material more in detail and a quantitative nondestructive measuring method which is applicable to various kinds of structures in order to prevent the corrosion damage. From the above viewpoint, studies have been made on the analytical method based on the theory of diffusion of chromium in austenitic stainless steels and on Electro-Potentiokinetics Reactivation Method (EPR Method) as a nondestructive measuring method, using 304 and 316 austenitic stainless steels having different carbon contents in base metals. This paper introduces the results of EPR test on the sensitization of austenitic stainless steels and the correlation between analytical and experimental results. (author)

  18. The Value of Qualitative Methods in Social Validity Research

    Science.gov (United States)

    Leko, Melinda M.

    2014-01-01

    One quality indicator of intervention research is the extent to which the intervention has a high degree of social validity, or practicality. In this study, I drew on Wolf's framework for social validity and used qualitative methods to ascertain five middle schoolteachers' perceptions of the social validity of System 44®--a phonics-based reading…

  19. Analytic Validation of Immunohistochemistry Assays: New Benchmark Data From a Survey of 1085 Laboratories.

    Science.gov (United States)

    Stuart, Lauren N; Volmar, Keith E; Nowak, Jan A; Fatheree, Lisa A; Souers, Rhona J; Fitzgibbons, Patrick L; Goldsmith, Jeffrey D; Astles, J Rex; Nakhleh, Raouf E

    2017-09-01

    - A cooperative agreement between the College of American Pathologists (CAP) and the United States Centers for Disease Control and Prevention was undertaken to measure laboratories' awareness and implementation of an evidence-based laboratory practice guideline (LPG) on immunohistochemical (IHC) validation practices published in 2014. - To establish new benchmark data on IHC laboratory practices. - A 2015 survey on IHC assay validation practices was sent to laboratories subscribed to specific CAP proficiency testing programs and to additional nonsubscribing laboratories that perform IHC testing. Specific questions were designed to capture laboratory practices not addressed in a 2010 survey. - The analysis was based on responses from 1085 laboratories that perform IHC staining. Ninety-six percent (809 of 844) always documented validation of IHC assays. Sixty percent (648 of 1078) had separate procedures for predictive and nonpredictive markers, 42.7% (220 of 515) had procedures for laboratory-developed tests, 50% (349 of 697) had procedures for testing cytologic specimens, and 46.2% (363 of 785) had procedures for testing decalcified specimens. Minimum case numbers were specified by 85.9% (720 of 838) of laboratories for nonpredictive markers and 76% (584 of 768) for predictive markers. Median concordance requirements were 95% for both types. For initial validation, 75.4% (538 of 714) of laboratories adopted the 20-case minimum for nonpredictive markers and 45.9% (266 of 579) adopted the 40-case minimum for predictive markers as outlined in the 2014 LPG. The most common method for validation was correlation with morphology and expected results. Laboratories also reported which assay changes necessitated revalidation and their minimum case requirements. - Benchmark data on current IHC validation practices and procedures may help laboratories understand the issues and influence further refinement of LPG recommendations.

  20. Analytical method of waste allocation in waste management systems: Concept, method and case study

    International Nuclear Information System (INIS)

    Bergeron, Francis C.

    2017-01-01

    Waste is not a rejected item to dispose anymore but increasingly a secondary resource to exploit, influencing waste allocation among treatment operations in a waste management (WM) system. The aim of this methodological paper is to present a new method for the assessment of the WM system, the “analytical method of the waste allocation process” (AMWAP), based on the concept of the “waste allocation process” defined as the aggregation of all processes of apportioning waste among alternative waste treatment operations inside or outside the spatial borders of a WM system. AMWAP contains a conceptual framework and an analytical approach. The conceptual framework includes, firstly, a descriptive model that focuses on the description and classification of the WM system. It includes, secondly, an explanatory model that serves to explain and to predict the operation of the WM system. The analytical approach consists of a step-by-step analysis for the empirical implementation of the conceptual framework. With its multiple purposes, AMWAP provides an innovative and objective modular method to analyse a WM system which may be integrated in the framework of impact assessment methods and environmental systems analysis tools. Its originality comes from the interdisciplinary analysis of the WAP and to develop the conceptual framework. AMWAP is applied in the framework of an illustrative case study on the household WM system of Geneva (Switzerland). It demonstrates that this method provides an in-depth and contextual knowledge of WM. - Highlights: • The study presents a new analytical method based on the waste allocation process. • The method provides an in-depth and contextual knowledge of the waste management system. • The paper provides a reproducible procedure for professionals, experts and academics. • It may be integrated into impact assessment or environmental system analysis tools. • An illustrative case study is provided based on household waste

  1. Analytical method of waste allocation in waste management systems: Concept, method and case study

    Energy Technology Data Exchange (ETDEWEB)

    Bergeron, Francis C., E-mail: francis.b.c@videotron.ca

    2017-01-15

    Waste is not a rejected item to dispose anymore but increasingly a secondary resource to exploit, influencing waste allocation among treatment operations in a waste management (WM) system. The aim of this methodological paper is to present a new method for the assessment of the WM system, the “analytical method of the waste allocation process” (AMWAP), based on the concept of the “waste allocation process” defined as the aggregation of all processes of apportioning waste among alternative waste treatment operations inside or outside the spatial borders of a WM system. AMWAP contains a conceptual framework and an analytical approach. The conceptual framework includes, firstly, a descriptive model that focuses on the description and classification of the WM system. It includes, secondly, an explanatory model that serves to explain and to predict the operation of the WM system. The analytical approach consists of a step-by-step analysis for the empirical implementation of the conceptual framework. With its multiple purposes, AMWAP provides an innovative and objective modular method to analyse a WM system which may be integrated in the framework of impact assessment methods and environmental systems analysis tools. Its originality comes from the interdisciplinary analysis of the WAP and to develop the conceptual framework. AMWAP is applied in the framework of an illustrative case study on the household WM system of Geneva (Switzerland). It demonstrates that this method provides an in-depth and contextual knowledge of WM. - Highlights: • The study presents a new analytical method based on the waste allocation process. • The method provides an in-depth and contextual knowledge of the waste management system. • The paper provides a reproducible procedure for professionals, experts and academics. • It may be integrated into impact assessment or environmental system analysis tools. • An illustrative case study is provided based on household waste

  2. Analytical method of polychlorinated biphenyls(PCBs) in transformer oil

    Energy Technology Data Exchange (ETDEWEB)

    Shin, S.K. [National Institute of Environmental Research, Incheon (Korea); Kim, H.J.; Chung, D.; Kim, K.S.; Kim, J.K.; Chung, Y.H.; Chung, I.R.

    2004-09-15

    Polychlorinated biphenyls (PCBs) is a chlorinated biphenyl compound with the general formula C{sub 12}H{sub 10-n}/Cl{sub n}. PCBs generally occur as mixtures, where n can vary from 1 to 10. The 10 sites available for possible chlorine substitution result in 209 possible PCB congeners. There is now considerable concern regarding; the presence of PCB congeners in insulating oils used within large-scale electrical supply systems. Due to its outstanding chemical and thermal stabilities and electrical insulation properties, the commercial and industrial products of polychlorinated biphenyls (PCBs), such as Aroclors, Kaneclors, Clophens, Phenaclors etc., had been widely used as thermal oil and transformer oil from 1930s until the 1970s. PCBs from a group of persistent organic pollutants of the environment, especially dangerous to living organisms due to high toxicity, persistency, and bio-concentration in adipose tissue. Despite of this fact, PCB-contaminated oils are still commonly encountered partly because PCBs used as dielectric liquids in transformer and condenser. The source of PCBs in environments can range from used transformer oils or dielectric liquids to liquid wastes, and some PCBs contamination is occurred due to the re-use of incompletely reconditioned oil. The current action plan of Republic of Korea dictates that organizations with electrical equipment contaminated with more than 2 mg/L PCBs will need to treat as PCBs-containing wastes, and 50mg/L of PCBs or PCBs equivalent to be treated as a pure PCB preparation. In this study, transformer oils analyzed based on guideline for PCBs analytical method of transformer oil in Korea.

  3. Transport methods: general. 1. The Analytical Monte Carlo Method for Radiation Transport Calculations

    International Nuclear Information System (INIS)

    Martin, William R.; Brown, Forrest B.

    2001-01-01

    We present an alternative Monte Carlo method for solving the coupled equations of radiation transport and material energy. This method is based on incorporating the analytical solution to the material energy equation directly into the Monte Carlo simulation for the radiation intensity. This method, which we call the Analytical Monte Carlo (AMC) method, differs from the well known Implicit Monte Carlo (IMC) method of Fleck and Cummings because there is no discretization of the material energy equation since it is solved as a by-product of the Monte Carlo simulation of the transport equation. Our method also differs from the method recently proposed by Ahrens and Larsen since they use Monte Carlo to solve both equations, while we are solving only the radiation transport equation with Monte Carlo, albeit with effective sources and cross sections to represent the emission sources. Our method bears some similarity to a method developed and implemented by Carter and Forest nearly three decades ago, but there are substantive differences. We have implemented our method in a simple zero-dimensional Monte Carlo code to test the feasibility of the method, and the preliminary results are very promising, justifying further extension to more realistic geometries. (authors)

  4. Evaluation and selection of energy technologies using an integrated graph theory and analytic hierarchy process methods

    Directory of Open Access Journals (Sweden)

    P. B. Lanjewar

    2016-06-01

    Full Text Available The evaluation and selection of energy technologies involve a large number of attributes whose selection and weighting is decided in accordance with the social, environmental, technical and economic framework. In the present work an integrated multiple attribute decision making methodology is developed by combining graph theory and analytic hierarchy process methods to deal with the evaluation and selection of energy technologies. The energy technology selection attributes digraph enables a quick visual appraisal of the energy technology selection attributes and their interrelationships. The preference index provides a total objective score for comparison of energy technologies alternatives. Application of matrix permanent offers a better appreciation of the considered attributes and helps to analyze the different alternatives from combinatorial viewpoint. The AHP is used to assign relative weights to the attributes. Four examples of evaluation and selection of energy technologies are considered in order to demonstrate and validate the proposed method.

  5. Analytical Validation of the ReEBOV Antigen Rapid Test for Point-of-Care Diagnosis of Ebola Virus Infection

    Science.gov (United States)

    Cross, Robert W.; Boisen, Matthew L.; Millett, Molly M.; Nelson, Diana S.; Oottamasathien, Darin; Hartnett, Jessica N.; Jones, Abigal B.; Goba, Augustine; Momoh, Mambu; Fullah, Mohamed; Bornholdt, Zachary A.; Fusco, Marnie L.; Abelson, Dafna M.; Oda, Shunichiro; Brown, Bethany L.; Pham, Ha; Rowland, Megan M.; Agans, Krystle N.; Geisbert, Joan B.; Heinrich, Megan L.; Kulakosky, Peter C.; Shaffer, Jeffrey G.; Schieffelin, John S.; Kargbo, Brima; Gbetuwa, Momoh; Gevao, Sahr M.; Wilson, Russell B.; Saphire, Erica Ollmann; Pitts, Kelly R.; Khan, Sheik Humarr; Grant, Donald S.; Geisbert, Thomas W.; Branco, Luis M.; Garry, Robert F.

    2016-01-01

    Background. Ebola virus disease (EVD) is a severe viral illness caused by Ebola virus (EBOV). The 2013–2016 EVD outbreak in West Africa is the largest recorded, with >11 000 deaths. Development of the ReEBOV Antigen Rapid Test (ReEBOV RDT) was expedited to provide a point-of-care test for suspected EVD cases. Methods. Recombinant EBOV viral protein 40 antigen was used to derive polyclonal antibodies for RDT and enzyme-linked immunosorbent assay development. ReEBOV RDT limits of detection (LOD), specificity, and interference were analytically validated on the basis of Food and Drug Administration (FDA) guidance. Results. The ReEBOV RDT specificity estimate was 95% for donor serum panels and 97% for donor whole-blood specimens. The RDT demonstrated sensitivity to 3 species of Ebolavirus (Zaire ebolavirus, Sudan ebolavirus, and Bundibugyo ebolavirus) associated with human disease, with no cross-reactivity by pathogens associated with non-EBOV febrile illness, including malaria parasites. Interference testing exhibited no reactivity by medications in common use. The LOD for antigen was 4.7 ng/test in serum and 9.4 ng/test in whole blood. Quantitative reverse transcription–polymerase chain reaction testing of nonhuman primate samples determined the range to be equivalent to 3.0 × 105–9.0 × 108 genomes/mL. Conclusions. The analytical validation presented here contributed to the ReEBOV RDT being the first antigen-based assay to receive FDA and World Health Organization emergency use authorization for this EVD outbreak, in February 2015. PMID:27587634

  6. A Newly Improved Modified Method Development and Validation of Bromofenac Sodium Sesquihydrate in Bulk Drug Manufacturing

    OpenAIRE

    Sunil Kumar Yelamanchi V; Useni Reddy Mallu; I. V Kasi Viswanath; D. Balasubramanyam; G. Narshima Murthy

    2016-01-01

    The main objective of this study was to develop a simple, efficient, specific, precise and accurate newly improved modified Reverse Phase High Performance Liquid Chromatographic Purity (or) Related substance method for bromofenac sodium sesquihydrate active pharmaceuticals ingredient dosage form. Validation of analytical method is the confirmation by examination and the provision of objective evidence that the particular requirements for a specific intended use are fulfilled as per ICH, USP...

  7. Analytical support of plant specific SAMG development validation of SAMG using MELCOR 1.8.5

    International Nuclear Information System (INIS)

    Duspiva, Jiri

    2006-01-01

    They are two NPPs in operation in Czech Republic. Both of NPPs operated in CR have already implemented EOPs, developed under collaboration with the WESE. The project on SAMG development has started and follows the previous one for EOPs also with the WESE as the leading organization. Plant specific SAMGs for the Temelin as well as Dukovany NPPs are based on the WOG generic SAMGs. The analytical support of plant specific SAMGs development is performed by the NRI Rez within the validation process. Basic conditions as well as their filling by NRI Rez are focused on analyst, analytical tools and their applications. More detail description is attended to the approach of the preparation of the MELCOR code application to the evaluation of hydrogen risk, validation of recent set of hydrogen passive autocatalytic recombiners and definition of proposals to amend system of hydrogen removal. Such kind of parametric calculations will request to perform very wide set of runs. It could not be possible with the whole plant model and decoupling of such calculation with storing of mass and energy sources into the containment is only one way. The example of this decoupling for the LOCA scenario is shown. It includes seven sources - heat losses from primary and secondary circuits, fluid blowndown through cold leg break, fission products blowndown through cold leg break, fluid blowndown through break in reactor pressure vessel bottom head, fission products through break in reactor pressure vessel bottom head, melt ejection from reactor pressure vessel to cavity and gas masses and heat losses from corium in cavity. The stand alone containment analysis was tested in two configurations - with or without taking of fission products into account. Testing showed very good agreement of all calculations until lower head failure and acceptable agreement after that. Also some problematic features appeared. The stand alone test with fission product was possible only after the changes in source code

  8. Validating and determining the weight of items used for evaluating clinical governance implementation based on analytic hierarchy process model.

    Science.gov (United States)

    Hooshmand, Elaheh; Tourani, Sogand; Ravaghi, Hamid; Vafaee Najar, Ali; Meraji, Marziye; Ebrahimipour, Hossein

    2015-04-08

    The purpose of implementing a system such as Clinical Governance (CG) is to integrate, establish and globalize distinct policies in order to improve quality through increasing professional knowledge and the accountability of healthcare professional toward providing clinical excellence. Since CG is related to change, and change requires money and time, CG implementation has to be focused on priority areas that are in more dire need of change. The purpose of the present study was to validate and determine the significance of items used for evaluating CG implementation. The present study was descriptive-quantitative in method and design. Items used for evaluating CG implementation were first validated by the Delphi method and then compared with one another and ranked based on the Analytical Hierarchy Process (AHP) model. The items that were validated for evaluating CG implementation in Iran include performance evaluation, training and development, personnel motivation, clinical audit, clinical effectiveness, risk management, resource allocation, policies and strategies, external audit, information system management, research and development, CG structure, implementation prerequisites, the management of patients' non-medical needs, complaints and patients' participation in the treatment process. The most important items based on their degree of significance were training and development, performance evaluation, and risk management. The least important items included the management of patients' non-medical needs, patients' participation in the treatment process and research and development. The fundamental requirements of CG implementation included having an effective policy at national level, avoiding perfectionism, using the expertise and potentials of the entire country and the coordination of this model with other models of quality improvement such as accreditation and patient safety. © 2015 by Kerman University of Medical Sciences.

  9. A Comparison of Two Approaches for the Ruggedness Testing of an Analytical Method

    International Nuclear Information System (INIS)

    Maestroni, Britt

    2016-01-01

    As part of an initiative under the “Red Analitica de Latino America y el Caribe” (RALACA) network the FAO/IAEA Food and Environmental Protection Laboratory validated a multi-residue method for pesticides in potato. One of the parameters to be assessed was the intra laboratory robustness or ruggedness. The objective of this work was to implement a worked example for RALACA laboratories to test for the robustness (ruggedness) of an analytical method. As a conclusion to this study, it is evident that there is a need for harmonization of the definition of the terms robustness/ruggedness, the limits, the methodology and the statistical treatment of the generated data. A worked example for RALACA laboratories to test for the robustness (ruggedness) of an analytical method will soon be posted on the RALACA website (www.red-ralaca.net). This study was carried out with collaborators from LVA (Austria), University of Antwerp (Belgium), University of Leuwen (The Netherlands), Universidad de la Republica (Uruguay) and Agilent technologies.

  10. The combination of four analytical methods to explore skeletal muscle metabolomics: Better coverage of metabolic pathways or a marketing argument?

    Science.gov (United States)

    Bruno, C; Patin, F; Bocca, C; Nadal-Desbarats, L; Bonnier, F; Reynier, P; Emond, P; Vourc'h, P; Joseph-Delafont, K; Corcia, P; Andres, C R; Blasco, H

    2018-01-30

    Metabolomics is an emerging science based on diverse high throughput methods that are rapidly evolving to improve metabolic coverage of biological fluids and tissues. Technical progress has led researchers to combine several analytical methods without reporting the impact on metabolic coverage of such a strategy. The objective of our study was to develop and validate several analytical techniques (mass spectrometry coupled to gas or liquid chromatography and nuclear magnetic resonance) for the metabolomic analysis of small muscle samples and evaluate the impact of combining methods for more exhaustive metabolite covering. We evaluated the muscle metabolome from the same pool of mouse muscle samples after 2 metabolite extraction protocols. Four analytical methods were used: targeted flow injection analysis coupled with mass spectrometry (FIA-MS/MS), gas chromatography coupled with mass spectrometry (GC-MS), liquid chromatography coupled with high-resolution mass spectrometry (LC-HRMS), and nuclear magnetic resonance (NMR) analysis. We evaluated the global variability of each compound i.e., analytical (from quality controls) and extraction variability (from muscle extracts). We determined the best extraction method and we reported the common and distinct metabolites identified based on the number and identity of the compounds detected with low analytical variability (variation coefficient<30%) for each method. Finally, we assessed the coverage of muscle metabolic pathways obtained. Methanol/chloroform/water and water/methanol were the best extraction solvent for muscle metabolome analysis by NMR and MS, respectively. We identified 38 metabolites by nuclear magnetic resonance, 37 by FIA-MS/MS, 18 by GC-MS, and 80 by LC-HRMS. The combination led us to identify a total of 132 metabolites with low variability partitioned into 58 metabolic pathways, such as amino acid, nitrogen, purine, and pyrimidine metabolism, and the citric acid cycle. This combination also showed

  11. Analytical method by high resolution liquid chromatography for the determination of carbamazepine in human plasma

    International Nuclear Information System (INIS)

    Jimenez Aleman, Narda M; Calero Carbonell, Jorge E; Padron Yaquis, Alejandro S; Izquierdo Lozano, Julio C

    2007-01-01

    One of the requirements to develop the studies of bioavailability and bioequivalence is to have analytic methodologies validated for the work with samples in biological fluids. A method was developed by high resolution liquid chromatography for the determination of carbamazepine in human plasma. A mixture of hydrogen phosphate of sodium: acetonitrile (65:35) adjusted to pH= 3.3 with phosphoric acid, flow of 1.2 mL/min and ultraviolet detection at 210 nm, was used as mobile phase. Propylparabene was used as an internal standard. According to the established regulations for the validation of the methods in biological fluids, the following parameters were studied: stability of the samples, lineality, specificity, precision, accuracy and limit of detection and quantification. The method proved to be specific and sensitive with a detection and quantification limit of 0.9 and 1.0 ng, respectively. The method was lineal, precise and exact in the range of concentrations of 1. 07 at 12.67 μg/mL. The mean recovery was not statistically different from 100.0 %. The analito in the proposed biological matrix remained in the studied period. The methodology described in this work is applied in our case to the study that evaluates the bioavailability and bioequivalence of a Cuban formulation of carbamazepine in healthy volunteers. (Author)

  12. Application of analytical quality by design principles for the determination of alkyl p-toluenesulfonates impurities in Aprepitant by HPLC. Validation using total-error concept.

    Science.gov (United States)

    Zacharis, Constantinos K; Vastardi, Elli

    2018-02-20

    In the research presented we report the development of a simple and robust liquid chromatographic method for the quantification of two genotoxic alkyl sulphonate impurities (namely methyl p-toluenesulfonate and isopropyl p-toluenesulfonate) in Aprepitant API substances using the Analytical Quality by Design (AQbD) approach. Following the steps of AQbD protocol, the selected critical method attributes (CMAs) were the separation criterions between the critical peak pairs, the analysis time and the peak efficiencies of the analytes. The critical method parameters (CMPs) included the flow rate, the gradient slope and the acetonitrile content at the first step of the gradient elution program. Multivariate experimental designs namely Plackett-Burman and Box-Behnken designs were conducted sequentially for factor screening and optimization of the method parameters. The optimal separation conditions were estimated using the desirability function. The method was fully validated in the range of 10-200% of the target concentration limit of the analytes using the "total error" approach. Accuracy profiles - a graphical decision making tool - were constructed using the results of the validation procedures. The β-expectation tolerance intervals did not exceed the acceptance criteria of±10%, meaning that 95% of future results will be included in the defined bias limits. The relative bias ranged between - 1.3-3.8% for both analytes, while the RSD values for repeatability and intermediate precision were less than 1.9% in all cases. The achieved limit of detection (LOD) and the limit of quantification (LOQ) were adequate for the specific purpose and found to be 0.02% (corresponding to 48μgg -1 in sample) for both methyl and isopropyl p-toluenesulfonate. As proof-of-concept, the validated method was successfully applied in the analysis of several Aprepitant batches indicating that this methodology could be used for routine quality control analyses. Copyright © 2017 Elsevier B

  13. Validation of a new analytical procedure for determination of residual solvents in [18F]FDG by gas chromatography

    International Nuclear Information System (INIS)

    Costa, Flávia M.; Costa, Cassiano L.S.; Silva, Juliana B.; Ferreira, Soraya M.Z.M.D.

    2017-01-01

    Fludeoxyglucose F 18 ([ 18 F]FDG) is the most used radiopharmaceutical for positron emission tomography, especially on oncology. Organic solvents such as ether, ethanol and acetonitrile might be used in the synthesis of [ 18 F]FDG; however, they might not be completely removed during purification steps. The determination of residual solvents in [ 18 F]FDG is required in the European Pharmacopoeia (EP) and the United States Pharmacopeia (USP) monographs. While the procedure described in the EP is quite general, the one described in the USP requires a long runtime (about 13 minutes). In this work a simple and fast (4-minute) analytical procedure was developed and validated for determination of residual solvents in [ 18 F]FDG. Analyses were carried out in a Perkin Elmer gas chromatograph equipped with a flame ionization detector. The separation was obtained on a 0.53-mm x 30 m fused-silica column. Validation included the evaluation of various parameters, such as: specificity, linearity and range, limits of detection and quantitation, precision (repeatability and intermediate precision), accuracy, and robustness. Results were found to be within acceptable limits, indicating the developed procedure is suitable for its intended application. Considering the short half-life of fluorine-18 (109.7 minutes), this new method could be a valuable alternative for routine quality control of [ 18 F]FDG. (author)

  14. Validation of a new analytical procedure for determination of residual solvents in [{sup 18}F]FDG by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Flávia M.; Costa, Cassiano L.S.; Silva, Juliana B.; Ferreira, Soraya M.Z.M.D., E-mail: flaviabiomedica@yahoo.com.br [Centro de Desenvolvimento da Tecnologia Nuclear (UPPR/CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Unidade de Pesquisa e Produção de Radiofármacos

    2017-07-01

    Fludeoxyglucose F 18 ([{sup 18}F]FDG) is the most used radiopharmaceutical for positron emission tomography, especially on oncology. Organic solvents such as ether, ethanol and acetonitrile might be used in the synthesis of [{sup 18}F]FDG; however, they might not be completely removed during purification steps. The determination of residual solvents in [{sup 18}F]FDG is required in the European Pharmacopoeia (EP) and the United States Pharmacopeia (USP) monographs. While the procedure described in the EP is quite general, the one described in the USP requires a long runtime (about 13 minutes). In this work a simple and fast (4-minute) analytical procedure was developed and validated for determination of residual solvents in [{sup 18}F]FDG. Analyses were carried out in a Perkin Elmer gas chromatograph equipped with a flame ionization detector. The separation was obtained on a 0.53-mm x 30 m fused-silica column. Validation included the evaluation of various parameters, such as: specificity, linearity and range, limits of detection and quantitation, precision (repeatability and intermediate precision), accuracy, and robustness. Results were found to be within acceptable limits, indicating the developed procedure is suitable for its intended application. Considering the short half-life of fluorine-18 (109.7 minutes), this new method could be a valuable alternative for routine quality control of [{sup 18}F]FDG. (author)

  15. A chromatographic method validation to quantify tablets Mephenesine of national production

    International Nuclear Information System (INIS)

    Suarez Perez, Yania; Izquierdo Castro, Adalberto; Milian Sanchez, Jana Daria

    2009-01-01

    Authors made validation of an analytical method by high performance liquid chromatography (HPLC) for quantification of Mephenesine in recently reformulated 500 mg tablets. With regard to its application to quality control, validation included the following parameters: linearity, accuracy, precision, and selectivity. Results were satisfactory within 50-150 % rank. In the case of its use in subsequent studies of chemical stability, the selectivity for stability and sensitivity was assessed. Estimated detection and quantification limits were appropriate, and the method was selective versus the possible degradation products. (Author)

  16. 40 CFR 136.6 - Method modifications and analytical requirements.

    Science.gov (United States)

    2010-07-01

    ... modifications and analytical requirements. (a) Definitions of terms used in this section. (1) Analyst means the..., oil and grease, total suspended solids, total phenolics, turbidity, chemical oxygen demand, and.... Except as set forth in paragraph (b)(3) of this section, an analyst may modify an approved test procedure...

  17. 77 FR 56176 - Analytical Methods Used in Periodic Reporting

    Science.gov (United States)

    2012-09-12

    ... informal rulemaking proceeding to consider changes in analytical principles (Proposals Six and Seven) used... (Proposals Six and Seven), September 4, 2012 (Petition). Proposal Six: Use of Foreign Postal Settlement System as Sole Source for Reporting of Inbound International Revenue, Pieces, and Weights. The Postal...

  18. Laser: a Tool for Optimization and Enhancement of Analytical Methods

    Energy Technology Data Exchange (ETDEWEB)

    Preisler, Jan [Iowa State Univ., Ames, IA (United States)

    1997-01-01

    In this work, we use lasers to enhance possibilities of laser desorption methods and to optimize coating procedure for capillary electrophoresis (CE). We use several different instrumental arrangements to characterize matrix-assisted laser desorption (MALD) at atmospheric pressure and in vacuum. In imaging mode, 488-nm argon-ion laser beam is deflected by two acousto-optic deflectors to scan plumes desorbed at atmospheric pressure via absorption. All absorbing species, including neutral molecules, are monitored. Interesting features, e.g. differences between the initial plume and subsequent plumes desorbed from the same spot, or the formation of two plumes from one laser shot are observed. Total plume absorbance can be correlated with the acoustic signal generated by the desorption event. A model equation for the plume velocity as a function of time is proposed. Alternatively, the use of a static laser beam for observation enables reliable determination of plume velocities even when they are very high. Static scattering detection reveals negative influence of particle spallation on MS signal. Ion formation during MALD was monitored using 193-nm light to photodissociate a portion of insulin ion plume. These results define the optimal conditions for desorbing analytes from matrices, as opposed to achieving a compromise between efficient desorption and efficient ionization as is practiced in mass spectrometry. In CE experiment, we examined changes in a poly(ethylene oxide) (PEO) coating by continuously monitoring the electroosmotic flow (EOF) in a fused-silica capillary during electrophoresis. An imaging CCD camera was used to follow the motion of a fluorescent neutral marker zone along the length of the capillary excited by 488-nm Ar-ion laser. The PEO coating was shown to reduce the velocity of EOF by more than an order of magnitude compared to a bare capillary at pH 7.0. The coating protocol was important, especially at an intermediate pH of 7.7. The increase of p

  19. Hanford environmental analytical methods: Methods as of March 1990. Volume 3, Appendix A2-I

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S.C.; McCulloch, M.; Daniel, J.L.

    1993-05-01

    This paper from the analytical laboratories at Hanford describes the method used to measure pH of single-shell tank core samples. Sludge or solid samples are mixed with deionized water. The pH electrode used combines both a sensor and reference electrode in one unit. The meter amplifies the input signal from the electrode and displays the pH visually.

  20. Analytical method for analysis of electromagnetic scattering from inhomogeneous spherical structures using duality principles

    Science.gov (United States)

    Kiani, M.; Abdolali, A.; Safari, M.

    2018-03-01

    In this article, an analytical approach is presented for the analysis of electromagnetic (EM) scattering from radially inhomogeneous spherical structures (RISSs) based on the duality principle. According to the spherical symmetry, similar angular dependencies in all the regions are considered using spherical harmonics. To extract the radial dependency, the system of differential equations of wave propagation toward the inhomogeneity direction is equated with the dual planar ones. A general duality between electromagnetic fields and parameters and scattering parameters of the two structures is introduced. The validity of the proposed approach is verified through a comprehensive example. The presented approach substitutes a complicated problem in spherical coordinate to an easy, well posed, and previously solved problem in planar geometry. This approach is valid for all continuously varying inhomogeneity profiles. One of the major advantages of the proposed method is the capability of studying two general and applicable types of RISSs. As an interesting application, a class of lens antenna based on the physical concept of the gradient refractive index material is introduced. The approach is used to analyze the EM scattering from the structure and validate strong performance of the lens.

  1. An active learning representative subset selection method using net analyte signal

    Science.gov (United States)

    He, Zhonghai; Ma, Zhenhe; Luan, Jingmin; Cai, Xi

    2018-05-01

    To guarantee accurate predictions, representative samples are needed when building a calibration model for spectroscopic measurements. However, in general, it is not known whether a sample is representative prior to measuring its concentration, which is both time-consuming and expensive. In this paper, a method to determine whether a sample should be selected into a calibration set is presented. The selection is based on the difference of Euclidean norm of net analyte signal (NAS) vector between the candidate and existing samples. First, the concentrations and spectra of a group of samples are used to compute the projection matrix, NAS vector, and scalar values. Next, the NAS vectors of candidate samples are computed by multiplying projection matrix with spectra of samples. Scalar value of NAS is obtained by norm computation. The distance between the candidate set and the selected set is computed, and samples with the largest distance are added to selected set sequentially. Last, the concentration of the analyte is measured such that the sample can be used as a calibration sample. Using a validation test, it is shown that the presented method is more efficient than random selection. As a result, the amount of time and money spent on reference measurements is greatly reduced.

  2. An analytical method for predicting the geometrical and optical properties of the human lens under accommodation.

    Science.gov (United States)

    Sheil, Conor J; Bahrami, Mehdi; Goncharov, Alexander V

    2014-05-01

    We present an analytical method to describe the accommodative changes in the human crystalline lens. The method is based on the geometry-invariant lens model, in which the gradient-index (GRIN) iso-indicial contours are coupled to the external shape. This feature ensures that any given number of iso-indicial contours does not change with accommodation, which preserves the optical integrity of the GRIN structure. The coupling also enables us to define the GRIN structure if the radii and asphericities of the external lens surfaces are known. As an example, the accommodative changes in lenticular radii and central thickness were taken from the literature, while the asphericities of the external surfaces were derived analytically by adhering to the basic physical conditions of constant lens volume and its axial position. The resulting changes in lens geometry are consistent with experimental data, and the optical properties are in line with expected values for optical power and spherical aberration. The aim of the paper is to provide an anatomically and optically accurate lens model that is valid for 3 mm pupils and can be used as a new tool for better understanding of accommodation.

  3. Validation of method in instrumental NAA for food products sample

    International Nuclear Information System (INIS)

    Alfian; Siti Suprapti; Setyo Purwanto

    2010-01-01

    NAA is a method of testing that has not been standardized. To affirm and confirm that this method is valid. it must be done validation of the method with various sample standard reference materials. In this work. the validation is carried for food product samples using NIST SRM 1567a (wheat flour) and NIST SRM 1568a (rice flour). The results show that the validation method for testing nine elements (Al, K, Mg, Mn, Na, Ca, Fe, Se and Zn) in SRM 1567a and eight elements (Al, K, Mg, Mn, Na, Ca, Se and Zn ) in SRM 1568a pass the test of accuracy and precision. It can be conclude that this method has power to give valid result in determination element of the food products samples. (author)

  4. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid chromatography (HPLC) method for the determination of cefadroxil monohydrate in human plasma. Methods: Schimadzu HPLC with LC solution software was used with Waters Spherisorb, C18 (5 μm, 150mm × 4.5mm) column. The mobile phase ...

  5. The implementation of a simplified spherical harmonics semi-analytic nodal method in PANTHER

    International Nuclear Information System (INIS)

    Hall, S.K.; Eaton, M.D.; Knight, M.P.

    2013-01-01

    Highlights: ► An SP N nodal method is proposed. ► Consistent CMFD derived and tested. ► Mark vacuum boundary conditions applied. ► Benchmarked against other diffusions and transport codes. - Abstract: In this paper an SP N nodal method is proposed which can utilise existing multi-group neutron diffusion solvers to obtain the solution. The semi-analytic nodal method is used in conjunction with a coarse mesh finite difference (CMFD) scheme to solve the resulting set of equations. This is compared against various nuclear benchmarks to show that the method is capable of computing an accurate solution for practical cases. A few different CMFD formulations are implemented and their performance compared. It is found that the effective diffusion coefficent (EDC) can provide additional stability and require less power iterations on a coarse mesh. A re-arrangement of the EDC is proposed that allows the iteration matrix to be computed at the beginning of a calculation. Successive nodal updates only modify the source term unlike existing CMFD methods which update the iteration matrix. A set of Mark vacuum boundary conditions are also derived which can be applied to the SP N nodal method extending its validity. This is possible due to a similarity transformation of the angular coupling matrix, which is used when applying the nodal method. It is found that the Marshak vacuum condition can also be derived, but would require the significant modification of existing neutron diffusion codes to implement it

  6. Thresholds for statistical and clinical significance in systematic reviews with meta-analytic methods

    DEFF Research Database (Denmark)

    Jakobsen, Janus Christian; Wetterslev, Jorn; Winkel, Per

    2014-01-01

    BACKGROUND: Thresholds for statistical significance when assessing meta-analysis results are being insufficiently demonstrated by traditional 95% confidence intervals and P-values. Assessment of intervention effects in systematic reviews with meta-analysis deserves greater rigour. METHODS......: Methodologies for assessing statistical and clinical significance of intervention effects in systematic reviews were considered. Balancing simplicity and comprehensiveness, an operational procedure was developed, based mainly on The Cochrane Collaboration methodology and the Grading of Recommendations...... Assessment, Development, and Evaluation (GRADE) guidelines. RESULTS: We propose an eight-step procedure for better validation of meta-analytic results in systematic reviews (1) Obtain the 95% confidence intervals and the P-values from both fixed-effect and random-effects meta-analyses and report the most...

  7. Recent Trends in Analytical Methods to Determine New Psychoactive Substances in Hair.

    Science.gov (United States)

    Kyriakou, Chrystalla; Pellegrini, Manuela; García-Algar, Oscar; Marinelli, Enrico; Zaami, Simona

    2017-01-01

    New Psychoactive Substances (NPS) belong to several chemical classes, including phenethylamines, piperazines, synthetic cathinones and synthetic cannabinoids. Development and validation of analytical methods for the determination of NPS both in traditional and alternative matrices is of crucial importance to study drug metabolism and to associate consumption to clinical outcomes and eventual intoxication symptoms. Among different biological matrices, hair is the one with the widest time window to investigate drug-related history and demonstrate past intake. The aim of this paper was to overview the trends of the rapidly evolving analytical methods for the determination of NPS in hair and the usefulness of these methods when applied to real cases. A number of rapid and sensitive methods for the determination of NPS in hair matrix has been recently published, most of them using liquid chromatography coupled to mass spectrometry. Hair digestion and subsequent solid phase extraction or liquid-liquid extraction were described as well as extraction in organic solvents. For most of the methods limits of quantification at picogram per milligram hair were obtained. The measured concentrations for most of the NPS in real samples were in the range of picograms of drug per milligram of hair. Interpretation of the results and lack of cut-off values for the discrimination between chronic consumption and occasional use or external contamination are still challenging. Methods for the determination of NPS in hair are continually emerging to include as many NPS as possible due to the great demand for their detection. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  8. Method validation using weighted linear regression models for quantification of UV filters in water samples.

    Science.gov (United States)

    da Silva, Claudia Pereira; Emídio, Elissandro Soares; de Marchi, Mary Rosa Rodrigues

    2015-01-01

    This paper describes the validation of a method consisting of solid-phase extraction followed by gas chromatography-tandem mass spectrometry for the analysis of the ultraviolet (UV) filters benzophenone-3, ethylhexyl salicylate, ethylhexyl methoxycinnamate and octocrylene. The method validation criteria included evaluation of selectivity, analytical curve, trueness, precision, limits of detection and limits of quantification. The non-weighted linear regression model has traditionally been used for calibration, but it is not necessarily the optimal model in all cases. Because the assumption of homoscedasticity was not met for the analytical data in this work, a weighted least squares linear regression was used for the calibration method. The evaluated analytical parameters were satisfactory for the analytes and showed recoveries at four fortification levels between 62% and 107%, with relative standard deviations less than 14%. The detection limits ranged from 7.6 to 24.1 ng L(-1). The proposed method was used to determine the amount of UV filters in water samples from water treatment plants in Araraquara and Jau in São Paulo, Brazil. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Analytical and Experimental Study for Validation of the Device to Confine BN Reactor Melted Fuel

    International Nuclear Information System (INIS)

    Rogozhkin, S.; Osipov, S.; Sobolev, V.; Shepelev, S.; Kozhaev, A.; Mavrin, M.; Ryabov, A.

    2013-01-01

    To validate the design and confirm the design characteristics of the special retaining device (core catcher) used for protection of BN reactor vessel in the case of a severe beyond-design basis accident with core melting, computational and experimental studies were carried out. The Tray test facility that uses water as coolant was developed and fabricated by OKBM; experimental studies were performed. To verify the methodical approach used for the computational study, experimental results obtained in the Tray test facility were compared with numerical simulation results obtained by the STAR-CCM+ CFD code

  10. Analytical methods of heat transfer compared with numerical methods as related to nuclear waste repositories

    International Nuclear Information System (INIS)

    Estrada-Gasca, C.A.

    1986-01-01

    Analytical methods were applied to the prediction of the far-field thermal impact of a nuclear waste repository. Specifically, the transformation of coordinates and the Kirchhoff transformation were used to solve one-dimensional nonlinear heat conduction problems. Calculations for the HLW and TRU nuclear waste with initial areal thermal loadings of 12 kW/acre and 0.7 kW/acre, respectively, are carried out for various models. Also, finite difference and finite element methods are applied. The last method is used to solve two-dimensional linear and nonlinear heat conduction problems. Results of the analysis are temperature distributions and temperature histories. Explicit analytical expressions of the maximum temperature rise as a function of the system parameters are presented. The theoretical approaches predict maximum temperature increases in the overburden with an error of 10%. When the finite solid one-dimensional NWR thermal problem is solved with generic salt and HLW thermal load as parameters, the maximum temperature rises predicted by the finite difference and finite element methods had maximum errors of 2.6 and 6.7%, respectively. In all the other cases the finite difference method also gave a smaller error than the finite element method

  11. Recent applications of nuclear analytical methods to the certification of elemental content in NIST standard reference materials

    International Nuclear Information System (INIS)

    Greenberg, R.R.; Zeisler, R.; Mackey, E.A.

    2006-01-01

    Well-characterized, certified reference materials (CRMs) play an essential role in assuring the quality of analytical measurements. NIST has been producing CRMs, currently called NIST Standard Reference Materials (SRMs), to validate analytical measurements for nearly one hundred years. The predominant mode of certifying inorganic constituents in complex-matrix SRMs is through the use of two critically evaluated, independent analytical techniques at NIST. These techniques should have no significant sources of error in common. The use of nuclear analytical methods in combination with one of the chemically based analytical method at NIST eliminates the possibility of any significant, common error source. The inherent characteristics of the various forms of nuclear analytical methods make them extremely valuable for SRM certification. Instrumental NAA is nondestructive, which eliminates the possibility of any dissolution problems, and often provides homogeneity information. Radiochemical NAA typically provides nearly blank-free determinations of some highly important, but difficult elements at very low levels. Prompt-gamma NAA complements INAA, and provides independent determinations of some key elements. In addition, all significant uncertainty components can be evaluated for these techniques, and we believe these methods can meet all the requirements of a primary method of measurement as defined by ISO and the CCQM. NIST has certified several SRMs using INAA and RNAA as primary methods. In addition, NIST has compared measurements by INAA and PGAA with other primary methods as part of the CCQM intercomparisons of national metrology institutes. Some significant SRMs recently certified for inorganic constituents with contributions from the nuclear analytical methods include: Toxic Substances in Urine (SRM 2670a), Lake Superior Fish Tissue (SRM 1946), Air Particulate on Filter Media (SRM 2783), Inorganics in Marine Sediment (SRM 2702), Sediment for Solid Sampling (Small

  12. Decentral gene expression analysis: analytical validation of the Endopredict genomic multianalyte breast cancer prognosis test

    International Nuclear Information System (INIS)

    Kronenwett, Ralf; Brase, Jan C; Weber, Karsten E; Fisch, Karin; Müller, Berit M; Schmidt, Marcus; Filipits, Martin; Dubsky, Peter; Petry, Christoph; Dietel, Manfred; Denkert, Carsten; Bohmann, Kerstin; Prinzler, Judith; Sinn, Bruno V; Haufe, Franziska; Roth, Claudia; Averdick, Manuela; Ropers, Tanja; Windbergs, Claudia

    2012-01-01

    EndoPredict (EP) is a clinically validated multianalyte gene expression test to predict distant metastasis in ER-positive, HER2-negative breast cancer treated with endocrine therapy alone. The test is based on the combined analysis of 12 genes in formalin-fixed, paraffin-embedded (FFPE) tissue by reverse transcription-quantitative real-time PCR (RT-qPCR). Recently, it was shown that EP is feasible for reliable decentralized assessment of gene expression. The aim of this study was the analytical validation of the performance characteristics of the assay and its verification in a molecular-pathological routine laboratory. Gene expression values to calculate the EP score were assayed by one-step RT-qPCR using RNA from FFPE tumor tissue. Limit of blank, limit of detection, linear range, and PCR efficiency were assessed for each of the 12 PCR assays using serial samples dilutions. Different breast cancer samples were used to evaluate RNA input range, precision and inter-laboratory variability. PCR assays were linear up to C q values between 35.1 and 37.2. Amplification efficiencies ranged from 75% to 101%. The RNA input range without considerable change of the EP score was between 0.16 and 18.5 ng/μl. Analysis of precision (variation of day, day time, instrument, operator, reagent lots) resulted in a total noise (standard deviation) of 0.16 EP score units on a scale from 0 to 15. The major part of the total noise (SD 0.14) was caused by the replicate-to-replicate noise of the PCR assays (repeatability) and was not associated with different operating conditions (reproducibility). Performance characteristics established in the manufacturer’s laboratory were verified in a routine molecular pathology laboratory. Comparison of 10 tumor samples analyzed in two different laboratories showed a Pearson coefficient of 0.995 and a mean deviation of 0.15 score units. The EP test showed reproducible performance characteristics with good precision and negligible laboratory

  13. Human Factors methods concerning integrated validation of nuclear power plant control rooms; Metodutveckling foer integrerad validering

    Energy Technology Data Exchange (ETDEWEB)

    Oskarsson, Per-Anders; Johansson, Bjoern J.E.; Gonzalez, Natalia (Swedish Defence Research Agency, Information Systems, Linkoeping (Sweden))

    2010-02-15

    The frame of reference for this work was existing recommendations and instructions from the NPP area, experiences from the review of the Turbic Validation and experiences from system validations performed at the Swedish Armed Forces, e.g. concerning military control rooms and fighter pilots. These enterprises are characterized by complex systems in extreme environments, often with high risks, where human error can lead to serious consequences. A focus group has been performed with representatives responsible for Human Factors issues from all Swedish NPP:s. The questions that were discussed were, among other things, for whom an integrated validation (IV) is performed and its purpose, what should be included in an IV, the comparison with baseline measures, the design process, the role of SSM, which methods of measurement should be used, and how the methods are affected of changes in the control room. The report brings different questions to discussion concerning the validation process. Supplementary methods of measurement for integrated validation are discussed, e.g. dynamic, psychophysiological, and qualitative methods for identification of problems. Supplementary methods for statistical analysis are presented. The study points out a number of deficiencies in the validation process, e.g. the need of common guidelines for validation and design, criteria for different types of measurements, clarification of the role of SSM, and recommendations for the responsibility of external participants in the validation process. The authors propose 12 measures for taking care of the identified problems

  14. Development and validation of a spectroscopic method for the ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... Purpose: To develop a new analytical method for the quantitative analysis of miconazole ... a simple, reliable and robust method for the characterization of a mixture of the drugs in a dosage form. ... By Country · List All Titles · Free To Read Titles This Journal is Open Access.

  15. Validated high performance liquid chromatographic (HPLC) method ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-22

    Feb 22, 2010 ... specific and accurate high performance liquid chromatographic method for determination of ZER in micro-volumes ... tional medicine as a cure for swelling, sores, loss of appetite and ... Receptor Activator for Nuclear Factor κ B Ligand .... The effect of ... be suitable for preclinical pharmacokinetic studies. The.

  16. Validation of qualitative microbiological test methods

    NARCIS (Netherlands)

    IJzerman-Boon, Pieta C.; van den Heuvel, Edwin R.

    2015-01-01

    This paper considers a statistical model for the detection mechanism of qualitative microbiological test methods with a parameter for the detection proportion (the probability to detect a single organism) and a parameter for the false positive rate. It is demonstrated that the detection proportion

  17. Validation Method of a Telecommunications Blackout Attack

    National Research Council Canada - National Science Library

    Amado, Joao; Nunes, Paulo

    2005-01-01

    ..., and to obtain the maximum disruptive effect over the services. The proposed method uses a top-down approach, starting on the service level and ending on the different network elements that can be identified in the end as the targets for the attack.

  18. Development and validation of stability indicating UPLC assay method for ziprasidone active pharma ingredient

    Directory of Open Access Journals (Sweden)

    Sonam Mittal

    2012-01-01

    Full Text Available Background: Ziprasidone, a novel antipsychotic, exhibits a potent highly selective antagonistic activity on D2 and 5HT2A receptors. Literature survey for ziprasidone revealed several analytical methods based on different techniques but no UPLC method has been reported so far. Aim: Aim of this research paper is to present a simple and rapid stability indicating isocratic, ultra performance liquid chromatographic (UPLC method which was developed and validated for the determination of ziprasidone active pharmaceutical ingredient. Forced degradation studies of ziprasidone were studied under acid, base, oxidative hydrolysis, thermal stress and photo stress conditions. Materials and Methods: The quantitative determination of ziprasidone drug was performed on a Supelco analytical column (100×2.1 mm i.d., 2.7 ΅m with 10 mM ammonium acetate buffer (pH: 6.7 and acetonitrile (ACN as mobile phase with the ratio (55:45-Buffer:ACN at a flow rate of 0.35 ml/ min. For UPLC method, UV detection was made at 318 nm and the run time was 3 min. Developed UPLC method was validated as per ICH guidelines. Results and Conclusion: Mild degradation of the drug substance was observed during oxidative hydrolysis and considerable degradation observed during basic hydrolysis. During method validation, parameters such as precision, linearity, ruggedness, stability, robustness, and specificity were evaluated, which remained within acceptable limits. Developed UPLC method was successfully applied for evaluating assay of Ziprasidone active Pharma ingredient.

  19. Valid methods: the quality assurance of test method development, validation, approval, and transfer for veterinary testing laboratories.

    Science.gov (United States)

    Wiegers, Ann L

    2003-07-01

    Third-party accreditation is a valuable tool to demonstrate a laboratory's competence to conduct testing. Accreditation, internationally and in the United States, has been discussed previously. However, accreditation is only I part of establishing data credibility. A validated test method is the first component of a valid measurement system. Validation is defined as confirmation by examination and the provision of objective evidence that the particular requirements for a specific intended use are fulfilled. The international and national standard ISO/IEC 17025 recognizes the importance of validated methods and requires that laboratory-developed methods or methods adopted by the laboratory be appropriate for the intended use. Validated methods are therefore required and their use agreed to by the client (i.e., end users of the test results such as veterinarians, animal health programs, and owners). ISO/IEC 17025 also requires that the introduction of methods developed by the laboratory for its own use be a planned activity conducted by qualified personnel with adequate resources. This article discusses considerations and recommendations for the conduct of veterinary diagnostic test method development, validation, evaluation, approval, and transfer to the user laboratory in the ISO/IEC 17025 environment. These recommendations are based on those of nationally and internationally accepted standards and guidelines, as well as those of reputable and experienced technical bodies. They are also based on the author's experience in the evaluation of method development and transfer projects, validation data, and the implementation of quality management systems in the area of method development.

  20. Validação em métodos cromatográficos e eletroforéticos Validation for chromatographic and electrophoretic methods

    Directory of Open Access Journals (Sweden)

    Marcelo Ribani

    2004-10-01

    Full Text Available The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the different Brazilian and international regulatory agencies.

  1. Validation of methods for the determination of radium in waters and soil

    International Nuclear Information System (INIS)

    Decaillon, J.-G.; Bickel, M.; Hill, C.; Altzitzoglou, T.

    2004-01-01

    This article describes the advantages and disadvantages of several analytical methods used to prepare the alpha-particle source. As a result of this study, a new method combining commercial extraction and ion chromatography prior to a final co-precipitation step is proposed. This method has been applied and validated on several matrices (soil, waters) in the framework of international intercomparisons. The integration of this method in a global procedure to analyze actinoids and radium from a single solution (or digested soil) is also described

  2. Fission product release from nuclear fuel II. Validation of ASTEC/ELSA on analytical and large scale experiments

    International Nuclear Information System (INIS)

    Brillant, G.; Marchetto, C.; Plumecocq, W.

    2013-01-01

    Highlights: • A wide range of experiments is presented for the ASTEC/ELSA code validation. • Analytical tests such as AECL, ORNL and VERCORS are considered. • A large-scale experiment, PHEBUS FPT1, is considered. • The good agreement with measurements shows the efficiency of the ASTEC modelling. • Improvements concern the FP release modelling from MOX and high burn-up UO 2 fuels. - Abstract: This article is the second of two articles dedicated to the mechanisms of fission product release from a degraded core. The models of fission product release from nuclear fuel in the ASTEC code have been described in detail in the first part of this work (Brillant et al., this issue). In this contribution, the validation of ELSA, the module of ASTEC that deals with fission product and structural material release from a degraded core, is presented. A large range of experimental tests, with various temperature and conditions for the fuel surrounding atmosphere (oxidising and reducing), is thus simulated with the ASTEC code. The validation database includes several analytical experiments with both bare fuel (e.g. MCE1 experiments) and cladded fuel (e.g. HCE3, VERCORS). Furthermore, the PHEBUS large-scale experiments are used for the validation of ASTEC. The rather satisfactory comparison between ELSA calculations and experimental measurements demonstrates the efficiency of the analytical models to describe fission product release in severe accident conditions

  3. Analytical methods for the evaluation of melamine contamination.

    Science.gov (United States)

    Cantor, Stuart L; Gupta, Abhay; Khan, Mansoor A

    2014-02-01

    There is an urgent need for the analysis of melamine in the global pharmaceutical supply chain to detect economically motivated adulteration or unintentional contamination using a simple, nondestructive analytical technique that confirms the extent of adulteration in a shorter time period. In this work, different analytical techniques (thermal analysis, X-ray diffraction, Fourier transform infrared (FT-IR), FT-Raman, and near-infrared (NIR) spectroscopy) were evaluated for their ability to detect a range of melamine levels in gelatin. While FT-IR and FT-Raman provided qualitative assessment of melamine contamination or adulteration, powder X-ray diffraction and NIR were able to detect and quantify the presence of melamine at levels as low as 1.0% w/w. Multivariate analysis of the NIR data yielded the most accurate model when three principal components were used. Data were pretreated using standard normal variate transformation to remove multiplicative interferences of scatter and particle size. The model had a root-mean-square error of calibration of 2.4 (R(2) = 0.99) and root-mean square error of prediction of 2.5 (R(2) = 0.96). The value of the paired t test for actual and predicted samples (1%-50% w/w) was 0.448 (p 5), further indicating the robustness of the model. Published 2013. This article is a U.S. Government work and is in the public domain in the USA.

  4. Fuzzy-logic based strategy for validation of multiplex methods: example with qualitative GMO assays.

    Science.gov (United States)

    Bellocchi, Gianni; Bertholet, Vincent; Hamels, Sandrine; Moens, W; Remacle, José; Van den Eede, Guy

    2010-02-01

    This paper illustrates the advantages that a fuzzy-based aggregation method could bring into the validation of a multiplex method for GMO detection (DualChip GMO kit, Eppendorf). Guidelines for validation of chemical, bio-chemical, pharmaceutical and genetic methods have been developed and ad hoc validation statistics are available and routinely used, for in-house and inter-laboratory testing, and decision-making. Fuzzy logic allows summarising the information obtained by independent validation statistics into one synthetic indicator of overall method performance. The microarray technology, introduced for simultaneous identification of multiple GMOs, poses specific validation issues (patterns of performance for a variety of GMOs at different concentrations). A fuzzy-based indicator for overall evaluation is illustrated in this paper, and applied to validation data for different genetically modified elements. Remarks were drawn on the analytical results. The fuzzy-logic based rules were shown to be applicable to improve interpretation of results and facilitate overall evaluation of the multiplex method.

  5. Examination of fast reactor fuels, FBR analytical quality assurance standards and methods, and analytical methods development: irradiation tests. Progress report, April 1--June 30, 1976, and FY 1976

    International Nuclear Information System (INIS)

    Baker, R.D.

    1976-08-01

    Characterization of unirradiated and irradiated LMFBR fuels by analytical chemistry methods will continue, and additional methods will be modified and mechanized for hot cell application. Macro- and microexaminations will be made on fuel and cladding using the shielded electron microprobe, emission spectrograph, radiochemistry, gamma scanner, mass spectrometers, and other analytical facilities. New capabilities will be developed in gamma scanning, analyses to assess spatial distributions of fuel and fission products, mass spectrometric measurements of burnup and fission gas constituents and other chemical analyses. Microstructural analyses of unirradiated and irradiated materials will continue using optical and electron microscopy and autoradiographic and x-ray techniques. Analytical quality assurance standards tasks are designed to assure the quality of the chemical characterizations necessary to evaluate reactor components relative to specifications. Tasks include: (1) the preparation and distribution of calibration materials and quality control samples for use in quality assurance surveillance programs, (2) the development of and the guidance in the use of quality assurance programs for sampling and analysis, (3) the development of improved methods of analysis, and (4) the preparation of continuously updated analytical method manuals. Reliable analytical methods development for the measurement of burnup, oxygen-to-metal (O/M) ratio, and various gases in irradiated fuels is described

  6. Update of Standard Practices for New Method Validation in Forensic Toxicology.

    Science.gov (United States)

    Wille, Sarah M R; Coucke, Wim; De Baere, Thierry; Peters, Frank T

    2017-01-01

    International agreement concerning validation guidelines is important to obtain quality forensic bioanalytical research and routine applications as it all starts with the reporting of reliable analytical data. Standards for fundamental validation parameters are provided in guidelines as those from the US Food and Drug Administration (FDA), the European Medicines Agency (EMA), the German speaking Gesellschaft fur Toxikologie und Forensische Chemie (GTFCH) and the Scientific Working Group of Forensic Toxicology (SWGTOX). These validation parameters include selectivity, matrix effects, method limits, calibration, accuracy and stability, as well as other parameters such as carryover, dilution integrity and incurred sample reanalysis. It is, however, not easy for laboratories to implement these guidelines into practice as these international guidelines remain nonbinding protocols, that depend on the applied analytical technique, and that need to be updated according the analyst's method requirements and the application type. In this manuscript, a review of the current guidelines and literature concerning bioanalytical validation parameters in a forensic context is given and discussed. In addition, suggestions for the experimental set-up, the pros and cons of statistical approaches and adequate acceptance criteria for the validation of bioanalytical applications are given. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  7. A manual of analytical methods used at MINTEK

    International Nuclear Information System (INIS)

    Stoch, H.; Dixon, K.

    1983-01-01

    The manual deals with various methods for a wide range of elemental analysis. Some of the methods that are used, include atomic absorption spectroscopy, optical emission spectroscopy and x-ray fluoresence spectroscopy. The basic charateristics of the method are given and the procedures are recorded step by step. One of the sections deals with methods associated with the recovery of uranium

  8. Development and Validation of a Learning Analytics Framework: Two Case Studies Using Support Vector Machines

    Science.gov (United States)

    Ifenthaler, Dirk; Widanapathirana, Chathuranga

    2014-01-01

    Interest in collecting and mining large sets of educational data on student background and performance to conduct research on learning and instruction has developed as an area generally referred to as learning analytics. Higher education leaders are recognizing the value of learning analytics for improving not only learning and teaching but also…

  9. Survey of Technetium Analytical Production Methods Supporting Hanford Nuclear Materials Processing

    International Nuclear Information System (INIS)

    TROYER, G.L.

    1999-01-01

    This document provides a historical survey of analytical methods used for measuring 99 Tc in nuclear fuel reprocessing materials and wastes at Hanford. Method challenges including special sludge matrices tested are discussed. Special problems and recommendations are presented

  10. Nuclear analytical methods in quality control of microanalysis

    International Nuclear Information System (INIS)

    Tian Weizhi

    2004-01-01

    Quantitative calibration and quality control have been a major bottleneck in microanalysis due to the lack of natural-matrix CRMs certified at sample sizes compatible with those of unknown samples. A solution is described to characterize sampling behavior for individual elements, so as to identify elements homogeneous enough at stated sample size levels in given CRMs/RMs. By using a combination of several nuclear analytical techniques, INAA-EDXRF-μPIXE, sampling behavior for individual elements can be characterized at sample size levels from grams down to pg. Natural-matrix CRMs specifically for QC of microanalysis may thus be created. Additional information in certificates of these new generation CRMs is imagined. (author)

  11. Evaluating water management strategies in watersheds by new hybrid Fuzzy Analytical Network Process (FANP) methods

    Science.gov (United States)

    RazaviToosi, S. L.; Samani, J. M. V.

    2016-03-01

    Watersheds are considered as hydrological units. Their other important aspects such as economic, social and environmental functions play crucial roles in sustainable development. The objective of this work is to develop methodologies to prioritize watersheds by considering different development strategies in environmental, social and economic sectors. This ranking could play a significant role in management to assign the most critical watersheds where by employing water management strategies, best condition changes are expected to be accomplished. Due to complex relations among different criteria, two new hybrid fuzzy ANP (Analytical Network Process) algorithms, fuzzy TOPSIS (Technique for Order Preference by Similarity to Ideal Solution) and fuzzy max-min set methods are used to provide more flexible and accurate decision model. Five watersheds in Iran named Oroomeyeh, Atrak, Sefidrood, Namak and Zayandehrood are considered as alternatives. Based on long term development goals, 38 water management strategies are defined as subcriteria in 10 clusters. The main advantage of the proposed methods is its ability to overcome uncertainty. This task is accomplished by using fuzzy numbers in all steps of the algorithms. To validate the proposed method, the final results were compared with those obtained from the ANP algorithm and the Spearman rank correlation coefficient is applied to find the similarity in the different ranking methods. Finally, the sensitivity analysis was conducted to investigate the influence of cluster weights on the final ranking.

  12. An analytical method to simulate the H I 21-cm visibility signal for intensity mapping experiments

    Science.gov (United States)

    Sarkar, Anjan Kumar; Bharadwaj, Somnath; Marthi, Visweshwar Ram

    2018-01-01

    Simulations play a vital role in testing and validating H I 21-cm power spectrum estimation techniques. Conventional methods use techniques like N-body simulations to simulate the sky signal which is then passed through a model of the instrument. This makes it necessary to simulate the H I distribution in a large cosmological volume, and incorporate both the light-cone effect and the telescope's chromatic response. The computational requirements may be particularly large if one wishes to simulate many realizations of the signal. In this paper, we present an analytical method to simulate the H I visibility signal. This is particularly efficient if one wishes to simulate a large number of realizations of the signal. Our method is based on theoretical predictions of the visibility correlation which incorporate both the light-cone effect and the telescope's chromatic response. We have demonstrated this method by applying it to simulate the H I visibility signal for the upcoming Ooty Wide Field Array Phase I.

  13. Five-point Element Scheme of Finite Analytic Method for Unsteady Groundwater Flow

    Institute of Scientific and Technical Information of China (English)

    Xiang Bo; Mi Xiao; Ji Changming; Luo Qingsong

    2007-01-01

    In order to improve the finite analytic method's adaptability for irregular unit, by using coordinates rotation technique this paper establishes a five-point element scheme of finite analytic method. It not only solves unsteady groundwater flow equation but also gives the boundary condition. This method can be used to calculate the three typical questions of groundwater. By compared with predecessor's computed result, the result of this method is more satisfactory.

  14. Analytical and numerical study of validation test-cases for multi-physic problems: application to magneto-hydro-dynamic

    Directory of Open Access Journals (Sweden)

    D Cébron

    2016-04-01

    Full Text Available The present paper is concerned with the numerical simulation of Magneto-Hydro-Dynamic (MHD problems with industrial tools. MHD has receivedattention some twenty to thirty years ago as a possible alternative inpropulsion applications; MHD propelled ships have even been designed forthat purpose. However, such propulsion systems have been proved of lowefficiency and fundamental researches in the area have progressivelyreceived much less attention over the past decades. Numerical simulationof MHD problem could however provide interesting solutions in the field ofturbulent flow control. The development of recent efficient numericaltechniques for multi-physic applications provide promising tool for theengineer for that purpose. In the present paper, some elementary testcases in laminar flow with magnetic forcing terms are analysed; equationsof the coupled problem are exposed, analytical solutions are derived ineach case and are compared to numerical solutions obtained with anumerical tool for multi-physic applications. The present work can be seenas a validation of numerical tools (based on the finite element method foracademic as well as industrial application purposes.

  15. Analytical validation of a melanoma diagnostic gene signature using formalin-fixed paraffin-embedded melanocytic lesions.

    Science.gov (United States)

    Warf, M Bryan; Flake, Darl D; Adams, Doug; Gutin, Alexander; Kolquist, Kathryn A; Wenstrup, Richard J; Roa, Benjamin B

    2015-01-01

    These studies were to validate the analytical performance of a gene expression signature that differentiates melanoma and nevi, using RNA expression from 14 signature genes and nine normalization genes that generates a melanoma diagnostic score (MDS). Formalin-fixed paraffin-embedded melanocytic lesions were evaluated in these studies. The overall SD of the assay was determined to be 0.69 MDS units. Individual amplicons within the signature had an average amplification efficiency of 92% and a SD less than 0.5 CT. The MDS was reproducible across a 2000-fold dilution range of input RNA. Melanin, an inhibitor of PCR, does not interfere with the signature. These studies indicate this signature is robust and reproducible and is analytically validated on formalin-fixed paraffin-embedded melanocytic lesions.

  16. Experimental validation of an analytical kinetic model for edge-localized modes in JET-ITER-like wall

    Science.gov (United States)

    Guillemaut, C.; Metzger, C.; Moulton, D.; Heinola, K.; O’Mullane, M.; Balboa, I.; Boom, J.; Matthews, G. F.; Silburn, S.; Solano, E. R.; contributors, JET

    2018-06-01

    The design and operation of future fusion devices relying on H-mode plasmas requires reliable modelling of edge-localized modes (ELMs) for precise prediction of divertor target conditions. An extensive experimental validation of simple analytical predictions of the time evolution of target plasma loads during ELMs has been carried out here in more than 70 JET-ITER-like wall H-mode experiments with a wide range of conditions. Comparisons of these analytical predictions with diagnostic measurements of target ion flux density, power density, impact energy and electron temperature during ELMs are presented in this paper and show excellent agreement. The analytical predictions tested here are made with the ‘free-streaming’ kinetic model (FSM) which describes ELMs as a quasi-neutral plasma bunch expanding along the magnetic field lines into the Scrape-Off Layer without collisions. Consequences of the FSM on energy reflection and deposition on divertor targets during ELMs are also discussed.

  17. Method validation for strobilurin fungicides in cereals and fruit

    DEFF Research Database (Denmark)

    Christensen, Hanne Bjerre; Granby, Kit

    2001-01-01

    Strobilurins are a new class of fungicides that are active against a broad spectrum of fungi. In the present work a GC method for analysis of strobilurin fungicides was validated. The method was based on extraction with ethyl acetate/cyclohexane, clean-up by gel permeation chromatography (GPC......) and determination of the content by gas chromatography (GC) with electron capture (EC-), nitrogen/phosphorous (NP-), and mass spectrometric (MS-) detection. Three strobilurins, azoxystrobin, kresoxim-methyl and trifloxystrobin were validated on three matrices, wheat, apple and grapes. The validation was based...

  18. Investigation by perturbative and analytical method of electronic properties of square quantum well under electric field

    Directory of Open Access Journals (Sweden)

    Mustafa Kemal BAHAR

    2010-06-01

    Full Text Available In this study, the effects of applied electric field on the isolated square quantum well was investigated by analytic and perturbative method. The energy eigen values and wave functions in quantum well were found by perturbative method. Later, the electric field effects were investigated by analytic method, the results of perturbative and analytic method were compared. As well as both of results fit with each other, it was observed that externally applied electric field changed importantly electronic properties of the system.

  19. A handbook of decomposition methods in analytical chemistry

    International Nuclear Information System (INIS)

    Bok, R.

    1984-01-01

    Decomposition methods of metals, alloys, fluxes, slags, calcine, inorganic salts, oxides, nitrides, carbides, borides, sulfides, ores, minerals, rocks, concentrates, glasses, ceramics, organic substances, polymers, phyto- and biological materials from the viewpoint of sample preparation for analysis have been described. The methods are systemitized according to decomposition principle: thermal with the use of electricity, irradiation, dissolution with participation of chemical reactions and without it. Special equipment for different decomposition methods is described. Bibliography contains 3420 references

  20. Determination of vitamin C in foods: current state of method validation.

    Science.gov (United States)

    Spínola, Vítor; Llorent-Martínez, Eulogio J; Castilho, Paula C

    2014-11-21

    Vitamin C is one of the most important vitamins, so reliable information about its content in foodstuffs is a concern to both consumers and quality control agencies. However, the heterogeneity of food matrixes and the potential degradation of this vitamin during its analysis create enormous challenges. This review addresses the development and validation of high-performance liquid chromatography methods for vitamin C analysis in food commodities, during the period 2000-2014. The main characteristics of vitamin C are mentioned, along with the strategies adopted by most authors during sample preparation (freezing and acidification) to avoid vitamin oxidation. After that, the advantages and handicaps of different analytical methods are discussed. Finally, the main aspects concerning method validation for vitamin C analysis are critically discussed. Parameters such as selectivity, linearity, limit of quantification, and accuracy were studied by most authors. Recovery experiments during accuracy evaluation were in general satisfactory, with usual values between 81 and 109%. However, few methods considered vitamin C stability during the analytical process, and the study of the precision was not always clear or complete. Potential future improvements regarding proper method validation are indicated to conclude this review. Copyright © 2014. Published by Elsevier B.V.

  1. Description of JNC's analytical method and its performance for FBR cores

    International Nuclear Information System (INIS)

    Ishikawa, M.

    2000-01-01

    The description of JNC's analytical method and its performance for FBR cores includes: an outline of JNC's Analytical System Compared with ERANOS; a standard data base for FBR Nuclear Design in JNC; JUPITER Critical Experiment; details of Analytical Method and Its Effects on JUPITER; performance of JNC Analytical System (effective multiplication factor k eff , control rod worth, and sodium void reactivity); design accuracy of a 600 MWe-class FBR Core. JNC developed a consistent analytical system for FBR core evaluation, based on JENDL library, f-table method, and three dimensional diffusion/transport theory, which includes comprehensive sensitivity tools to improve the prediction accuracy of core parameters. JNC system was verified by analysis of JUPITER critical experiment, and other facilities. Its performance can be judged quite satisfactory for FBR-core design work, though there is room for further improvement, such as more detailed treatment of cross-section resonance regions

  2. Application of an analytical method for solution of thermal hydraulic conservation equations

    Energy Technology Data Exchange (ETDEWEB)

    Fakory, M.R. [Simulation, Systems & Services Technologies Company (S3 Technologies), Columbia, MD (United States)

    1995-09-01

    An analytical method has been developed and applied for solution of two-phase flow conservation equations. The test results for application of the model for simulation of BWR transients are presented and compared with the results obtained from application of the explicit method for integration of conservation equations. The test results show that with application of the analytical method for integration of conservation equations, the Courant limitation associated with explicit Euler method of integration was eliminated. The results obtained from application of the analytical method (with large time steps) agreed well with the results obtained from application of explicit method of integration (with time steps smaller than the size imposed by Courant limitation). The results demonstrate that application of the analytical approach significantly improves the numerical stability and computational efficiency.

  3. International Harmonization and Cooperation in the Validation of Alternative Methods.

    Science.gov (United States)

    Barroso, João; Ahn, Il Young; Caldeira, Cristiane; Carmichael, Paul L; Casey, Warren; Coecke, Sandra; Curren, Rodger; Desprez, Bertrand; Eskes, Chantra; Griesinger, Claudius; Guo, Jiabin; Hill, Erin; Roi, Annett Janusch; Kojima, Hajime; Li, Jin; Lim, Chae Hyung; Moura, Wlamir; Nishikawa, Akiyoshi; Park, HyeKyung; Peng, Shuangqing; Presgrave, Octavio; Singer, Tim; Sohn, Soo Jung; Westmoreland, Carl; Whelan, Maurice; Yang, Xingfen; Yang, Ying; Zuang, Valérie

    The development and validation of scientific alternatives to animal testing is important not only from an ethical perspective (implementation of 3Rs), but also to improve safety assessment decision making with the use of mechanistic information of higher relevance to humans. To be effective in these efforts, it is however imperative that validation centres, industry, regulatory bodies, academia and other interested parties ensure a strong international cooperation, cross-sector collaboration and intense communication in the design, execution, and peer review of validation studies. Such an approach is critical to achieve harmonized and more transparent approaches to method validation, peer-review and recommendation, which will ultimately expedite the international acceptance of valid alternative methods or strategies by regulatory authorities and their implementation and use by stakeholders. It also allows achieving greater efficiency and effectiveness by avoiding duplication of effort and leveraging limited resources. In view of achieving these goals, the International Cooperation on Alternative Test Methods (ICATM) was established in 2009 by validation centres from Europe, USA, Canada and Japan. ICATM was later joined by Korea in 2011 and currently also counts with Brazil and China as observers. This chapter describes the existing differences across world regions and major efforts carried out for achieving consistent international cooperation and harmonization in the validation and adoption of alternative approaches to animal testing.

  4. An Analytical Method for Measuring Competence in Project Management

    Science.gov (United States)

    González-Marcos, Ana; Alba-Elías, Fernando; Ordieres-Meré, Joaquín

    2016-01-01

    The goal of this paper is to present a competence assessment method in project management that is based on participants' performance and value creation. It seeks to close an existing gap in competence assessment in higher education. The proposed method relies on information and communication technology (ICT) tools and combines Project Management…

  5. Tank 48H Waste Composition and Results of Investigation of Analytical Methods

    Energy Technology Data Exchange (ETDEWEB)

    Walker , D.D. [Westinghouse Savannah River Company, AIKEN, SC (United States)

    1997-04-02

    This report serves two purposes. First, it documents the analytical results of Tank 48H samples taken between April and August 1996. Second, it describes investigations of the precision of the sampling and analytical methods used on the Tank 48H samples.

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

    NARCIS (Netherlands)

    Lou, X.; Waal, de B.F.M.; Milroy, L.G.; Dongen, van J.L.J.

    2015-01-01

    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

  7. Practical procedure for method validation in INAA- A tutorial

    Energy Technology Data Exchange (ETDEWEB)

    Petroni, Robson; Moreira, Edson G., E-mail: robsonpetroni@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    This paper describes the procedure employed by the Neutron Activation Laboratory at the Nuclear and Energy Research Institute (LAN, IPEN - CNEN/SP) for validation of Instrumental Neutron Activation Analysis (INAA) methods. According to recommendations of ISO/IEC 17025 the method performance characteristics (limit of detection, limit of quantification, trueness, repeatability, intermediate precision, reproducibility, selectivity, linearity and uncertainties budget) were outline in an easy, fast and convenient way. The paper presents step by step how to calculate the required method performance characteristics in a process of method validation, what are the procedures, adopted strategies and acceptance criteria for the results, that is, how to make a method validation in INAA. In order to exemplify the methodology applied, obtained results for the method validation of mass fraction determination of Co, Cr, Fe, Rb, Se and Zn in biological matrix samples, using an internal reference material of mussel tissue were presented. It was concluded that the methodology applied for validation of INAA methods is suitable, meeting all the requirements of ISO/IEC 17025, and thereby, generating satisfactory results for the studies carried at LAN, IPEN - CNEN/SP. (author)

  8. Practical procedure for method validation in INAA- A tutorial

    International Nuclear Information System (INIS)

    Petroni, Robson; Moreira, Edson G.

    2015-01-01

    This paper describes the procedure employed by the Neutron Activation Laboratory at the Nuclear and Energy Research Institute (LAN, IPEN - CNEN/SP) for validation of Instrumental Neutron Activation Analysis (INAA) methods. According to recommendations of ISO/IEC 17025 the method performance characteristics (limit of detection, limit of quantification, trueness, repeatability, intermediate precision, reproducibility, selectivity, linearity and uncertainties budget) were outline in an easy, fast and convenient way. The paper presents step by step how to calculate the required method performance characteristics in a process of method validation, what are the procedures, adopted strategies and acceptance criteria for the results, that is, how to make a method validation in INAA. In order to exemplify the methodology applied, obtained results for the method validation of mass fraction determination of Co, Cr, Fe, Rb, Se and Zn in biological matrix samples, using an internal reference material of mussel tissue were presented. It was concluded that the methodology applied for validation of INAA methods is suitable, meeting all the requirements of ISO/IEC 17025, and thereby, generating satisfactory results for the studies carried at LAN, IPEN - CNEN/SP. (author)

  9. Downstream processing and chromatography based analytical methods for production of vaccines, gene therapy vectors, and bacteriophages

    Science.gov (United States)

    Kramberger, Petra; Urbas, Lidija; Štrancar, Aleš

    2015-01-01

    Downstream processing of nanoplexes (viruses, virus-like particles, bacteriophages) is characterized by complexity of the starting material, number of purification methods to choose from, regulations that are setting the frame for the final product and analytical methods for upstream and downstream monitoring. This review gives an overview on the nanoplex downstream challenges and chromatography based analytical methods for efficient monitoring of the nanoplex production. PMID:25751122

  10. Manual of analytical methods for the Industrial Hygiene Chemistry Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Greulich, K.A.; Gray, C.E. (comp.)

    1991-08-01

    This Manual is compiled from techniques used in the Industrial Hygiene Chemistry Laboratory of Sandia National Laboratories in Albuquerque, New Mexico. The procedures are similar to those used in other laboratories devoted to industrial hygiene practices. Some of the methods are standard; some, modified to suit our needs; and still others, developed at Sandia. The authors have attempted to present all methods in a simple and concise manner but in sufficient detail to make them readily usable. It is not to be inferred that these methods are universal for any type of sample, but they have been found very reliable for the types of samples mentioned.

  11. Manual of analytical methods for the Industrial Hygiene Chemistry Laboratory

    International Nuclear Information System (INIS)

    Greulich, K.A.; Gray, C.E.

    1991-08-01

    This Manual is compiled from techniques used in the Industrial Hygiene Chemistry Laboratory of Sandia National Laboratories in Albuquerque, New Mexico. The procedures are similar to those used in other laboratories devoted to industrial hygiene practices. Some of the methods are standard; some, modified to suit our needs; and still others, developed at Sandia. The authors have attempted to present all methods in a simple and concise manner but in sufficient detail to make them readily usable. It is not to be inferred that these methods are universal for any type of sample, but they have been found very reliable for the types of samples mentioned

  12. Potential of accuracy profile for method validation in inductively coupled plasma spectrochemistry

    International Nuclear Information System (INIS)

    Mermet, J.M.; Granier, G.

    2012-01-01

    Method validation is usually performed over a range of concentrations for which analytical criteria must be verified. One important criterion in quantitative analysis is accuracy, i.e. the contribution of both trueness and precision. The study of accuracy over this range is called an accuracy profile and provides experimental tolerance intervals. Comparison with acceptability limits fixed by the end user defines a validity domain. This work describes the computation involved in the building of the tolerance intervals, particularly for the intermediate precision with within-laboratory experiments and for the reproducibility with interlaboratory studies. Computation is based on ISO 5725‐4 and on previously published work. Moreover, the bias uncertainty is also computed to verify the bias contribution to accuracy. The various types of accuracy profile behavior are exemplified with results obtained by using ICP-MS and ICP-AES. This procedure allows the analyst to define unambiguously a validity domain for a given accuracy. However, because the experiments are time-consuming, the accuracy profile method is mainly dedicated to method validation. - Highlights: ► An analytical method is defined by its accuracy, i.e. both trueness and precision. ► The accuracy as a function of an analyte concentration is an accuracy profile. ► Profile basic concepts are explained for trueness and intermediate precision. ► Profile-based tolerance intervals have to be compared with acceptability limits. ► Typical accuracy profiles are given for both ICP-AES and ICP-MS techniques.

  13. Analytical method for the evaluation of the outdoor air contamination by emerging pollutants using tree leaves as bioindicators.

    Science.gov (United States)

    Barroso, Pedro José; Martín, Julia; Santos, Juan Luis; Aparicio, Irene; Alonso, Esteban

    2018-01-01

    In this work, an analytical method, based on sonication-assisted extraction, clean-up by dispersive solid-phase extraction and determination by liquid chromatography-tandem mass spectrometry, has been developed and validated for the simultaneous determination of 15 emerging pollutants in leaves from four ornamental tree species. Target compounds include perfluorinated organic compounds, plasticizers, surfactants, brominated flame retardant, and preservatives. The method was optimized using Box-Behnken statistical experimental design with response surface methodology and validated in terms of recovery, accuracy, precision, and method detection and quantification limits. Quantification of target compounds was carried out using matrix-matched calibration curves. The highest recoveries were achieved for the perfluorinated organic compounds (mean values up to 87%) and preservatives (up to 88%). The lowest recoveries were achieved for plasticizers (51%) and brominated flame retardant (63%). Method detection and quantification limits were in the ranges 0.01-0.09 ng/g dry matter (dm) and 0.02-0.30 ng/g dm, respectively, for most of the target compounds. The method was successfully applied to the determination of the target compounds on leaves from four tree species used as urban ornamental trees (Citrus aurantium, Celtis australis, Platanus hispanica, and Jacaranda mimosifolia). Graphical abstract Analytical method for the biomonitorization of emerging pollutants in outdoor air.

  14. EVALUATION OF ANALYTICAL METHODS FOR DETERMINING PESTICIDES IN BABY FOOD

    Science.gov (United States)

    Three extraction methods and two detection techniques for determining pesticides in baby food were evaluated. The extraction techniques examined were supercritical fluid extraction (SFE), enhanced solvent extraction (ESE), and solid phase extraction (SPE). The detection techni...

  15. Analytical methods for measuring 10Be in marine sediments

    International Nuclear Information System (INIS)

    Graham, I.J.; Ditchburn, R.G.; Sparks, R.J.; Whitehead, N.E.

    1995-01-01

    A suite of marine sediments from the Wanganui Basin (Graham et al. 1995) has provided excellent material to further develop methods for 10 Be analysis at the Institute of Geological and Nuclear Sciences AMS facility. Chemical methods for Be extraction have been streamlined and there has been some reduction of backgrounds and contamination peaks for 1 0Be isotopic analysis. (authors) 12 refs., 5 figs., 1 tab

  16. Testing and Validation of Computational Methods for Mass Spectrometry.

    Science.gov (United States)

    Gatto, Laurent; Hansen, Kasper D; Hoopmann, Michael R; Hermjakob, Henning; Kohlbacher, Oliver; Beyer, Andreas

    2016-03-04

    High-throughput methods based on mass spectrometry (proteomics, metabolomics, lipidomics, etc.) produce a wealth of data that cannot be analyzed without computational methods. The impact of the choice of method on the overall result of a biological study is often underappreciated, but different methods can result in very different biological findings. It is thus essential to evaluate and compare the correctness and relative performance of computational methods. The volume of the data as well as the complexity of the algorithms render unbiased comparisons challenging. This paper discusses some problems and challenges in testing and validation of computational methods. We discuss the different types of data (simulated and experimental validation data) as well as different metrics to compare methods. We also introduce a new public repository for mass spectrometric reference data sets ( http://compms.org/RefData ) that contains a collection of publicly available data sets for performance evaluation for a wide range of different methods.

  17. Optimal analytic method for the nonlinear Hasegawa-Mima equation

    Science.gov (United States)

    Baxter, Mathew; Van Gorder, Robert A.; Vajravelu, Kuppalapalle

    2014-05-01

    The Hasegawa-Mima equation is a nonlinear partial differential equation that describes the electric potential due to a drift wave in a plasma. In the present paper, we apply the method of homotopy analysis to a slightly more general Hasegawa-Mima equation, which accounts for hyper-viscous damping or viscous dissipation. First, we outline the method for the general initial/boundary value problem over a compact rectangular spatial domain. We use a two-stage method, where both the convergence control parameter and the auxiliary linear operator are optimally selected to minimize the residual error due to the approximation. To do the latter, we consider a family of operators parameterized by a constant which gives the decay rate of the solutions. After outlining the general method, we consider a number of concrete examples in order to demonstrate the utility of this approach. The results enable us to study properties of the initial/boundary value problem for the generalized Hasegawa-Mima equation. In several cases considered, we are able to obtain solutions with extremely small residual errors after relatively few iterations are computed (residual errors on the order of 10-15 are found in multiple cases after only three iterations). The results demonstrate that selecting a parameterized auxiliary linear operator can be extremely useful for minimizing residual errors when used concurrently with the optimal homotopy analysis method, suggesting that this approach can prove useful for a number of nonlinear partial differential equations arising in physics and nonlinear mechanics.

  18. Development and validation of simple RP-HPLC-PDA analytical protocol for zileuton assisted with Design of Experiments for robustness determination

    OpenAIRE

    Saurabh B. Ganorkar; Dinesh M. Dhumal; Atul A. Shirkhedkar

    2017-01-01

    A simple, rapid, sensitive, robust, stability-indicating RP-HPLC-PDA analytical protocol was developed and validated for the analysis of zileuton racemate in bulk and in tablet formulation. Development of method and resolution of degradation products from forced; hydrolytic (acidic, basic, neutral), oxidative, photolytic (acidic, basic, neutral, solid state) and thermal (dry heat) degradation was achieved on a LC – GC Qualisil BDS C18 column (250 mm × 4.6 mm × 5 μm) by isocratic mode at ambie...

  19. Analytical methods for quantitative evaluation of the radiocardiagram

    Energy Technology Data Exchange (ETDEWEB)

    Wolberg, J R [Technion-Israel Inst. of Tech., Haifa; Freedman, G S [Yale Univ., New Haven, Conn. (USA). School of Medicine; Dwyer, A [St. Raphael Hospital, New Haven, Conn., U.S.A.

    1975-01-01

    Radiocardiagrams are obtained by monitoring a radioisotope after injection as it passes through the heart and lungs. The purpose of this paper is to discuss several methods used to evaluate cardiac performance from radiocardiagram data. Mathematical models are developed for extracting two parameters of interest to cardiologists: cardiac chamber flow to volume ratio (F/V) and left ventricle ejection fraction (E.F.). The model used to characterize F/V is continuous and provides good agreement with data obtained by other physiological methods for the right heart. A discrete model is used to characterize the left heart and obtain E.F. Comparison has been made with other methods for obtaining E.F. for twelve patients with various types of cardiac disease. An important aspect of the E.F. model is that background interference is taken into consideration. The analyses include calculations of the statistical uncertainties associated with the computed values of both parameters.

  20. Fast analytical method for the addition of random variables

    International Nuclear Information System (INIS)

    Senna, V.; Milidiu, R.L.; Fleming, P.V.; Salles, M.R.; Oliveria, L.F.S.

    1983-01-01

    Using the minimal cut sets representation of a fault tree, a new approach to the method of moments is proposed in order to estimate confidence bounds to the top event probability. The method utilizes two or three moments either to fit a distribution (the normal and lognormal families) or to evaluate bounds from standard inequalities (e.g. Markov, Tchebycheff, etc.) Examples indicate that the results obtained by the log-normal family are in good agreement with those obtained by Monte Carlo simulation

  1. Development and Validation of Improved Method for Fingerprint ...

    African Journals Online (AJOL)

    Purpose: To develop and validate an improved method by capillary zone electrophoresis with photodiode array detection for the fingerprint analysis of Ligusticum chuanxiong Hort. (Rhizoma Chuanxiong). Methods: The optimum high performance capillary electrophoresis (HPCE) conditions were 30 mM borax containing 5 ...

  2. Development and Validation of a Bioanalytical Method for Direct ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a user-friendly spiked plasma method for the extraction of diclofenac potassium that reduces the number of treatments with plasma sample, in order to minimize human error. Method: Instead of solvent evaporation technique, the spiked plasma sample was modified with H2SO4 and NaCl, ...

  3. Triangulation, Respondent Validation, and Democratic Participation in Mixed Methods Research

    Science.gov (United States)

    Torrance, Harry

    2012-01-01

    Over the past 10 years or so the "Field" of "Mixed Methods Research" (MMR) has increasingly been exerting itself as something separate, novel, and significant, with some advocates claiming paradigmatic status. Triangulation is an important component of mixed methods designs. Triangulation has its origins in attempts to validate research findings…

  4. An Analytical framework of social learning facilitated by participatory methods

    NARCIS (Netherlands)

    Scholz, G.; Dewulf, A.; Pahl-Wostl, C.

    2014-01-01

    Social learning among different stakeholders is often a goal in problem solving contexts such as environmental management. Participatory methods (e.g., group model-building and role playing games) are frequently assumed to stimulate social learning. Yet understanding if and why this assumption is

  5. Analytic Method for Pressure Recovery in Truncated Diffusers ...

    African Journals Online (AJOL)

    A prediction method is presented for the static pressure recovery in subsonic axisymmetric truncated conical diffusers. In the analysis, a turbulent boundary layer is assumed at the diffuser inlet and a potential core exists throughout the flow. When flow separation occurs, this approach cannot be used to predict the maximum ...

  6. Analytic method for solitary solutions of some partial differential equations

    Energy Technology Data Exchange (ETDEWEB)

    Ugurlu, Yavuz [Firat University, Department of Mathematics, 23119 Elazig (Turkey); Kaya, Dogan [Firat University, Department of Mathematics, 23119 Elazig (Turkey)], E-mail: dkaya@firat.edu.tr

    2007-10-22

    In this Letter by considering an improved tanh function method, we found some exact solutions of the clannish random walker's parabolic equation, the modified Korteweg-de Vries (KdV) equation, and the Sharma-Tasso-Olver (STO) equation with its fission and fusion, the Jaulent-Miodek equation.

  7. Analytic method for solitary solutions of some partial differential equations

    International Nuclear Information System (INIS)

    Ugurlu, Yavuz; Kaya, Dogan

    2007-01-01

    In this Letter by considering an improved tanh function method, we found some exact solutions of the clannish random walker's parabolic equation, the modified Korteweg-de Vries (KdV) equation, and the Sharma-Tasso-Olver (STO) equation with its fission and fusion, the Jaulent-Miodek equation

  8. Pressurised liquid extraction of flavonoids in onions. Method development and validation

    DEFF Research Database (Denmark)

    Søltoft, Malene; Christensen, J.H.; Nielsen, J.

    2009-01-01

    A rapid and reliable analytical method for quantification of flavonoids in onions was developed and validated. Five extraction methods were tested on freeze-dried onions and subsequently high performance liquid chromatography (HPLC) with UV detection was used for quantification of seven flavonoids...... extraction methods. However. PLE was the preferred extraction method because the method can be highly automated, use only small amounts of solvents, provide the cleanest extracts, and allow the extraction of light and oxygen-sensitive flavonoids to be carried out in an inert atmosphere protected from light......-step PLE method showed good selectivity, precision (RSDs = 3.1-11%) and recovery of the extractable flavonoids (98-99%). The method also appeared to be a multi-method, i.e. generally applicable to, e.g. phenolic acids in potatoes and carrots....

  9. Validation of Land Cover Products Using Reliability Evaluation Methods

    Directory of Open Access Journals (Sweden)

    Wenzhong Shi

    2015-06-01

    Full Text Available Validation of land cover products is a fundamental task prior to data applications. Current validation schemes and methods are, however, suited only for assessing classification accuracy and disregard the reliability of land cover products. The reliability evaluation of land cover products should be undertaken to provide reliable land cover information. In addition, the lack of high-quality reference data often constrains validation and affects the reliability results of land cover products. This study proposes a validation schema to evaluate the reliability of land cover products, including two methods, namely, result reliability evaluation and process reliability evaluation. Result reliability evaluation computes the reliability of land cover products using seven reliability indicators. Process reliability evaluation analyzes the reliability propagation in the data production process to obtain the reliability of land cover products. Fuzzy fault tree analysis is introduced and improved in the reliability analysis of a data production process. Research results show that the proposed reliability evaluation scheme is reasonable and can be applied to validate land cover products. Through the analysis of the seven indicators of result reliability evaluation, more information on land cover can be obtained for strategic decision-making and planning, compared with traditional accuracy assessment methods. Process reliability evaluation without the need for reference data can facilitate the validation and reflect the change trends of reliabilities to some extent.

  10. Semi-Analytical method for the pricing of barrier options in case of time-dependent parameters (with Matlab® codes

    Directory of Open Access Journals (Sweden)

    Guardasoni C.

    2018-03-01

    Full Text Available A Semi-Analytical method for pricing of Barrier Options (SABO is presented. The method is based on the foundations of Boundary Integral Methods which is recast here for the application to barrier option pricing in the Black-Scholes model with time-dependent interest rate, volatility and dividend yield. The validity of the numerical method is illustrated by several numerical examples and comparisons.

  11. Analytical method to evaluate fuel consumption of hybrid electric vehicles at balanced energy content of the electric storage devices

    Energy Technology Data Exchange (ETDEWEB)

    Katrasnik, Tomaz [University of Ljubljana, Faculty of Mechanical Engineering, Askerceva 6, 1000 Ljubljana (Slovenia)

    2010-11-15

    Innovative analytically based method to calculate corrected fuel consumption of parallel and series hybrid electric vehicles (HEVs) at balanced energy content of the electric storage devices is proposed and validated in the paper. The proposed analytical method is generally applicable and features highly accurate corrected fuel consumption results. It enables calculation of the corrected fuel consumption out of a single fuel consumption test run in a single analytic post-processing step. An additional fuel consumption test run might be needed to obtain highly accurate results if ratio of the energy content deviation of the electric storage devices to the energy used for vehicle propulsion over the test cycle is high. Proposed method enables consideration of non-linear energy flow changes and non-linear HEV component efficiency changes caused by the energy management strategy or by the component characteristics. The method therefore features highly accurate results out of the minimum number of fuel consumption test runs and thus optimizes workload for development or optimization of HEVs. The input data of the method are characteristic energy flows and efficiencies that are derived from the energy flows on selected energy paths of HEVs. (author)

  12. Validación de un método de análisis para la determinación de hidrocarburos aromáticos policíclicos por cromatografía líquida de alta eficiencia en partículas PM10 Y PM2,5 Validation of an analytical method for the determination of polycyclic aromatic hydrocarbons by high efficiency liquid chromatography in PM10 and PM2, 5

    Directory of Open Access Journals (Sweden)

    Jorge Herrera Murillo

    2012-11-01

    Full Text Available Se validó un método analítico para la determinación de hidrocarburos aromáticos policíclicos presentes en partículas PM10 y PM 2,5 recolectadas en el aire mediante cromatografía líquida de alta resolución (CLAR. Los HPA incluidos en la metodología comprenden: Naftaleno, Acenaftileno, Fluoreno, Acenafteno, Fenantreno, Antraceno, Fluoranteno, Pireno, Benzo (aantraceno, Criseno, Benzo (bfluoranteno, Benzo (kfluoranteno, Benzo (apireno, Dibenzo (a,h antraceno, Benzo (g,h,iperileno y Indeno (1,2,3- C.D pireno. Para estos compuestos, los límites de detección y cuantificación estuvieron entre 0,02 y 0,1 mg/l utilizando un equipo marca Dionex modelo ICS- 3000, el cual consta de dos detectores en serie, un ultravioleta modelo VWD-1 y un detector de fluorescencia modelo RF-2000, permitiendo diferenciar las distintas señales de absorción y emisión para la debida identificación de los distintos compuestos. Para todos los compuestos analizados, el factor de recuperación resultó no ser significativamente diferente de uno y la repetibilidad y reproducibilidad resultó ser adecuada para un método analítico, especialmente para los HPA más ligeros.An analytical method for polycyclic aromatic hydrocarbons in PM10 and PM 2.5 par ticles collected from air by high performance liquid chromatography (HPLC was validated. The PAHs analyzed in the methodology include: Naphthalene, Acenaphthylene, Fluorene, Acenaphthene, Phenanthrene, Anthracene, fluoranthene,pyrene,Benzo(aanthracene,Chrysene, Benzo (bfluoranthene, Benzo (kfluoranthene, Benzo (apyrene Dibenzo (a, hanthracene, Benzo (g, h, iperylene and Indeno (1,2,3-CDpyrene. For these compounds, the detection limit and quantification limit were between 0,02 and 0,1 mg/l using a DIONEX ICS 3000 model cromatograph, that has two in serie detectors: UV/Vis and Fluorescense, separating the different absorption and emission signals for proper identification of individual compounds. For all the compounds

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

    Science.gov (United States)

    Ermacora, Alessia; Hrnčiřík, Karel

    2014-01-01

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

  14. Analytic model for ultrasound energy receivers and their optimal electric loads II: Experimental validation

    Science.gov (United States)

    Gorostiaga, M.; Wapler, M. C.; Wallrabe, U.

    2017-10-01

    In this paper, we verify the two optimal electric load concepts based on the zero reflection condition and on the power maximization approach for ultrasound energy receivers. We test a high loss 1-3 composite transducer, and find that the measurements agree very well with the predictions of the analytic model for plate transducers that we have developed previously. Additionally, we also confirm that the power maximization and zero reflection loads are very different when the losses in the receiver are high. Finally, we compare the optimal load predictions by the KLM and the analytic models with frequency dependent attenuation to evaluate the influence of the viscosity.

  15. Approximate Analytic Solutions for the Two-Phase Stefan Problem Using the Adomian Decomposition Method

    Directory of Open Access Journals (Sweden)

    Xiao-Ying Qin

    2014-01-01

    Full Text Available An Adomian decomposition method (ADM is applied to solve a two-phase Stefan problem that describes the pure metal solidification process. In contrast to traditional analytical methods, ADM avoids complex mathematical derivations and does not require coordinate transformation for elimination of the unknown moving boundary. Based on polynomial approximations for some known and unknown boundary functions, approximate analytic solutions for the model with undetermined coefficients are obtained using ADM. Substitution of these expressions into other equations and boundary conditions of the model generates some function identities with the undetermined coefficients. By determining these coefficients, approximate analytic solutions for the model are obtained. A concrete example of the solution shows that this method can easily be implemented in MATLAB and has a fast convergence rate. This is an efficient method for finding approximate analytic solutions for the Stefan and the inverse Stefan problems.

  16. Assessment of Two Analytical Methods in Solving the Linear and Nonlinear Elastic Beam Deformation Problems

    DEFF Research Database (Denmark)

    Barari, Amin; Ganjavi, B.; Jeloudar, M. Ghanbari

    2010-01-01

    and fluid mechanics. Design/methodology/approach – Two new but powerful analytical methods, namely, He's VIM and HPM, are introduced to solve some boundary value problems in structural engineering and fluid mechanics. Findings – Analytical solutions often fit under classical perturbation methods. However......, as with other analytical techniques, certain limitations restrict the wide application of perturbation methods, most important of which is the dependence of these methods on the existence of a small parameter in the equation. Disappointingly, the majority of nonlinear problems have no small parameter at all......Purpose – In the last two decades with the rapid development of nonlinear science, there has appeared ever-increasing interest of scientists and engineers in the analytical techniques for nonlinear problems. This paper considers linear and nonlinear systems that are not only regarded as general...

  17. Numerical Validation of the Delaunay Normalization and the Krylov-Bogoliubov-Mitropolsky Method

    Directory of Open Access Journals (Sweden)

    David Ortigosa

    2014-01-01

    Full Text Available A scalable second-order analytical orbit propagator programme based on modern and classical perturbation methods is being developed. As a first step in the validation and verification of part of our orbit propagator programme, we only consider the perturbation produced by zonal harmonic coefficients in the Earth’s gravity potential, so that it is possible to analyze the behaviour of the mathematical expressions involved in Delaunay normalization and the Krylov-Bogoliubov-Mitropolsky method in depth and determine their limits.

  18. Validation of a method to determine methylmercury in fish tissues using gas chromatography

    International Nuclear Information System (INIS)

    Vega Bolannos, Luisa O.; Arias Verdes, Jose A.; Beltran Llerandi, Gilberto; Castro Diaz, Odalys; Moreno Tellez, Olga L.

    2000-01-01

    We validated a method to determine methylmercury in fish tissues using gas chromatography with an electron capture detector as described by the Association of Official Analytical Chemist (AOAC) International. The linear curve range was 0.02 to 1 g/ml and linear correlation coefficient was 0.9979. A 1 mg/kg methylmercury-contaminated fish sample was analyzed 20 times to determine repeatability of the method. The quantification limit was 0.16 mg/kg and detection limit was 0.06 ppm. Fish samples contaminated with 0.2 to 10 mg/kg methylmercury showed recovery indexes from 94.66 to 108.8%

  19. A new robust method for the treatment of analytical data

    International Nuclear Information System (INIS)

    Pearton, D.C.G.

    1982-01-01

    A new robust method is proposed for the calculation of the median and the relative standard deviation for a set of data containing unsymmetrically placed outliers. Examples of the advantages of the new method are given, the findings being confirmed by Monte Carlo tests. At Mintek mass-spectrometric data are often unsymmetrical, and all outliers are often at one of the extremities, either all high or all low. In some instances the outliers can be seen visually, and would therefore be rejected on sight. However, when large sets of results are processed, such as those from mass-spectrometric, X-ray fluorescence, and neutron-activation analyses, or in fields such as the assignment of values to reference materials, the sets of results are often too large for visual inspection and are processed within the computer

  20. The analytic method for calculating the control rod worth

    International Nuclear Information System (INIS)

    Kim, Han Gon; Lee, Byeong Ho; Chang, Soon Heung

    1989-01-01

    We calculated the control rod worth in this paper. To avoid complexity, we did not consider burnable poisons and soluble boron. The system was localized within one assembly. The control rod was treated as not an absorber but an another boundary. Thus all of the group constants were unchanged before and after control rod insertion. And we discussed the method for calculation of the reactivity of the whole core

  1. Analytical methods applied to diverse types of Brazilian propolis

    Directory of Open Access Journals (Sweden)

    Marcucci Maria

    2011-06-01

    Full Text Available Abstract Propolis is a bee product, composed mainly of plant resins and beeswax, therefore its chemical composition varies due to the geographic and plant origins of these resins, as well as the species of bee. Brazil is an important supplier of propolis on the world market and, although green colored propolis from the southeast is the most known and studied, several other types of propolis from Apis mellifera and native stingless bees (also called cerumen can be found. Propolis is usually consumed as an extract, so the type of solvent and extractive procedures employed further affect its composition. Methods used for the extraction; analysis the percentage of resins, wax and insoluble material in crude propolis; determination of phenolic, flavonoid, amino acid and heavy metal contents are reviewed herein. Different chromatographic methods applied to the separation, identification and quantification of Brazilian propolis components and their relative strengths are discussed; as well as direct insertion mass spectrometry fingerprinting. Propolis has been used as a popular remedy for several centuries for a wide array of ailments. Its antimicrobial properties, present in propolis from different origins, have been extensively studied. But, more recently, anti-parasitic, anti-viral/immune stimulating, healing, anti-tumor, anti-inflammatory, antioxidant and analgesic activities of diverse types of Brazilian propolis have been evaluated. The most common methods employed and overviews of their relative results are presented.

  2. Survey of analytical methods for environmental monitoring of krypton-85

    International Nuclear Information System (INIS)

    Jaquish, R.E.; Moghissi, A.A.

    1973-01-01

    Numerous methods have been developed for measuring krypton-85 in air as krypton ultimately accumulates in air once it is released into the environment. However, krypton-85 can be present in other media such as natural gas from wells stimulated with nuclear devices or in water when krypton-85 is used for aeration studies. Methods for the measurement of ambient levels of krypton-85 require a concentration of krypton from a large air sample of one m 3 or more. If elevated levels are to be measured, carrier krypton may be used provided the contamination of atmospheric krypton with krypton-85 does not interfere with the measurement. In certain cases, such as in the vicinity of nuclear fuel processing plants, direct measurement techniques may be used. A variety of techniques are employed for krypton-85 counting. At low levels, internal gas counting or organic scintillation is used to measure the beta emission of this radionuclide. At higher levels the gamma emission of krypton-85 may be measured using scintillation or solid state gamma spectroscopic methods. Techniques for collection of the sample, concentration of krypton, and radioactivity measurement of krypton-85 are discussed and various processes are critically evaluated and compared

  3. [Progress in sample preparation and analytical methods for trace polar small molecules in complex samples].

    Science.gov (United States)

    Zhang, Qianchun; Luo, Xialin; Li, Gongke; Xiao, Xiaohua

    2015-09-01

    Small polar molecules such as nucleosides, amines, amino acids are important analytes in biological, food, environmental, and other fields. It is necessary to develop efficient sample preparation and sensitive analytical methods for rapid analysis of these polar small molecules in complex matrices. Some typical materials in sample preparation, including silica, polymer, carbon, boric acid and so on, are introduced in this paper. Meanwhile, the applications and developments of analytical methods of polar small molecules, such as reversed-phase liquid chromatography, hydrophilic interaction chromatography, etc., are also reviewed.

  4. 76 FR 28664 - Method 301-Field Validation of Pollutant Measurement Methods From Various Waste Media

    Science.gov (United States)

    2011-05-18

    ... . d m = The mean of the paired sample differences. n = Total number of paired samples. 7.4.2 t Test... being compared to a validated test method as part of the Method 301 validation and an audit sample for... tighten the acceptance criteria for the precision of candidate alternative test methods. One commenter...

  5. Review and evaluation of spark source mass spectrometry as an analytical method

    International Nuclear Information System (INIS)

    Beske, H.E.

    1981-01-01

    The analytical features and most important fields of application of spark source mass spectrometry are described with respect to the trace analysis of high-purity materials and the multielement analysis of technical alloys, geochemical and cosmochemical, biological and radioactive materials, as well as in environmental analysis. Comparisons are made to other analytical methods. The distribution of the method as well as opportunities for contract analysis are indicated and developmental tendencies discussed. (orig.) [de

  6. Critical node treatment in the analytic function expansion method for Pin Power Reconstruction

    International Nuclear Information System (INIS)

    Gao, Z.; Xu, Y.; Downar, T.

    2013-01-01

    Pin Power Reconstruction (PPR) was implemented in PARCS using the eight term analytic function expansion method (AFEN). This method has been demonstrated to be both accurate and efficient. However, similar to all the methods involving analytic functions, such as the analytic node method (ANM) and AFEN for nodal solution, the use of AFEN for PPR also has potential numerical issue with critical nodes. The conventional analytic functions are trigonometric or hyperbolic sine or cosine functions with an angular frequency proportional to buckling. For a critic al node the buckling is zero and the sine functions becomes zero, and the cosine function become unity. In this case, the eight terms of the analytic functions are no longer distinguishable from ea ch other which makes their corresponding coefficients can no longer be determined uniquely. The mode flux distribution of critical node can be linear while the conventional analytic functions can only express a uniform distribution. If there is critical or near critical node in a plane, the reconstructed pin power distribution is often be shown negative or very large values using the conventional method. In this paper, we propose a new method to avoid the numerical problem wit h critical nodes which uses modified trigonometric or hyperbolic sine functions which are the ratio of trigonometric or hyperbolic sine and its angular frequency. If there are no critical or near critical nodes present, the new pin power reconstruction method with modified analytic functions are equivalent to the conventional analytic functions. The new method is demonstrated using the L336C5 benchmark problem. (authors)

  7. Critical node treatment in the analytic function expansion method for Pin Power Reconstruction

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Z. [Rice University, MS 318, 6100 Main Street, Houston, TX 77005 (United States); Xu, Y. [Argonne National Laboratory, 9700 South Case Ave., Argonne, IL 60439 (United States); Downar, T. [Department of Nuclear Engineering, University of Michigan, 2355 Bonisteel blvd., Ann Arbor, MI 48109 (United States)

    2013-07-01

    Pin Power Reconstruction (PPR) was implemented in PARCS using the eight term analytic function expansion method (AFEN). This method has been demonstrated to be both accurate and efficient. However, similar to all the methods involving analytic functions, such as the analytic node method (ANM) and AFEN for nodal solution, the use of AFEN for PPR also has potential numerical issue with critical nodes. The conventional analytic functions are trigonometric or hyperbolic sine or cosine functions with an angular frequency proportional to buckling. For a critic al node the buckling is zero and the sine functions becomes zero, and the cosine function become unity. In this case, the eight terms of the analytic functions are no longer distinguishable from ea ch other which makes their corresponding coefficients can no longer be determined uniquely. The mode flux distribution of critical node can be linear while the conventional analytic functions can only express a uniform distribution. If there is critical or near critical node in a plane, the reconstructed pin power distribution is often be shown negative or very large values using the conventional method. In this paper, we propose a new method to avoid the numerical problem wit h critical nodes which uses modified trigonometric or hyperbolic sine functions which are the ratio of trigonometric or hyperbolic sine and its angular frequency. If there are no critical or near critical nodes present, the new pin power reconstruction method with modified analytic functions are equivalent to the conventional analytic functions. The new method is demonstrated using the L336C5 benchmark problem. (authors)

  8. HPLC method validated for the simultaneous analysis of cichoric acid and alkamides in Echinacea purpurea plants and products

    DEFF Research Database (Denmark)

    Mølgaard, Per; Johnsen, Søren; Christensen, Peter

    2003-01-01

    phenolics as well as the lipophilic alkamides are released from the samples, followed by the analytical HPLC procedure for quantitative determination of these compounds. The method is the first one validated for the determination of these two groups of compounds in the same procedure. Naringenin has been...

  9. Validation of a chromatographic method for quantitation of 50 μg/mL Latanoprost in a Cuban eye drops

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad Margarita; Martinez Espinosa, Vivian; Gonzalez Cortezon, Ania

    2012-01-01

    Latanoprost is indicated to treat high intraocular pressure in patients suffering from ocular hypertension or from open angle glaucoma. To develop and to validate a high performance liquid chromatography-based analytical method for quality control of 50 μg/mL Latanoprost eye drops

  10. JRC Guidelines for 1 - Selecting and/or validating analytical methods for cosmetics 2 - Recommending standardization steps of analytical methods

    OpenAIRE

    VINCENT Ursula

    2015-01-01

    The analysis of cosmetics constitutes a challenge mainly due to the large variety of ingredients and formulations, and to the complexity of cosmetic products, in particular due to huge matrix variability. In 2009, the European Commission issued a Regulation (Regulation (EC) N° 1223/2009 of the European Parliament and of the Council) establishing the requisites for cosmetic products and the responsibilities of the stakeholders. While the manufacturers' are responsible to ensure the safety of t...

  11. A Vocal-Based Analytical Method for Goose Behaviour Recognition

    Directory of Open Access Journals (Sweden)

    Henrik Karstoft

    2012-03-01

    Full Text Available Since human-wildlife conflicts are increasing, the development of cost-effective methods for reducing damage or conflict levels is important in wildlife management. A wide range of devices to detect and deter animals causing conflict are used for this purpose, although their effectiveness is often highly variable, due to habituation to disruptive or disturbing stimuli. Automated recognition of behaviours could form a critical component of a system capable of altering the disruptive stimuli to avoid this. In this paper we present a novel method to automatically recognise goose behaviour based on vocalisations from flocks of free-living barnacle geese (Branta leucopsis. The geese were observed and recorded in a natural environment, using a shielded shotgun microphone. The classification used Support Vector Machines (SVMs, which had been trained with labeled data. Greenwood Function Cepstral Coefficients (GFCC were used as features for the pattern recognition algorithm, as they can be adjusted to the hearing capabilities of different species. Three behaviours are classified based in this approach, and the method achieves a good recognition of foraging behaviour (86–97% sensitivity, 89–98% precision and a reasonable recognition of flushing (79–86%, 66–80% and landing behaviour(73–91%, 79–92%. The Support Vector Machine has proven to be a robust classifier for this kind of classification, as generality and non-linearcapabilities are important. We conclude that vocalisations can be used to automatically detect behaviour of conflict wildlife species, and as such, may be used as an integrated part of awildlife management system.

  12. [Analytic methods for seed models with genotype x environment interactions].

    Science.gov (United States)

    Zhu, J

    1996-01-01

    Genetic models with genotype effect (G) and genotype x environment interaction effect (GE) are proposed for analyzing generation means of seed quantitative traits in crops. The total genetic effect (G) is partitioned into seed direct genetic effect (G0), cytoplasm genetic of effect (C), and maternal plant genetic effect (Gm). Seed direct genetic effect (G0) can be further partitioned into direct additive (A) and direct dominance (D) genetic components. Maternal genetic effect (Gm) can also be partitioned into maternal additive (Am) and maternal dominance (Dm) genetic components. The total genotype x environment interaction effect (GE) can also be partitioned into direct genetic by environment interaction effect (G0E), cytoplasm genetic by environment interaction effect (CE), and maternal genetic by environment interaction effect (GmE). G0E can be partitioned into direct additive by environment interaction (AE) and direct dominance by environment interaction (DE) genetic components. GmE can also be partitioned into maternal additive by environment interaction (AmE) and maternal dominance by environment interaction (DmE) genetic components. Partitions of genetic components are listed for parent, F1, F2 and backcrosses. A set of parents, their reciprocal F1 and F2 seeds is applicable for efficient analysis of seed quantitative traits. MINQUE(0/1) method can be used for estimating variance and covariance components. Unbiased estimation for covariance components between two traits can also be obtained by the MINQUE(0/1) method. Random genetic effects in seed models are predictable by the Adjusted Unbiased Prediction (AUP) approach with MINQUE(0/1) method. The jackknife procedure is suggested for estimation of sampling variances of estimated variance and covariance components and of predicted genetic effects, which can be further used in a t-test for parameter. Unbiasedness and efficiency for estimating variance components and predicting genetic effects are tested by

  13. Validation of calculational methods for nuclear criticality safety - approved 1975

    International Nuclear Information System (INIS)

    Anon.

    1977-01-01

    The American National Standard for Nuclear Criticality Safety in Operations with Fissionable Materials Outside Reactors, N16.1-1975, states in 4.2.5: In the absence of directly applicable experimental measurements, the limits may be derived from calculations made by a method shown to be valid by comparison with experimental data, provided sufficient allowances are made for uncertainties in the data and in the calculations. There are many methods of calculation which vary widely in basis and form. Each has its place in the broad spectrum of problems encountered in the nuclear criticality safety field; however, the general procedure to be followed in establishing validity is common to all. The standard states the requirements for establishing the validity and area(s) of applicability of any calculational method used in assessing nuclear criticality safety

  14. A Complete Validated Learning Analytics Framework: Designing Issues from Data Preparation Perspective

    Science.gov (United States)

    Tlili, Ahmed; Essalmi, Fathi; Jemni, Mohamed; Kinshuk; Chen, Nian-Shing

    2018-01-01

    With the rapid growth of online education in recent years, Learning Analytics (LA) has gained increasing attention from researchers and educational institutions as an area which can improve the overall effectiveness of learning experiences. However, the lack of guidelines on what should be taken into consideration during application of LA hinders…

  15. Selected methods of waste monitoring using modern analytical techniques

    International Nuclear Information System (INIS)

    Hlavacek, I.; Hlavackova, I.

    1993-11-01

    Issues of the inspection and control of bituminized and cemented waste are discussed, and some methods of their nondestructive testing are described. Attention is paid to the inspection techniques, non-nuclear spectral techniques in particular, as employed for quality control of the wastes, waste concentrates, spent waste leaching solutions, as well as for the examination of environmental samples (waters and soils) from the surroundings of nuclear power plants. Some leaching tests used abroad for this purpose and practical analyses by the ICP-AES technique are given by way of example. The ICP-MS technique, which is unavailable in the Czech Republic, is routinely employed abroad for alpha nuclide measurements; examples of such analyses are also given. The next topic discussed includes the monitoring of organic acids and complexants to determine the degree of their thermal decomposition during the bituminization of wastes on an industrial line. All of the methods and procedures highlighted can be used as technical support during the monitoring of radioactive waste properties in industrial conditions, in the chemical and radiochemical analyses of wastes and related matter, in the calibration of nondestructive testing instrumentation, in the monitoring of contamination of the surroundings of nuclear facilities, and in trace analysis. (author). 10 tabs., 1 fig., 14 refs

  16. Applications of Nuclear Analytical Methods for High Tech Industry

    International Nuclear Information System (INIS)

    Hossain, T.

    2013-01-01

    Silicon based semiconductor chip manufacturing is a worldwide high technology industry with numerous measurement issues. One of the major concerns in the semiconductor manufacturing is contamination such as the trace metal impurities. This concern is vividly illustrated by the fact that the manufacturing in this industry is done in ultra clean environment where the entire manufacturing facility or “Fab” is a clean room facility or each and every manufacturing tool is enclosed in a mini-environment Although semiconductor devices are fabricated on the surface of the Si wafers contamination in the bulk material is a major concern. Nuclear methods of analysis are uniquely suited for the contamination analysis in such a matrix. Many opportunities in the semiconductor manufacturing field exist for the nuclear methods to provide support services. Contamination analysis by NAA, depth profiles by NDP and prompt gamma analysis of H in thin films are a few examples. These needs are on-going and require commitment from the lab so that a manufacturing operation can rely on the delivery of these services when required

  17. An analytical investigation on unsteady motion of vertically falling spherical particles in non-Newtonian fluid by Collocation Method

    Directory of Open Access Journals (Sweden)

    M. Rahimi-Gorji

    2015-06-01

    Full Text Available An analytical investigation is applied for unsteady motion of a rigid spherical particle in a quiescent shear-thinning power-law fluid. The results were compared with those obtained from Collocation Method (CM and the established Numerical Method (Fourth order Runge–Kutta scheme. It was shown that CM gave accurate results. Collocation Method (CM and Numerical Method are used to solve the present problem. We obtained that the CM which was used to solve such nonlinear differential equation with fractional power is simpler and more accurate than series method such as HPM which was used in some previous works by others but the new method named Akbari-Ganji’s Method (AGM is an accurate and simple method which is slower than CM for solving such problems. The terminal settling velocity—that is the velocity at which the net forces on a falling particle eliminate—for three different spherical particles (made of plastic, glass and steel and three flow behavior index n, in three sets of power-law non-Newtonian fluids was investigated, based on polynomial solution (CM. Analytical results obtained indicated that the time of reaching the terminal velocity in a falling procedure is significantly increased with growing of the particle size that validated with Numerical Method. Further, with approaching flow behavior to Newtonian behavior from shear-thinning properties of flow (n → 1, the transient time to achieving the terminal settling velocity is decreased.

  18. Using an analytical geometry method to improve tiltmeter data presentation

    Science.gov (United States)

    Su, W.-J.

    2000-01-01

    The tiltmeter is a useful tool for geologic and geotechnical applications. To obtain full benefit from the tiltmeter, easy and accurate data presentations should be used. Unfortunately, the most commonly used method for tilt data reduction now may yield inaccurate and low-resolution results. This article describes a simple, accurate, and high-resolution approach developed at the Illinois State Geological Survey for data reduction and presentation. The orientation of tiltplates is determined first by using a trigonometric relationship, followed by a matrix transformation, to obtain the true amount of rotation change of the tiltplate at any given time. The mathematical derivations used for the determination and transformation are then coded into an integrated PC application by adapting the capabilities of commercial spreadsheet, database, and graphics software. Examples of data presentation from tiltmeter applications in studies of landfill covers, characterizations of mine subsidence, and investigations of slope stability are also discussed.

  19. Manual of analytical methods for the Environmental Health Laboratory

    International Nuclear Information System (INIS)

    Gray, C.E.

    1975-06-01

    The manual contains four sections: absorption spectrophotometry; general radiochemical procedures; instrumental analysis; and calibration of field instruments. Included in the individual analyses using absorption spectrophotometry is one for total iodine in oil. Radiochemical procedures are given for: actinides in urine and water; 137 Cs in soil and vegetation; 137 Cs in soil, urine, vegetation, and water; enriched uranium in urine; gross beta activity in soil, urine, vegetation, and water; plutonium in urine and soil; 210 Po in urine and water; 24 Na in air, blood, urine, and water; 90 Sr in soil, vegetation, and water; tritium in urine, water, and on swipes; and total uranium on fallout trays and in soil, urine, and water. Among the individual instrumental analyses is a spectrographic method for determining beryllium in air samples and swipes. (U.S.)

  20. Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 4, Organic methods

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    This interim notice covers the following: extractable organic halides in solids, total organic halides, analysis by gas chromatography/Fourier transform-infrared spectroscopy, hexadecane extracts for volatile organic compounds, GC/MS analysis of VOCs, GC/MS analysis of methanol extracts of cryogenic vapor samples, screening of semivolatile organic extracts, GPC cleanup for semivolatiles, sample preparation for GC/MS for semi-VOCs, analysis for pesticides/PCBs by GC with electron capture detection, sample preparation for pesticides/PCBs in water and soil sediment, report preparation, Florisil column cleanup for pesticide/PCBs, silica gel and acid-base partition cleanup of samples for semi-VOCs, concentrate acid wash cleanup, carbon determination in solids using Coulometrics` CO{sub 2} coulometer, determination of total carbon/total organic carbon/total inorganic carbon in radioactive liquids/soils/sludges by hot persulfate method, analysis of solids for carbonates using Coulometrics` Model 5011 coulometer, and soxhlet extraction.