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Sample records for analytical methods validation

  1. Validation of analytical methods

    Directory of Open Access Journals (Sweden)

    Xavier Rius, F.

    2002-03-01

    Full Text Available In this paper we shall discuss the concept of method validation, describe the various elements and explain its close relationship with fitness for purpose. Method validation is based on the assumption that a series of requirements are fulfilled and we shall explain how these requirements are selected, the way in which evidence is supplied and what work has to be carried out in the laboratory. The basic principles of method validation and the different ways to validate a methodology, by inter-laboratory comparison or performing an in-house validation, are also described.En este artículo se discute el concepto de validación del método, se describen los elementos que la componen y se explica la fuerte relación entre la validación y las características de ajuste. El método de validación se basa en el cumplimiento de una serie de requerimientos, se explica como seleccionar esos requerimientos, la forma en que se suministran evidencias, y que trabajo se debe llevar a cabo en el laboratorio. También se describen, los principios básicos del método de validación y los diferentes caminos para validar una metodología, tanto en la comparación entre laboratorios o como cuando se lleva a cabo una validación dentro del laboratorio.

  2. ANALYTICAL METHOD VALIDATION: AN UPDATED REVIEW

    Directory of Open Access Journals (Sweden)

    G. Lavanya, M. Sunil, M.M. Eswarudu*, M. C. Eswaraiah, K. Harisudha and B. Naga Spandana

    2013-04-01

    Full Text Available ABSTRACT: The development of sound Analytical method(s is of supreme importance during the process of drug discovery, release to market and development, culminating in a marketing approval. The objective of this paper is to review the method development, optimize and validation of the method for the drug product from the developmental stage of the formulation to commercial batch of the product. Method development for the interested component in finished product or in process tests and the sample preparation of drug product and to provide practical approaches for determining selectivity, specificity, limit of detection, limit of quantitation, linearity, range accuracy, precision, recovery solution stability, ruggedness, and robustness of liquid chromatographic methods to support the Routine, in process and stability analysis.

  3. Development and validation of analytical methods for dietary supplements

    International Nuclear Information System (INIS)

    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. Oxcarbazepine: validation and application of an analytical method

    OpenAIRE

    Paula Cristina Rezende Enéas; Renata Barbosa de Oliveira; Gerson Antônio Pianetti

    2010-01-01

    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 ...

  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 Method Development & Validation for Related Substances Method of Busulfan Injection by Ion Chromatography Method

    Directory of Open Access Journals (Sweden)

    Rewaria S

    2013-05-01

    Full Text Available A new simple, accurate, precise and reproducible Ion chromatography method has been developed forthe estimation of Methane sulfonic acid in Busulfan injectable dosage. The method which is developedis also validated in complete compliance with the current regulatory guidelines by using well developedanalytical method validation techniques and tools which comprises with the analytical method validationparameters like Linearity, LOD and LOQ determination, Accuracy, Method precision, Specificity,System suitability, Robustness, Ruggedness etc. by adopting the current method the linearity obtained isnear to 0.999 and thus this shows that the method is capable to give a good detector response, therecovery calculated was within the range of 85% to 115% of the specification limits.

  7. Validation of analytical methods involved in dissolution assays: acceptance limits and decision methodologies.

    Science.gov (United States)

    Rozet, E; Ziemons, E; Marini, R D; Boulanger, B; Hubert, Ph

    2012-11-01

    Dissolution tests are key elements to ensure continuing product quality and performance. The ultimate goal of these tests is to assure consistent product quality within a defined set of specification criteria. Validation of an analytical method aimed at assessing the dissolution profile of products or at verifying pharmacopoeias compliance should demonstrate that this analytical method is able to correctly declare two dissolution profiles as similar or drug products as compliant with respect to their specifications. It is essential to ensure that these analytical methods are fit for their purpose. Method validation is aimed at providing this guarantee. However, even in the ICHQ2 guideline there is no information explaining how to decide whether the method under validation is valid for its final purpose or not. Are the entire validation criterion needed to ensure that a Quality Control (QC) analytical method for dissolution test is valid? What acceptance limits should be set on these criteria? How to decide about method's validity? These are the questions that this work aims at answering. Focus is made to comply with the current implementation of the Quality by Design (QbD) principles in the pharmaceutical industry in order to allow to correctly defining the Analytical Target Profile (ATP) of analytical methods involved in dissolution tests. Analytical method validation is then the natural demonstration that the developed methods are fit for their intended purpose and is not any more the inconsiderate checklist validation approach still generally performed to complete the filing required to obtain product marketing authorization. PMID:23084050

  8. Development and Validation of HPLC Methods for Analytical and Preparative Purposes

    OpenAIRE

    Lindholm, Johan

    2004-01-01

    This thesis concerns the development and validation of high performance liquid chromatography (HPLC) methods aimed for two industrially important areas: (i) analysis of biotechnological synthesis and (ii) determination of adsorption isotherm parameters. There is today a lack of detailed recommendations for analytical procedures in the field of biotechnological production of drugs. Therefore, guidelines were given for analytical development and validation in this field; the production of 9α-hy...

  9. Analytical Method Validation of Gamma Spectrometric Procedure for the Determination of γ-Emitters in Environmental Samples

    International Nuclear Information System (INIS)

    It is internationally recognized that validation is necessary in analytical laboratories. The use of validated methods is important for an analytical laboratory to show its qualification and competency. This work describes the methods for validation of gamma spectrometric analytical procedure in the determination of some gamma emitters in environmental samples. The method was tested and validated in terms of repeatability, trueness, reproducibility in accordance with ISO guidelines using IAEA reference materials with different matrixes and compositions

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

    International Nuclear Information System (INIS)

    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)

  11. Validation of analytical methods for food control. Report of a Joint FAO/IAEA expert consultation

    International Nuclear Information System (INIS)

    There is a continuing need for reliable analytical methods for use in determining compliance with national regulations as well as international requirements in all areas of food quality and safety. The reliability of a method is determined by some form of a validation procedure. The Codex Alimentarius Commission (CAC), for example, requires that in order for a method of analysis to be included in a Codex commodity standard, certain method performance information should be available. This includes specificity, accuracy, precision (repeatability, reproducibility), limit of detection, sensitivity, applicability and practicability, as appropriate. This very often requires an extensive collaborative study be undertaken to obtain the necessary data. Methods which have successfully undergone this performance review testing have been considered to be validated for purposes of analyses under Codex commodity standards. Within this environment, the entire area of validation of analytical methods used in food control for Codex purposes has been discussed at length by the CCMAS, as well as the CCRVDF and the Codex Committee on Pesticide Residues (CCPR). All three Committees supported the holding of a consultation to provide expert advice and guidance in this area. The present Joint FAO/lAEA Consultation on Validation of Analytical Methods for Food Control was convened for that purpose

  12. Development and Validation of Analytical Method for Determination of Uranium Enrichment in Standard Nuclear Material

    International Nuclear Information System (INIS)

    A non-destructive analytical method has been developed for determination of uranium enrichment using hyper pure germanium (HPGe) gamma ray detector. The absolute efficiency was measured experimentally by different radioactive sources at different distances from the detector crystal. The variation of the absolute peak efficiency for 185.7 keV with source to detector distances has been determined and used to estimate the absolute peak efficiency for the nuclear material samples at 185 keV with the help of analytical method. The validity of the developed analytical method has been confirmed by measuring the 235U enrichment of uranium oxide powders (U3O8) contained in cylindrical aluminum cans

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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

  15. New Analytical Methods and Their Validation for the Estimation of Etodolac in Bulk and Marketed Formulations

    Directory of Open Access Journals (Sweden)

    Mona Bhalani

    2015-02-01

    Full Text Available Etodolac is non-steroidal anti-inflammatory drug. It is used for the management of mild to moderate pain, fever and inflammation. Purpose: Analytical methods are required to characterize drug substances and drug products composition during all phases of pharmaceutical development. Development of methods to achieve the final goal of ensuring the quality of drug substances and drug products must be implemented. This determination requires highly sophisticated instruments and methods like HPLC, HPTLC and Spectrophotometer. Hence there was a need for the development of newer, simple, sensitive, rapid, accurate and reproducible analytical methods for the routine estimation of etodolac in bulk and pharmaceutical dosage form. Methods: Two simple, sensitive, specific and validated methods (method A and method B have been developed for the quantitative estimation of etodolac in bulk and pharmaceutical dosage form. Method A is based on reaction of etodolac with p-dimethylaminocinnamaldehyde to produce orange colour chromogen which showed λmax at 526.8 nm. In method B, etodolac oxidizes in presence of ferric chloride and hydrogen peroxide which absorbs at λmax at 537.2 nm. Reults: The linearity was found in concentration range of 5-30μg/ml and 2-12μg/ml for method A and method B respectively. The correlation coefficient was found to be 0.9990 and 0.9966 for method A and method B respectively. The methods were validated as per ICH guidelines. The LOD and LOQ for estimation of etodolac were found as 0.0824, 0.0230 for method A and 0.2498, 0.0699 for method B respectively. Conclusions: Proposed methods were successfully applied for the quantitative estimation of etodolac in marketed formulations.

  16. 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. PMID:24360478

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

    International Nuclear Information System (INIS)

    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

  18. NEW ANALYTICAL METHODS AND THEIR VALIDATION FOR THE ESTIMATION OF CARVEDILOL IN BULK AND MARKETED FORMULATION

    Directory of Open Access Journals (Sweden)

    Viral Bechara

    2015-02-01

    Full Text Available Carvedilol is cardiovascular agent. Mainly used for the treatment of hypertension, heart failure, and cardiovascular diseases. Purpose: Analytical methods are required to characterize drug substances and drug products composition during all phases of pharmaceutical development. Development of methods to achieve the final goal of ensuring the quality of drug substances and drug products must be implemented in conjunction with an understanding of the chemical behavior and physicochemical properties of the drug substance. This determination requires highly sophisticated instruments and methods like HPLC, HPTLC and Spectrophotometer. Hence there was a need for the development of newer, simple, sensitive, rapid, accurate and reproducible analytical methods for the routine estimation of metoprolol succinate in bulk and pharmaceutical dosage form. Methods: The present work describes two new spectrophotometric methods for the determination of carvedilol in bulk and marketed formulations. Method A is based on oxidation of Carvedilol with ferric ammonium sulphate followed by complex formation of resulting ferrous ion (Fe2+ with potassium ferricyanide to form bluish green coloured chromogen which showed λmax at 582 nm. In Method B is based on the oxidation of 2, 4- Dinitrophenylhydrazine and coupling of the oxidized product with drugs to give brown coloured chromogen which showed λmax at 500.8 nm. Results: The linearity was found in concentration range of 5-30 μg/ml for both Method A and Method B. The correlation coefficient was found 0.997 and 0.9997 for both Method A and Method B respectively. The methods were validated as per ICH guidelines. The LOD and LOQ for estimation of Carvedilol were found as 0.0840, 0.2545 for method A and 0.0667, 0.2021 for method B respectively. Conclusion: Proposed methods were successfully applied for the quantitative estimation of Carvedilol in marketed formulations.

  19. Development and validation of an analytical method for the determination of 4-hexylresorcinol in food.

    Science.gov (United States)

    Kim, Young-Hyun; Kim, Jae-Min; Lee, Jong Seok; Gang, Seong-Ran; Lim, Ho-Soo; Kim, Meehye; Lee, Ok-Hwan

    2016-01-01

    This study presents a method validation for extraction and quantitative analysis of 4-hexylresorcinol residues in shrimp and crab meat using HPLC-FLD. We were focused on the collaboratively analysis of each shrimp and crab meat samples, and developed LC-MS/MS method for the correct confirmation of the identity of compound. Validation parameters; selectivity, linearity, LOD, LOQ, accuracy, precision, and measurement of uncertainty were attained. The measurement of uncertainty was based on the precision study, data related to the performance of the analytical process and quantification of 4-hexylresorcinol. For HPLC-FLD analysis, the recoveries of 4-hexylresorcinol from spiked samples at levels of 0.2-10.0 ppm ranged from 92.54% to 97.67% with RSDs between 0.07% and 1.88%. According to these results, the method has been proven to be appropriate for extraction and determination of 4-hexylresorcinol, and can be used to maintain the safety of shrimp and crab products containing 4-hexylresorcinol residues. PMID:26213080

  20. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF TRIMETAZIDINE BY EXTRACTIVE SPECTROPHOTOMETRY

    Directory of Open Access Journals (Sweden)

    Y. Naga Prasanna*, S. Archana, G.S. Sowjanya, S. Lalitha, M. Lalitha

    2013-03-01

    Full Text Available ABSTRACT: Rapid, simple, sensitive and accurate spectrophotometric methods have been developed for the determination of Trimetazidine in pure and pharmaceutical formulations. Various methods were developed for estimation of trimetazidine .but a simple extractive photometric method using has not been developed .This method is based on the formation of chloroform soluble ion pair complex of Trimetazidine with bromothymol blue (BTB in buffer of pH 5.0 with absorption maximum at 409nm. Reaction conditions were optimised to obtain the maximum colour intensity. The absorbance was found to increase linearly with increase in concentration of Trimetazidine. Calibration graph was plotted and the correlation coefficient was found to be 0.998.Beer's law was obeyed in the concentration range of 1- 7 µg/ml with molar absorptivity of 30*10^3 l /mol /cm .Various analytical parameters have been evaluated and the results have been validated by statistical data. This method has been successfully applied for the assay of drug in pharmaceutical formulations. No interference was observed from common pharmaceutical adjuvant. The proposed method is simple, accurate and suitable for quality control applications.

  1. Validation of analytical methods for ethyl carbamate in nine food matrices.

    Science.gov (United States)

    Ryu, Dayeon; Choi, Bogyoung; Kim, Nayoung; Koh, Eunmi

    2016-11-15

    Ethyl carbamate (EC) is formed through a reaction between ethanol and either cyanate or N-carbamyl compounds. This study aimed to develop and validate analytical methods for EC determination in nine food matrices: apple juice, soju, milk, corn oil, rice porridge, peanut butter, beef, flat fish, and sea mustard. Differences from AOAC procedure were use of d5-EC as internal standard, dilution of alcohol content, removal of lipophilic compounds by hexane, and removal of hydrophilic polysaccharides by gel-forming. Standard curves had a good linearity (R(2)>0.997) in all matrices tested. LOD and LOQ were in the range of 0.69-6.08μg/kg and 2.10-18.43μg/kg, respectively. Recovery rates ranged from 80.75 to 121.82% for intra-day and ranged from 78.84 to 116.98% for inter-day. The relative standard deviations (RSDs) were below 14%. These results indicate that the established methods can be applied to determine EC in a variety of foods. PMID:27283695

  2. Development and Validation of a Terbium-Sensitized LuminescenceAnalytical Method for Deferiprone

    OpenAIRE

    Manzoori Lashkar, Jamshid; Amjadi, Mohammad; Soleymani, Jafar; Tamizi, Elnaz; Panahi-Azar, Vahid; Jouyban, Abolghasem

    2012-01-01

    A sensitive fluorometric method for the determination of deferiprone (DFP) based on the formation of a luminescent complex with Tb3+ ions in aqueous solutions is reported. The maximum excitation and emission wavelengths were 295 and 545 nm, respectively. The effects of various factors on the luminescence intensity of the system were investigated and optimized, then under the optimum conditions, the method was validated. The method validation results indicated that the relative intensity at 54...

  3. 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.

  4. 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.

  5. Comparison of statistical validation parameters for three analytical methods for determination of total uranium fluorometric

    International Nuclear Information System (INIS)

    Three analytical methods for determination of uranium in environmental samples by fluorescent technique have been compared. The first method depends on uranium purification from iron using the mercury anode technique, while, in the second method, uranium was purified from iron using the ion exchange technique (Dowex 1x4), employing a solution of hydrochloric acid (4.5 mol l-1), ascorbic acid (7%) and hydrazine hydrate (1.8%). The third method was performed using the ion exchange technique followed by uranium elution using a diluted sulfuric acid. The results have showed that the third method was the best among the studied methods. This is due to better values for detection limits, repeatability, replicability and recovery coefficient, in addition to low quantities of consumed chemical materials and less analytical time being required. (author)

  6. Comparison and validation of two analytical methods for measurement of urinary sucrose and fructose excretion

    OpenAIRE

    Song, Xiaoling; Navarro, Sandi L.; Diep, Pho; Thomas, Wendy K.; Razmpoosh, Elena C.; Schwarz, Yvonne; Wang, Ching-Yun; Kratz, Mario; Neuhouser, Marian L; Lampe, Johanna W.

    2013-01-01

    Urinary sugars excretion has been proposed as a potential biomarker for intake of sugars. In this study we compared two analytical methods [gas chromatography (GC) and enzymatic reactions – UV absorption] for quantifying urinary fructose and sucrose using 24-hour urine samples from a randomized cross-over controlled feeding study. All samples were successfully quantified by the GC method; however 21% and 1.9% of samples were below the detection limit of the enzymatic method for sucrose and fr...

  7. Development and validation of analytical methods for monomeric and oligomeric migrants from nylon 12 packaging materials.

    NARCIS (Netherlands)

    Stoffers, N.H.; Brandl, F.; Linssen, J.P.H.; Franz, R.

    2003-01-01

    Analytical methods for the determination of laurolactam-the monomer of nylon 12-as well as the cyclic dimer and trimer were established. High performance liquid chromatography using ultraviolet (HPLC-UV) and mass spectrometric detection (HPLC-MS) were both found suitable to identify and quantify mon

  8. Development and Validation of Analytical method for Lopinavir and Ritonavir by HPLC

    Directory of Open Access Journals (Sweden)

    R. Arun

    2013-06-01

    Full Text Available This paper describes the development and validation of the HPLC method (254nm for the quantitation of lopinavir and ritonavir in pure form and pharmaceutical formulations. The method showed to be linear (r2 > 0.999, precise (R.S.D. < 0.21%, accurate (recovery of 100.11% for lopinavir and 99.96% for ritonavir, specific and robust. Three batches of lopinavir and ritonavir tablets were assayed by the validated method. The lopinavir contents in the tablets varied from 99.87 to 100.52%, while ritonavir contents showed 99.61 to 100.57%.

  9. Analytical Method Development and Validation of Related Substance Method for Bortezomib for Injection 3.5 mg/Vial by RP-HPLC Method

    Directory of Open Access Journals (Sweden)

    Utage M

    2013-04-01

    Full Text Available An accurate, precise, simple and economical High Performance Liquid Chromatographic method for therelated substance determination of Bortezomib in its lyophilized dosage form has been developed. Themethod developed is Reverse Phase High Performance Liquid Chromatographic method using HypersilBDS C18 column (Length: 150mm, Diameter: 4.6mm, Particle size: 5μ with Gradient programmed anda simple Acetonitrile, Water and Formic acid in the ratio of 30:70:0.1 (v/v/v respectively as mobilephase A and Acetonitrile, Water and Formic acid in the ratio of 80:20:0.1 (v/v/v respectively. Themethod so developed was validated in compliance with the regulatory guidelines by using welldeveloped analytical method validation tool which comprises with the analytical method validationparameters like Linearity, Accuracy, Method precision, Specificity with forced degradation, Systemsuitability, Robustness, LOD, LOQ and Ruggedness. The results obtained were well within theacceptance criteria.

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

    International Nuclear Information System (INIS)

    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 (HNO3) 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% RDSr. 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)

  11. 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.

  12. Experimental validation of an analytical method to obtain the response function of an alpha particle spectrometer

    International Nuclear Information System (INIS)

    In a previous paper, one of the authors suggested an analytical method for calculation of the response function of an alpha spectrometer for the case of large solid angles. This paper describes the experimental verification of the method. Spectra of a well-known natural uranium sample were measured with a 450 mm2 Si detector and compared to the theoretical predictions. The measurements were carried out with two different geometrical configurations. In both cases a good agreement was observed between experimental and theoretical results

  13. Analytical Method Validation of Selected Organochlorine Pesticides in Fortified Rice Using Gas Chromatography with Electron Capture Detector

    Directory of Open Access Journals (Sweden)

    Mutia Kusuma Wardani

    2014-01-01

    Full Text Available Gas chromatography with electron capture detector (GC-ECD has been validated for simultaneous determination of selected organochlorine pesticides namely heptachlor, endosulfan, dieldrin, dan p,p’-dichlorodiphenyltrichloroethane (p,p’-DDT using aldrin as standard internal. Some parameters for analytical method validation were evaluated, i.e. linearity, precision, sensitivity expressed with limit of detection and limit of quantification, and recovery. GC-ECD was linear for determination of these pesticides with r values ≥ 0.99. The values of LOD obtained were 2.50, 2.97, 1.61, and 2.54 ng/mL for heptachlor, endosulphan, dieldrin, and p,p’-DDT, respectively. Furthermore, the relative standard deviation (RSD values obtained for the assessment of analytical precision were lower than those required by Horwitz. Finally, the used GC-ECD method was accurate for determination of these organochlorine psticides in fortified rice samples which were indicated by the acceptable recovery percentages.

  14. Validation Study for Analytical Method of Diarrhetic Shellfish Poisons in 9 Kinds of Shellfish.

    Science.gov (United States)

    Yamaguchi, Mizuka; Yamaguchi, Takahiro; Kakimoto, Kensaku; Nagayoshi, Haruna; Okihashi, Masahiro; Kajimura, Keiji

    2016-01-01

    A method was developed for the simultaneous determination of okadaic acid, dinophysistoxin-1 and dinophysistoxin-2 in shellfish using ultra performance liquid chromatography with tandem mass spectrometry. Shellfish poisons in spiked samples were extracted with methanol and 90% methanol, and were hydrolyzed with 2.5 mol/L sodium hydroxide solution. Purification was done on an HLB solid-phase extraction column. This method was validated in accordance with the notification of Ministry of Health, Labour and Welfare of Japan. As a result of the validation study in nine kinds of shellfish, the trueness, repeatability and within-laboratory reproducibility were 79-101%, less than 12 and 16%, respectively. The trueness and precision met the target values of notification. PMID:26936305

  15. Analytical Method Development and Validation for Simultaneous Estimation of Clotrimazole and Tinidazole by RP-HPLC

    Directory of Open Access Journals (Sweden)

    Joshi S

    2015-12-01

    Full Text Available An isocratic reverse phase High Performance Liquid Chromatographic (RP-HPLC method was developed and validated for simultaneous determination of Clotrimazole and Tinidazole in combined pharmaceutical dosage form. The successful separation of Clotrimazole and Tinidazole was achieved using Purospher® C18 (250 mm x 4.6 mm i.d., 5 μm column, with mobile phase consisting Phosphate buffer (pH 3.5: Acetonitrile (45:55. The mobile phase flow rate was 1.0 ml/min and the detection wavelength was 240 nm. The developed RP-HPLC method was validated according to ICH guidelines with respect to linearity, accuracy, precision, specificity and robustness and also the LOD and LOQ values were determined.

  16. Analytical Method Validation of an Herbal Formulation by Headspace Gas Chromatography Using QbD

    OpenAIRE

    Joydeep Mazumder; Devender Pathak; Rachna Kumria

    2014-01-01

    Essential oils are rich sources of biologically active compounds possessing diverse medicinal properties. These form integral part of a number of herbal formulations. The most challenging part of commercialization of herbal formulation is to ensure consistency in quality from batch to batch. The aim of present study was to develop a validated gas chromatographic method based on quality by design (QbD) for routine quality control purpose. A blend of essential oils possessing synergistic ca...

  17. 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.

  18. Analytical Method Validation of an Herbal Formulation by Headspace Gas Chromatography Using QbD

    Directory of Open Access Journals (Sweden)

    Joydeep Mazumder

    2014-10-01

    Full Text Available Essential oils are rich sources of biologically active compounds possessing diverse medicinal properties. These form integral part of a number of herbal formulations. The most challenging part of commercialization of herbal formulation is to ensure consistency in quality from batch to batch. The aim of present study was to develop a validated gas chromatographic method based on quality by design (QbD for routine quality control purpose. A blend of essential oils possessing synergistic carminative properties was formulated in oily base. Ajowan oil, cardamom oil, caraway oil, coriander and fennel oil were selected for development of formulation. A gas chromatography method was developed for routine quality control purpose of the developed formulation by quality by design techniques (QbD. Each oil was characterized making use of a marker compound which was linalool for coriander oil, cineol for cardamom oil, anethol for fennel oil, carvone for caraway oil, thymol for ajowan oil and menthol for peppermint oil. Marker compound was characterized using mass spectroscopy. Chromatography method was established by quality by design approach and validated based on ICH guidelines.

  19. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR ESTIMATION OF CILNIDIPINE AND METOPROLOL SUCCINATE

    Directory of Open Access Journals (Sweden)

    Mo.Salauddin A Shaikh

    2015-07-01

    Full Text Available A simple, specific, accurate and precise reversed phase high performance liquid chromatographic method was developed and validated for the simultaneous estimation of Cilnidipine and Metoprolol Succinate, using a Cosmosil C18 (250 х 4.6 mm i.d. column and a mobile phase composed of 0.05M potassium dihydrogen phosphate buffer: Methanol (70:30 pH 3.5 adjusted with ophosphoric acid and at flow rate of 1.0 ml/min. The retention times of Cilnidipine and Metoprolol Succinate were found to be 3.493 min and 5.960 min, respectively. Linearity was established for Cilnidipine and Metoprolol Succinate in the range of 12.5-37.5 μg/ml and 2.5-7.5 μg/ml, respectively. The percentage recoveries of Cilnidipine and Metoprolol Succinate were found to be in the range of 100.13-100.40 % and 99.24-100.29 %, respectively. The correlation coefficients for both components were found to be 0.999. The developed methods were validated according to ICH guidelines and values of linearity, accuracy, precision and other analysis were found to be in good accordance with the prescribed values. This method can be successfully employed for simultaneous quantitative analysis of Cilnidipine and Metoprolol Succinate in its dosage form. The developed HPLC method was subjected to stability indicating studies for marketed formulation. Interfering peak from degraded products or solvent did not interfere with estimation of drugs and the developed method was found to be specific for estimation of Cilnidipine and Metoprolol Succinate.

  20. 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. PMID:27443214

  1. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF SIMULTANEOUS ESTIMATION OF AMLODIPINE AND ATORVASTATIN BY RP-UPLC

    Directory of Open Access Journals (Sweden)

    Waghmare A. N

    2014-02-01

    Full Text Available To develop and validate simple, sensitive, robust, rapid and specific isocratic RP-UPLC method for simultaneous estimation of Amlodipine and Atorvastatin in tablet dosage form. Methods: The developed method consisting the mobile phase of acetonitrile and 0.02 M Potassium dihydrogen phosphate (55:45 with isocratic programming, BEH C18 (100mm×2.1mm, 1.7μm column as stationary phase with a flow rate of 0.3 mL/minute. Results and discussion: Proposed method was found to be linear for Amlodipine and Atorvastatin in the concentration range of 0.5 to 40.0 μg/mL with r2 of 0.9999 for Amlodipine and 0.9997 for Atorvastatin respectively. Precision study showed that the percentage relative standard deviation was within the range of acceptable limits, and the mean recovery was found to be 100.79 % for assay of Amlodipine and 99.87% for Atorvastatin in tablet dosage form .The LOD and LOQ of Amlodipine and Atorvastatin were found to be 0.062 and 0.078μg/ml and 0.020 and 0.026 μg/mL.

  2. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF SIMULTANEOUS ESTIMATION OF AMLODIPINE AND ATORVASTATIN BY RP-UPLC

    Directory of Open Access Journals (Sweden)

    Waghmare A. N

    2014-02-01

    Full Text Available Objective: To develop and validate simple, sensitive, robust, rapid and specific isocratic RP-UPLC method for simultaneous estimation of Amlodipine and Atorvastatin in tablet dosage form. Methods: The developed method consisting the mobile phase of acetonitrile and 0.02 M Potassium dihydrogen phosphate (55:45 with isocratic programming, BEH C18 (100mm×2.1mm, 1.7μm column as stationary phase with a flow rate of 0.3 mL/minute. Results and discussion: Proposed method was found to be linear for Amlodipine and Atorvastatin in the concentration range of 0.5 to 40.0 μg/mL with r2 of 0.9999 for Amlodipine and 0.9997 for Atorvastatin respectively. Precision study showed that the percentage relative standard deviation was within the range of acceptable limits, and the mean recovery was found to be 100.79 % for assay of Amlodipine and 99.87% for Atorvastatin in tablet dosage form .The LOD and LOQ of Amlodipine and Atorvastatin were found to be 0.062 and 0.078μg/ml and 0.020 and 0.026 μg/mL.

  3. Development and validation of a rapid analytical method to quantify naled residue.

    Science.gov (United States)

    Zhong, H; Latham, M

    2001-12-01

    A rapid gas chromatographic method for detecting residues of the thio-organophosphate naled was developed and subsequently validated in laboratory and field studies. More than 90% of naled was recovered by a gas chromatograph when equipped with a DB-5 capillary column and a thermionic specific detector. The limit of detection was 0.01 microg/ml with direct injection. Stabilization of naled under a variety of storage conditions also was examined. Analysis of field data showed that naled broke down rapidly in the environment but was stable when stored in hexane solvent at 4 degrees C and 23 degrees C for at least 7 days. Range of percentage matrix spike recovery was 31-49% for filter paper samples exposed under field conditions for 14 h. A field study was also initiated that collected naled droplets trapped on 6.7-m acrylic mohair-look yarn strands in addition to residue on filter paper after aerial ultra-low-volume mosquito adulticide application. Spike recovery was 79% for filter paper samples and 93% for yarn samples. Average naled residue concentrations with these methods were 373 microg/m2 and 11.28-73.77 microg/yarn, respectively. PMID:11804458

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

    International Nuclear Information System (INIS)

    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 (r2=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

  5. NEW ANALYTICAL METHODS AND THEIR VALIDATION FOR THE ESTIMATION OF METOPROLOL SUCCINATE IN BULK AND MARKETED FORMULATION

    Directory of Open Access Journals (Sweden)

    Viral Bechara

    2015-02-01

    Full Text Available Metoprolol succinate is cardiovascular agent. Mainly used for the treatment of hypertension, heart failure, and cardiovascular diseases. Purpose: Analytical methods are required to characterize drug substances and drug products composition during all phases of pharmaceutical development. Development of methods to achieve the final goal of ensuring the quality of drug substances and drug products must be implemented in conjunction with an understanding of the chemical behavior and physicochemical properties of the drug substance. This determination requires highly sophisticated instruments and methods like HPLC, HPTLC and Spectrophotometer. Hence there was a need for the development of newer, simple, sensitive, rapid, accurate and reproducible analytical methods for the routine estimation of metoprolol succinate in bulk and pharmaceutical dosage form. Methods: The present work describes two new spectrophotometric methods for the determination of metoprolol succinate in bulk and marketed formulations. Method A is based on oxidation reaction. Metoprolol succinate in presence of acidic medium reacts with excess amount of chloramine-T and remaining chloramine-T react with malachite green to produce orange colour chromogen which showed λmax at 516 nm. In Method B, the drug was diazotised with sodium nitrite in presence of hydrochloric acid and then it was coupled with β-naphthol in alkaline medium. Which produce red colour chromogen which showed λmax at 688 nm. Results: The linearity was found in concentration range of 5-30μg/ml for both method A and method B. The correlation coefficient was found to be 0.9983 and 0.9993 for method A and method B respectively. The methods were validated as per ICH guidelines. The LOD and LOQ for estimation of Metoprolol succinate were found as 0.0773, 0.2343 for method A and 0.0667, 0.2021 for method B respectively. Conclusion: Proposed methods were successfully applied for the quantitative estimation of

  6. Estimating the Coefficient of Cross-validity in Multiple Regression: A Comparison of Analytical and Empirical Methods.

    Science.gov (United States)

    Kromrey, Jeffrey D.; Hines, Constance V.

    1996-01-01

    The accuracy of three analytical formulas for shrinkage estimation and four empirical techniques were investigated in a Monte Carlo study of the coefficient of cross-validity in multiple regression. Substantial statistical bias was evident for all techniques except the formula of M. W. Brown (1975) and multicross-validation. (SLD)

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

    International Nuclear Information System (INIS)

    The Ketotiphen eyedrop is prescribed to relief the signs and symptoms of allergic conjunctivitis due to its potent H1antihistaminic 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

  8. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF TRIMETAZIDINE BY EXTRACTIVE SPECTROPHOTOMETRY

    OpenAIRE

    Y. Naga Prasanna*, S. Archana, G.S. Sowjanya, S. Lalitha, M. Lalitha

    2013-01-01

    ABSTRACT: Rapid, simple, sensitive and accurate spectrophotometric methods have been developed for the determination of Trimetazidine in pure and pharmaceutical formulations. Various methods were developed for estimation of trimetazidine .but a simple extractive photometric method using has not been developed .This method is based on the formation of chloroform soluble ion pair complex of Trimetazidine with bromothymol blue (BTB) in buffer of pH 5.0 with absorption maximum at 409nm. Reaction ...

  9. Validation of analytical method for dopamine determination by high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Dopamine is an endogenous hormone in the catecholamine group, which is used to simulate the sympathetic nervous system action and to raise the heart rate and the blood pressure. However, this drug has high genotoxicity and is associated with the treatment of diseases such as schizophrenia and Parkinson's disease. For this reason, the determination of dopamine in wastewaters coming from its production has been of great interest. The validation used a RP-18 250 x 4.6 mm 5 μm column, mobile phase: 1 % NaH2PO4 /CH3OH (90/10), 1.0 ml/min flow rate and a visible ultraviolet detector at 280 nm. Detection limits and quantitation were estimated in addition to evaluating the drug stability under the analysis conditions

  10. 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)

    This work presents a low cost, simple and new methodology for direct determination uranium in different matrices uranium: organic phase (UO2(NO3)2.2TBP - uranyl nitrate complex) and aqueous phase (UO2(NO3)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 (UO2(NO3)2.2TBP in hexane/embedded in KBr) was linear (r=0.9989) over the range of 1.0 g L-1a 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 (UO2(NO3)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)

  11. 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)

    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

  12. Validation of an HPLC Analytical Method for Determination of Biogenic Amines in Agricultural Products and Monitoring of Biogenic Amines in Korean Fermented Agricultural Products

    OpenAIRE

    Yoon, Hyeock; Park, Jung Hyuck; Choi, Ari; Hwang, Han-Joon; Mah, Jae-Hyung

    2015-01-01

    An HPLC analytical method was validated for the quantitative determination of biogenic amines in agricultural products. Four agricultural foods, including apple juice, Juk, corn oil and peanut butter, were selected as food matrices based on their water and fat contents (i.e., non-fatty liquid, non-fatty solid, fatty liquid and fatty solid, respectively). The precision, accuracy, recovery, limit of detection (LOD) and quantification (LOQ) were determined to test the validity of an HPLC procedu...

  13. Determination of aflatoxin in processed dried cassava root: validation of a new analytical method for cassava flour.

    Science.gov (United States)

    Gnonlonfin, G J Benoit; Katerere, David R; Adjovi, Yann; Brimer, Leon; Shephard, Gordon S; Sanni, Ambaliou

    2010-01-01

    A new method that uses HPLC with a photochemical reactor for enhanced detection was developed and validated for the determination of aflatoxins in cassava flour. Samples were spiked with a mixture of four aflatoxins at 5, 10, and 20 microg/kg mixed with either 1 or 5 g NaCI and extracted with methanol-water (80 + 20, v/v) by shaking for 10 or 30 min. An immunoaffinity column was used for cleanup. HPLC with postcolumn derivatization, for enhancement of aflatoxin fluorescence, and fluorescence determination were used for quantitation of the toxin concentration. The method was validated for recovery, linearity, and precision at the three concentrations tested. Recovery ranges were 52-70, 69-85, and 80-89% for the spiking levels of 5.0, 10.0, and 20.0 microg/kg, respectively. It appears that the amount of salt (NaCl) and the shaking time are critical factors in this method; optimal performance was obtained when 1 g salt was used and the shaking time was 10 min. The good linearity and precision of the method allowed baseline separation from interferences, e.g., coumarins. PMID:21313816

  14. 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)

  15. 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)

    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 2k 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

    Institute of Scientific and Technical Information of China (English)

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

    2012-01-01

    The most suitable bio-analytical method based on liquid liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mm × 50 mm, 3.5 um) 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 lotal 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.

  17. The forensic validity of visual analytics

    Science.gov (United States)

    Erbacher, Robert F.

    2008-01-01

    The wider use of visualization and visual analytics in wide ranging fields has led to the need for visual analytics capabilities to be legally admissible, especially when applied to digital forensics. This brings the need to consider legal implications when performing visual analytics, an issue not traditionally examined in visualization and visual analytics techniques and research. While digital data is generally admissible under the Federal Rules of Evidence [10][21], a comprehensive validation of the digital evidence is considered prudent. A comprehensive validation requires validation of the digital data under rules for authentication, hearsay, best evidence rule, and privilege. Additional issues with digital data arise when exploring digital data related to admissibility and the validity of what information was examined, to what extent, and whether the analysis process was sufficiently covered by a search warrant. For instance, a search warrant generally covers very narrow requirements as to what law enforcement is allowed to examine and acquire during an investigation. When searching a hard drive for child pornography, how admissible is evidence of an unrelated crime, i.e. drug dealing. This is further complicated by the concept of "in plain view". When performing an analysis of a hard drive what would be considered "in plain view" when analyzing a hard drive. The purpose of this paper is to discuss the issues of digital forensics and the related issues as they apply to visual analytics and identify how visual analytics techniques fit into the digital forensics analysis process, how visual analytics techniques can improve the legal admissibility of digital data, and identify what research is needed to further improve this process. The goal of this paper is to open up consideration of legal ramifications among the visualization community; the author is not a lawyer and the discussions are not meant to be inclusive of all differences in laws between states and

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

    Directory of Open Access Journals (Sweden)

    Kerusha Govender

    2016-02-01

    Full Text Available 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.

  19. 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

  20. 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.

  1. 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)

    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)

  2. Development and analytical validation of a screening method for simultaneous detection of five adulterants in raw milk using mid-infrared spectroscopy and PLS-DA.

    Science.gov (United States)

    Botelho, Bruno G; Reis, Nádia; Oliveira, Leandro S; Sena, Marcelo M

    2015-08-15

    This paper proposed a new screening method for the simultaneous detection of five common adulterants in raw cow milk by using attenuated total reflectance (ATR) mid infrared spectroscopy and multivariate supervised classification (partial least squares discrimination analysis - PLSDA). The method was able to detect the presence of the adulterants water, starch, sodium citrate, formaldehyde and sucrose in milk samples containing from one up to five of these analytes, in the range of 0.5-10% w/v. A multivariate qualitative validation was performed, estimating specific figures of merit, such as false positive and false negative rates, selectivity, specificity and efficiency rates, accordance and concordance. The proposed method does not need any sample pretreatment, requires a small amount of sample (30 μL), is fast and simple, being suitable for the control of raw milk in a dairy industry or for the quality inspection of commercialized milk. PMID:25794717

  3. 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). PMID:27230427

  4. 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

    2015-01-01

    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. PMID:25556930

  5. Validation of an HPLC Analytical Method for Determination of Biogenic Amines in Agricultural Products and Monitoring of Biogenic Amines in Korean Fermented Agricultural Products.

    Science.gov (United States)

    Yoon, Hyeock; Park, Jung Hyuck; Choi, Ari; Hwang, Han-Joon; Mah, Jae-Hyung

    2015-09-01

    An HPLC analytical method was validated for the quantitative determination of biogenic amines in agricultural products. Four agricultural foods, including apple juice, Juk, corn oil and peanut butter, were selected as food matrices based on their water and fat contents (i.e., non-fatty liquid, non-fatty solid, fatty liquid and fatty solid, respectively). The precision, accuracy, recovery, limit of detection (LOD) and quantification (LOQ) were determined to test the validity of an HPLC procedure for the determination of biogenic amines, including tryptamine, β-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine, in each matrix. The LODs and LOQs for the biogenic amines were within the range of 0.01~0.10 mg/kg and 0.02~0.31 mg/kg, respectively. The relative standard deviation (RSD) of intraday for biogenic amine concentrations ranged from 1.86 to 5.95%, whereas the RSD of interday ranged from 2.08 to 5.96%. Of the matrices spiked with biogenic amines, corn oil with tyramine and Juk with putrescine exhibited the least accuracy of 84.85% and recovery rate of 89.63%, respectively, at the lowest concentration (10 mg/kg). Therefore, the validation results fulfilled AOAC criteria and recommendations. Subsequently, the method was applied to the analysis of biogenic amines in fermented agricultural products for a total dietary survey in Korea. Although the results revealed that Korean traditional soy sauce and Doenjang contained relatively high levels of histamine, the amounts are of no concern if these fermented agricultural products serve as condiments. PMID:26483889

  6. 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. PMID:26320872

  7. 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; Moreira, Otacilio da Cruz; 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; Guedes, Paulo Marcos da Matta; 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; Galvão, Lúcia Maria da Cunha; da Câmara, Antonia Cláudia Jácome; Espinoza, Bertha; de Noya, Belkisyole Alarcón; Puerta, Concepción; Riarte, Adelina; Diosque, Patricio; Sosa-Estani, Sergio; Guhl, Felipe; Ribeiro, Isabela; Aznar, Christine; Britto, Constança; Yadón, Zaida Estela; Schijman, Alejandro G.

    2015-01-01

    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. PMID:26320872

  8. Chromatographic development of validated analytical method for the estimation of tapentadol and paracetamol in combined dosage form

    OpenAIRE

    Manoj S. Charde; Ashwini A. Patil; Jitendra Kumar; A. S. Welankiwar; R. D. Chakole

    2014-01-01

    A simple, sensitive an isocratic RP-HPLC method for the estimation of  TAP (Tapentadol) and PARA (Paracetamol) in combined dosage form using Inertsil ODS C-18 column (250×4.6 mm, 5 µ) in an isocratic mode with mobile phase comprising  Buffer (1mL TEA) :  ACN : MeOH in the ratio of (75:20:5 v/v/v). The flow rate was 1.2 mL/ min and effluent was monitored at 220 nm. The retention times were found to be 6.88 min for TAP and 3.78 min for PARA. The assay exhibited a linear dynamic range of 11.89- ...

  9. Chromatographic development of validated analytical method for the estimation of tapentadol and paracetamol in combined dosage form

    Directory of Open Access Journals (Sweden)

    Manoj S. Charde

    2014-01-01

    Full Text Available A simple, sensitive an isocratic RP-HPLC method for the estimation of  TAP (Tapentadol and PARA (Paracetamol in combined dosage form using Inertsil ODS C-18 column (250×4.6 mm, 5 µ in an isocratic mode with mobile phase comprising  Buffer (1mL TEA :  ACN : MeOH in the ratio of (75:20:5 v/v/v. The flow rate was 1.2 mL/ min and effluent was monitored at 220 nm. The retention times were found to be 6.88 min for TAP and 3.78 min for PARA. The assay exhibited a linear dynamic range of 11.89- 28.55 µg/mL for TAP and 64.95- 155.90 µg/mL for PARA.

  10. 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. PMID:24912721

  11. Analytic Methods for Cosmological Likelihoods

    OpenAIRE

    Taylor, A. N.; Kitching, T. D.

    2010-01-01

    We present general, analytic methods for Cosmological likelihood analysis and solve the "many-parameters" problem in Cosmology. Maxima are found by Newton's Method, while marginalization over nuisance parameters, and parameter errors and covariances are estimated by analytic marginalization of an arbitrary likelihood function with flat or Gaussian priors. We show that information about remaining parameters is preserved by marginalization. Marginalizing over all parameters, we find an analytic...

  12. 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.

  13. Fast and simple procedure for fractionation of zinc in soil using an ultrasound probe and FAAS detection. Validation of the analytical method and evaluation of the uncertainty budget.

    Science.gov (United States)

    Leśniewska, Barbara; Kisielewska, Katarzyna; Wiater, Józefa; Godlewska-Żyłkiewicz, Beata

    2016-01-01

    A new fast method for determination of mobile zinc fractions in soil is proposed in this work. The three-stage modified BCR procedure used for fractionation of zinc in soil was accelerated by using ultrasounds. The working parameters of an ultrasound probe, a power and a time of sonication, were optimized in order to acquire the content of analyte in soil extracts obtained by ultrasound-assisted sequential extraction (USE) consistent with that obtained by conventional modified Community Bureau of Reference (BCR) procedure. The content of zinc in extracts was determined by flame atomic absorption spectrometry. The developed USE procedure allowed for shortening the total extraction time from 48 h to 27 min in comparison to conventional modified BCR procedure. The method was fully validated, and the uncertainty budget was evaluated. The trueness and reproducibility of the developed method was confirmed by analysis of certified reference material of lake sediment BCR-701. The applicability of the procedure for fast, low costs and reliable determination of mobile zinc fraction in soil, which may be useful for assessing of anthropogenic impacts on natural resources and environmental monitoring purposes, was proved by analysis of different types of soil collected from Podlaskie Province (Poland). PMID:26666658

  14. Validation and application of an analytical method for the determination of selected acidic pharmaceuticals and estrogenic hormones in wastewater and sludge.

    Science.gov (United States)

    Zhang, Mengtao; Mao, Qianhui; Feng, Jingwei; Yuan, Shoujun; Wang, Qiquan; Huang, Deying; Zhang, Jibiao

    2016-09-18

    This study was undertaken to develop an extraction method for seven acidic pharmaceuticals and five steroidal estrogens from wastewater, treated wastewater and sludge samples. The temperature and time of sample derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide was optimized. Our results show that pretreatment combined with solid phase extraction (SPE) for wastewater samples (using an ENVI-C18 cartridge) and liquid-solid extraction combined with SPE (using an HLB cartridge) for sludge samples increased the analytical efficiency for acidic pharmaceuticals and estrogenic hormones using gas chromatography-mass spectrometry (GC-MS). The derivatization conditions were optimized at 40°C for 2 h. In addition, the derivatized samples were stable at ambient temperature. The new method was validated and applied to the analysis of real wastewater and discharged sludge samples from a local wastewater treatment plant. Except for 17α-ethinylestradiol, all acidic pharmaceuticals and estrogens were detected in the influent, effluent and discharged sludge samples. The concentrations of these compounds were particularly high in the discharged sludge samples. PMID:27314419

  15. Analytical Method Development and Validation for Simultaneous Estimation of Artemether and Lumefantrine in Pure And Pharmaceutical Dosage Form Using Rp-Hplc Method

    International Nuclear Information System (INIS)

    A simple, rapid, precise and cost effective reversed phase-high performance liquid chromatography (RP-HPLC) method was developed for the simultaneous estimation of Artemether (AT) and Lumefantrine (LU) in pure drug and pharmaceutical dosage forms. The separation was carried out using BDS Hypersil C18 (150 x 4.6 mm i.d. 3 μm particle size) column, with mobile phase comprising of 0.01M tetra butyl ammonium hydrogen sulphate and acetonitrile in the ratio of 20 : 80 (v/ v). The flow rate was 1.0 ml/ min and the detection was carried out using UV-visible detector at 222 nm. The method was validated by evaluation of different parameters such as accuracy, precision, linearity, ruggedness, and robustness, limit of detection (LOD) and limit of quantification (LOQ). The retention time were found to be 4.19 and 5.22 min for AT and LU, respectively. Correlation coefficient (r2) of 0.999 for both over concentration range of 3.2-19.2 μg/ ml and 16-96 μg/ ml for AT and LU, respectively. Parameters like mobile phase ratio, wavelength, flow rate and others were deliberately varied. It was observed that there were no marked changes in chromatograms, which demonstrated that the developed RP-HPLC method is robust. Intra and inter day precision reproducibility study was carried out and it was checked by determining precision on the same instrument, but by a different analyst. The percentage recovery for AT and LU were ranged between 99.18-100.19 and 99.96-100.07, respectively. The LOD for AT and LU were found to be 0.201 and 2.99 μg/ ml and the LOQ were 0.609 and 9.086 μg/ml respectively. Method was found to be reproducible with relative standard deviation (RSD) for intra and inter day precision less than 2 %. (author)

  16. Development and validation of an HPLC-MS/MS analytical method for quantitative analysis of TCBA-TPQ, a novel anticancer makaluvamine analog, and application in a pharmacokinetic study in rats

    OpenAIRE

    Jun-Xian, YU; Voruganti, Sukesh; Dan-Dan, LI; Qin, Jiang-Jiang; Nag, Subhasree; Xu, Su; Velu, Sadanandan E.; Wang, Wei; Zhang, Ruiwen

    2015-01-01

    We have recently designed and synthesized several novel iminoquinone anticancer agents that have entered preclinical development for the treatment of human cancers. Herein we developed and validated a quantitative HPLC-MS/MS analytical method for one of the lead novel anticancer makaluvamine analog, TCBA-TPQ, and conducted a pharmacokinetic study in laboratory rats. Our results indicated that the HPLC-MS/MS method was precise, accurate, and specific. Using this method, we carried out in vitro...

  17. Analytical Method Development, Validation and Simultaneous Estimation of Guaifenesin, Levocetirizine Hydrochloride, and Ambroxol Hydrochloride in Syrup Dosage form by RP-HPLC

    Directory of Open Access Journals (Sweden)

    Konagala Sravanthi

    2016-05-01

    Full Text Available In the present study a validated stability indicating RP-HPLC method for quantification of GFS, LCZ and ABX was established. Compared with the reported methods, this method represents the first report about a stability indicating method for the determination of GFS, LCZ and ABX. With the proposed method a satisfactory separation of three drugs from the degradation products and impurities, extended linear range and rapid analysis time were carried out. A high recovery of GFS, LCZ and ABX in formulation was achieved. The proposed method ensured a precise and accurate determination of GFS, LCZ and ABX in formulation. No interference from the excipients was noticed.

  18. Validation of a confirmatory analytical method for the determination of aflatoxins B1, B2, G1 and G2 in foods and feed materials by HPLC with on-line photochemical derivatization and fluorescence detection

    OpenAIRE

    Muscarella, Marilena; Iammarino, Marco; Nardiello, Donatella; Lo Magro, Sonia; Palermo, Carmen; Centonze, Diego; Palermo, Domenico

    2009-01-01

    Abstract A sensitive and selective analytical method for the simultaneous separation and quantitative determination of aflatoxins B1, B2, G1 and G2 in foodstuffs and materials for feed has been validated. The method is based on high performance liquid chromatography with on-line post-column photochemical derivatization and fluorescence detection. The chromatographic separation of aflatoxins was accomplished by using a C18 column eluted with an isocratic mobile phase consisting of w...

  19. Analytical methods under emergency conditions

    International Nuclear Information System (INIS)

    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

  20. Analytic Methods in Nonperturbative QCD

    OpenAIRE

    Simonov, Yu.A.

    2000-01-01

    Recently developed analytic methods in the framework of the Field Correlator Method are reviewed in this series of four lectures and results of calculations are compared to lattice data and experiment. Recent lattice data demonstrating the Casimir scaling of static quark interaction strongly support the FCM and leave very little space for all other theoretical models, e.g. instanton gas/liquid model. Results of calculations for mesons, baryons, quark-gluon plasma and phase transition temperat...

  1. Determination of serum levels of imatinib mesylate in patients with chronic myeloid leukemia: validation and application of a new analytical method to monitor treatment compliance

    Directory of Open Access Journals (Sweden)

    Vinícius Marcondes Rezende

    2013-01-01

    Full Text Available OBJECTIVE: The goal of this study was to monitor imatinib mesylate therapeutically in the Tumor Biology Laboratory, Department of Hematology and Hemotherapy, Hospital das Clínicas, Faculdade de Medicina, Universidade de São Paulo (USP. A simple and sensitive method to quantify imatinib and its metabolite (CGP74588 in human serum was developed and fully validated in order to monitor treatment compliance. METHODS: The method used to quantify these compounds in serum included protein precipitation extraction followed by instrumental analysis using high performance liquid chromatography coupled with mass spectrometry. The method was validated for several parameters, including selectivity, precision, accuracy, recovery and linearity. RESULTS: The parameters evaluated during the validation stage exhibited satisfactory results based on the Food and Drug Administration and the Brazilian Health Surveillance Agency (ANVISA guidelines for validating bioanalytical methods. These parameters also showed a linear correlation greater than 0.99 for the concentration range between 0.500 µg/mL and 10.0 µg/mL and a total analysis time of 13 minutes per sample. This study includes results (imatinib serum concentrations for 308 samples from patients being treated with imatinib mesylate. CONCLUSION: The method developed in this study was successfully validated and is being efficiently used to measure imatinib concentrations in samples from chronic myeloid leukemia patients to check treatment compliance. The imatinib serum levels of patients achieving a major molecular response were significantly higher than those of patients who did not achieve this result. These results are thus consistent with published reports concerning other populations.

  2. Ruggedness testing and validation of a practical analytical method for > 100 veterinary drug residues in bovine muscle by ultrahigh performance liquid chromatography – tandem mass spectrometry

    Science.gov (United States)

    In this study, optimization, extension, and validation of a streamlined, qualitative and quantitative multiclass, multiresidue method was conducted to monitor great than100 veterinary drug residues in meat using ultrahigh-performance liquid chromatography – tandem mass spectrometry (UHPLC-MS/MS). I...

  3. Waste minimization in analytical methods

    International Nuclear Information System (INIS)

    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. Fast and simple procedure for fractionation of zinc in soil using an ultrasound probe and FAAS detection. Validation of the analytical method and evaluation of the uncertainty budget

    OpenAIRE

    Leśniewska, Barbara; Kisielewska, Katarzyna; Wiater, Józefa; Godlewska-Żyłkiewicz, Beata

    2015-01-01

    A new fast method for determination of mobile zinc fractions in soil is proposed in this work. The three-stage modified BCR procedure used for fractionation of zinc in soil was accelerated by using ultrasounds. The working parameters of an ultrasound probe, a power and a time of sonication, were optimized in order to acquire the content of analyte in soil extracts obtained by ultrasound-assisted sequential extraction (USE) consistent with that obtained by conventional modified Community Burea...

  5. Validation of a UHPLC-FLD analytical method for the simultaneous quantification of aflatoxin B1 and ochratoxin a in rat plasma, liver and kidney

    OpenAIRE

    Corcuera, L.A. (Laura Ana); Ibañez-Vea, M. (María); Vettorazzi, A; Gonzalez-Peñas, E. (Elena); Lopez-de-Cerain, A. (Adela)

    2011-01-01

    A rapid and simple method for the simultaneous quantification of AFB1 and OTA in rat plasma, liver and kidney by UHPLC-FLD has been successfully validated according to the following criteria: selectivity, stability, linearity, precision, accuracy, recovery, robustness and limits of quantification and detection. The extraction method, calibration curves and chromatographic conditions are common for the three matrices. Plasma and homogenized tissue samples (100 μL) were extracted...

  6. 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.

  7. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR SIMULTANEOUS ESTIMATION OF MUPIROCIN AND MOMETASONE FUROATE IN TOPICAL FORMULATION BY RP-HPLC

    Directory of Open Access Journals (Sweden)

    Arti P. Parmar

    2015-04-01

    Full Text Available Purpose: To develop simple, precise, rapid RP-HPLC (Reverse-phase High Performance Liquid Chromatography method for estimation of marketed combination formulation of Mupirocin and Mometasone Furoate. Methods: The Chromatographic separation was achieved on a reversed-phase Phenomenax-luna C18 (250 x 4.6mm, 5 μm column using a mobile phase consisting of acetonitrile : Sodium dihydrogen phosphate buffer (pH 6.8 (70:30 v/v at a flow rate of 1 mL/min and UV detection at 240 nm. Developed methods were validated according to ICH Q2 (R1 guidelines. The methods were found to be linear between the range of 10 - 60 μg/ml for Mupirocin and 1 – 6 μg/ml for Mometasone Furoate. Results: An intra-day precision for Mupirocin was found to be 0.6788% - 0.9820% and for Mometasone Furoate 0.6758%- 0.7532%, inter-day precision for Mupirocin was found to be 0.9775% - 1.1277% for Mometasone Furoate 0.9114% - 1.0765%. Accuracy was determined by recovery studies and showed % recovery between 98 to 102%. Conclusions: A simple, accurate and precise HPLC method was developed and validated for the routine analysis of Mometasone Furoate and Mupirocin in ointment topical formulation. The results make known that the proposed method could be successfully useful for the routine analysis and quality control of pharmaceutical dosage forms containing Mometasone Furoate and Mupirocin. NOVELTY OF THE WORK - The proposed HPLC method was validated as per ICH guidelines. The drug was extracted from an ointment and there is no any interference of excipients was founded. The results of the recovery studies performed show the high degree of accuracy of the proposed method, hence proposed method will useful to routine analysis of Mometasone Furoate and Mupirocin.

  8. Decision analytic methods in RODOS

    International Nuclear Information System (INIS)

    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

  9. Valid, legally defensible data from your analytical laboratories

    International Nuclear Information System (INIS)

    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

  10. A new validated analytical method for the determination of tributyltin in water samples at the quantification level set by the European Union.

    Science.gov (United States)

    Devos, Christophe; David, Frank; Sandra, Pat

    2012-10-26

    According to recent directives of the European Union (EU), limits of quantification (LOQ) for the determination of tributyltin (TBT) in surface waters should be ca. 60 pg/L (ppq). This put very stringent requirements on analytical methodologies; definitely when they have to be applied in a routine environment. Stir bar sorptive extraction (SBSE), followed by thermal desorption (TD) and capillary gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) can provide accurate and precise data at the 2 ng/L level (ppt). For lower concentrations, matrix and reagent interferences together with contamination may provide too high TBT values. A two-dimensional heart-cut GC method was developed to fractionate TBT from interferences. The GC-GC-MS/MS method shows excellent linearity in the range 50 pg/L-4 ng/L, good repeatability (RSD<20% at 200 pg/L), and a limit of detection of 11 pg/L. The method performance is demonstrated with representative samples i.e. harbor water and waste water samples. PMID:22889600

  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...

  12. 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...

  13. 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...

  14. Validation of a UHPLC-FLD analytical method for the simultaneous quantification of aflatoxin B1 and ochratoxin a in rat plasma, liver and kidney.

    Science.gov (United States)

    Corcuera, Laura-Ana; Ibáñez-Vea, María; Vettorazzi, Ariane; González-Peñas, Elena; Cerain, Adela López de

    2011-09-15

    A rapid and simple method for the simultaneous quantification of AFB1 and OTA in rat plasma, liver and kidney by UHPLC-FLD has been successfully validated according to the following criteria: selectivity, stability, linearity, precision, accuracy, recovery, robustness and limits of quantification and detection. The extraction method, calibration curves and chromatographic conditions are common for the three matrices. Plasma and homogenized tissue samples (100 μL) were extracted with acetonitrile:formic acid mixture (99:1) (300 μL). Chromatographic separation was performed with a mixture of water and acetonitrile:methanol (50:50), both acidified with 0.5% of formic acid using a gradient profile. The method avoids the use of immunoaffinity columns and allows reduction of sample and solvent volumes as well as toxic wastes. The detection is based on a photochemical reaction which enhances the AFB1 response without affecting the OTA signal before reaching the fluorescent detector. The mycotoxin recovery for each matrix was very efficient, between 93% and 96% for AFB1 and between 94% and 96% for OTA. For both mycotoxins the LOQs were 2μg/L in plasma and 8μg/kg in liver and kidney. The method has successfully been applied to rat samples after a single oral administration of a mixture of AFB1 and OTA and it could be a useful tool in toxicokinetic and toxicological studies. PMID:21868292

  15. Comparison and validation of 2 analytical methods for the determination of free fatty acids in dairy products by gas chromatography with flame ionization detection.

    Science.gov (United States)

    Mannion, David T; Furey, Ambrose; Kilcawley, Kieran N

    2016-07-01

    Accurate quantification of free fatty acids (FFA) in dairy products is important for quality control, nutritional, antimicrobial, authenticity, legislative, and flavor purposes. In this study, the performance of 2 widely used gas chromatographic flame ionization detection methods for determination of FFA in dairy products differing in lipid content and degree of lipolysis were evaluated. We used a direct on-column approach where the isolated FFA extract was injected directly and a derivatization approach where the FFA were esterified in the injector to methyl esters using tetramethylammonium hydroxide as a catalyst. A comprehensive validation was undertaken to establish method linearity, limits of detection, limits of quantification, accuracy, and precision. Linear calibrations of 3 to 700mg/L (R(2)>0.999) and 20 to 700mg/L (R(2)>0.997), and limits of detection and limits of quantification of 0.7 and 3mg/L and 5 and 20mg/L were obtained for the direct injection on-column and the derivatization method, respectively. Intraday precision of 1.5 to 7.2% was obtained for both methods. The direct injection on-column method had the lower levels of limits of detection and quantification, because FFA are directly injected onto the GC as opposed to the split injection used in the derivatization method. However, the direct injection on-column method experienced accumulative column phase deterioration and irreversible FFA absorption because of the acidic nature of the injection extract, which adversely affected method robustness and the quantification of some longer chain FFA. The derivatization method experienced issues with quantification of butyric acid at low concentrations because of coelution with the injection solvent peak, loss of polyunsaturated FFA due to degradation by tetramethylammonium hydroxide, and the periodic emergence of by-product peaks of the tetramethylammonium hydroxide reaction that interfered with the quantification of some short-chain FFA. The

  16. 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...

  17. 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...

  18. 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)

    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 range

  19. Analytical methods used at model facility

    International Nuclear Information System (INIS)

    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

  20. Development and validation of an HPLC-MS/MS analytical method for quantitative analysis of TCBA-TPQ, a novel anticancer makaluvamine analog, and application in a pharmacokinetic study in rats.

    Science.gov (United States)

    Yu, Jun-Xian; Voruganti, Sukesh; Li, Dan-Dan; Qin, Jiang-Jiang; Nag, Subhasree; Xu, Su; Velu, Sadanandan E; Wang, Wei; Zhang, Ruiwen

    2015-07-01

    We have recently designed and synthesized several novel iminoquinone anticancer agents that have entered preclinical development for the treatment of human cancers. Herein we developed and validated a quantitative HPLC-MS/MS analytical method for one of the lead novel anticancer makaluvamine analog, TCBA-TPQ, and conducted a pharmacokinetic study in laboratory rats. Our results indicated that the HPLC-MS/MS method was precise, accurate, and specific. Using this method, we carried out in vitro and in vivo evaluations of the pharmacological properties of TCBA-TPQ and plasma pharmacokinetics in rats. Our results provide a basis for future preclinical and clinical development of this promising anticancer marine analog. PMID:26233847

  1. Analytical mechanics methods for solving Whittaker equations

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The purpose of this paper is to study the solution of the celebrated Whittaker equations by using analytical mechanics methods, including the Lagrange-Noether method, Hamilton-Poisson method and potential integral method.

  2. [Validation and verfication of microbiology methods].

    Science.gov (United States)

    Camaró-Sala, María Luisa; Martínez-García, Rosana; Olmos-Martínez, Piedad; Catalá-Cuenca, Vicente; Ocete-Mochón, María Dolores; Gimeno-Cardona, Concepción

    2015-01-01

    Clinical microbiologists should ensure, to the maximum level allowed by the scientific and technical development, the reliability of the results. This implies that, in addition to meeting the technical criteria to ensure their validity, they must be performed with a number of conditions that allows comparable results to be obtained, regardless of the laboratory that performs the test. In this sense, the use of recognized and accepted reference methodsis the most effective tool for these guarantees. The activities related to verification and validation of analytical methods has become very important, as there is continuous development, as well as updating techniques and increasingly complex analytical equipment, and an interest of professionals to ensure quality processes and results. The definitions of validation and verification are described, along with the different types of validation/verification, and the types of methods, and the level of validation necessary depending on the degree of standardization. The situations in which validation/verification is mandatory and/or recommended is discussed, including those particularly related to validation in Microbiology. It stresses the importance of promoting the use of reference strains as controls in Microbiology and the use of standard controls, as well as the importance of participation in External Quality Assessment programs to demonstrate technical competence. The emphasis is on how to calculate some of the parameters required for validation/verification, such as the accuracy and precision. The development of these concepts can be found in the microbiological process SEIMC number 48: «Validation and verification of microbiological methods» www.seimc.org/protocols/microbiology. PMID:24958671

  3. 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

    -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......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...

  4. 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.

  5. 7 CFR 91.23 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 91.23 Section 91.23 Agriculture... SERVICES AND GENERAL INFORMATION Method Manuals § 91.23 Analytical methods. Most analyses are performed according to approved procedures described in manuals of standardized methodology. These standard...

  6. 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,...

  7. 7 CFR 93.13 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture... PROCESSED FRUITS AND VEGETABLES Peanuts, Tree Nuts, Corn and Other Oilseeds § 93.13 Analytical methods... manuals: (a) Approved Methods of the American Association of Cereal Chemists (AACC), American...

  8. Planilha de validação: uma nova ferramenta para estimar figuras de mérito na validação de métodos analíticos univariados Validation spreadsheet: a new tool for estimating the analytical figures of merit for the validation of univariate methods

    Directory of Open Access Journals (Sweden)

    Fabiana Alves de Lima Ribeiro

    2008-01-01

    Full Text Available This work presents the VALIDATION SPREADSHEET, a public domain tool that can be used to evaluate the figures of merit for univariate analytical methods. A real example of BTEX determination in environmental samples is included to illustrate its use. The spreadsheet has been developed for Excel® and Open Office®, and is available on the internet at http//lqta.iqm.unicamp.br.

  9. Validation of the General Electric pressure suppression analytical model

    International Nuclear Information System (INIS)

    The GE Company's analytical model for pressure suppression system transient response has evolved over more than 15 years. This paper describes the validation process and results from qualification of the latest version of this model. A general description of the model, validation activities, test data used for qualification, and model/data comparisons are included. Based on drywell pressure response, the model is shown to be about 3% conservative when run in the best estimate mode, and approximately 15% conservative when run in the design basis mode. (orig.)

  10. Development and validation of a new analytical method for the determination of 1,4-dichlorobenzene in honey by gas chromatography-isotope dilution mass spectrometry after steam-distillation

    International Nuclear Information System (INIS)

    A simple, fast, sensitive and robust analytical method using gas chromatography (GC)-isotope dilution mass spectrometry (MS) was developed and validated for the identification and quantification of 1,4-dichlorobenzene (p-DCB) residues in honey samples. The proposed methodology is based on steam-distillation using a Clevenger-type apparatus followed by gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring (SIM) mode employing the isotopically labeled analogue D 4-1,4-dichlorobenzene (D 4-p-DCB) as internal standard (IS). Validation of the method was performed in two different GC-MS systems, using quadrupole MS (QMS) and ion-trap MS (ITMS) detectors, with no statistically significant differences between two. Recoveries were better than 91% with percent relative standard deviations lower than 12%. The instrumental limits of detection were 1 μg kg-1 in the GC-ITMS system and 0.6 μg kg-1 in the GC-QMS system. The expanded uncertainty was estimated as 17% at the currently accepted 'action level' of 10 μg kg-1. The method was applied to the analysis of 310 honey samples in an extensive national monitoring study. A quality control (QC) system applied during the assays has demonstrated a good performance and long-term stability over a period of more than 8 months of continuous operation

  11. Alternative methods in toxicology: pre-validated and validated methods

    OpenAIRE

    Kandárová, Helena; Letašiová, Silvia

    2011-01-01

    The development of alternative methods to animal experimentation has progressed rapidly over the last 20 years. Today, in vitro and in silico methods have an important role in the hazard identification and assessment of toxicology profile of compounds. Advanced alternative methods and their combinations are also used for safety assessment of final products. Several alternative methods, which were scientifically validated and accepted by competent regulatory bodies, can be used for regulatory ...

  12. 40 CFR 141.704 - Analytical methods.

    Science.gov (United States)

    2010-07-01

    ... Federal Register approves this incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 CFR... 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...

  13. HTGR analytical methods and design verification

    International Nuclear Information System (INIS)

    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. Analytical detection methods for irradiated foodstuff

    International Nuclear Information System (INIS)

    Some analytical detection methods are used in the world. A detail of establishment of CEN Standards in 1996, one of them, is explained. Nine standards of CEN are adopted by the Codex Standards (General Codex Methods for detection of irradiated Food). Main analytical technologies and the standard method are stated. As the physical methods, ESR (Electron Spin Resonance), TL and PSL (Photostimulated Luminescence) method are described. On chemical methods, hydrocarbons method, 2-alkylcyclobutanone method and other methods are discussed. DNA method, DEFT/APC, LAL/GNB and DEFT/APC method are explained as the biological methods. The application methods of irradiated food and classification of analytical detection methods are shown. References after 1996 are reviewed. (S.Y.)

  15. 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. PMID:23993492

  16. Validation of an analytical method for the determination of valsartan in human plasma by HPLC/UV with addition standard using losartan as an internal standard.

    Directory of Open Access Journals (Sweden)

    Milena Pérez

    2009-11-01

    Full Text Available Introducción: El concepto de validación se refiere a la evaluación estadística de los resultados obtenidos en la aplicación de técnicas analíticas, mediante pruebas convenientemente documentadas y demostrativas de que un método es lo suficientemente fiable a fin de producir el resultado previsto bajo condiciones definidas, como son: sistema analítico, intervalo de concentración, infraestructura y talento humano. Objetivo: Describir el proceso de validación del método analítico para la cuantificación de valsartán en plasma humano por HPLC-UV y su aplicación en estudios farmacocinéticos, de biodisponibilidad y bioequivalencia de medicamentos que contengan valsartán como principio activo. Metodología: Se desarrolló un método para la detección y cuantificación de valsartán en plasma humano, con elución isocrática por cromatografía líquida de fase reversa, con detección ultravioleta a 265 nm, mediante el método de adición de estándar. Se utilizó losartán como estándar interno. El método implica una extracción en fase sólida de los principios activos (valsartán y losartán con cartuchos C8. La separación se realizó en una columna C18 en fase reversa y la fase móvil fue una mezcla de acetonitrilo: buffer fosfato  (45:55 v/v ajustado a pH 2.7±0.1 con ácido fosfórico concentrado. El método se validó en el rango de concentraciones de 0.05 a 20 µg/ml con adición de estándar de valsartán de 2.5 µg/ml. Resultados y conclusiones: La curva de calibración fue lineal en el rango de concentraciones establecido. Se evaluó la reproducibilidad, estabilidad y porcentaje de recuperación del método. El método para determinar el valsartán en plasma humano por HPLC/UV fue preciso y exacto con un límite de cuantificación de 1.485 µg/ml. Este método fue suficientemente sensible para su aplicación en estudios farmacocinéticos de valsartán.

  17. Validation of a confirmatory analytical method for the determination of aflatoxins B₁, B₂, G₁ and G₂ in foods and feed materials by HPLC with on-line photochemical derivatization and fluorescence detection.

    Science.gov (United States)

    Muscarella, Marilena; Iammarino, Marco; Nardiello, Donatella; Magro, Sonia Lo; Palermo, Carmen; Centonze, Diego; Palermo, Domenico

    2009-10-01

    A sensitive and selective analytical method for the simultaneous separation and quantitative determination of aflatoxins B1, B2, G1 and G2 in foodstuffs and materials for feed has been validated. The method is based on high performance liquid chromatography with on-line post-column photochemical derivatization and fluorescence detection. The chromatographic separation of aflatoxins was accomplished using a C18 column eluted with an isocratic mobile phase consisting of water, methanol and acetonitrile. The sample preparation required a simple extraction of aflatoxins with MeOH/H2O (80:20, v/v) and a purification step by immunoaffinity column cleanup. The total analysis time, including sample preparation and chromatographic separation, did not exceed 40 min with a run time of 10 min. The on-line photochemical derivatization ensures better results in terms of simplicity, sensitivity and reproducibility with respect to chemical derivatization techniques, and provides an increase of the peak resolution and an extent of automation in comparison with the electrochemical ones. The procedure for the determination of aflatoxins in food samples and cereals for animal consumption was extensively validated following Regulation (EC) No. 882/2004. Detection limits in wheat bran samples of 0.08 μg kg1 for AFB1, 0.02 μg kg1 for AFB2, 0.16 μg kg1 for AFG1 and 0.04 μg kg1 for AFG2 were attained. The method allows high recovery with mean values ranging from 72 to 94% and it satisfies the necessary requirements for sensitivity, linearity, selectivity, precision and ruggedness, demonstrating the conformity of the method with provisions of Regulation (EC) No. 401/2006. PMID:21462585

  18. 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...

  19. Analytical Methods in Mesoscopic Systems

    Science.gov (United States)

    Mason, Douglas Joseph

    The prospect of designing technologies around the quantum behavior of mesoscopic devices is enticing. This thesis present several tools to facilitate the process of calculating and analyzing the quantum properties of such devices - resonance, boundary conditions, and the quantum-classical correspondence are major themes that we study with these tools. In Chapter 1, we begin by laying the groundwork for the tools that follow by defining the Hamiltonian, the Green's function, the scattering matrix, and the Landauer formalism for ballistic conduction. In Chapter 2, we present an efficient and easy-to-implement algorithm called the Outward Wave Algorithm, which calculates the conductance function and scattering density matrix when a system is coupled to an environment in a variety of geometries and contexts beyond the simple two-lead schematic. In Chapter 3, we present a unique geometry and numerical method called the Boundary Reflectin Matrix that allows us to calculate the full scattering matrix from arbitrary boundaries of a lattice system, and introduce the phenomenon of internal Bragg diffraction. In Chapter 4, we present a new method for visualizing wavefunctions called the Husimi map, which uses measurement by coherent states to form a bridge between the quantum flux operator and semiclassics. We extend the formalism from Chapter 4 to lattice systems in Chapter 5, and comment on our results in Chapter 3 and other work in the literature. These three tools - the Outward Wave Algorithm, the Boundary Reflection Matrix, and the Husimi map - work together to throw light on our interpretation of resonance and scattering in quantum systems, effectively codifying the expertise developed in semiclassics over the past few decades in an efficient and robust package. The data and images that they make available promise to help design better technologies based on quantum scattering.

  20. METHODS FOR TESTING DISCRIMINANT VALIDITY

    Directory of Open Access Journals (Sweden)

    Adriana ZAIŢ

    2011-01-01

    Full Text Available The study presents three methods which can be used to assess discriminant validity for multi-item scales. Q-sorting is presented as a method that can be used in early stages of research, being more exploratory, while the chi-square difference test and the average variance extracted analysis are recommended for the confirmatory stages of research. The paper describes briefly the three methods and presents evidence from two surveys that aimed to develop a scale for measuring perceived risk in e-commerce.

  1. Analytical Approach Validation for the Spin-Stabilized Satellite Attitude

    Science.gov (United States)

    Zanardi, Maria Cecilia F. P. S.; Garcia, Roberta Veloso; Kuga, Helio Koiti

    2007-01-01

    An analytical approach for spin-stabilized spacecraft attitude prediction is presented for the influence of the residual magnetic torques and the satellite in an elliptical orbit. Assuming a quadripole model for the Earth s magnetic field, an analytical averaging method is applied to obtain the mean residual torque in every orbital period. The orbit mean anomaly is used to compute the average components of residual torque in the spacecraft body frame reference system. The theory is developed for time variations in the orbital elements, giving rise to many curvature integrals. It is observed that the residual magnetic torque does not have component along the spin axis. The inclusion of this torque on the rotational motion differential equations of a spin stabilized spacecraft yields conditions to derive an analytical solution. The solution shows that the residual torque does not affect the spin velocity magnitude, contributing only for the precession and the drift of the spin axis of the spacecraft. The theory developed has been applied to the Brazilian s spin stabilized satellites, which are quite appropriated for verification and comparison of the theory with the data generated and processed by the Satellite Control Center of Brazil National Research Institute. The results show the period that the analytical solution can be used to the attitude propagation, within the dispersion range of the attitude determination system performance of Satellite Control Center of Brazil National Research Institute.

  2. 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

  3. Validated Analytical Model of a Pressure Compensation Drip Irrigation Emitter

    Science.gov (United States)

    Shamshery, Pulkit; Wang, Ruo-Qian; Taylor, Katherine; Tran, Davis; Winter, Amos

    2015-11-01

    This work is focused on analytically characterizing the behavior of pressure-compensating drip emitters in order to design low-cost, low-power irrigation solutions appropriate for off-grid communities in developing countries. There are 2.5 billion small acreage farmers worldwide who rely solely on their land for sustenance. Drip, compared to flood, irrigation leads to up to 70% reduction in water consumption while increasing yields by 90% - important in countries like India which are quickly running out of water. To design a low-power drip system, there is a need to decrease the pumping pressure requirement at the emitters, as pumping power is the product of pressure and flow rate. To efficiently design such an emitter, the relationship between the fluid-structure interactions that occur in an emitter need to be understood. In this study, a 2D analytical model that captures the behavior of a common drip emitter was developed and validated through experiments. The effects of independently changing the channel depth, channel width, channel length and land height on the performance were studied. The model and the key parametric insights presented have the potential to be optimized in order to guide the design of low-pressure, clog-resistant, pressure-compensating emitters.

  4. 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).

  5. 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.

  6. Analytic compensation methods in dynamic tomography

    International Nuclear Information System (INIS)

    Recent progresses in X-ray tomography allow to study some organs dynamically. The aim of this work is to analyze the deformation compensation algorithms used to integrate dynamical evolution models into the image reconstruction processes. An exact and efficient analytical method of movement compensation is presented and applied to simulated data. Abstract only. (J.S.)

  7. Numerical and analytical methods with Matlab

    CERN Document Server

    Bober, William; Masory, Oren

    2013-01-01

    Numerical and Analytical Methods with MATLAB® presents extensive coverage of the MATLAB programming language for engineers. It demonstrates how the built-in functions of MATLAB can be used to solve systems of linear equations, ODEs, roots of transcendental equations, statistical problems, optimization problems, control systems problems, and stress analysis problems. These built-in functions are essentially black boxes to students. By combining MATLAB with basic numerical and analytical techniques, the mystery of what these black boxes might contain is somewhat alleviated. This classroom-tested

  8. Analytical detection methods for irradiated foods

    International Nuclear Information System (INIS)

    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

  9. Rat brain polyamines: an analytical method validation Poliaminas no cérebro do rato: validação de método analítico

    OpenAIRE

    Valdomiro de Freitas Sampaio; Gilberto J. Padovan; Julio Sérgio Marchini; Luiz Marcellino de Oliveira; Sebastião de Sousa Almeida

    2010-01-01

    The validation of the analytical technique for the determination of polyamines in cerebral tissue using HPLC based on o-phthalaldehyde post-column derivatization is described. The polyamines were separated in a LiChrospher100 RP18 column. Elution gradient was formed with two mobile phases: A (sodium acetate 0.1 M + sodium octanesulphonate 0.01 M, pH = 4.5) and B (sodium acetate 0.2 M + sodium octanesulphonate 0.01 M)/acetonitrile (10:3), pH = 4.5) in a 1.2 ml/min flow rate. The derivative elu...

  10. Nuclear analytical methods for platinum group elements

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    The aim of this study was to validate analytical method for determination of total radioactivity and radioactive concentration of 125I-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)

  12. Wavelet Analytical Forecasting Method of Water Consumption

    Institute of Scientific and Technical Information of China (English)

    刘洪波; 张宏伟

    2004-01-01

    A new method of short-term forecasting for water consumption in municipal supply water networks based on wavelet transformation is introduced. By wavelet decomposing commonly used in the signal field, water consumption per hour is decomposed into many series. Trend item, cycle item and random item are separated from the original time series in this way.Then by analyzing, building a model, forecasting every series and composing the results, the forecasting value of the original consumption is received. Simulation results show that this forecasting method is faster and more accurate, of which the error is less than 20%,indicating that the wavelet analytical method is practicable.

  13. Secondary waste minimization in analytical methods

    International Nuclear Information System (INIS)

    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

  14. Analytical crashworthiness methods applied to composite structures

    OpenAIRE

    Lehnhardt, Keith W.

    1999-01-01

    CIVINS Several shell deformation models are developed for use in crashworthiness analysis of rotationally symmetric structures. These models use analytical techniques to predict the crushing force versus axial crush distance characteristics of both a rigid-plastic, hemispherical shell and an elastic, cylindrical shell loaded axially by a rigid flat plate. Additional methods are proposed to determine the effects of cutout sections and internal stiffening members on the crushing force capaci...

  15. A New Analytic Alignment Method for a SINS

    Directory of Open Access Journals (Sweden)

    Caiming Tan

    2015-11-01

    Full Text Available Analytic alignment is a type of self-alignment for a Strapdown inertial navigation system (SINS that is based solely on two non-collinear vectors, which are the gravity and rotational velocity vectors of the Earth at a stationary base on the ground. The attitude of the SINS with respect to the Earth can be obtained directly using the TRIAD algorithm given two vector measurements. For a traditional analytic coarse alignment, all six outputs from the inertial measurement unit (IMU are used to compute the attitude. In this study, a novel analytic alignment method called selective alignment is presented. This method uses only three outputs of the IMU and a few properties from the remaining outputs such as the sign and the approximate value to calculate the attitude. Simulations and experimental results demonstrate the validity of this method, and the precision of yaw is improved using the selective alignment method compared to the traditional analytic coarse alignment method in the vehicle experiment. The selective alignment principle provides an accurate relationship between the outputs and the attitude of the SINS relative to the Earth for a stationary base, and it is an extension of the TRIAD algorithm. The selective alignment approach has potential uses in applications such as self-alignment, fault detection, and self-calibration.

  16. Comparison of nuclear analytical methods with competitive methods

    International Nuclear Information System (INIS)

    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

  17. 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.

  18. Directory of Analytical Methods, Department 1820

    Energy Technology Data Exchange (ETDEWEB)

    Whan, R.E. (ed.)

    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.

  19. Directory of Analytical Methods, Department 1820

    International Nuclear Information System (INIS)

    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

  20. SELECTION OF ONLINE SHOPPING SITE BASED ON ANALYTIC HIERARCHY PROCESS AND ANALYTIC NETWORK PROCESS METHODS

    OpenAIRE

    ÖMÜRBEK, Nuri; ŞİMŞEK, Ali

    2014-01-01

    Analytic Hierarchy Process and Analytic Network Process are common multi criteria decision-making methods. Analytic Hierarchy Process identifies the degree of importance of effective decision making criteria and ranks decision alternatives by making pairwise comparisons. Analytic Network Process, however, identifies the relationship and its direction between the criteria and the alternatives in order to solve problems in a network. In this study, Analytic Hierarchy Process and Analytic Networ...

  1. Analytical methods to identify irradiated food--a review

    International Nuclear Information System (INIS)

    The ability to analytically identify irradiated food - complementary to certification - helps to enhance consumers confidence. It makes it possible to check compliance with existing regulations (e.g. enforcement of labelling, control of prohibition) and to facilitate international food trade. An enormous effort--both at the world-wide international level (ADMIT) and at European (BCR)/national level--has led to several validated and even standardized (CEN) detection methods for a large number of different food products. In this short review, the present methods are summarized, limitations and new developments drafted

  2. An inverse and analytic lens design method

    CERN Document Server

    Lu, Yang

    2016-01-01

    Traditional lens design is a numerical and forward process based on ray tracing and aberration theory. This method has limitations because the initial configuration of the lens has to be specified and the aberrations of the lenses have to considered. This paper is an initial attempt to investigate an analytic and inverse lens design method, called Lagrange, to overcome these barriers. Lagrange method tries to build differential equations in terms of the system parameters and the system input and output (object and image). The generalized Snell's law in three dimensional space and the normal of a surface in fundamental differential geometry are applied. Based on the Lagrange method equations for a single surface system are derived which can perfectly image a point object.

  3. 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.

  4. 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....

  5. Analytical Methods for Uranium Concentration Measurements

    International Nuclear Information System (INIS)

    A survey of analytical procedures for the determination of uranium, as performed for NMM in the United States of America, is presented. Methods are outlined for the measurement of the element in a variety of materials, i.e. ores, concentrates, uranium metal, alloys, ceramics, compounds of uranium, scrap processing solutions, residues, and waste stream products. It is not intended as a complete résumé dealing with the subject, but it does offer measurement methods believed to give precise and accurate results of a high order. Because of the monetary value of the materials, and the transfer activities from one installation to another, involving payments or credits, burn-up charges, use charges, etc., it is essential that such methods are used. Methods of analysis to a large extent are dictated by the types of material to be analysed. The use of gravimetric methods are reviewed pertaining to product materials, which are generally defined as uranium metal, or compounds of the metal, such as oxides, halides, or nitrates. A pyro-hydrolysis technique is included under this heading. Non-volatile metallic impurities are determined spectroscopically, and the gravimetric results are corrected accordingly. Volumetric procedures, the ''workhorse'' methods for determining uranium, are thoroughly explored. The technique is applicable to all types of material, providing the uranium available for measurement is present in milligram quantities. Due to the valence states of uranium, reduction-oxidation schemes are particularly attractive. Dissolution problems, separation of interfering elements, reduction steps, and oxidation titrations of reduced uranium are discussed. The application of certain spectrophotometric and fluorometric procedures for analysing low-grade materials are included. Various separation steps incorporated in the procedures before the determination of uranium are reviewed. Along these lines the utilization of differential colorimetry is examined for determining

  6. Optimization and validation of a GC-MS analytical method for the determination of alkylated phenols and bisphenol A in sea water and suspended matter; Optimierung und Validierung einer GC-MS-Analysenmethode zur Bestimmung alkylierter Phenole und Bisphenol A in Meerwasser und Schwebstoffen

    Energy Technology Data Exchange (ETDEWEB)

    Theobald, N.; Meyer, C.

    2001-12-01

    A method for the determination of alkylated phenols, phenol ethoxylates and bisphenol A in surface and sea water was optimized and validated. The analytical procedure consists of a liquid/liquid extraction with dichloromethane, a derivatisation with bis(heptafluorobutyric) anhydride and a GC-MS determination in EI-mode under selected ion monitoring condition. The validation parameters such as measuring precision, method precision, linearity, limits of determination, accuracy and robustness were determined. Very good results were achieved for all parameters. It turned out that the problem of contamination has to be observed very carefully. The method validation was supported by organising and performing two ring tests. For the first test, spiked samples of ultra-clean water were analysed. For the second test spiked river and sea water samples were investigated. The results show that the presented method is capable for monitoring purposes within the Bund-Laender-Messprogramm. (orig.)

  7. The analytic nodal method in cylindrical geometry

    International Nuclear Information System (INIS)

    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

  8. 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.

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

    International Nuclear Information System (INIS)

    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)

  10. Numerical methods: Analytical benchmarking in transport theory

    International Nuclear Information System (INIS)

    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

  11. Analytical methods to assess nanoparticle toxicity.

    Science.gov (United States)

    Marquis, Bryce J; Love, Sara A; Braun, Katherine L; Haynes, Christy L

    2009-03-01

    During the past 20 years, improvements in nanoscale materials synthesis and characterization have given scientists great control over the fabrication of materials with features between 1 and 100 nm, unlocking many unique size-dependent properties and, thus, promising many new and/or improved technologies. Recent years have found the integration of such materials into commercial goods; a current estimate suggests there are over 800 nanoparticle-containing consumer products (The Project on Emerging Nanotechnologies Consumer Products Inventory, , accessed Oct. 2008), accounting for 147 billion USD in products in 2007 (Nanomaterials state of the market Q3 2008: stealth success, broad impact, Lux Research Inc., New York, NY, 2008). Despite this increase in the prevalence of engineered nanomaterials, there is little known about their potential impacts on environmental health and safety. The field of nanotoxicology has formed in response to this lack of information and resulted in a flurry of research studies. Nanotoxicology relies on many analytical methods for the characterization of nanomaterials as well as their impacts on in vitro and in vivo function. This review provides a critical overview of these techniques from the perspective of an analytical chemist, and is intended to be used as a reference for scientists interested in conducting nanotoxicological research as well as those interested in nanotoxicological assay development. PMID:19238274

  12. 77 FR 41336 - Analytical Methods Used in Periodic Reporting

    Science.gov (United States)

    2012-07-13

    ... 39 CFR Part 3050 Analytical Methods Used in Periodic Reporting AGENCY: Postal Regulatory Commission... initiate an informal rulemaking proceeding to consider changes in analytical methods used in periodic... the Commission initiate an informal rulemaking proceeding to consider changes in the...

  13. Evolution of microbiological analytical methods for dairy industry needs

    Directory of Open Access Journals (Sweden)

    Daniele eSohier

    2014-02-01

    Full Text Available Traditionally, culture-based methods have been used to enumerate microbial populations in dairy products. Recent developments in molecular methods now enable faster and more sensitive analyses than classical microbiology procedures. These molecular tools allow a detailed characterization of cell physiological states and bacterial fitness and thus, offer new perspectives to integration of microbial physiology monitoring to improve industrial processes. This review summarizes the methods described to enumerate and characterize physiological states of technological microbiota in dairy products, and discusses the current deficiencies in relation to the industry’s needs. Recent studies show that PCR-based methods can successfully be applied to quantify fermenting microbes and probiotics in dairy products. Flow cytometry and omics technologies also show interesting analytical potentialities. However, they still suffer from a lack of validation and standardization for quality control analyses, as reflected by the absence of performance studies and official international standards.

  14. 40 CFR 161.180 - Enforcement analytical method.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Enforcement analytical method. 161.180 Section 161.180 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS... § 161.180 Enforcement analytical method. An analytical method suitable for enforcement purposes must...

  15. 40 CFR 158.355 - Enforcement analytical method.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Enforcement analytical method. 158.355... DATA REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.355 Enforcement analytical method. An analytical method suitable for enforcement purposes must be provided for each active ingredient in...

  16. ANALYTICAL METHODS FOR CALCULATING FAN AERODYNAMICS

    Directory of Open Access Journals (Sweden)

    Jan Dostal

    2015-12-01

    Full Text Available This paper presents results obtained between 2010 and 2014 in the field of fan aerodynamics at the Department of Composite Technology at the VZLÚ aerospace research and experimental institute in Prague – Letnany. The need for rapid and accurate methods for the preliminary design of blade machinery led to the creation of a mathematical model based on the basic laws of turbomachine aerodynamics. The mathematical model, the derivation of which is briefly described below, has been encoded in a computer programme, which enables the theoretical characteristics of a fan of the designed geometry to be determined rapidly. The validity of the mathematical model is assessed continuously by measuring model fans in the measuring unit, which was developed and manufactured specifically for this purpose. The paper also presents a comparison between measured characteristics and characteristics determined by the mathematical model as the basis for a discussion on possible causes of measured deviations and calculation deviations.

  17. Catalyst Kinetics Analytical Method Study of Ruthenium

    Institute of Scientific and Technical Information of China (English)

    Kou ming-ze; Zhan hui-ying; Kou zong-yan

    2004-01-01

    Color reactions are used to determine ruthenium utilizing spectrophotometer, but the process need high temperature, long time pyrogenation and miscellaneous extraction and it contaminates the enviroment. As the sensitive degree and simple apparatus of catalyst kinetics analytical method, it was extensively attentcd. The fundmental principle means to determinn a certain chemistry reaction rate accelerated by homogeneous catalyst and determine substantial content using the function of the numerical value of of its and the catalyst concentration. Color acid double azo-reagents (chloro-phosphor group, arsenic group and carboxylic acid group) are sensitive color reagent determining uranium and thorium of lanthanon, but the report is few that it is used to determine ruthenium. Since 1990s, the author studied that the ruthenium was possessed evident catalysis to the fade reaction of oxidant (KIO4, KBrO3) oxidating color acid double azo-reagent in acitidy medium and provided the catalyst kinetics analytical method to determine trace ruthenium.sensitive degree was increased 1 ~2 amount than color reaction. The reaction as:The original concentration of color acid double azo-reagents is A. The instantaneous absorbency after t reaction time is At. In homogeneous catalyst reaction: log(A0/At) = KCRu3+t. Reaction time t is invarible, so log(A0/At) = K' CRu3+t.Color acid double azo-reagents, such as: chlor-azochlorphosphor(CPA-TC),bromic-azochlorphosphor (CPA-TB), DBS-azochlorphosphor(DBS-CPA), DBC-azochlorphosphor (DBC-CPA), DBOK-azochlorpho sphor (DBOK-CPA), p-iodineazochlorphosphor(CPA-PI),p-acetylazochlorphosphor (CPA-PA), azochlorpho sphorⅢ(CPAⅢ), chlor-azoarsenic (TC-AsA),bromic-azoarsenic (TB-AsA), DBS-azoarsenic(DCS-AsA), DCS-azoarsenic(DCS-AsA),azoarsenicⅢ(AsAⅢ), bromicnityrlazoarsenic (DBN-AsA), P-acetylcarboxy lazo-p,P-acetylcarboxylazo, were utilized in catalyst kinetics system. The author obtains the satisfactory results that color acid double azo-rea gents

  18. Reactor analysis methods. 1. Removal of Numerical Singularity in Analytical Nodal Methods via Continued Factoring

    International Nuclear Information System (INIS)

    nearly no-net-leakage nodes. An algebraically exact method is proposed in this paper to eliminate the numerical singularity. The method is based on factoring out the singular components from the nonsingular components in the highly ill conditioned system that can arise in analytical nodal formulation. The method does not require a priori identification of the singular nodes to treat separately and is valid for all nodes. The proposed method was implemented in AFEN and tested in the rectangular and hexagonal geometries. It should be straightforward to implement the method in ANM

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

    International Nuclear Information System (INIS)

    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. 77 FR 56176 - Analytical Methods Used in Periodic Reporting

    Science.gov (United States)

    2012-09-12

    ... 39 CFR Part 3001 Analytical Methods Used in Periodic Reporting AGENCY: Postal Regulatory Commission... Service petition to initiate an informal rulemaking proceeding to consider changes in analytical... consider changes in the analytical methods approved for use in periodic reporting.\\1\\ \\1\\ Petition of...

  1. 40 CFR 136.6 - Method modifications and analytical requirements.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Method modifications and analytical... modifications and analytical requirements. (a) Definitions of terms used in this section. (1) Analyst means the person or laboratory using a test procedure (analytical method) in this Part. (2) Chemistry of the...

  2. Method validation for phthalate analysis from water

    OpenAIRE

    Irina Dumitraşc

    2013-01-01

    The goal of method validation is to provide objective evidence that the evaluated method will show acceptable reproducibility and accuracy so as to be applicable. The objective of this paper is to present a validation method for quantitative phthalates analysis from water by solid phase extraction (SPE) and determination by gas chromatography in combination with mass spectrometry detector (GC–MS) in electronic ionization mode (EI) with selected -ion monitoring (SIM) acquisition...

  3. Design for validation, based on formal methods

    Science.gov (United States)

    Butler, Ricky W.

    1990-01-01

    Validation of ultra-reliable systems decomposes into two subproblems: (1) quantification of probability of system failure due to physical failure; (2) establishing that Design Errors are not present. Methods of design, testing, and analysis of ultra-reliable software are discussed. It is concluded that a design-for-validation based on formal methods is needed for the digital flight control systems problem, and also that formal methods will play a major role in the development of future high reliability digital systems.

  4. Analytical bootstrap methods for censored data

    OpenAIRE

    Alan D. Hutson

    2002-01-01

    Analytic bootstrap estimators for the moments of survival quantities are derived. By using these expressions recommendations can be made as to the appropriateness of bootstrap estimation under censored data conditions.

  5. Analytical prediction and field validation of transient temperature field in asphalt pavements

    Institute of Scientific and Technical Information of China (English)

    陈嘉祺; 李亮; 汪浩

    2015-01-01

    This work presented the development and validation of an analytical method to predict the transient temperature field in the asphalt pavement. The governing equation for heat transfer was based on heat conduction radiation and convection. An innovative time-dependent function was proposed to predict the pavement surface temperature with solar radiation and air temperature using dimensional analysis in order to simplify the complex heat exchange on the pavement surface. The parameters for the time-dependent pavement surface temperature function were obtained through the regression analysis of field measurement data. Assuming that the initial pavement temperature distribution was linear and the influence of the base course materials on the temperature of the upper asphalt layers was negligible, a close-form analytical solution of the temperature in asphalt layers was derived using Green’s function. Finally, two numerical examples were presented to validate the model solutions with field temperature measurements. Analysis results show that the solution accuracy is in agreement with field data and the relative errors at a shallower depth are greater than those at a deeper one. Although the model is not sensitive to dramatic changes in climatic factors near the pavement surface, it is applicable for predicting pavement temperature field in cloudless days.

  6. Validation of analytical breast cancer microarray analysis in medical laboratory.

    Science.gov (United States)

    Darweesh, Amal Said; Louka, Manal Louis; Hana, Maha; Rashad, Shaymaa; El-Shinawi, Mohamed; Sharaf-Eldin, Ahmed; Kassim, Samar Kamal

    2014-10-01

    A previously reported microarray data analysis by RISS algorithm on breast cancer showed over-expression of the growth factor receptor (Grb7) and it also highlighted Tweety (TTYH1) gene to be under expressed in breast cancer for the first time. Our aim was to validate the results obtained from the microarray analysis with respect to these genes. Also, the relationship between their expression and the different prognostic indicators was addressed. RNA was extracted from the breast tissue of 30 patients with primary malignant breast cancer. Control samples from the same patients were harvested at a distance of ≥5 cm from the tumour. Semi-quantitative RT-PCR analysis was done on all samples. There was a significant difference between the malignant and control tissues as regards Grb7 expression. It was significantly related to the presence of lymph node metastasis, stage and histological grade of the malignant tumours. There was a significant inverse relation between expression of Grb7 and expression of both oestrogen and progesterone receptors. Grb7 was found to be significantly related to the biological classification of breast cancer. TTYH1 was not expressed in either the malignant or the control samples. The RISS by our group algorithm developed was laboratory validated for Grb7, but not for TTYH1. The newly developed software tool needs to be improved. PMID:25182704

  7. Fracture mechanics life analytical methods verification testing

    Science.gov (United States)

    Favenesi, J. A.; Clemons, T. G.; Riddell, W. T.; Ingraffea, A. R.; Wawrzynek, P. A.

    1994-01-01

    The objective was to evaluate NASCRAC (trademark) version 2.0, a second generation fracture analysis code, for verification and validity. NASCRAC was evaluated using a combination of comparisons to the literature, closed-form solutions, numerical analyses, and tests. Several limitations and minor errors were detected. Additionally, a number of major flaws were discovered. These major flaws were generally due to application of a specific method or theory, not due to programming logic. Results are presented for the following program capabilities: K versus a, J versus a, crack opening area, life calculation due to fatigue crack growth, tolerable crack size, proof test logic, tearing instability, creep crack growth, crack transitioning, crack retardation due to overloads, and elastic-plastic stress redistribution. It is concluded that the code is an acceptable fracture tool for K solutions of simplified geometries, for a limited number of J and crack opening area solutions, and for fatigue crack propagation with the Paris equation and constant amplitude loads when the Paris equation is applicable.

  8. Fracture mechanics life analytical methods verification testing

    Science.gov (United States)

    Favenesi, J. A.; Clemons, T. G.; Riddell, W. T.; Ingraffea, A. R.; Wawrzynek, P. A.

    1994-09-01

    The objective was to evaluate NASCRAC (trademark) version 2.0, a second generation fracture analysis code, for verification and validity. NASCRAC was evaluated using a combination of comparisons to the literature, closed-form solutions, numerical analyses, and tests. Several limitations and minor errors were detected. Additionally, a number of major flaws were discovered. These major flaws were generally due to application of a specific method or theory, not due to programming logic. Results are presented for the following program capabilities: K versus a, J versus a, crack opening area, life calculation due to fatigue crack growth, tolerable crack size, proof test logic, tearing instability, creep crack growth, crack transitioning, crack retardation due to overloads, and elastic-plastic stress redistribution. It is concluded that the code is an acceptable fracture tool for K solutions of simplified geometries, for a limited number of J and crack opening area solutions, and for fatigue crack propagation with the Paris equation and constant amplitude loads when the Paris equation is applicable.

  9. 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.)

  10. Analytic methods for calculating coupling impedances

    International Nuclear Information System (INIS)

    These lecture notes describe a variety of analytic techniques to calculate the longitudinal and transverse impedances of obstacles in a beam pipe. They also treat the effort to shield these impedances from the beam by appropriate use of thin conducting layers. (orig.)

  11. Analytical validation of anti-toxoplasma IgG immunoassays

    Directory of Open Access Journals (Sweden)

    Guenael Freire de Souza

    2012-12-01

    Full Text Available There are often discrepancies when using different methods to measure anti-Toxoplasma gondii IgG levels in patient samples. The diagnostic performance of a chemiluminescent immunoassay (CLIA and an enzyme-linked fluorescent assay (ELFA used as confirmatory tests for samples identified as positive or equivocal by an electrochemiluminescent immunoassay (ECLIA were examined. Cut-off values were those stated by the manufacturer, and Western blot was used to confirm the results of all methods. All samples identified as positive by ECLIA (n = 93 were confirmed as positive by Western blot, as were 14 of the 28 samples identified as equivocal. When these 121 samples were retested, the sensitivities of CLIA and ELFA were 64.4% and 73.8%, respectively. Both methods exhibited a specificity of 100%. This study confirms that the results obtained from the different immunoassays are not comparable, and neither CLIA nor ELFA should be used to confirm ECLIA results, which should instead be confirmed by methods such as Western blot or Sabin-Feldman dye test.

  12. 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...

  13. Analytical solution methods for geodesic motion

    CERN Document Server

    Hackmann, Eva

    2015-01-01

    The observation of the motion of particles and light near a gravitating object is until now the only way to explore and to measure the gravitational field. In the case of exact black hole solutions of the Einstein equations the gravitational field is characterized by a small number of parameters which can be read off from the observables related to the orbits of test particles and light rays. Here we review the state of the art of analytical solutions of geodesic equations in various space--times. In particular we consider the four dimensional black hole space--times of Pleba\\'nski--Demia\\'nski type as far as the geodesic equation separates, as well as solutions in higher dimensions, and also solutions with cosmic strings. The mathematical tools used are elliptic and hyperelliptic functions. We present a list of analytic solutions which can be found in the literature.

  14. Experimental validation of structural optimization methods

    Science.gov (United States)

    Adelman, Howard M.

    1992-01-01

    The topic of validating structural optimization methods by use of experimental results is addressed. The need for validating the methods as a way of effecting a greater and an accelerated acceptance of formal optimization methods by practicing engineering designers is described. The range of validation strategies is defined which includes comparison of optimization results with more traditional design approaches, establishing the accuracy of analyses used, and finally experimental validation of the optimization results. Examples of the use of experimental results to validate optimization techniques are described. The examples include experimental validation of the following: optimum design of a trussed beam; combined control-structure design of a cable-supported beam simulating an actively controlled space structure; minimum weight design of a beam with frequency constraints; minimization of the vibration response of helicopter rotor blade; minimum weight design of a turbine blade disk; aeroelastic optimization of an aircraft vertical fin; airfoil shape optimization for drag minimization; optimization of the shape of a hole in a plate for stress minimization; optimization to minimize beam dynamic response; and structural optimization of a low vibration helicopter rotor.

  15. 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.

  16. Verification of an Analytical Method for Measuring Crystal Nucleation Rates in Glasses from DTA Data

    Science.gov (United States)

    Ranasinghe, K. S.; Wei, P. F.; Kelton, K. F.; Ray, C. S.; Day, D. E.

    2004-01-01

    A recently proposed analytical (DTA) method for estimating the nucleation rates in glasses has been evaluated by comparing experimental data with numerically computed nucleation rates for a model lithium disilicate glass. The time and temperature dependent nucleation rates were predicted using the model and compared with those values from an analysis of numerically calculated DTA curves. The validity of the numerical approach was demonstrated earlier by a comparison with experimental data. The excellent agreement between the nucleation rates from the model calculations and fiom the computer generated DTA data demonstrates the validity of the proposed analytical DTA method.

  17. How to assess the quality of your analytical method?

    Science.gov (United States)

    Topic, Elizabeta; Nikolac, Nora; Panteghini, Mauro; Theodorsson, Elvar; Salvagno, Gian Luca; Miler, Marijana; Simundic, Ana-Maria; Infusino, Ilenia; Nordin, Gunnar; Westgard, Sten

    2015-10-01

    Laboratory medicine is amongst the fastest growing fields in medicine, crucial in diagnosis, support of prevention and in the monitoring of disease for individual patients and for the evaluation of treatment for populations of patients. Therefore, high quality and safety in laboratory testing has a prominent role in high-quality healthcare. Applied knowledge and competencies of professionals in laboratory medicine increases the clinical value of laboratory results by decreasing laboratory errors, increasing appropriate utilization of tests, and increasing cost effectiveness. This collective paper provides insights into how to validate the laboratory assays and assess the quality of methods. It is a synopsis of the lectures at the 15th European Federation of Clinical Chemistry and Laboratory Medicine (EFLM) Continuing Postgraduate Course in Clinical Chemistry and Laboratory Medicine entitled "How to assess the quality of your method?" (Zagreb, Croatia, 24-25 October 2015). The leading topics to be discussed include who, what and when to do in validation/verification of methods, verification of imprecision and bias, verification of reference intervals, verification of qualitative test procedures, verification of blood collection systems, comparability of results among methods and analytical systems, limit of detection, limit of quantification and limit of decision, how to assess the measurement uncertainty, the optimal use of Internal Quality Control and External Quality Assessment data, Six Sigma metrics, performance specifications, as well as biological variation. This article, which continues the annual tradition of collective papers from the EFLM continuing postgraduate courses in clinical chemistry and laboratory medicine, aims to provide further contributions by discussing the quality of laboratory methods and measurements and, at the same time, to offer continuing professional development to the attendees. PMID:26408611

  18. Structural damage localization by outlier analysis of signal-processed mode shapes - Analytical and experimental validation

    Science.gov (United States)

    Ulriksen, M. D.; Damkilde, L.

    2016-02-01

    Contrary to global modal parameters such as eigenfrequencies, mode shapes inherently provide structural information on a local level. Therefore, this particular modal parameter and its derivatives are utilized extensively for damage identification. Typically, more or less advanced mathematical methods are employed to identify damage-induced discontinuities in the spatial mode shape signals, hereby, potentially, facilitating damage detection and/or localization. However, by being based on distinguishing damage-induced discontinuities from other signal irregularities, an intrinsic deficiency in these methods is the high sensitivity towards measurement noise. In the present paper, a damage localization method which, compared to the conventional mode shape-based methods, has greatly enhanced robustness towards measurement noise is proposed. The method is based on signal processing of a spatial mode shape by means of continuous wavelet transformation (CWT) and subsequent application of a generalized discrete Teager-Kaiser energy operator (GDTKEO) to identify damage-induced mode shape discontinuities. In order to evaluate whether the identified discontinuities are in fact damage-induced, outlier analysis is conducted by applying the Mahalanobis metric to major principal scores of the sensor-located bands of the signal-processed mode shape. The method is tested analytically and benchmarked with other mode shape-based damage localization approaches on the basis of a free-vibrating beam and validated experimentally in the context of a residential-sized wind turbine blade subjected to an impulse load.

  19. Traveling wave analysis of partial differential equations numerical and analytical methods with Matlab and Maple

    CERN Document Server

    Griffiths, Graham

    2010-01-01

    Although the Partial Differential Equations (PDE) models that are now studied are usually beyond traditional mathematical analysis, the numerical methods that are being developed and used require testing and validation. This is often done with PDEs that have known, exact, analytical solutions. The development of analytical solutions is also an active area of research, with many advances being reported recently, particularly traveling wave solutions for nonlinear evolutionary PDEs. Thus, the current development of analytical solutions directly supports the development of numerical methods by p

  20. Analytical method of elements in humic acid phase

    International Nuclear Information System (INIS)

    A method of rapid extraction of humic acid, determination of carbon in the humic acid and a phase analytical method of major relevant elements such as uranium, gold etc, in the humic acid phase are described. Good results are achieved in exploration of hidden uranium ores by using this phase analytical technique

  1. 40 CFR 766.16 - Developing the analytical test method.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Developing the analytical test method. 766.16 Section 766.16 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC... analytical test method. Because of the matrix differences of the chemicals listed for testing, no one...

  2. 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... § 425.03 Sulfide analytical methods and applicability. (a) The potassium ferricyanide titration...

  3. Analytic Methods of Sound Field Synthesis

    CERN Document Server

    Ahrens, Jens

    2012-01-01

    This book treats the topic of sound field synthesis with a focus on serving human listeners though the approach can be also exploited in other areas such as underwater acoustics or ultrasonics. The author derives a fundamental formulation based on standard integral equations and the single-layer potential approach is identified as a useful tool in order to derive a general solution. He also proposes extensions to the single-layer potential approach which allow for a derivation of solutions for non-enclosing distributions of secondary sources such as circular, planar, and linear ones. Based on above described formulation it is shown that the two established analytic approaches of Wave Field Synthesis and Near-field Compensated Higher Order Ambisonics constitute specific solutions to the general problem which are covered by the single-layer potential solution and its extensions. The consequences spatial discretization are analyzed in detail for all elementary geometries of secondary source distributions and app...

  4. Analytical methods for predicting contaminant transport

    International Nuclear Information System (INIS)

    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. Validation of analytical models for the design of basal reinforced piled embankments

    NARCIS (Netherlands)

    Van Eekelen, S.J.M.; Bezuijen, A.; Van Tol, A.F.

    2014-01-01

    Van Eekelen et al., 2012a, Van Eekelen et al., 2012b and Van Eekelen et al., 2013) have introduced an analytical model for the design of the geosynthetic reinforcement (GR) in a piled embankment. This paper further validates this model with measurements from seven full-scale tests and four series of

  6. Intercalibration of analytical methods on marine environmental samples

    International Nuclear Information System (INIS)

    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

  7. Determination of aluminum by four analytical methods

    International Nuclear Information System (INIS)

    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

  8. Physical analytical methods for uranium hexafluoride

    International Nuclear Information System (INIS)

    Various physical methods of analysis currently used or still under investigation such as: sound analysis, vapor pressure measurements, fractional distillation, cryogenics, micro-sublimation, ultra-violet, visible and infra-red absorption spectrophotometry, nuclear magnetic resonance and mass spectrometry are reviewed. For each method, principle and applications are given, and results obtained concerning reproducibility, application limits and rapidity are discussed. (author)

  9. Validation of qualitative microbiological test methods.

    Science.gov (United States)

    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 and the bacterial density cannot be estimated separately, not even in a multiple dilution experiment. Only the product can be estimated, changing the interpretation of the most probable number estimator. The asymptotic power of the likelihood ratio statistic for comparing an alternative method with the compendial method, is optimal for a single dilution experiment. The bacterial density should either be close to two CFUs per test unit or equal to zero, depending on differences in the model parameters between the two test methods. The proposed strategy for method validation is to use these two dilutions and test for differences in the two model parameters, addressing the validation parameters specificity and accuracy. Robustness of these two parameters might still be required, but all other validation parameters can be omitted. A confidence interval-based approach for the ratio of the detection proportions for the two methods is recommended, since it is most informative and close to the power of the likelihood ratio test. PMID:25412584

  10. Validation of analytical procedures using HPLC-ELSD to determine six sesquiterpene lactones in Eremanthus species.

    Science.gov (United States)

    Sousa, João Paulo B; Nogueira, Elídia F; Ferreira, Leandro S; Lopes, Norberto P; Lopes, João Luis C

    2016-03-01

    Eremanthus species display sesquiterpene lactones with therapeutic potential. We are proposing the development of a new analytical method that has been completely validated to qualify Eremanthus species and its main lactones in raw material using HPLC-ELSD. For the sample preparation, 10.0 mg of powdered Eremanthus leaves was extracted with a 5 mL MeOH/H2 O (9:1 v/v) solution containing scopoletin at 140 µg/mL as the internal standard. For the separation of eight compounds, six of which were lactones, one internal (IS) and one secondary standard were performed utilizing monolithic columns with a nonlinear gradient. The selectivity, stability, precision and matrix effects parameters showed values of RSD of  0.9987. The limits of detection and quantitation ranged from 2.00 to 6.79 µg/mL and from 6.00 to 20.40 µg/mL, respectively. Assessing the robustness study, this method can be used in inter-laboratory studies. Using the HPLC-ELSD method, six sesquiterpene lactones including 4β,5-dihydro-2',3'-dihydroxy-15-deoxy-goyazensolide, goyazensolide, 4β,5-dihydro-2',3'-epoxy-15-deoxy-goyazensolide, centratherin, 4β,5-dihydro-15-deoxy-goyazensolide and lychnofolide, were detected and quantified from distinct Eremanthus species, which were collected in different regions. PMID:26234655

  11. Advancing Analytical Methods for Characterization of Anionic Carbohydrate Biopolymers

    OpenAIRE

    Langeslay, Derek Joseph

    2013-01-01

    The focus of this dissertation is on the development of improved analytical methods for the characterization of anionic carbohydrate biopolymers. Our goal is to extract important information from complex mixtures of heterogeneous polysaccharides by characterizing their substituent oligosaccharides in terms of monosaccharide composition and primary and secondary structure. This work focuses on the application of two major analytical platforms: spectroscopy and chromatography. The development ...

  12. Recent developments in radio-analytic methods for radiation protection. A resume

    International Nuclear Information System (INIS)

    The review covers recent developments in radio-analytic methods for radiation protection. Te validation and verification of radio-analytic methodologies for radionuclide determination in a variety of matrices is related to the appropriate sample preparation. Modern techniques are described from rotation evaporators, microwave systems to automated separation columns. New testing technologies allow the extension of detectable radionuclides and to reduce the detection limit significantly. These techniques are of importance for incorporation surveillance purposes but also for emergency management in case of radiation accidents. The modern radio-analytical techniques allow a sophisticated quality assurance in the frame of international cooperation and projects. A specific contribution covers the capability of alpha spectrometry.

  13. Optimization of reversed-phase chromatography methods for peptide analytics.

    Science.gov (United States)

    Khalaf, Rushd; Baur, Daniel; Pfister, David

    2015-12-18

    The analytical description and quantification of peptide solutions is an essential part in the quality control of peptide production processes and in peptide mapping techniques. Traditionally, an important tool is analytical reversed phase liquid chromatography. In this work, we develop a model-based tool to find optimal analytical conditions in a clear, efficient and robust manner. The model, based on the Van't Hoff equation, the linear solvent strength correlation, and an analytical solution of the mass balance on a chromatographic column describing peptide retention in gradient conditions is used to optimize the analytical scale separation between components in a peptide mixture. The proposed tool is then applied in the design of analytical reversed phase liquid chromatography methods of five different peptide mixtures. PMID:26620597

  14. Analytical methods for RE-Co alloys

    International Nuclear Information System (INIS)

    Total RE, Co and Fe in mischmetal and its cobalt alloys are determined by visual complexometric methods and instrumental x-ray fluorescence techniques. As Fe causes interference in the determinations of RE and Co and its own determination is affected by the presence of Co, it is removed by precipitation. The iron is determined from the precipitate and RE and Co from the filtrate. Accuracy of the method is checked by analysing synthetic mixtures of RE, Co and Fe. The individual REs in mischmetal are determined by x-ray fluorescence method. The analysis technique is based on comparison of the oxides of the test samples with standards (both in pressed pellet form) in the appropriate composition range. The total RE content of mischmetal determined through complexometric analysis is compared with the total RE determined through x-ray fluorescence. (auth.)

  15. Method validation for methanol quantification present in working places

    International Nuclear Information System (INIS)

    Given the widespread use of methanol by different industry sectors and high toxicity associated with this substance, it is necessary to use an analytical method able to determine in a sensitive, precise and accurate levels of methanol in the air of working environments. Based on the methodology established by the National Institute for Occupational Safety and Health (NIOSH), it was validated a methodology for determination of methanol in silica gel tubes which had demonstrated its effectiveness based on the participation of the international collaborative program sponsored by the American Industrial Hygiene Association (AIHA)

  16. 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

  17. Analytical modeling and experimental validation of a structurally integrated piezoelectric energy harvester on a thin plate

    Science.gov (United States)

    Aridogan, U.; Basdogan, I.; Erturk, A.

    2014-04-01

    Vibration-based energy harvesting using piezoelectric cantilevers has been extensively studied over the past decade. As an alternative to cantilevered harvesters, piezoelectric patch harvesters integrated to thin plates can be more convenient for use in marine, aerospace and automotive applications since these systems are often composed of thin plate-like structures with various boundary conditions. In this paper, we present analytical electroelastic modeling of a piezoelectric energy harvester structurally integrated to a thin plate along with experimental validations. The distributed-parameter electroelastic model of the thin plate with the piezoceramic patch harvester is developed based on Kirchhoff’s plate theory for all-four-edges clamped (CCCC) boundary conditions. Closed-form steady-state response expressions for coupled electrical output and structural vibration are obtained under transverse point force excitation. Analytical electroelastic frequency response functions (FRFs) relating the voltage output and vibration response to force input are derived and generalized for different boundary conditions. Experimental validation and extensive theoretical analysis efforts are then presented with a case study employing a thin PZT-5A piezoceramic patch attached on the surface of a rectangular aluminum CCCC plate. The importance of positioning of the piezoceramic patch harvester is discussed through an analysis of dynamic strain distribution on the overall plate surface. The electroelastic model is validated by a comparison of analytical and experimental FRFs for a wide range of resistive electrical boundary conditions. Finally, power generation performance of the structurally integrated piezoceramic patch harvester from multiple vibration modes is investigated analytically and experimentally.

  18. 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)

  19. Bioanalytical method validation: An updated review.

    Science.gov (United States)

    Tiwari, Gaurav; Tiwari, Ruchi

    2010-10-01

    The development of sound bioanalytical method(s) is of paramount importance during the process of drug discovery and development, culminating in a marketing approval. The objective of this paper is to review the sample preparation of drug in biological matrix and to provide practical approaches for determining selectivity, specificity, limit of detection, lower limit of quantitation, linearity, range, accuracy, precision, recovery, stability, ruggedness, and robustness of liquid chromatographic methods to support pharmacokinetic (PK), toxicokinetic, bioavailability, and bioequivalence studies. Bioanalysis, employed for the quantitative determination of drugs and their metabolites in biological fluids, plays a significant role in the evaluation and interpretation of bioequivalence, PK, and toxicokinetic studies. Selective and sensitive analytical methods for quantitative evaluation of drugs and their metabolites are critical for the successful conduct of pre-clinical and/or biopharmaceutics and clinical pharmacology studies. PMID:23781413

  20. Analytical techniques for instrument design - matrix methods

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, R.A. [Los Alamos National Lab., NM (United States)

    1997-09-01

    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 ({Delta}k{sub I},{Delta}k{sub F} to {Delta}E, {Delta}Q & 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.

  1. Analytical techniques for instrument design - matrix methods

    International Nuclear Information System (INIS)

    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 (ΔkI,ΔkF 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

  2. Design and structural verification of locomotive bogies using combined analytical and experimental methods

    Science.gov (United States)

    Manea, I.; Popa, G.; Girnita, I.; Prenta, G.

    2015-11-01

    The paper presents a practical methodology for design and structural verification of the locomotive bogie frames using a modern software package for design, structural verification and validation through combined, analytical and experimental methods. In the initial stage, the bogie geometry is imported from a CAD program into a finite element analysis program, such as Ansys. The analytical model validation is done by experimental modal analysis carried out on a finished bogie frame. The bogie frame own frequencies and own modes by both experimental and analytic methods are determined and the correlation analysis of the two types of models is performed. If the results are unsatisfactory, the structural optimization should be performed. If the results are satisfactory, the qualification procedures follow by static and fatigue tests carried out in a laboratory with international accreditation in the field. This paper presents an application made on bogie frames for the LEMA electric locomotive of 6000 kW.

  3. 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.

  4. Analytical and experimental validation of the Oblique Detonation Wave Engine concept

    Science.gov (United States)

    Adelman, Henry G.; Cambier, Jean-Luc; Menees, Gene P.; Balboni, John A.

    1988-01-01

    The Oblique Detonation Wave Engine (ODWE) for hypersonic flight has been analytically studied by NASA using the CFD codes which fully couple finite rate chemistry with fluid dynamics. Fuel injector designs investigated included wall and strut injectors, and the in-stream strut injectors were chosen to provide good mixing with minimal stagnation pressure losses. Plans for experimentally validating the ODWE concept in an arc-jet hypersonic wind tunnel are discussed. Measurements of the flow field properties behind the oblique wave will be compared to analytical predictions.

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

    OpenAIRE

    Eloy Yordad Companioni Damas; Miriam Odette Cora Medina; Ana Catalina Núñez Clemente; Miguel Ángel Díaz Díaz; Luis González Bravo; Rolando Marbot Ramada; Rodny Montes de Oca Porto

    2009-01-01

    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(a)...

  6. Spacecraft early design validation using formal methods

    International Nuclear Information System (INIS)

    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)

  7. 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 PMID:25420055

  8. Analytical instruments, ionization sources, and ionization methods

    Science.gov (United States)

    Atkinson, David A.; Mottishaw, Paul

    2006-04-11

    Methods and apparatus for simultaneous vaporization and ionization of a sample in a spectrometer prior to introducing the sample into the drift tube of the analyzer are disclosed. The apparatus includes a vaporization/ionization source having an electrically conductive conduit configured to receive sample particulate which is conveyed to a discharge end of the conduit. Positioned proximate to the discharge end of the conduit is an electrically conductive reference device. The conduit and the reference device act as electrodes and have an electrical potential maintained between them sufficient to cause a corona effect, which will cause at least partial simultaneous ionization and vaporization of the sample particulate. The electrical potential can be maintained to establish a continuous corona, or can be held slightly below the breakdown potential such that arrival of particulate at the point of proximity of the electrodes disrupts the potential, causing arcing and the corona effect. The electrical potential can also be varied to cause periodic arcing between the electrodes such that particulate passing through the arc is simultaneously vaporized and ionized. The invention further includes a spectrometer containing the source. The invention is particularly useful for ion mobility spectrometers and atmospheric pressure ionization mass spectrometers.

  9. A Probabilistic Method for Certification of Analytically Redundant Systems

    Directory of Open Access Journals (Sweden)

    Hu Bin

    2015-03-01

    Full Text Available Analytical fault detection algorithms have the potential to reduce the size, power and weight of safety-critical aerospace systems. Analytical redundancy has been successfully applied in many non-safety critical applications. However, acceptance for aerospace applications will require new methods to rigorously certify the impact of such algorithms on the overall system reliability. This paper presents a theoretical method to assess the probabilistic performance for an analytically redundant system. Specifically, a fault tolerant actuation system is considered. The system consists of dual-redundant actuators and an analytical fault detection algorithm to switch between the hardware components. The exact system failure rate per hour is computed using the law of total probability. This analysis requires knowledge of the failure rates for the hardware components. In addition, knowledge of specific probabilistic performance metrics for the fault detection logic is needed. Numerical examples are provided to demonstrate the proposed analysis method.

  10. A heterogeneous analytical benchmark for particle transport methods development

    International Nuclear Information System (INIS)

    A heterogeneous analytical benchmark has been designed to provide a quality control measure for large-scale neutral particle computational software. Assurance that particle transport methods are efficiently implemented and that current codes are adequately maintained for reactor and weapons applications is a major task facing today's transport code developers. An analytical benchmark, as used here, refers to a highly accurate evaluation of an analytical solution to the neutral particle transport equation. Because of the requirement of an analytical solution, however, only relatively limited transport scenarios can be treated. To some this may seem to be a major disadvantage of analytical benchmarks. However, to the code developer, simplicity by no means diminishes the usefulness of these benchmarks since comprehensive transport codes must perform adequately for simple as well as comprehensive transport scenarios

  11. An Analytical Method of Auxiliary Sources Solution for Plane Wave Scattering by Impedance Cylinders - A Reference Solution for the Numerical Method of Auxiliary Sources

    DEFF Research Database (Denmark)

    Larsen, Niels Vesterdal; Breinbjerg, Olav

    2004-01-01

    To facilitate the validation of the numerical Method of Auxiliary Sources an analytical Method of Auxiliary Sources solution is derived in this paper. The Analytical solution is valid for transverse magnetic, and electric, plane wave scattering by circular impedance Cylinders, and it is derived by...... singularities at different positions away from the origin. The transformation necessitates a truncation of the wave transformation but the inaccuracy introduced hereby is shown to be negligible. The analytical Method of Auxiliary Sources solution is employed as a reference to investigate the accuracy of the...... numerical Method of Auxiliary Sources for a range of scattering configurations....

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

    International Nuclear Information System (INIS)

    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 T0 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

  13. 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.

  14. Comparative Analytical Methods for the Measurment of Chlorine Dioxide

    OpenAIRE

    Desai, Unmesh Jeetendra

    2002-01-01

    Four commercially available methods used for the analysis of low-level Chlorine Dioxide (ClO2) concentrations in drinking water were evaluated for accuracy and precision and ranked according to cost, efficiency and ease of the methods under several conditions that might be encountered at water treatment plants. The different analytical methods included: 1.The DPD (N, N-diethyl-p-phenylenediamine) method 2.Lissamine Green B (LGB) wet-chemical method 3.Palintest® kit LGB 4.A...

  15. 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;…

  16. A validated stability indicating rapid LC method for duloxetine HCl.

    Science.gov (United States)

    Srinivasulu, P; Srinivas, K S V; Reddy, R S; Mukkanti, K; Buchireddy, R

    2009-01-01

    The present paper describes the development of a reversed phase liquid chromatographic (RPLC) analytical method for duloxetine HCl in the presence of its impurities and degradation products generated from forced decomposition studies. The drug substance was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The degradation of duloxetine HCl was observed under acid hydrolysis. The drug was found to be stable in other stress conditions studied. Successful separation of the drug from the synthetic impurities and degradation products formed under stress conditions was achieved on a Zorabax XDB C18, 50 mm x 4.6 mm, 5.0 micron column using a mixture of aqueous 0.1% trifluroacetic acid, methanol, tetrahydrofuran (60:20:20, v/v/v) as mobile phase. The HPLC method developed was validated with respect to linearity, accuracy, precisions, specificity and ruggedness. To our knowledge, a rapid stability indicating LC method for duloxetine HCl has not been published elsewhere. PMID:19216224

  17. Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry

    OpenAIRE

    Ornatsky, Olga I.; Kinach, Robert; Bandura, Dmitry R.; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I.; Nitz, Mark; Mitchell A. Winnik

    2008-01-01

    Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for...

  18. New concept of analytical method for two-phase flow

    International Nuclear Information System (INIS)

    The authors are developing a new analytical method for vertical upward two-phase flow based on a concept that two-phase flow with minimum pressure energy consumption rate is the most stable and easily flowable two-phase flow for the given boundary conditions and, thus, such two-phase flow should be realized actually. Although this concept is applied basically one-dimensionally in the analytical method, gravity convection effect due to density difference between liquid film on the channel wall and two-phase flow core in the central region of the channel is taken into account through a two-dimensional turbulent flow analysis. An air-water two-phase flow experiment was performed to verify the proposed analytical method. In the present paper, results of the experimental analysis with the proposed method are reported. (author)

  19. Application of EU guidelines for the validation of screening methods for veterinary drugs.

    Science.gov (United States)

    Stolker, Alida A M Linda

    2012-08-01

    Commission Decision (CD) 2002/657/EC describes detailed rules for method validation within the framework of residue monitoring programmes. The approach described in this CD is based on criteria. For (qualitative) screening methods, the most important criteria is that the CCβ has to be below any regulatory limit. Especially when microbiological or immunochemical methods are involved, the approach described in the CD is not easily applied. For example, by those methods, a large number of analytes (all antibiotics) within several different matrices (meat, milk, fish, eggs, etc.) are detected. It is not completely clear whether all those analytes and all matrices have to be taken into account during method validation. To clarify this, a working group - from EU Reference Laboratories - came up with a practical approach to validate multi-analyte multi-matrix screening methods. It describes how many analyte/matrix combinations have to be tested and how these combinations are selected. Furthermore it describes how to determine CCβ for screening methods in relation to a large list of compounds and maximum residue limits (MRLs). First for each analyte/matrix combination the 'cut-off' level - i.e. the level at which the method separates blanks from contaminated samples - is established. The validation is preferably at the concentration of 50% of the regulatory limit. A minimum set of 20 different samples has to be tested. From the experiences with applying these guidelines it was concluded that the validation approach is very 'practical'; however, there are some remarks. One has to be careful with selecting 'representative' analytes and matrices and it is strongly recommended to collect additional validation data during the routine application of the method. PMID:22851358

  20. On Approximate Analytical Solutions of Nonlinear Vibrations of Inextensible Beams using Parameter-Expansion Method

    DEFF Research Database (Denmark)

    Kimiaeifar, Amin; Lund, Erik; Thomsen, Ole Thybo; Barari, Amin

    2010-01-01

    In this work, an analytical method, which is referred to as Parameter-expansion Method is used to obtain the exact solution for the problem of nonlinear vibrations of an inextensible beam. It is shown that one term in the series expansion is sufficient to obtain a highly accurate solution, which is...... valid for the whole domain of the problem. A comparison of the obtained the numerical solution demonstrates that PEM is effective and convenient for solving such problems. After validation of the obtained results, the system response and stability are also discussed....

  1. A preliminary investigation of PSA validation methods

    International Nuclear Information System (INIS)

    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

  2. ASSESSMENT OF CONSTRUCTION INVESTMENT PROJECTS USING OF ANALYTIC HIERARCHY METHOD

    OpenAIRE

    AYTEKİN, Osman; İlker ÖZDEMİR; KUŞAN, Hakan; TEZCAN, Ömür

    2012-01-01

    In this study, it has been researched the applicability of AHP method (Analytic Hierarchy Method) that is one of multi-criteria decision-making methods, in assessment of construction investment projects. For this aim, it has been considered an application having shopping center, housing estate and residence alternatives. For application of AHP method, a binary comparison matrices have been established using main criteria which have financial conditions, sales and marketing, location and contr...

  3. NON-SPECIFIC METHODS FOR DETECTING RESIDUES OF CLEANING AGENTS DURING CLEANING VALIDATION

    OpenAIRE

    DRAGAN M. MILENOVIĆ; DRAGAN S. PEŠIĆ; SNEŽANA S. MITIĆ

    2011-01-01

    Cleaning validation procedures are carried out in order to assure that residues of cleaning agents are within acceptable limits after the cleaning process. Cleaning agents often consist of a mixture of various surfactants which are in a highly diluted state after the water rinsing procedure has been completed. This makes it difficult to find appropriate analytical methods that are sensitive enough to detect the cleaning agents. In addition, it is advantageous for the analytical methods to be ...

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

    International Nuclear Information System (INIS)

    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

  5. 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.

  6. Analysis profile of the fully grouted rock bolt in jointed rock using analytical and numerical methods

    Institute of Scientific and Technical Information of China (English)

    Ghadimi Mostafa; Shahriar Kourosh; Jalalifar Hossein

    2014-01-01

    The purpose of this study was to investigate the effect of bolt profile on load transfer mechanism of fully grouted bolts in jointed rocks using analytical and numerical methods. Based on the analytical method with development of methods, a new model is presented. To validate the analytical model, five different profiles modeled by ANSYS software. The profile of rock bolts T3 and T4 with load transfer capacity, respectively 180 and 195 kN in the jointed rocks was selected as the optimum profiles. Finally, the selected profiles were examined in Tabas Coal Mine. FLAC analysis indicates that patterns 6+7 with 2NO flexi bolt 4 m better than other patterns within the faulted zone.

  7. 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.

  8. Beamforming and holography image formation methods: an analytic study.

    Science.gov (United States)

    Solimene, Raffaele; Cuccaro, Antonio; Ruvio, Giuseppe; Tapia, Daniel Flores; O'Halloran, Martin

    2016-04-18

    Beamforming and holographic imaging procedures are widely used in many applications such as radar sensing, sonar, and in the area of microwave medical imaging. Nevertheless, an analytical comparison of the methods has not been done. In this paper, the Point Spread Functions pertaining to the two methods are analytically determined. This allows a formal comparison of the two techniques, and to easily highlight how the performance depends on the configuration parameters, including frequency range, number of scatterers, and data discretization. It is demonstrated that the beamforming and holography basically achieve the same resolution but beamforming requires a cheaper (less sensors) configuration.. PMID:27137336

  9. Method Development and Validation of Dapagliflozin in API by RP-HPLC and UV-Spectroscopy

    OpenAIRE

    Sanagapati Manasa; Dhanalakshmi K; Nagarjuna Reddy G; Sreenivasa S

    2014-01-01

    In the present study, two analytical methods were developed for the estimation of Dapagliflozin in API. Method A: RP-HPLC method, Method B: UV spectroscopic method. In method A, the drug showed linearity in the range of 25-150µg/ml with a correlation coefficient (r2) of 0.999, where as in method B, the linearity range was found to be 1-5µg/ml with a correlation coefficient of (r2) 0.999. Both the methods were validated for different validation parameters such as linearity, accuracy, precision...

  10. Desenvolvimento e validação de um método analítico simples e rápido por espectroscopia UV para quantificação de aciclovir em matrizes hidrofílicas de liberação prolongada Development and validation of a simple and rapid analytical method by UV spectroscopy for acyclovir quantification in hydrophilic matrices for sustained release

    Directory of Open Access Journals (Sweden)

    Fernanda Malaquias Barboza

    2010-01-01

    Full Text Available This work reports the validation of an analytical UV spectrophotometric method to assay acyclovir in hydrophilic matrices (assay and dissolution studies. The method was linear in the range between 2.5-20 µg mL-1, presenting a good correlation coefficient ( r = 0,9999. Precision and accuracy analysis showed low relative standart deviation (< 2.0 % and a good recoveries percentual (98.9-100 %. The procedure was linear, accurate, and robust. The method is simple and cheap. It does not use polluting reagents and can be applied in dissolution studies, being an adequate alternative to assay acyclovir in hydrophilic matrices tablets.

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

    Energy Technology Data Exchange (ETDEWEB)

    Farah, J; Bonfrate, A; Donadille, L; Martinetti, F; Trompier, F; Clairand, I [IRSN, Fontenay-aux-roses, Ile-de-France (France); De Olivera, A; Delacroix, S [Institut Curie - Centre de Protontherapie d Orsay, Orsay (France); Herault, J [Centre Antoine Lacassagne, Nice (France); Piau, S; Vabre, I [Institut de Physique Nucleaire d Orsay, Orsay (France)

    2014-06-01

    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

  12. 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.

  13. Multi basin desalination using biomass heat source and analytical validation using RSM

    International Nuclear Information System (INIS)

    Highlights: • Biomass boiler is coupled with multi basin solar still. • Top basin is divided into small stepped basins. • Surface response method is used for analytical validation. • Biomass is eco-friendly. • Higher productivity than conventional still. - Abstract: In this field a multi basin solar still is, used to heighten the productivity. The concept of integrating the multi basin still with biomass heat source is introduced in this research area. In the multi basin still heat exchanger is placed at the bottom end of the watershed region. The heat exchanger is connected to the biomass boiler heat source to create heat energy. This system increases the water temperature in the sword and also increases the productivity in the blade. The upper watershed is separated into small stepped basins. So the flat plate collector and stepped basin are used to increase the turnout in this work. The heat from lower basin is used by the upper basin for desalination. Experiments are conducted with various water depths. In this work the solar still behaves like a capacitor. A conventional still is fabricated and run parallel with the experimental setup for comparison. Sensible heat storage materials such as cement blocks, sand, glass eggs are added to the tail end and top basins to increase water temperature. Latent heat storage materials such as water, wax are introduced in the material body of small pellets to increase productivity. Biomass such as wood, wood wastes, palm wastes is tried in this workplace. A higher productivity is obtained for sensible storage materials when compared to latent heat storage. Theoretical analysis is performed by using RSM (response surface methodology) well agrees with experimental values. The efficiency of the system is compared with conventional still. Experiments are conducted in once flow mode, continuous stream mode and solar modes. Output from RSM are compared with experimental values for error analysis

  14. 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

  15. Analytical Evaluation of Beam Deformation Problem Using Approximate Methods

    DEFF Research Database (Denmark)

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

    2010-01-01

    , 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......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...... 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....

  16. 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

  17. Pulsed plane wave analytic solutions for generic shapes and the validation of Maxwell's equations solvers

    Science.gov (United States)

    Yarrow, Maurice; Vastano, John A.; Lomax, Harvard

    1992-01-01

    Generic shapes are subjected to pulsed plane waves of arbitrary shape. The resulting scattered electromagnetic fields are determined analytically. These fields are then computed efficiently at field locations for which numerically determined EM fields are required. Of particular interest are the pulsed waveform shapes typically utilized by radar systems. The results can be used to validate the accuracy of finite difference time domain Maxwell's equations solvers. A two-dimensional solver which is second- and fourth-order accurate in space and fourth-order accurate in time is examined. Dielectric media properties are modeled by a ramping technique which simplifies the associated gridding of body shapes. The attributes of the ramping technique are evaluated by comparison with the analytic solutions.

  18. An analytical software for NAA by using K0-method

    International Nuclear Information System (INIS)

    An analytical software has been designed for a personal computer in DOS environment to do reactor NAA by using K0-method. The system has functions of radionuclide identification, f and α calculation, K0-value calculation, quantitative calculation of elemental concentrations, nuclides' data management, experiment design, computer simulation etc. The analytical methods used in this system include absolute method, relative method and K0-method. Using this system, three gamma-ray spectra for NAA of Au, Zr samples and GBW07107 rock standard sample have been analyzed. The analysis results are in agreement with the certified results in the scope of uncertainties and the f and α values at the irradiation site in the UZrH pulse reactor are 36.6 and 0.044 respectively. (author)

  19. 40 CFR 141.25 - Analytical methods for radioactivity.

    Science.gov (United States)

    2010-07-01

    ... was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part... January 1, 2005 to satisfy the radium-226 and radium-228 monitoring requirements specified at 40 CFR 141... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Analytical methods for...

  20. 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.

  1. ANALYSIS OF SELECTION INDICATORS OF BADMINTON PLAYERS BY THE DELPHI METHOD AND ANALYTIC HIERARCHY PROCESS

    OpenAIRE

    Han-Chen Huang; Chun-Ta Lin,; Chia-Sen Hu

    2015-01-01

    This study aims to clarify the selection standard of potential badminton players and construct an evaluation model of badminton players. Through literature review and the Delphi Method, this study validated the selection indicators of badminton team players: body type, physical qualities, physical functions, psychological qualities, and intelligence level, including a total of 17 detailed indicators. The researcher then interviewed badminton coaches and applied Analytic Hierarchy ...

  2. Thresholds for statistical and clinical significance in systematic reviews with meta-analytic methods

    DEFF Research Database (Denmark)

    Jakobsen, Janus Christian; Wetterslev, Jorn; Winkel, Per; Lange, Theis; Gluud, Christian

    2014-01-01

    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......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...... proposed eight-step procedure will increase the validity of assessments of intervention effects in systematic reviews of randomised clinical trials....

  3. Prediction of polymer flooding performance using an analytical method

    International Nuclear Information System (INIS)

    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

    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.

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

    International Nuclear Information System (INIS)

    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

  6. A certain analytical method used for solving the Stefan problem

    OpenAIRE

    Grzymkowski Radoslaw; Hetmaniok Edyta; Pleszczynski Mariusz; Slota Damian

    2013-01-01

    The paper presents an analytic method applied for finding the approximate solution of Stefan problem 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 extension of a sought function describing the field of temperature into the power series, some coefficients of which can be determined with the aid of boundary conditions, a...

  7. AIR: fused Analytical and Iterative Reconstruction method for computed tomography

    CERN Document Server

    Yang, Liu; Qi, Sharon X; Gao, Hao

    2013-01-01

    Purpose: CT image reconstruction techniques have two major categories: analytical reconstruction (AR) method and iterative reconstruction (IR) method. AR reconstructs images through analytical formulas, such as filtered backprojection (FBP) in 2D and Feldkamp-Davis-Kress (FDK) method in 3D, which can be either mathematically exact or approximate. On the other hand, IR is often based on the discrete forward model of X-ray transform and formulated as a minimization problem with some appropriate image regularization method, so that the reconstructed image corresponds to the minimizer of the optimization problem. This work is to investigate the fused analytical and iterative reconstruction (AIR) method. Methods: Based on IR with L1-type image regularization, AIR is formulated with a AR-specific preconditioner in the data fidelity term, which results in the minimal change of the solution algorithm that replaces the adjoint X-ray transform by the filtered X-ray transform. As a proof-of-concept 2D example of AIR, FB...

  8. Recent progress of analytical methods of spent nuclear fuel (Review)

    International Nuclear Information System (INIS)

    Analytical methods for the spent nuclear fuel (SF) have been greatly innovated recently. This methodological innovation is mainly caused by rapid and remarkable progress of induced coupled plasma-mass spectrometry (ICP-MS) which is utilized for the isotopic analysis of actinoid elements (U, Np, Pu, Am, Cm) and fission product elements in the SF samples. The quantity of the objective element as well as the volume of the sample solution needed for the ICP-MS measurement are, in principle, much less than required for the measurement by other analytical methods. Because of its highly sensitive characteristic, the ICP-MS becomes the most powerful method for the analysis of radioactive samples such as SF. The utilization of the analytical method based on the ICP-MS makes it possible to reduce the radiation dose of the operator and to minimize the amount of the radioactive wastes generated from the analytical work. For the precise and accurate isotopic analysis of the objective element in the SF sample by mass spectrometry, the interfering element having isobars needs to be separated prior to the measurement. The separation method has also made remarkable progress in recent years. Most of the advancement of the separation method involves the improvement of the conventional method such as ion-chromatography, high performance liquid chromatography or extraction chromatography so that the separation method conforms to the detection using advanced ICP-MS. Furthermore, the application of such new method as the capillary electrophoresis chromatography to the separation of the element in the SF is examined. Ultimately, the analytical system with the chromatographic separation process combined on-line with the ICP-MS detection is considered to be the most suitable and has been developed and employed to the sensitive, precise and rapid analysis of the many isotopes of various elements in the SF. In Institute of Transuranium (EU) and Argonne National Laboratory (USA), the analyses

  9. 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…

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

    International Nuclear Information System (INIS)

    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

  11. A simple analytical method for deflation prediction of inflatable structures

    Institute of Scientific and Technical Information of China (English)

    李庆松; 卿强; 龚景海

    2015-01-01

    The static performance of inflatable structures has been well studied and the dynamic deployment simulation has received much attention. However, very few studies focus on its deflation behavior. Although there are several dynamic finite element algorithms that can be applied to the deflation simulation, their computation costs are expensive, especially for large scale structures. In this work, a simple method based on classic thermodynamics and the analytical relationship between air and membrane was proposed to efficiently analyze the air state variables under the condition of ventilation. Combined with failure analysis of static bearing capacity, a fast incremental analytical method was presented to predict both elastic and post wrinkling deflation process of inflatable structures. Comparisons between simplified analysis, dynamic finite element simulation, and a full-scale experimental test are presented and the suitability of this simple method for solving the air state and predicting the deflation behavior of inflatable structures is proved.

  12. Developments and retrospectives in Lie theory geometric and analytic methods

    CERN Document Server

    Penkov, Ivan; Wolf, Joseph

    2014-01-01

    This volume reviews and updates a prominent series of workshops in representation/Lie theory, and reflects the widespread influence of those  workshops in such areas as harmonic analysis, representation theory, differential geometry, algebraic geometry, and mathematical physics.  Many of the contributors have had leading roles in both the classical and modern developments of Lie theory and its applications. This Work, entitled Developments and Retrospectives in Lie Theory, and comprising 26 articles, is organized in two volumes: Algebraic Methods and Geometric and Analytic Methods. This is the Geometric and Analytic Methods volume. The Lie Theory Workshop series, founded by Joe Wolf and Ivan Penkov and joined shortly thereafter by Geoff Mason, has been running for over two decades. Travel to the workshops has usually been supported by the NSF, and local universities have provided hospitality. The workshop talks have been seminal in describing new perspectives in the field covering broad areas of current re...

  13. Validation of spectrophotometric method for lactulose assay in syrup preparation

    Science.gov (United States)

    Mahardhika, Andhika Bintang; Novelynda, Yoshella; Damayanti, Sophi

    2015-09-01

    Lactulose is a synthetic disaccharide widely used in food and pharmaceutical fields. In the pharmaceutical field, lactulose is used as osmotic laxative in a syrup dosage form. This research was aimed to validate the spectrophotometric method to determine the levels of lactulose in syrup preparation and the commercial sample. Lactulose is hydrolyzed by hydrochloric acid to form fructose and galactose. The fructose was reacted with resorcinol reagent, forming compounds that give absorption peak at 485 nm. Analytical methods was validated, hereafter lactulose content in syrup preparation were determined. The calibration curve was linear in the range of 30-100 μg/mL with a correlation coefficient (r) of 0.9996, coefficient of variance (Vxo) of 1.1 %, limit of detection of 2.32 μg/mL, and limit of quantitation of 7.04 μg/mL. The result of accuracy test for the lactulose assay in the syrup preparation showed recoveries of 96.6 to 100.8 %. Repeatability test of lactulose assay in standard solution of lactulose and sample preparation syrup showed the coefficient of variation (CV) of 0.75 % and 0.7 %. Intermediate precision (interday) test resulted in coefficient of variation 1.06 % on the first day, the second day by 0.99 %, and 0.95 % for the third day. This research gave a valid analysis method and levels of lactulose in syrup preparations of samples A, B, C were 101.6, 100.5, and 100.6 %, respectively.

  14. 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.

  15. Methods for developing and validating survivability distributions

    Energy Technology Data Exchange (ETDEWEB)

    Williams, R.L.

    1993-10-01

    A previous report explored and discussed statistical methods and procedures that may be applied to validate the survivability of a complex system of systems that cannot be tested as an entity. It described a methodology where Monte Carlo simulation was used to develop the system survivability distribution from the component distributions using a system model that registers the logical interactions of the components to perform system functions. This paper discusses methods that can be used to develop the required survivability distributions based upon three sources of knowledge. These are (1) available test results; (2) little or no available test data, but a good understanding of the physical laws and phenomena which can be applied by computer simulation; and (3) neither test data nor adequate knowledge of the physics are known, in which case, one must rely upon, and quantify, the judgement of experts. This paper describes the relationship between the confidence bounds that can be placed on survivability and the number of tests conducted. It discusses the procedure for developing system level survivability distributions from the distributions for lower levels of integration. It demonstrates application of these techniques by defining a communications network for a Hypothetical System Architecture. A logic model for the performance of this communications network is developed, as well as the survivability distributions for the nodes and links based on two alternate data sets, reflecting the effects of increased testing of all elements. It then shows how this additional testing could be optimized by concentrating only on those elements contained in the low-order fault sets which the methodology identifies.

  16. Substantive provisions of Numeral-analytical boundary elements method

    Directory of Open Access Journals (Sweden)

    V.F. Orobey

    2011-06-01

    Full Text Available Substantive propositions of the new method of design calculation, that got the name "Numeral-analytical of boundary elements method", offered by authors, are brought. A method consists of development of the fundamental system of decisions (analytically and Green functions (also analytically for every examined task.For the account of certain border terms, or terms of contact between the separate modules (the separate element of the system is so named the small system of linear algebraic equalizations, that must be decided numeral, is made.Discretisation only of border of the area occupied by an object, sharply diminishes the order of the system of resolvent equalizations; there is possibility of decline of regularity of the decided task. A method is strictly reasonable mathematically, as uses the fundamental decisions of differential equalizations, and, means, within the framework of the accepted hypotheses allows to get the exact meaning of parameters of task (efforts, moving, tensions, currents, frequencies of eigentones, critical forces of loss of stability et cetera into an area.Simplicity of logic of algorithm, good convergence of decision, high stability and small accumulation of errors at numeral operations, are marked also.

  17. Analytical methods to calculate correlation functions in quantum statistical physics

    International Nuclear Information System (INIS)

    In the work there is presented a brief but clear and quite reserved account of two analytical methods to calculate correlation functions in quantum statistical physics, proceeding from the first principles, i.e., the most broadly used at present two-time temperature Green's functions method and a new, so-called 'direct algebraic' method (DAM). The aim of this work is to show on the concrete examples of live the most broadly used models of quantum statistical physics, mathematical and technical clarity and simplicity of DAM and hence its practical value

  18. 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.

  19. Analytical validation of serum bone alkaline phosphatase (BAP OSTASE) on Liaison

    OpenAIRE

    Cavalier, Etienne; Rozet, Eric; Carlisi, Agnès; Bekaert, Anne-Catherine; ROUSSELLE, Olivier; Hubert, Philippe; Chapelle, Jean-Paul; Delanaye, Pierre

    2009-01-01

    Background: The goal of this study was to validate the DiaSorin Liaison BAP OSTASE, a new method for measurement of bone alkaline phosphatase (BAP), and to compare this method with the Beckman-Coulter Access Ostase. We also wanted to establish the reference range for BAP in adults and children. Methods: We determined the precision, functional sensitivity, recovery, linearity and measurement uncertainty, accuracy profile and β-expectation limits. We defined an adult reference interval using i...

  20. Scoping analytical usability evaluation methods: A case study

    OpenAIRE

    Blandford, A. E.; Hyde, J K; Green, T. R. G.; Connell, I.

    2008-01-01

    Analytical usability evaluation methods (UEMs) can complement empirical evaluation of systems: for example, they can often be used earlier in design and can provide accounts of why users might experience difficulties, as well as what those difficulties are. However, their properties and value are only partially understood. One way to improve our understanding is by detailed comparisons using a single interface or system as a target for evaluation, but we need to look deeper than simple proble...

  1. DEVELOPMENT AND METHOD VALIDATION OF AESCULUS HIPPOCASTANUM EXTRACT

    OpenAIRE

    Biradar sanjivkumar; Dhumansure Rajkumar; Patil Mallikarjun; Biradar Karankumar; K Sreenivasa Rao

    2012-01-01

    Aesculus hippocastanum is highly regarded for their medicinal properties in the indigenous system of medicine. The objectives of the present study include the validation of Aesculus hippocastanum extract. Authenticated extract of seeds of the plant was collected and the method was developed for the validation. In this the extract was subjected to check the Accuracy, Precision, Linearity and Specificity. For the validation UV spectrophotometer was used. The proposed UV validation method for ...

  2. Method validation and analysis of nine dithiocarbamates in fruits and vegetables by LC-MS/MS

    DEFF Research Database (Denmark)

    Schmidt, Bjørn; Christensen, Hanne Bjerre; Petersen, Annette;

    2013-01-01

    An analytical method for separation and quantitative determination of nine dithiocarbamates (DTCs) in fruits and vegetables by using LC-MS/MS was developed, validated and applied to samples purchased in local supermarkets. The nine DTCs were ziram, ferbam, thiram, maneb, zineb, nabam, metiram...

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

    International Nuclear Information System (INIS)

    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

  4. 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.

  5. 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)

    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

  6. Random Qualitative Validation: A Mixed-Methods Approach to Survey Validation

    Science.gov (United States)

    Van Duzer, Eric

    2012-01-01

    The purpose of this paper is to introduce the process and value of Random Qualitative Validation (RQV) in the development and interpretation of survey data. RQV is a method of gathering clarifying qualitative data that improves the validity of the quantitative analysis. This paper is concerned with validity in relation to the participants'…

  7. SRXRF Experiments and Analytical Methods of Mineral Individual Fluid Inclusions

    Institute of Scientific and Technical Information of China (English)

    Wu Chunxue; Huang Yuying; Li Hongkui; Chen Chuanren; He Wei; Li Kuifa

    2007-01-01

    This paper focuses on the micro-beam and trace element non-destructive experiment and analytical method of mineral fluid inclusions by synchrotron radiation X-ray fluorescence (SRXRF) microprobe at Beijing Synchrotron Radiation Facility (BSRF). The experimental instrument, measurement process and calculating method are introduced. A set of oil- and gas-containing typical mineral fluid inclusions taken from the Tazhong and Lunnan oilfields in the Tarim Basin were analyzed non-destructively. The trace element contents in the fluid inclusions may provide guidance for oil and gas exploration and development.

  8. Determination of methylmercury in marine biota samples: method validation.

    Science.gov (United States)

    Carrasco, Luis; Vassileva, Emilia

    2014-05-01

    Regulatory authorities are expected to measure concentration of contaminants in foodstuffs, but the simple determination of total amount cannot be sufficient for fully judging its impact on the human health. In particular, the methylation of metals generally increases their toxicity; therefore validated analytical methods producing reliable results for the assessment of methylated species are highly needed. Nowadays, there is no legal limit for methylmercury (MeHg) in food matrices. Hence, no standardized method for the determination of MeHg exists within the international jurisdiction. Contemplating the possibility of a future legislative limit, a method for low level determination of MeHg in marine biota matrixes, based on aqueous-phase ethylation followed by purge and trap and gas chromatography (GC) coupled to pyrolysis-atomic fluorescence spectrometry (Py-AFS) detection, has been developed and validated. Five different extraction procedures, namely acid and alkaline leaching assisted by microwave and conventional oven heating, as well as enzymatic digestion, were evaluated in terms of their efficiency to extract MeHg from Scallop soft tissue IAEA-452 Certified Reference Material. Alkaline extraction with 25% (w/w) KOH in methanol, microwave-assisted extraction (MAE) with 5M HCl and enzymatic digestion with protease XIV yielded the highest extraction recoveries. Standard addition or the introduction of a dilution step were successfully applied to overcome the matrix effects observed when microwave-assisted extraction using 25% (w/w) KOH in methanol or 25% (w/v) aqueous TMAH were used. ISO 17025 and Eurachem guidelines were followed to perform the validation of the methodology. Accordingly, blanks, selectivity, calibration curve, linearity (0.9995), working range (1-800pg), recovery (97%), precision, traceability, limit of detection (0.45pg), limit of quantification (0.85pg) and expanded uncertainty (15.86%, k=2) were assessed with Fish protein Dorm-3 Certified

  9. 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.

  10. Development and validation of analytical methodology with focus on the qualification of powder mixers

    Directory of Open Access Journals (Sweden)

    Pedro de Freitas Fiorante

    2015-06-01

    Full Text Available This study aims at developing an analytical procedure capable of quantifying the ferric oxide present in the mixture of ferric oxide/lactose monohydrate (0.4% w/w. The analytical procedure was checked for specificity, linearity, precision (system repeatability, procedure repeatability and intermediate precision, accuracy, stability of solutions and robustness of the procedure. The concentration of Fe (III was determined by spectrophotometry at 480 nm based on calibration curves. The specificity was verified. The linearity was obtained in the range of 11.2 to 16.8 µg of ferric oxide/mL. The relative standard deviation (RSD of the system repeatability, procedure repeatability and intermediate precision, were not more than 2%. The RSD of the accuracy values were less than 0.75%. The stability of the samples was checked over a 24 hours assay. In the robustness evaluation, the wavelength and the concentration of hydrochloric acid varied. The maximum absorbance deviation due to wavelength variation was 0.14 percent, and the maximum deviation due to the hydrochloric acid concentration variation was 2.4%, indicating that the concentration of hydrochloric acid is critical to the analysis of ferric oxide. The procedure developed was validated and is suitable to the performance qualification of powder mixers.

  11. An Analytical Method for the Response of Coated Plates Subjected to One-Dimensional Underwater Weak Shock Wave

    Directory of Open Access Journals (Sweden)

    Zeyu Jin

    2014-01-01

    Full Text Available An analytical method based on the wave theory is proposed to calculate the pressure at the interfaces of coated plate subjected to underwater weak shock wave. The method is carried out to give analytical results by summing up the pressure increment, which can be calculated analytically, in time sequence. The results are in very good agreement with the finite element (FE predictions for the coating case and Taylor’s results for the noncoating case, which validate the method that is suitable for underwater weak shock problem. On the other hand, Taylor’s results for the coating case are invalid, which indicates a potential application field for the method. The extension of the analytical method to q-layer systems and dissipation case is also outlined.

  12. Organic analysis and analytical methods development: FY 1995 progress report

    Energy Technology Data Exchange (ETDEWEB)

    Clauss, S.A.; Hoopes, V.; Rau, J. [and others

    1995-09-01

    This report describes the status of organic analyses and developing analytical methods to account for the organic components in Hanford waste tanks, with particular emphasis on tanks assigned to the Flammable Gas Watch List. The methods that have been developed are illustrated by their application to samples obtained from Tank 241-SY-103 (Tank 103-SY). The analytical data are to serve as an example of the status of methods development and application. Samples of the convective and nonconvective layers from Tank 103-SY were analyzed for total organic carbon (TOC). The TOC value obtained for the nonconvective layer using the hot persulfate method was 10,500 {mu}g C/g. The TOC value obtained from samples of Tank 101-SY was 11,000 {mu}g C/g. The average value for the TOC of the convective layer was 6400 {mu}g C/g. Chelator and chelator fragments in Tank 103-SY samples were identified using derivatization. gas chromatography/mass spectrometry (GC/MS). Organic components were quantified using GC/flame ionization detection. Major components in both the convective and nonconvective-layer samples include ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), succinic acid, nitrosoiminodiacetic acid (NIDA), citric acid, and ethylenediaminetriacetic acid (ED3A). Preliminary results also indicate the presence of C16 and C18 carboxylic acids in the nonconvective-layer sample. Oxalic acid was one of the major components in the nonconvective layer as determined by derivatization GC/flame ionization detection.

  13. Gaussian Analytic Centroiding method of star image of star tracker

    Science.gov (United States)

    Wang, Haiyong; Xu, Ershuai; Li, Zhifeng; Li, Jingjin; Qin, Tianmu

    2015-11-01

    The energy distribution of an actual star image coincides with the Gaussian law statistically in most cases, so the optimized processing algorithm about star image centroiding should be constructed also by following Gaussian law. For a star image spot covering a certain number of pixels, the marginal distribution of the gray accumulation on rows and columns are shown and analyzed, based on which the formulas of Gaussian Analytic Centroiding method (GAC) are deduced, and the robustness is also promoted due to the inherited filtering effect of gray accumulation. Ideal reference star images are simulated by the PSF (point spread function) with integral form. Precision and speed tests for the Gaussian Analytic formulas are conducted under three scenarios of Gaussian radius (0.5, 0.671, 0.8 pixel), The simulation results show that the precision of GAC method is better than that of the other given algorithms when the Gaussian radius is not bigger than 5 × 5 pixel window, a widely used parameter. Above all, the algorithm which consumes the least time is still the novel GAC method. GAC method helps to promote the comprehensive performance in the attitude determination of a star tracker.

  14. An Approximate Analytical Method of the Nonlinear Vibroacoustic Coupling System

    Directory of Open Access Journals (Sweden)

    Qizheng Zhou

    2014-01-01

    Full Text Available An approximate analytical method of the nonlinear vibroacoustic coupling system is proposed for the first time. Taking the Duffing oscillator-plate-medium system as an example, the nonlinear vibroacoustic coupling equations are developed using variational principle. The two major difficulties which lie in solving the coupling equations are the uncertain motion of the oscillator and the surface acoustic pressure on the plate, a system for which the fluid-structure coupling cannot be neglected. Based on the incremental harmonic balance (IHB method, the motion of the oscillator is expressed in the form of the Fourier series, and then the modal expression method and the incoherent assumption are employed to discretize the displacement and the surface pressure of the plate. Then the approximate analytical solution is given by the IHB method. The characteristics of acoustic radiation and surface quadratic velocity of the plate, the nonlinear characteristics of oscillator, and the influence of the excitation frequency and the nonlinear stiffness on the results are investigated by the numerical simulation. The results show that the excitation at the frequency close to the natural frequency of the oscillator can produce a significant response of the third-harmonic generation which determines the vibroacoustic characteristics of the plate.

  15. 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)

  16. 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.

  17. Stiffness matrix formulation for double row angular contact ball bearings: Analytical development and validation

    Science.gov (United States)

    Gunduz, Aydin; Singh, Rajendra

    2013-10-01

    Though double row angular contact ball bearings are widely used in industrial, automotive, and aircraft applications, the scientific literature on double row bearings is sparse. It is also shown that the stiffness matrices of two single row bearings may not be simply superposed to obtain the stiffness matrix of a double row bearing. To overcome the deficiency in the literature, a new, comprehensive, analytical approach is proposed based on the Hertzian theory for back-to-back, face-to-face, and tandem arrangements. The elements of the five-dimensional stiffness matrix for double row angular contact ball bearings are computed given either the mean bearing displacement or the mean load vector. The diagonal elements of the proposed stiffness matrix are verified with a commercial code for all arrangements under three loading scenarios. Some changes in stiffness coefficients are investigated by varying critical kinematic and geometric parameters to provide more insight. Finally, the calculated natural frequencies of a shaft-bearing experiment are successfully compared with measurements, thus validating the proposed stiffness formulation. For double row angular contact ball bearings, the moment stiffness and cross-coupling stiffness terms are significant, and the contact angle changes under loads. The proposed formulation is also valid for paired (duplex) bearings which behave as an integrated double row unit when the surrounding structural elements are sufficiently rigid.

  18. 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.

  19. Implementation of the Maximum Entropy Method for Analytic Continuation

    CERN Document Server

    Levy, Ryan; Gull, Emanuel

    2016-01-01

    We present $\\texttt{Maxent}$, a tool for performing analytic continuation of spectral functions using the maximum entropy method. The code operates on discrete imaginary axis datasets (values with uncertainties) and transforms this input to the real axis. The code works for imaginary time and Matsubara frequency data and implements the 'Legendre' representation of finite temperature Green's functions. It implements a variety of kernels, default models, and grids for continuing bosonic, fermionic, anomalous, and other data. Our implementation is licensed under GPLv2 and extensively documented. This paper shows the use of the programs in detail.

  20. Performance of analytical methods for tomographic gamma scanning

    International Nuclear Information System (INIS)

    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

  1. Analytical methods used by the geochemical section: water

    International Nuclear Information System (INIS)

    The authors describe the analytical methods used by the C.E.A. Geochemical Section to determine the chemical composition of natural waters encountered during the prospecting of uraniferous deposits or in the course of mining operations. Because of the diversity of the samples and the different items of information requested, methods were selected and adapted to answer to the demands peculiar to mining research. Methods and know-how concerning the quantitative analysis of natural water to find out the concentration of the following chemicals are reviewed: carbonates and bicarbonates, calcium, magnesium, chlorides, sodium and potassium, sulfates, nitrates, silica, phosphates, iron, manganese, aluminium, fluorides, dissolved oxygen, CO2, SH2 and sulphur, and uranium. (authors)

  2. Analytical method of spectra calculations in the Bargmann representation

    International Nuclear Information System (INIS)

    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

  3. VALIDATED SPECTROPHOTMETRIC METHOD FOR THE DETERMINATION OF SALBUTAMOL SULPHATE IN BULK AND PHARMACEUTICAL DOSAGE FORMS

    Directory of Open Access Journals (Sweden)

    Eswarudu.M.M

    2012-04-01

    Full Text Available A new, simple, accurate and sensitive spectrophotometric method has been developed for the estimation of Salbutamol sulphate in bulk and in pharmaceutical formulations. Salbutamol sulphate shows ʎ max at 292 nm. The drug follows the beer’s lambert’s law in the concentration range of 20-100µ ml. the method was validated by following the analytical performance parameters as suggested by the international conference on harmonization which included accuracy, precision, linearity. All validation parameters were with in the acceptable range. The developed method was successfully applied to estimate the amount of Salbutamol sulphate in bulk and pharmaceutical dosage forms.

  4. Using analytic network process for evaluating mobile text entry methods.

    Science.gov (United States)

    Ocampo, Lanndon A; Seva, Rosemary R

    2016-01-01

    This paper highlights a preference evaluation methodology for text entry methods in a touch keyboard smartphone using analytic network process (ANP). Evaluation of text entry methods in literature mainly considers speed and accuracy. This study presents an alternative means for selecting text entry method that considers user preference. A case study was carried out with a group of experts who were asked to develop a selection decision model of five text entry methods. The decision problem is flexible enough to reflect interdependencies of decision elements that are necessary in describing real-life conditions. Results showed that QWERTY method is more preferred than other text entry methods while arrangement of keys is the most preferred criterion in characterizing a sound method. Sensitivity analysis using simulation of normally distributed random numbers under fairly large perturbation reported the foregoing results reliable enough to reflect robust judgment. The main contribution of this paper is the introduction of a multi-criteria decision approach in the preference evaluation of text entry methods. PMID:26360215

  5. The evolution of analytical chemistry methods in foodomics.

    Science.gov (United States)

    Gallo, Monica; Ferranti, Pasquale

    2016-01-01

    The methodologies of food analysis have greatly evolved over the past 100 years, from basic assays based on solution chemistry to those relying on the modern instrumental platforms. Today, the development and optimization of integrated analytical approaches based on different techniques to study at molecular level the chemical composition of a food may allow to define a 'food fingerprint', valuable to assess nutritional value, safety and quality, authenticity and security of foods. This comprehensive strategy, defined foodomics, includes emerging work areas such as food chemistry, phytochemistry, advanced analytical techniques, biosensors and bioinformatics. Integrated approaches can help to elucidate some critical issues in food analysis, but also to face the new challenges of a globalized world: security, sustainability and food productions in response to environmental world-wide changes. They include the development of powerful analytical methods to ensure the origin and quality of food, as well as the discovery of biomarkers to identify potential food safety problems. In the area of nutrition, the future challenge is to identify, through specific biomarkers, individual peculiarities that allow early diagnosis and then a personalized prognosis and diet for patients with food-related disorders. Far from the aim of an exhaustive review of the abundant literature dedicated to the applications of omic sciences in food analysis, we will explore how classical approaches, such as those used in chemistry and biochemistry, have evolved to intersect with the new omics technologies to produce a progress in our understanding of the complexity of foods. Perhaps most importantly, a key objective of the review will be to explore the development of simple and robust methods for a fully applied use of omics data in food science. PMID:26363946

  6. 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

  7. 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.

  8. ANALYSIS OF SELECTION INDICATORS OF BADMINTON PLAYERS BY THE DELPHI METHOD AND ANALYTIC HIERARCHY PROCESS

    Directory of Open Access Journals (Sweden)

    Han-Chen Huang

    2015-02-01

    Full Text Available This study aims to clarify the selection standard of potential badminton players and construct an evaluation model of badminton players. Through literature review and the Delphi Method, this study validated the selection indicators of badminton team players: body type, physical qualities, physical functions, psychological qualities, and intelligence level, including a total of 17 detailed indicators. The researcher then interviewed badminton coaches and applied Analytic Hierarchy process (AHP to determine the importance of the indicators of potential badminton players for badminton coaches. A selection model of badminton players was constructed. The results can serve as reference for badminton coaches’ scientific and objective selection of players.

  9. The use of graphic-analytical method in investment design

    Directory of Open Access Journals (Sweden)

    Musatova Tatiana

    2016-04-01

    Full Text Available We investigate the possibility of using the network planning method for the goals and objectives of the investment project. The author suggests a network model of implementing the investment project related to the manufacture of aluminum structures. Insufficient study of adaptation of methodological issues of organization of technological processes to the investment project of socio-economic activities has led to the relevance and identified the purpose of the present study. The presented network model allows project participants to optimize the time and costs of various types of project resources. It includes the calculation of the parameters of the network schedule and the actual model of interrelated events and activities. Scientific and practical significance of the results of research is related to the possibility of practical application of graphic-analytical method for the preparation of technical and economic documentation for the investment project.

  10. Friedmann--Lemaitre Cosmologies via Roulettes and Other Analytic Methods

    CERN Document Server

    Chen, Shouxin; Yang, Yisong

    2015-01-01

    In this work a series of methods are developed for understanding the Friedmann equation when it is beyond the reach of the Chebyshev theorem. First it will be demonstrated that every solution of the Friedmann equation admits a representation as a roulette such that information on the latter may be used to obtain that for the former. Next the Friedmann equation is integrated for a quadratic equation of state and for the Randall--Sundrum II universe, leading to a harvest of a rich collection of new interesting phenomena. Finally an analytic method is used to isolate the asymptotic behavior of the solutions of the Friedmann equation, when the equation of state is of an extended form which renders the integration impossible, and to establish a universal exponential growth law.

  11. Potentialities and possible applications of a new analytical method (PIXE)

    International Nuclear Information System (INIS)

    In 1970, a new method was introduced for trace analysis, namely, the X-ray emission induced by charged particles (PIXE). It has been shown that when protons in the few MeV range are used for the excitation of inner shell electrons and solid state detectors for the detection of the characteristic X-rays, we dispose of a powerful multi-elemental analytical tool of high sensitivity. In contrast to activation spectrometry, this is an in beam technique, irradiation and measuring being performed at the same time. The foundations of the method are described experimental arrangements and problems related to beam transport, target preparation an spectrum analysis. A detailed discussion on precision, accuracy and sensitivity is presented. Applications in biology, medicine, environmental and materials sciences are discussed. (Author)

  12. 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 ...

  13. A novel unified coding analytical method for Internet of Things

    Science.gov (United States)

    Sun, Hong; Zhang, JianHong

    2013-08-01

    This paper presents a novel unified coding analytical method for Internet of Things, which abstracts out the `displacement goods' and `physical objects', and expounds the relationship thereof. It details the item coding principles, establishes a one-to-one relationship between three-dimensional spatial coordinates of points and global manufacturers, can infinitely expand, solves the problem of unified coding in production phase and circulation phase with a novel unified coding method, and further explains how to update the item information corresponding to the coding in stages of sale and use, so as to meet the requirement that the Internet of Things can carry out real-time monitoring and intelligentized management to each item.

  14. A general multigroup formulation of the analytic nodal method

    International Nuclear Information System (INIS)

    In this paper the theoretical description of an alternative approach to the Analytic Nodal Method is given, in which a full multigroup formulations is developed. This approach differs from the well known QUANDRY approach in three aspects. Firstly, a notation which is more widely used in Quantum Mechanics has been adopted to enable a clear and concise presentation of this multigroup approach. A basis transformation is then used to reduce the directional equations to a scalar form and finally, Green's secondary identity is used to rewrite each of the resulting scalar equations in a form which eventually leads to a response matrix, as opposed to using classical methods to actually solve the coupled multigroup directional equations

  15. A Review on Supercritical Fluid Extraction as New Analytical Method

    Directory of Open Access Journals (Sweden)

    K. A. Abbas

    2008-01-01

    Full Text Available This review study summarized the Supercritical Fluid Extraction (SFE as new analytical method. The advantage and disadvantage of CO2 (SC-CO2 as well as special applications of SFE in food processing such as removal of fat from food, enrichment of vitamin E from natural sources, removal of alcohol from wine and beer, encapsulation of liquids for engineering solid products and extraction and characterization of functional compounds were also highlighted. The study also covered the application of SFE in food safety such as rapid analysis for fat content, rapid analysis for pesticides in foods as well as the recent applications of SFE in food such as supercritical particle formation and nan particle formation and ssupercritical drying. The outcome finding confirmed that SFE was found to be advance, fast, reliable, clean and cheap methods for routine food analysis.

  16. Analytical support of plant specific SAMG development validation of SAMG using MELCOR 1.8.5

    International Nuclear Information System (INIS)

    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

  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. Pressurised liquid extraction of flavonoids in onions. Method development and validation

    OpenAIRE

    Søltoft, Malene; Christensen, J.H.; Nielsen, J.; Knuthsen, Pia

    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. The extraction efficiencies were lowest for the conventional water bath extraction compared to pressurized liquid extraction (PLE), ultrasonication, ultrasonic liquid processor, and microwave e...

  19. Development and Validation of Liquid Chromatographic Method for Estimation of Naringin in Nanoformulation

    OpenAIRE

    Musmade, Kranti P.; Trilok, M.; Swapnil J. Dengale; Krishnamurthy Bhat; Reddy, M. S.; Prashant B Musmade; N Udupa

    2014-01-01

    A simple, precise, accurate, rapid, and sensitive reverse phase high performance liquid chromatography (RP-HPLC) method with UV detection has been developed and validated for quantification of naringin (NAR) in novel pharmaceutical formulation. NAR is a polyphenolic flavonoid present in most of the citrus plants having variety of pharmacological activities. Method optimization was carried out by considering the various parameters such as effect of pH and column. The analyte was separated by e...

  20. Validation methods for flight crucial systems

    Science.gov (United States)

    Holt, H. M.

    1983-01-01

    Research to develop techniques that can aid in determining the reliability and performance of digital electronic fault-tolerant systems, that have probability of catastrophic system failure on the order of 10 to the -9th at 10 hours, is reviewed. The computer-aided reliability estimation program (CARE III) provides general-purpose reliability analysis and a design tool for fault-tolerant systems; large reduction of state size; and a fault-handling model based on probabilistic description of detection, isolation, and recovery mechanisms. The application of design proof techniques as part of the design and development of the software implemented fault-tolerance computer is mentioned. Emulation techniques and experimental procedures are verified using specimens of fault-tolerant computers and the capabilities of the validation research laboratory, AIRLAB.

  1. Algebraic and analytic reconstruction methods for dynamic tomography.

    OpenAIRE

    Desbat, Laurent; Rit, S; Clackdoyle, R.; Mennessier, C; Promayon, Emmanuel; Ntalampeki, S.

    2007-01-01

    In this work, we discuss algebraic and analytic approaches for dynamic tomography. We present a framework of dynamic tomography for both algebraic and analytic approaches. We finally present numerical experiments.

  2. Algebraic and analytic reconstruction methods for dynamic tomography.

    Science.gov (United States)

    Desbat, L; Rit, S; Clackdoyle, R; Mennessier, C; Promayon, E; Ntalampeki, S

    2007-01-01

    In this work, we discuss algebraic and analytic approaches for dynamic tomography. We present a framework of dynamic tomography for both algebraic and analytic approaches. We finally present numerical experiments. PMID:18002059

  3. Towards in-vivo K-edge imaging using a new semi-analytical calibration method

    Science.gov (United States)

    Schirra, Carsten; Thran, Axel; Daerr, Heiner; Roessl, Ewald; Proksa, Roland

    2014-03-01

    Flat field calibration methods are commonly used in computed tomography (CT) to correct for system imperfections. Unfortunately, they cannot be applied in energy-resolving CT when using bow-tie filters owing to spectral distortions imprinted by the filter. This work presents a novel semi-analytical calibration method for photon-counting spectral CT systems, which is applicable with a bow-tie filter in place and efficiently compensates pile-up effects at fourfold increased photon flux compared to a previously published method without degradation of image quality. The achieved reduction of the scan time enabled the first K-edge imaging in-vivo. The method employs a calibration measurement with a set of flat sheets of only a single absorber material and utilizes an analytical model to predict the expected photon counts, taking into account factors such as x-ray spectrum and detector response. From the ratios of the measured x-ray intensities and the corresponding simulated photon counts, a look-up table is generated. By use of this look-up table, measured photon-counts can be corrected yielding data in line with the analytical model. The corrected data show low pixel-to-pixel variations and pile-up effects are mitigated. Consequently, operations like material decomposition based on the same analytical model yield accurate results. The method was validated on a experimental spectral CT system equipped with a bow-tie filter in a phantom experiment and an in-vivo animal study. The level of artifacts in the resulting images is considerably lower than in images generated with a previously published method. First in-vivo K-edge images of a rabbit selectively depict vessel occlusion by an ytterbium-based thermoresponsive polymer.

  4. Validated Explicit and Implicit Runge-Kutta Methods

    OpenAIRE

    Alexandre Dit Sandretto, Julien; Chapoutot, Alexandre

    2015-01-01

    A set of validated numerical integration methods based on explicit and implicit Runge-Kutta schemes is presented to solve, in a guaranteed way, initial value problems of ordinary differential equations. Runge-Kutta methods are well-known to have strong stability properties which make them appealing to be the basis of validated numerical integration methods. A new approach to bound the local truncation error of any Runge-Kutta methods is the main contribution of this article which pushes back ...

  5. DEVELOPMENT AND METHOD VALIDATION OF AESCULUS HIPPOCASTANUM EXTRACT

    Directory of Open Access Journals (Sweden)

    Biradar sanjivkumar

    2012-07-01

    Full Text Available Aesculus hippocastanum is highly regarded for their medicinal properties in the indigenous system of medicine. The objectives of the present study include the validation of Aesculus hippocastanum extract. Authenticated extract of seeds of the plant was collected and the method was developed for the validation. In this the extract was subjected to check the Accuracy, Precision, Linearity and Specificity. For the validation UV spectrophotometer was used. The proposed UV validation method for the extract is accurate, linear, precise, linear, specific and within the range. Further isolation and in-vitro studies are needed.

  6. Development and experimental validation of an analytical model to predict the demoulding force in hot embossing

    International Nuclear Information System (INIS)

    During the demoulding stage of the hot embossing process, the force required to separate a polymer part from the mould should be minimized to avoid the generation of structural defects for the produced micro structures. However, the demoulding force is dependent on a number of process factors, which include the material properties, the demoulding temperature, the polymer pressure history and the design of the mould structures. In particular, these factors affect the chemical, physical and mechanical interactions between a polymer and the replication master during demoulding. The focus of the reported research is on the development and validation of an analytical model that takes into account the adhesion, friction and deformation phenomena to predict the required demoulding force in hot embossing under different processing conditions. The results indicate that the model predictions agree well with the experimental data obtained and confirm that the design of the mould affects the resulting demoulding force. In addition, the applied embossing load was observed to have a significant effect on demoulding. More specifically, the increase in pressure within the polymer raises the adhesion force while it also reduces the friction force due to the decrease in the thermal stress. (paper)

  7. Development and validation of a path analytic model of students' performance in chemistry

    Science.gov (United States)

    Anamuah-Mensah, Jophus; Erickson, Gaalen; Gaskell, Jim

    This article reports the development and validation of an integrated model of performance on a chemical concept - volumetric analysis. From the chemical literature a path-analytic model of performance on volumetric analysis calculation was postulated based on studies utilizing the proportional reasoning schema of Piaget and the Cumulative learning theory of Gagne. This integrated model hypothesized some relationships among the variables: direct proportional reasoning, inverse proportional reasoning, prerequisite concepts (content) and performance on volumetric analysis calculations. This model was postulated for the two groups of students involved in the study - that is those who use algorithms with understanding and those who use algorithms without understanding. Two hundred and sixty-five grade twelve chemistry students in eight schools (14 classes) in the lower mainland of British Columbia, Canada participated fully in the study. With the exception of the test on volumetric analysis calculations all the other tests were administered prior to the teaching of the unit on volumetric analysis. The results of the study indicate that for subjects using algorithms without understanding, their performance on VA problems is not influenced by proportional reasoning strategies while for those who use algorithms with understanding, their performance is influenced by proportional reasoning strategies.

  8. A chromatographic method validation to quantify tablets Mephenesine of national production

    International Nuclear Information System (INIS)

    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)

  9. Development and Validation of a UV - Spectrophotometric Method for Quantification of Atorvastatin in Tablets

    Directory of Open Access Journals (Sweden)

    Mondal A

    2012-01-01

    Full Text Available A UV-spectrophotometric method has been developed for the quantitativeestimation of atorvastatin in tablet. The present study describes development and validation of UV-spectroscopic method for estimationof atorvastatin in tablet dosage form and validation of newlydeveloped method. During development of analytical method methanol:phosphate buffer (20:80,methanol:water(20:80,methanol:water (50:50,acetonitrile:water (10:90were tried but drug was found to be solublein methanol:water (50:50. Standard stock solution was prepared in methanol: water (50:50. The detection wave length (λmax was found tobe 248nm.Calibration curves were prepared.The proposed method obeysBeer's law in the range of 5-15μg/ml. Absorption maxima was determinedwith 10 μg/ml by scanning in the range of 200-400nm.Percent recoverystudies are in the range of 98.78%-100.36%. The method was validated in terms specificity,linearity,accuracy,range,precision,repeatability,robustness,system suitability,stability of analytical solution.Results of analysis were validated statistically and by specificity studies.From that it was observed that there is no interference of blank,excipients during the estimation of drug in formulation. This showsthe adaptability of the method for routine estimation of atorvastatinin tablet dosage form.

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

    International Nuclear Information System (INIS)

    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 C13) have been developed for solvent titration and to evaluate the percentage of degradation and to identify some of the degradation products

  11. Laser induced uranium fluorescence as an analytical method

    International Nuclear Information System (INIS)

    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)

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

    International Nuclear Information System (INIS)

    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 19F(p,ag)16O 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

  13. Modelling of packet traffic with matrix analytic methods

    DEFF Research Database (Denmark)

    Andersen, Allan T.

    1995-01-01

    The dissertation is concerned with modelling various performance aspects pertaining to packet switched telecommunication networks. The emphsis has been put on versatile modelling of the packet arrival process which is a very relevant issue in cotext with the future Broadband Integrated Service Data...... network services i.e. 800 and 900 calls and advanced mobile communication services. The Markovian Arrival Process (MAP) has been used as a versatile tool to model the packet arrival process. Applying the MAP facilitates the use of Matrix Analytic methods to obtain performance measures associated with for...... example the single server queue with a MAP arrival process and a general service time distribution. Measured SS7 traffic data has been analyzed as a part of this study. Recently there has been expressed concern regarding adverse behaviour of measured SS7 traffic i.e. long range dependence. Our studies did...

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

    DEFF Research Database (Denmark)

    Larsen, Niels Vesterdal; Breinbjerg, Olav

    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...

  15. Comparison of the Helicobacter Pylori Diagnosis Methods with Analytic Network Process

    Directory of Open Access Journals (Sweden)

    Hacer KONAKLI

    2015-11-01

    Full Text Available Helicobacter pylori is infecting %70-80 of the world’s population and is assumed to cause gastric diseases. Diagnosis of the bacteria is crucial for the treatment of the bacteria related infections. Histology, culture, urea breath test, stool antigen test some of the diagnosis methods each having specific strength and weaknesses as sensitivity, specificity, cost, easiness, time, effectiveness in the treatment and laboratory requirements. In this study, three of the commonly used H. pylori diagnosis methods: histology, culture and urea breath test, are evaluated with Analytic network process (ANP and the rank of the criteria and alternatives are obtained. The evaluation of the methods and the rank of the diagnosis methods can reduce time, cost, and validity of the test results.

  16. Comparative assessment of bioanalytical method validation guidelines for pharmaceutical industry.

    Science.gov (United States)

    Kadian, Naveen; Raju, Kanumuri Siva Rama; Rashid, Mamunur; Malik, Mohd Yaseen; Taneja, Isha; Wahajuddin, Muhammad

    2016-07-15

    The concepts, importance, and application of bioanalytical method validation have been discussed for a long time and validation of bioanalytical methods is widely accepted as pivotal before they are taken into routine use. United States Food and Drug Administration (USFDA) guidelines issued in 2001 have been referred for every guideline released ever since; may it be European Medical Agency (EMA) Europe, National Health Surveillance Agency (ANVISA) Brazil, Ministry of Health and Labour Welfare (MHLW) Japan or any other guideline in reference to bioanalytical method validation. After 12 years, USFDA released its new draft guideline for comments in 2013, which covers the latest parameters or topics encountered in bioanalytical method validation and approached towards the harmonization of bioanalytical method validation across the globe. Even though the regulatory agencies have general agreement, significant variations exist in acceptance criteria and methodology. The present review highlights the variations, similarities and comparison between bioanalytical method validation guidelines issued by major regulatory authorities worldwide. Additionally, other evaluation parameters such as matrix effect, incurred sample reanalysis including other stability aspects have been discussed to provide an ease of access for designing a bioanalytical method and its validation complying with the majority of drug authority guidelines. PMID:27179186

  17. Method Development and Validation of Dapagliflozin in API by RP-HPLC and UV-Spectroscopy

    Directory of Open Access Journals (Sweden)

    Sanagapati Manasa

    2014-07-01

    Full Text Available In the present study, two analytical methods were developed for the estimation of Dapagliflozin in API. Method A: RP-HPLC method, Method B: UV spectroscopic method. In method A, the drug showed linearity in the range of 25-150µg/ml with a correlation coefficient (r2 of 0.999, where as in method B, the linearity range was found to be 1-5µg/ml with a correlation coefficient of (r2 0.999. Both the methods were validated for different validation parameters such as linearity, accuracy, precision, detection limit, quantitation limit, robustness and ruggedness and the results were found to be within the acceptance limits as per the guidelines of International Conference on Harmonization (ICH.

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

    International Nuclear Information System (INIS)

    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

  19. Guidelines for validation of qualitative real-time PCR methods

    OpenAIRE

    Broeders, Sylvia; Huber, Ingrid; GROHMANN Lutz; Berben, Gilbert; Taverniers, Isabel; Mazzara, Marco; Roosens, Nancy; Morisset, Dany

    2014-01-01

    As for many areas of molecular testing, detection of Genetically Modified Organisms (GMO) relies on the real-time Polymerase Chain Reaction (qPCR) technology. Due to the increasing number of GMO, a screening approach using qualitative screening methods has become an integrated part of GMO detection. However, specific guidelines for the validation of these methods are lacking. Here, a pragmatic approach to conduct in-house and inter-laboratory validation studies for GMO screening methods, is p...

  20. Analytical methods for (oxidized) plasmalogens: Methodological aspects and applications.

    Science.gov (United States)

    Fuchs, B

    2015-05-01

    Plasmalogens are a unique class of glycerophospholipids (GPLs) containing a fatty alcohol linked by a vinyl-ether moiety at the sn-1 position of the glycerol backbone. There is normally a polyunsaturated fatty acyl residue at the sn-2 position. These two features provide interesting properties to the plasmalogen GPL. Their physiological roles have been challenging to elucidate, although plasmalogens represent up to 20% of the total membrane GPLs in humans. Recent studies have revealed plasmalogen deficiencies associated with several human disorders; therefore, plasmalogens are likely to be specific to different tissues, metabolic processes, and developmental stages. The first chapter of this review will discuss the molecular structure and chemistry of plasmalogens, their biological roles, and their distributions in cells and tissues in different species. In the second chapter, currently used methods of analyzing plasmalogens and their degradation products are described. Although chromatographic methods will be also discussed, special attention will be given to ((31)P) nuclear magnetic resonance spectroscopy and soft ionization mass spectrometry (MS) techniques such as electrospray ionization and matrix-assisted laser desorption and ionization time-of-flight MS. Finally, in the third chapter of this review selected human diseases and disorders, which are presumably characterized by changes in plasmalogen contents and compositions, are described and the analytical methods used are discussed. PMID:25536419

  1. Analytical performance of radiochemical method for americium determination in urine

    International Nuclear Information System (INIS)

    This paper presents an analytical method developed and adapted for separation and analysis of Plutonium (Pu) isotopes and Americium (Am) in urine samples. The proposed method will attend the demand of internal exposure monitoring program for workers involved mainly with dismantling rods and radioactive smoke detectors. In this experimental procedure four steps are involved as preparation of samples, sequential radiochemical separation, preparation of the source for electroplating and quantification by alpha spectrometry. In the first stage of radiochemical separation, plutonium is conventionally isolated employing the anion exchange technique. Americium isolation is achieved sequentially by chromatographic extraction (Tru.spec column) from the load and rinse solutions coming from the anion exchange column. The 243Am tracer is added into the sample as chemical yield monitors and to correct the results improving the precision and accuracy. The mean recovery obtained is 60%, and the detection limit for 24h urine sample is 1.0 mBq L-1 in accordance with the literature. Based in the preliminary results, the method is appropriate to be used in monitoring programme of workers with a potential risk of internal contamination. (author)

  2. Analytical methods associated with the recovery of uranium

    International Nuclear Information System (INIS)

    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

  3. Study of analytical methods concerning storage effect of underground dam

    Energy Technology Data Exchange (ETDEWEB)

    Hirama, Kunioki; Kuwahara, Toru; Kushima, Masatoshi (Obayashi Corp., Osaka, (Japan))

    1989-08-10

    Information on water balance concerning a catchment area of an underground dam is necessary for effective survey, design, construction and maintenance of the underground dam. Since the observation data of the underground water for about 5 years at some underground dam was obtained this time, they were used for evaluation of the storage effect of the underground dam by using the following four analytical methods, namely water balance equation, combination of tank model and water balance equation, numerical calculation by finite element method and hybrid model of finite element method and tank model. As a result, in case when permeable layers consist of sand and conglomerate of an alluvial system, it was found that evaluation of the storage at the underground dam and its characteristics was feasible and the following points were important for such evaluation; accumulation of observation data over a certain long period, correct information on hydrogeology, suitable composition of tank model, preparation of reasonable numerical model, and combination of analyses such as hybridization of tank models, etc.. 6 refs., 8 figs., 4 tabs.

  4. 21 CFR 530.40 - Safe levels and availability of analytical methods.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Safe levels and availability of analytical methods... Safe levels and availability of analytical methods. (a) In accordance with § 530.22, the following safe... accordance with § 530.22, the following analytical methods have been accepted by FDA:...

  5. 40 CFR 260.21 - Petitions for equivalent testing or analytical methods.

    Science.gov (United States)

    2010-07-01

    ... analytical methods. 260.21 Section 260.21 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... Petitions for equivalent testing or analytical methods. (a) Any person seeking to add a testing or analytical method to part 261, 264, or 265 of this chapter may petition for a regulatory amendment under...

  6. 21 CFR 320.29 - Analytical methods for an in vivo bioavailability or bioequivalence study.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 5 2010-04-01 2010-04-01 false Analytical methods for an in vivo bioavailability... Analytical methods for an in vivo bioavailability or bioequivalence study. (a) The analytical method used in... ingredient or therapeutic moiety, or its active metabolite(s), achieved in the body. (b) When the...

  7. Analytic initialization method for xenon oscillation in power reactor simulation

    International Nuclear Information System (INIS)

    The purpose of simulating nuclear power reactor core transients is to predict variations in core behavior due to changes in operating conditions. In the simulation, the initial condition of the core transient should be consistent with the real core state. Especially, the initial conditions of iodine and xenon distributions, which cannot be measured in the core, have dominant effects on the accuracy of the simulation for the transients related with xenon dynamics. If the transient starts from non-equilibrium xenon condition, the accurate initialization of the non-equilibrium iodine and xenon distributions is essential for the prediction of the core transient behavior. In this study, a simple initialization method of non-equilibrium iodine and xenon distributions for the core transient simulation was developed using axial power difference, which is the only measurable parameter related with the non-equilibrium state of the core. For this purpose, the spatial distribution of two-group one-dimensional neutron diffusion equation combined with xenon dynamics equation was expanded with Fourier sine series. It was found that the nonlinearly combined terms of flux and xenon distributions in the equations were canceled by the orthogonal characteristics of the Fourier series using adequate approximation. Therefore, the dynamics equations for axial difference parameters of power, iodine and xenon can be completely linearized and can be converted into an equation system which can be solved analytically. Because the equation system provides with an analytic relationship between the axial differences of power, iodine and xenon, the non-equilibrium iodine and xenon can be represented as functions of the axial power difference. It implies that the initial condition of the transient starting from a non-equilibrium state can be determined from the initial condition of the axial power difference which is a measurable parameter of the core. Using the analytic solution obtained in this

  8. Validation of uranium determination by SF-ICP-MS from QC samples from the IAEA Safeguards Analytical Laboratory

    International Nuclear Information System (INIS)

    Full text: A high-resolution sector field ICP-MS (SF-ICP-MS) (ThermoElectron ELEMENT2) with an ESI Apex high sensitivity inlet system and ESI autosampler was installed at the IAEA Safeguards Analytical Laboratory (SAL) in late 2005. The instrument has at least three intended uses: (1) quality control in the form of uranium determinations from room blank samples collected in the IAEA Clean Laboratory and process blank samples from U-Pu chemical separations of environmental safeguards samples, (2) forensics in the form of trace element determinations in nuclear samples collected by IAEA Safeguards inspectors, and (3) rapid determination of uranium isotopic composition from diluted samples collected from uranium enrichment facilities. The validation of the methods for (2) and (3) will be reported at a later date. The importance of (1) bears on the frequency of QC measurements and therefore the confidence of cleanliness of the critical working areas within the Clean Laboratory. Here we report the results of method validation quality control samples collected in the SAL Clean Laboratory. The ELEMENT2 is located in the nuclear chemistry area of the SAL, therefore the validation, which requires the analysis of uranium concentrations down to 10 ppq, was envisioned as a significant challenge. The need for careful chemical treatment and standard preparation techniques was recognized in order to mitigate potential external contamination effects. A series of uranium standards covering the concentration level from 1000 ppq down to 10 ppq was prepared gravimetrically in the SAL Clean Laboratory and transferred and measured on the ELEMENT2. Although the measurements were not made under clean room conditions, uranium down to 10 ppq was measured with good linearity and repeatability. The associated standard deviations were typically below 10%. Due to the uranium background in the lab, concentration measurements below 10 ppq were much more variable, and therefore the reliable

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

    International Nuclear Information System (INIS)

    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 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. The EP test showed reproducible performance characteristics with good precision and negligible laboratory

  10. Thrust measurement method verification and analytical studies on a liquid-fueled pulse detonation engine

    Directory of Open Access Journals (Sweden)

    Lu Jie

    2014-06-01

    Full Text Available In order to test the feasibility of a new thrust stand system based on impulse thrust measurement method, a liquid-fueled pulse detonation engine (PDE is designed and built. Thrust performance of the engine is obtained by direct thrust measurement with a force transducer and indirect thrust measurement with an eddy current displacement sensor (ECDS. These two sets of thrust data are compared with each other to verify the accuracy of the thrust performance. Then thrust data measured by the new thrust stand system are compared with the verified thrust data to test its feasibility. The results indicate that thrust data from the force transducer and ECDS system are consistent with each other within the range of measurement error. Though the thrust data from the impulse thrust measurement system is a litter lower than that from the force transducer due to the axial momentum losses of the detonation jet, the impulse thrust measurement method is valid when applied to measure the averaged thrust of PDE. Analytical models of PDE are also discussed in this paper. The analytical thrust performance is higher than the experimental data due to ignoring the losses during the deflagration to detonation transition process. Effect of equivalence ratio on the engine thrust performance is investigated by utilizing the modified analytical model. Thrust reaches maximum at the equivalence ratio of about 1.1.

  11. An analytical method for predicting postwildfire peak discharges

    Science.gov (United States)

    Moody, John A.

    2012-01-01

    An analytical method presented here that predicts postwildfire peak discharge was developed from analysis of paired rainfall and runoff measurements collected from selected burned basins. Data were collected from 19 mountainous basins burned by eight wildfires in different hydroclimatic regimes in the western United States (California, Colorado, Nevada, New Mexico, and South Dakota). Most of the data were collected for the year of the wildfire and for 3 to 4 years after the wildfire. These data provide some estimate of the changes with time of postwildfire peak discharges, which are known to be transient but have received little documentation. The only required inputs for the analytical method are the burned area and a quantitative measure of soil burn severity (change in the normalized burn ratio), which is derived from Landsat reflectance data and is available from either the U.S. Department of Agriculture Forest Service or the U.S. Geological Survey. The method predicts the postwildfire peak discharge per unit burned area for the year of a wildfire, the first year after a wildfire, and the second year after a wildfire. It can be used at three levels of information depending on the data available to the user; each subsequent level requires either more data or more processing of the data. Level 1 requires only the burned area. Level 2 requires the burned area and the basin average value of the change in the normalized burn ratio. Level 3 requires the burned area and the calculation of the hydraulic functional connectivity, which is a variable that incorporates the sequence of soil burn severity along hillslope flow paths within the burned basin. Measurements indicate that the unit peak discharge response increases abruptly when the 30-minute maximum rainfall intensity is greater than about 5 millimeters per hour (0.2 inches per hour). This threshold may relate to a change in runoff generation from saturated-excess to infiltration-excess overland flow. The

  12. 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.

  13. Modern analytic methods applied to the art and archaeology

    International Nuclear Information System (INIS)

    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)

  14. 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.

  15. Simplex and duplex event-specific analytical methods for functional biotech maize.

    Science.gov (United States)

    Lee, Seong-Hun; Kim, Su-Jeong; Yi, Bu-Young

    2009-08-26

    Analytical methods are very important in the control of genetically modified organism (GMO) labeling systems or living modified organism (LMO) management for biotech crops. Event-specific primers and probes were developed for qualitative and quantitative analysis for biotech maize event 3272 and LY 038 on the basis of the 3' flanking regions, respectively. The qualitative primers confirmed the specificity by a single PCR product and sensitivity to 0.05% as a limit of detection (LOD). Simplex and duplex quantitative methods were also developed using TaqMan real-time PCR. One synthetic plasmid was constructed from two taxon-specific DNA sequences of maize and two event-specific 3' flanking DNA sequences of event 3272 and LY 038 as reference molecules. In-house validation of the quantitative methods was performed using six levels of mixing samples, from 0.1 to 10.0%. As a result, the biases from the true value and the relative deviations were all within the range of +/-30%. Limits of quantitation (LOQs) of the quantitative methods were all 0.1% for simplex real-time PCRs of event 3272 and LY 038 and 0.5% for duplex real-time PCR of LY 038. This study reports that event-specific analytical methods were applicable for qualitative and quantitative analysis for biotech maize event 3272 and LY 038. PMID:19650633

  16. 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.

  17. Validação em laboratório de método analítico para determinação do teor de adipato e ftalato de di-(2-etil-hexila utilizados como plastificantes em filmes flexíveis de PVC Validation in laboratory of the analytical method to determine di-(2-ethylhexyl phthalate and adipate utilized as plasticizers in pvc films

    Directory of Open Access Journals (Sweden)

    Andreia Artur Esteves

    2007-02-01

    Full Text Available The validation of analytical methods was carried out for di-(ethylhexyl phthalate (DEHP and adipate (DEHA the determination of in PVC films. The level of DEHP and DEHA in samples was determined by leaving the film in contact with n-heptane during 48 hours and analysis in a gas chromatograph (GC equipped with a flame ionization detector and fused silica column with 5% phenylmethyl silicone in the dimensions 30 m x 0.53 mm x 2.65 mm. The results for detection and the quantification limits were smaller than the restriction limits. The recovery rates of DEHP and DEHA were, respectively, 69.10 and 75.30 %.

  18. Validação de metodologia analítica para determinação de mercúrio total em amostras de urina por espectrometria de absorção atômica com geração de vapor frio (CV-AAS: estudo de caso Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS: case study

    Directory of Open Access Journals (Sweden)

    Sabine Neusatz Guilhen

    2010-01-01

    Full Text Available Mercury is a toxic metal used in a variety of substances over the course history. One of its more dubious uses is in dental amalgam restorations. It is possible to measure very small concentrations of this metal in the urine of exposed subjects by the cold vapor atomic absorption technique. The present work features the validation as an essential tool to confirm the suitability of the analytical method chosen to accomplish such determination. An initial analysis will be carried out in order to evaluate the environmental and occupational levels of exposure to mercury in 39 members of the auxiliary dental staff at public consulting rooms in the city of Araguaína (TO.

  19. Validação de métodos analíticos na quantificação de comprimidos de Captopril - comparação de metodologias para um programa de garantia de qualidade - DOI: 10.4025/actascihealthsci.v26i2.1590 Validation of analytical methods for quantifying captopril in tablets – a comparison of methodologies for a quality control program - DOI: 10.4025/actascihealthsci.v26i2.1590

    Directory of Open Access Journals (Sweden)

    Graciette Matioli

    2004-04-01

    Full Text Available Atualmente, quando todos os caminhos levam à busca da qualidade total, torna-se indispensável conhecer perfeitamente cada fase de um processo produtivo. Neste caso, a validação é a ferramenta adequada para garantir a confiabilidade de instalação de um processo produtivo, de equipamento e, inclusive, da metodologia analítica. Dessa forma, o presente trabalho teve por objetivo analisar os principais aspectos da validação de métodos analíticos na quantificação do captopril. Foi realizada a validação e a comparação dos seguintes métodos: titulométrico por óxido-redução, espectrofotométrico por Folin-Ciocalteau e cromatográfico por cromatografia líquida de alta eficiência - CLAE. Os atributos de exatidão, precisão, linearidade, especificidade e robustez foram estudados para cada metodologia. Os resultados obtidos demonstraram que o método cromatográfico foi o mais adequado para as análises dos comprimidos de Captopril 25 mg, enquanto que os métodos espectrofotométrico e titulométrico demonstraram valores que satisfazem os critérios de aceitação, porém, com maior variabilidade e menor sensibilidade.Nowadays, when all approaches lead to the search for total quality, a thorough knowledge of every stage of a production process is vital. Validation is an appropriate tool to guarantee the reliabilities of: productive process installation, equipment and also analytical methodology. The aim of the present study was to analyze the main aspects of analytical methods validation for quantifying captopril. Validation and comparison of the following methods were carried out: titrimetric for oxide-reduction, spectrophotometry for Folin-Ciocalteau and high-efficiency liquid chromatography - HPLC. The attributes of accuracy, precision, linearity, specificity and robustness were studied for each methodology. The results show that the chromatographic method was the most suitable for Captopril 25 mg tablets evaluation, while the

  20. Analytical Validation of AmpliChip p53 Research Test for Archival Human Ovarian FFPE Sections.

    Directory of Open Access Journals (Sweden)

    Matthew J Marton

    Full Text Available The p53 tumor suppressor gene (TP53 is reported to be mutated in nearly half of all tumors and plays a central role in genome integrity. Detection of mutations in p53 can be accomplished by many assays, including the AmpliChip p53 Research Test. The AmpliChip p53 Research Test has been successfully used to determine p53 status in hematologic malignancies and fresh frozen solid tissues but there are few reports of using the assay with formalin fixed, paraffin-embedded (FFPE tissue. The objective of this study was to describe analytical performance characterization of the AmpliChip p53 Research Test to detect p53 mutations in genomic DNA isolated from archival FFPE human ovarian tumor tissues. Method correlation with sequencing showed 96% mutation-wise agreement and 99% chip-wise agreement. We furthermore observed 100% agreement (113/113 of the most prevalent TP53 mutations. Workflow reproducibility was 96.8% across 8 samples, with 2 operators, 2 reagent lots and 2 instruments. Section-to-section reproducibility was 100% for each sample across a 60 μm region of the FFPE block from ovarian tumors. These data indicate that the AmpliChip p53 Research Test is an accurate and reproducible method for detecting mutations in TP53 from archival FFPE human ovarian specimens.

  1. Nuclear Analytical Methods on Archaeological Glass in Thailand

    International Nuclear Information System (INIS)

    Full text: Due to the complex nature of archaeological objects, their analysis needs to use extremely sensitive, spatially resolved and versatile methods that should be as non invasive as possible and give complementary information at different scales; from the macroscopic to the nanometer scales. In this work, SEM-EDS, PIXE and SRXRF were used to analyze the chemical composition of the archaeological glass bead samples that excavated from various historical sites in Thailand. There were number of differences in shade between the glass beads of different colors. The results revealed different in glass types; soda- and potash-, mixed-alkali-, and lead-based glasses. It was noticed that it has been difficult to interpret because of a long period covering and weathering effects. This study may be led to the historical link of the long distance trade and exchange networks in maritime between South-East Asia, South Asia, East Asia and Asia Minor. These analytical measurements in combination are proved useful to investigate the glassy materials and to answer questions posted by archaeologists

  2. Analytical method to estimate resin cement diffusion into dentin

    Science.gov (United States)

    de Oliveira Ferraz, Larissa Cristina; Ubaldini, Adriana Lemos Mori; de Oliveira, Bruna Medeiros Bertol; Neto, Antonio Medina; Sato, Fracielle; Baesso, Mauro Luciano; Pascotto, Renata Corrêa

    2016-05-01

    This study analyzed the diffusion of two resin luting agents (resin cements) into dentin, with the aim of presenting an analytical method for estimating the thickness of the diffusion zone. Class V cavities were prepared in the buccal and lingual surfaces of molars (n=9). Indirect composite inlays were luted into the cavities with either a self-adhesive or a self-etch resin cement. The teeth were sectioned bucco-lingually and the cement-dentin interface was analyzed by using micro-Raman spectroscopy (MRS) and scanning electron microscopy. Evolution of peak intensities of the Raman bands, collected from the functional groups corresponding to the resin monomer (C–O–C, 1113 cm-1) present in the cements, and the mineral content (P–O, 961 cm-1) in dentin were sigmoid shaped functions. A Boltzmann function (BF) was then fitted to the peaks encountered at 1113 cm-1 to estimate the resin cement diffusion into dentin. The BF identified a resin cement-dentin diffusion zone of 1.8±0.4 μm for the self-adhesive cement and 2.5±0.3 μm for the self-etch cement. This analysis allowed the authors to estimate the diffusion of the resin cements into the dentin. Fitting the MRS data to the BF contributed to and is relevant for future studies of the adhesive interface.

  3. 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.

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

    International Nuclear Information System (INIS)

    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

  5. 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)

    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

  6. 75 FR 49930 - Stakeholder Meeting Regarding Re-Evaluation of Currently Approved Total Coliform Analytical Methods

    Science.gov (United States)

    2010-08-16

    ... From the Federal Register Online via the Government Publishing Office ENVIRONMENTAL PROTECTION AGENCY Stakeholder Meeting Regarding Re-Evaluation of Currently Approved Total Coliform Analytical...) analytical methods. At these meetings, stakeholders will be given an opportunity to discuss...

  7. Reliability and validity of optoelectronic method for biophotonical measurements

    Science.gov (United States)

    Karpienko, Katarzyna; Wróbel, Maciej S.; UrniaŻ, Rafał

    2013-11-01

    Reliability and validity of measurements is of utmost importance when assessing measuring capability of instruments developed for research. In order to perform an experiment which is legitimate, used instruments must be both reliable and valid. Reliability estimates the degree of precision of measurement, the extent to which a measurement is internally consistent. Validity is the usefulness of an instrument to perform accurate measurements of quantities it was designed to measure. Statistical analysis for reliability and validity control of low-coherence interferometry method for refractive index measurements of biological fluids is presented. The low-coherence interferometer is sensitive to optical path difference between interfering beams. This difference depends on the refractive index of measured material. To assess the validity and reliability of proposed method for blood measurements, the statistical analysis of the method was performed on several substances with known refractive indices. Analysis of low-coherence interferograms considered the mean distances between fringes. Performed statistical analysis for validity and reliability consisted of Grubb's test for outliers, Shapiro-Wilk test for normal distribution, T-Student test, standard deviation, coefficient of determination and r-Pearson correlation. Overall the tests proved high statistical significance of measurement method with confidence level < 0.0001 of measurement method.

  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. Evaluating protocols and analytical methods for peptide adsorption experiments.

    Science.gov (United States)

    Fears, Kenan P; Petrovykh, Dmitri Y; Clark, Thomas D

    2013-12-01

    This paper evaluates analytical techniques that are relevant for performing reliable quantitative analysis of peptide adsorption on surfaces. Two salient problems are addressed: determining the solution concentrations of model GG-X-GG, X5, and X10 oligopeptides (G = glycine, X = a natural amino acid), and quantitative analysis of these peptides following adsorption on surfaces. To establish a uniform methodology for measuring peptide concentrations in water across the entire GG-X-GG and X n series, three methods were assessed: UV spectroscopy of peptides having a C-terminal tyrosine, the bicinchoninic acid (BCA) protein assay, and amino acid (AA) analysis. Due to shortcomings or caveats associated with each of the different methods, none were effective at measuring concentrations across the entire range of representative model peptides. In general, reliable measurements were within 30% of the nominal concentration based on the weight of as-received lyophilized peptide. In quantitative analysis of model peptides adsorbed on surfaces, X-ray photoelectron spectroscopy (XPS) data for a series of lysine-based peptides (GGKGG, K5, and K10) on Au substrates, and for controls incubated in buffer in the absence of peptides, suggested a significant presence of aliphatic carbon species. Detailed analysis indicated that this carbonaceous contamination adsorbed from the atmosphere after the peptide deposition. The inferred adventitious nature of the observed aliphatic carbon was supported by control experiments in which substrates were sputter-cleaned by Ar(+) ions under ultra-high vacuum (UHV) then re-exposed to ambient air. In contrast to carbon contamination, no adventitious nitrogen species were detected on the controls; therefore, the relative surface densities of irreversibly-adsorbed peptides were calculated by normalizing the N/Au ratios by the average number of nitrogen atoms per residue. PMID:24706133

  10. Analytic compensation methods in dynamic tomography; Methodes analytiques de compensation des deformations en tomographie dynamique

    Energy Technology Data Exchange (ETDEWEB)

    Roux, S.; Desbat, L.; Koenig, A.; Grangeat, P. [Laboratoire TIMC-IMAG UMR CNRS 5525, Faculte de Medecine de Grenoble, 38 - La Tronche (France)]|[CEA Grenoble, Lab. Electronique et de Technologie de l' Informatique (LETI), 38 (France)

    2004-07-01

    Recent progresses in X-ray tomography allow to study some organs dynamically. The aim of this work is to analyze the deformation compensation algorithms used to integrate dynamical evolution models into the image reconstruction processes. An exact and efficient analytical method of movement compensation is presented and applied to simulated data. Abstract only. (J.S.)

  11. Semi-analytic treatment of the three-dimensional Poisson equation via a Galerkin BIE method

    Energy Technology Data Exchange (ETDEWEB)

    Nintcheu Fata, Sylvain [ORNL

    2011-01-01

    A systematic treatment of the three-dimensional Poisson equation via singular and hypersingular boundary integral equation techniques is investigated in the context of a Galerkin approximation. Developed to conveniently deal with domain integrals without a volume-fitted mesh, the proposed method initially converts domain integrals featuring the Newton potential and its gradient into equivalent surface integrals. Then, the resulting boundary integrals are evaluated by means of well-established cubature methods. In this transformation, weakly-singular domain integrals, defined over simply- or multiply-connected domains with Lipschitz boundaries, are rigorously converted into weakly-singular surface integrals. Combined with the semi-analytic integration approach developed for potential problems to accurately calculate singular and hypersingular Galerkin surface integrals, this technique can be employed to effectively deal with mixed boundary-value problems without the need to partition the underlying domain into volume cells. Sample problems are included to validate the proposed approach.

  12. The criterion-related validity of personality measures for predicting GPA: a meta-analytic validity competition.

    Science.gov (United States)

    McAbee, Samuel T; Oswald, Frederick L

    2013-06-01

    Interest in the role of personality traits in predicting academic performance outcomes has steadily increased over the last several decades, enough to produce a number of meta-analyses that summarize this research (e.g., Poropat, 2009; Richardson, Abraham, & Bond, 2012). These previous meta-analyses combine a variety of alternative personality measures under the assumption that they all reflect the same personality traits and thus predict outcomes similarly. The current meta-analysis tests this assumption by comparing different personality measures when predicting postsecondary grade point average (GPA). The operational validities (r+) of 5 frequently used measures of the Big Five personality traits were compared: the NEO Personality Inventory--Revised (NEO-PI-R; Costa & McCrae, 1992), the NEO Five-Factor Inventory (NEO-FFI; Costa & McCrae, 1992), the Big Five Inventory (BFI; e.g., Benet-Martínez & John, 1998), Goldberg's (1992) unipolar Big Five Factor Markers (Markers), and the Big Five International Personality Item Pool (IPIP; Goldberg, 1999). A systematic review of the psychological literature from 1992 to 2012 was conducted, identifying 51 studies containing 274 correlations. Conscientiousness demonstrated the strongest criterion-related validity for predicting GPA (r+ = .23), consistent with previous meta-analyses; in addition, this overall validity was found to be robust across measures (r(BFI)(+) = .24, r(IPIP)(+) = .21, r(Markers)(+) = .15, r(NEO-FFI)(+) = .24, r(NEO-PI-R)(+) = .26). Although the criterion-related validities for Extraversion, Agreeableness, Neuroticism, and Openness to Experience (Intellect) differed by measure, they were generally low (r+s < .10). Practical implications of the findings and directions for future research are discussed. PMID:23397931

  13. 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)

  14. Practical procedure for method validation in INAA- A tutorial

    International Nuclear Information System (INIS)

    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)

  15. Selected Parallel and Scalable Methods for Scientific Big Data Analytics

    OpenAIRE

    Riedel, Morris

    2015-01-01

    The goal of this talk is to inform participants about two concrete and widely used data analytics techniques that are suitable to analyse ‘big data’ for scientific and engineering applications. After a brief introduction to the general approach of using machine learning, data mining, and statistical computing in data analytics, the talk will offer details on the ‘clustering’ technique that partitions datasets into subgroups (i.e. clusters) previously unknown. From the broad class of available...

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

    International Nuclear Information System (INIS)

    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

  17. 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.

  18. Analytical method by high resolution liquid chromatography for the determination of carbamazepine in human plasma

    International Nuclear Information System (INIS)

    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)

  19. Parametric design-based modal damped vibrational piezoelectric energy harvesters with arbitrary proof mass offset: Numerical and analytical validations

    Science.gov (United States)

    Lumentut, Mikail F.; Howard, Ian M.

    2016-02-01

    This paper focuses on the primary development of novel numerical and analytical techniques of the modal damped vibration energy harvesters with arbitrary proof mass offset. The key equations of electromechanical finite element discretisation using the extended Lagrangian principle are revealed and simplified to give matrix and scalar forms of the coupled system equations, indicating the most relevant numerical technique for the power harvester research. To evaluate the performance of the numerical study, the analytical closed-form boundary value equations have been developed using the extended Hamiltonian principle. The results from the electromechanical frequency response functions (EFRFs) derived from two theoretical studies show excellent agreement with experimental studies. The benefit of the numerical technique is in providing effective and quick predictions for analysing parametric designs and physical properties of piezoelectric materials. Although analytical technique provides a challenging process for analysing the complex smart structure, it shows complementary study for validating the numerical technique.

  20. An Analytic Method for the Kinematics and Dynamics of a Multiple-Backbone Continuum Robot

    Directory of Open Access Journals (Sweden)

    Bin He

    2013-01-01

    Full Text Available Continuum robots have been the subject of extensive research due to their potential use in a wide range of applications. In this paper, we propose a new continuum robot with three backbones, and provide a unified analytic method for the kinematics and dynamics of a multiple‐backbone continuum robot. The robot achieves actuation by independently pulling three backbones to carry out a bending motion of two‐degrees‐of‐freedom (DoF. A three‐dimensional CAD model of the robot is built and the kinematical equation is established on the basis of the Euler‐Bernoulli beam. The dynamical model of the continuum robot is constructed by using the Lagrange method. The simulation and the experiment’s validation results show the continuum robot can exactly bend into pre‐set angles in the two‐dimensional space (the maximum error is less than 5% of the robot length and can make a circular motion in three‐dimensional space. The results demonstrate that the proposed analytic method for the kinematics and dynamics of a continuum robot is feasible.

  1. 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 on...... reproducibility were within the limits for repeatability and reproducibility given by the Horwitz equation. Validation was not accepted for azoxystrobin in grapes on all three detectors and for azoxystrobin in apple for the MS-detector. A comparison of matrix-matched standards versus standards in solvent showed...

  2. A simple parallel analytical method of prenatal screening.

    Science.gov (United States)

    Li, Ding; Yang, Hao; Zhang, Wen-Hong; Pan, Hao; Wen, Dong-Qing; Han, Feng-Chan; Guo, Hui-Fang; Wang, Xiao-Ming; Yan, Xiao-Jun

    2006-01-01

    Protein microarray has progressed rapidly in the past few years, but it is still hard to popularize it in many developing countries or small hospitals owing to the technical expertise required in practice. We developed a cheap and easy-to-use protein microarray based on dot immunogold filtration assay for parallel analysis of ToRCH-related antibodies including Toxoplasma gondii, rubella virus, cytomegalovirus and herpes simplex virus type 1 and 2 in sera of pregnant women. It does not require any expensive instruments and the assay results can be clearly recognized by the naked eye. We analyzed 186 random sera of outpatients at the gynecological department with our microarray and commercial ELISA kit, and the results showed there was no significant difference between the two detection methods. Validated by clinical application, the microarray is easy to use and has a unique advantage in cost and time. It is more suitable for mass prenatal screening or epidemiological screening than the ELISA format. PMID:16791006

  3. Validation procedures for quantitative gluten ELISA methods: AOAC allergen community guidance and best practices.

    Science.gov (United States)

    Koerner, Terry B; Abbott, Michael; Godefroy, Samuel Benrejeb; Popping, Bert; Yeung, Jupiter M; Diaz-Amigo, Carmen; Roberts, James; Taylor, Steve L; Baumert, Joseph L; Ulberth, Franz; Wehling, Paul; Koehler, Peter

    2013-01-01

    The food allergen analytical community is endeavoring to create harmonized guidelines for the validation of food allergen ELISA methodologies to help protect food-sensitive individuals and promote consumer confidence. This document provides additional guidance to existing method validation publications for quantitative food allergen ELISA methods. The gluten-specific criterion provided in this document is divided into sections for information required by the method developer about the assay and information for the implementation of the multilaboratory validation study. Many of these recommendations and guidance are built upon the widely accepted Codex Alimentarius definitions and recommendations for gluten-free foods. The information in this document can be used as the basis of a harmonized validation protocol for any ELISA method for gluten, whether proprietary or nonproprietary, that will be submitted to AOAC andlor regulatory authorities or other bodies for status recognition. Future work is planned for the implementation of this guidance document for the validation of gluten methods and the creation of gluten reference materials. PMID:24282943

  4. An analytical method for the measurement of nonviable bioaerosols.

    Science.gov (United States)

    Menetrez, M Y; Foarde, K K; Ensor, D S

    2001-10-01

    Exposures from indoor environments are a major issue for evaluating total long-term personal exposures to the fine fraction (airborne, IAQ could be significantly deteriorated. The airborne biocontaminants or their metabolites can induce irritational, allergic, infectious, and chemical responses in exposed individuals. Biocontaminants, such as some mold spores or pollen grains, because of their size and mass, settle rapidly within the indoor environment. Over time they may become nonviable and fragmented by the process of desiccation. Desiccated nonviable fragments of organisms are common and can be toxic or allergenic, depending upon the specific organism or organism component. Once these smaller and lighter fragments of biological PM become suspended in air, they have a greater tendency to stay suspended. Although some bioaerosols have been identified, few have been quantitatively studied for their prevalence within the total indoor PM with time, or for their affinity to penetrate indoors. This paper describes a preliminary research effort to develop a methodology for the measurement of nonviable biologically based PM, analyzing for mold and ragweed antigens and endotoxins. The research objectives include the development of a set of analytical methods and the comparison of impactor media and sample size, and the quantification of the relationship between outdoor and indoor levels of bioaerosols. Indoor and outdoor air samples were passed through an Andersen nonviable cascade impactor in which particles from 0.2 to 9.0 microm were collected and analyzed. The presence of mold, ragweed, and endotoxin was found in all eight size ranges. The presence of respirable particles of mold and pollen found in the fine particle size range from 0.2 to 5.25 microm is evidence of fragmentation of larger source particles that are known allergens. PMID:11686248

  5. Development and validation of an UV spectrophotometric method for the determination of aliskiren in tablets

    OpenAIRE

    Micheli Wrasse-Sangoi; Leonardo Trevisan Secretti; Isabel Fração Diefenbach; Clarice Madalena Bueno Rolim; Maximiliano da Silva Sangoi

    2010-01-01

    For determination of aliskiren in commercial samples, an analytical UV spectrophotometric method was developed and validate according to ICH guideline. The method was linear in the range between 40 and 100 μg mL-1 (r² = 0.9997, n = 7) and exhibited suitable specificity, accuracy, precision, and robustness. It is simple, it has low cost, and it has low use polluting reagents. Therefore, the proposed method was successfully applied for the assay and dissolution studies of aliskiren in tabl...

  6. Analysis of the validity of the transcendental method for heavy nucleus

    International Nuclear Information System (INIS)

    In this paper, the degree and structure of the exactness of the transcedental method for the process of neutron slowing down on heavy nucleus (A>80) is studied in some detail. An original indirect method of genesis of the general form of the analytical equation of error is applied. This, together with the known solution for the constant function of cross-section constitutes the exact proof of the validity of the transcedental method for heavy nucleaus. The conditions of th exact solution are discussed. (author)

  7. Validation of a simple and rapid UV spectrophotometric method for dexamethasone assay in tablets

    Directory of Open Access Journals (Sweden)

    Rossana Barcellos Friedrich

    2009-01-01

    Full Text Available This work reports the validation of an analytical UV spectrophotometric method to assay dexamethasone in tablets (assay and dissolution studies. The method was linear in the range between 1 and 30 µg mL-1 presenting a good correlation coefficient (r = 0.9998, n = 7. Precision and accuracy analysis showed low relative standard deviation (< 2.00% and good percentual recoveries (95-105%. The procedure was linear, accurate, precise, and robust. The method is simple, and it has low cost. It does not use polluting reagents and can be applied in dissolution studies, being an adequate alternative to assay dexamethasone in tablets.

  8. Standardization of Chemical Analytical Techniques for Pyrolysis Bio-Oil: History, Challenges, and Current Status of Methods

    Energy Technology Data Exchange (ETDEWEB)

    Ferrell, Jack R., III; Olarte, Mariefel V.; Christensen, Earl D.; Padmaperuma, Asanga B.; Connatser, Raynella M.; Stankovikj, Filip; Meier, Dietrich; Paasikallio, Ville

    2016-09-01

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

  9. Validation of a streamlined multiclass, multiresidue method for determination of veterinary drug residues in bovine muscle by liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    Multiclass, multiresidue methods are becoming increasingly popular in regulatory monitoring programs due to their increased analytical scope and laboratory efficiency. In this work, we report the development and validation of a new high-throughput analytical method to monitor up to 131 veterinary d...

  10. 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

    2016-03-01

    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. PMID:26549429

  11. 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.

  12. 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…

  13. 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) an...

  14. Chemometric approach to open validation protocols: Prediction of validation parameters in multi-residue ultra-high performance liquid chromatography-tandem mass spectrometry methods.

    Science.gov (United States)

    Alladio, Eugenio; Pirro, Valentina; Salomone, Alberto; Vincenti, Marco; Leardi, Riccardo

    2015-06-01

    The recent technological advancements of liquid chromatography-tandem mass spectrometry allow the simultaneous determination of tens, or even hundreds, of target analytes. In such cases, the traditional approach to quantitative method validation presents three major drawbacks: (i) it is extremely laborious, repetitive and rigid; (ii) it does not allow to introduce new target analytes without starting the validation from its very beginning and (iii) it is performed on spiked blank matrices, whose very nature is significantly modified by the addition of a large number of spiking substances, especially at high concentration. In the present study, several predictive chemometric models were developed from closed sets of analytes in order to estimate validation parameters on molecules of the same class, but not included in the original training set. Retention time, matrix effect, recovery, detection and quantification limits were predicted with partial least squares regression method. In particular, iterative stepwise elimination, iterative predictors weighting and genetic algorithms approaches were utilized and compared to achieve effective variables selection. These procedures were applied to data reported in our previously validated ultra-high performance liquid chromatography-tandem mass spectrometry multi-residue method for the determination of pharmaceutical and illicit drugs in oral fluid samples in accordance with national and international guidelines. Then, the partial least squares model was successfully tested on naloxone and lormetazepam, in order to introduce these new compounds in the oral fluid validated method, which adopts reverse-phase chromatography. Retention time, matrix effect, recovery, limit of detection and limit of quantification parameters for naloxone and lormetazepam were predicted by the model and then positively compared with their corresponding experimental values. The whole study represents a proof-of-concept of chemometrics potential to

  15. Potential of accuracy profile for method validation in inductively coupled plasma spectrochemistry

    Energy Technology Data Exchange (ETDEWEB)

    Mermet, J.M., E-mail: jeanmichel.mermet@wanadoo.fr [Spectroscopy Forever, 624, Chemin du Colombier, F-01390 Tramoyes (France); Granier, G. [CEA Marcoule, DRCP/CETAMA, BP 17171, F-30207 Bagnols sur Ceze (France)

    2012-10-15

    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: Black-Right-Pointing-Pointer An analytical method is defined by its accuracy, i.e. both trueness and precision. Black-Right-Pointing-Pointer The accuracy as a function of an analyte concentration is an accuracy profile. Black-Right-Pointing-Pointer Profile basic concepts are explained for trueness and intermediate precision. Black-Right-Pointing-Pointer Profile-based tolerance intervals have to be compared with acceptability limits. Black-Right-Pointing-Pointer Typical accuracy profiles are given for both ICP-AES and ICP-MS techniques.

  16. Potential of accuracy profile for method validation in inductively coupled plasma spectrochemistry

    International Nuclear Information System (INIS)

    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.

  17. Semi-physiologic model validation and bioequivalence trials simulation to select the best analyte for acetylsalicylic acid.

    Science.gov (United States)

    Cuesta-Gragera, Ana; Navarro-Fontestad, Carmen; Mangas-Sanjuan, Victor; González-Álvarez, Isabel; García-Arieta, Alfredo; Trocóniz, Iñaki F; Casabó, Vicente G; Bermejo, Marival

    2015-07-10

    The objective of this paper is to apply a previously developed semi-physiologic pharmacokinetic model implemented in NONMEM to simulate bioequivalence trials (BE) of acetyl salicylic acid (ASA) in order to validate the model performance against ASA human experimental data. ASA is a drug with first-pass hepatic and intestinal metabolism following Michaelis-Menten kinetics that leads to the formation of two main metabolites in two generations (first and second generation metabolites). The first aim was to adapt the semi-physiological model for ASA in NOMMEN using ASA pharmacokinetic parameters from literature, showing its sequential metabolism. The second aim was to validate this model by comparing the results obtained in NONMEM simulations with published experimental data at a dose of 1000 mg. The validated model was used to simulate bioequivalence trials at 3 dose schemes (100, 1000 and 3000 mg) and with 6 test formulations with decreasing in vivo dissolution rate constants versus the reference formulation (kD 8-0.25 h (-1)). Finally, the third aim was to determine which analyte (parent drug, first generation or second generation metabolite) was more sensitive to changes in formulation performance. The validation results showed that the concentration-time curves obtained with the simulations reproduced closely the published experimental data, confirming model performance. The parent drug (ASA) was the analyte that showed to be more sensitive to the decrease in pharmaceutical quality, with the highest decrease in Cmax and AUC ratio between test and reference formulations. PMID:25869458

  18. Analytical and numerical methods for wave propagation in fluid media

    CERN Document Server

    Murawski, K

    2002-01-01

    This book surveys analytical and numerical techniques appropriate to the description of fluid motion with an emphasis on the most widely used techniques exhibiting the best performance.Analytical and numerical solutions to hyperbolic systems of wave equations are the primary focus of the book. In addition, many interesting wave phenomena in fluids are considered using examples such as acoustic waves, the emission of air pollutants, magnetohydrodynamic waves in the solar corona, solar wind interaction with the planet venus, and ion-acoustic solitons.

  19. A validated LC-MS-MS method for simultaneous identification and quantitation of rodenticides in blood.

    Science.gov (United States)

    Bidny, Sergei; Gago, Kim; David, Mark; Duong, Thanh; Albertyn, Desdemona; Gunja, Naren

    2015-04-01

    A rapid, highly sensitive and specific analytical method for the extraction, identification and quantification of nine rodenticides from whole blood has been developed and validated. Commercially available rodenticides in Australia include coumatetralyl, warfarin, brodifacoum, bromadiolone, difenacoum, flocoumafen, difethialone, diphacinone and chlorophacinone. A Waters ACQUITY UPLC TQD system operating in multiple reaction monitoring mode was used to conduct the analysis. Two different ionization techniques, ES+ and ES-, were examined to achieve optimal sensitivity and selectivity resulting in detection by MS-MS using electrospray ionization in positive mode for difenacoum and brodifacoum and in negative mode for all other analytes. All analytes were extracted from 200 µL of whole blood with ethylacetate and separated on a Waters ACQUITY UPLC BEH-C18 column using gradient elution. Ammonium acetate (10 mM, pH 7.5) and methanol were used as mobile phases with a total run time of 8 min. Recoveries were between 70 and 105% with limits of detection ranging from 0.5 to 1 ng/mL. The limit of quantitation was 2 ng/mL for all analytes. Calibration curves were linear within the range 2-200 ng/mL for all analytes with the coefficient of determination ≥0.98. The application of the proposed method using liquid-liquid extraction in a series of clinical investigations and forensic toxicological analyses was successful. PMID:25595137

  20. Semi-analytical and numerical methods for computing transient waves in 2D acoustic / poroelastic stratified media

    CERN Document Server

    Lefeuve-Mesgouez, Gaëlle; Chiavassa, Guillaume; Lombard, Bruno

    2012-01-01

    Wave propagation in a stratified fluid / porous medium is studied here using analytical and numerical methods. The semi-analytical method is based on an exact stiffness matrix method coupled with a matrix conditioning procedure, preventing the occurrence of poorly conditioned numerical systems. Special attention is paid to calculating the Fourier integrals. The numerical method is based on a high order finite-difference time-domain scheme. Mesh refinement is applied near the interfaces to discretize the slow compressional diffusive wave predicted by Biot's theory. Lastly, an immersed interface method is used to discretize the boundary conditions. The numerical benchmarks are based on realistic soil parameters and on various degrees of hydraulic contact at the fluid / porous boundary. The time evolution of the acoustic pressure and the porous velocity is plotted in the case of one and four interfaces. The excellent level of agreement found to exist between the two approaches confirms the validity of both metho...

  1. Quantitative assessment of gene expression network module-validation methods.

    Science.gov (United States)

    Li, Bing; Zhang, Yingying; Yu, Yanan; Wang, Pengqian; Wang, Yongcheng; Wang, Zhong; Wang, Yongyan

    2015-01-01

    Validation of pluripotent modules in diverse networks holds enormous potential for systems biology and network pharmacology. An arising challenge is how to assess the accuracy of discovering all potential modules from multi-omic networks and validating their architectural characteristics based on innovative computational methods beyond function enrichment and biological validation. To display the framework progress in this domain, we systematically divided the existing Computational Validation Approaches based on Modular Architecture (CVAMA) into topology-based approaches (TBA) and statistics-based approaches (SBA). We compared the available module validation methods based on 11 gene expression datasets, and partially consistent results in the form of homogeneous models were obtained with each individual approach, whereas discrepant contradictory results were found between TBA and SBA. The TBA of the Zsummary value had a higher Validation Success Ratio (VSR) (51%) and a higher Fluctuation Ratio (FR) (80.92%), whereas the SBA of the approximately unbiased (AU) p-value had a lower VSR (12.3%) and a lower FR (45.84%). The Gray area simulated study revealed a consistent result for these two models and indicated a lower Variation Ratio (VR) (8.10%) of TBA at 6 simulated levels. Despite facing many novel challenges and evidence limitations, CVAMA may offer novel insights into modular networks. PMID:26470848

  2. Validation of seismic probabilistic risk analysis (PRA) methods

    International Nuclear Information System (INIS)

    The objective of validation research is to obtain information that can be used by the NRC to develop acceptance criteria for seismic probabilistic risk assessment (PRA's) and thus improve the regulatory process. The needs for validation and experimental data in seismic PRA methodologies are assessed to be in the following areas: 1) definition of seismic hazards; 2) capacity and failure data for equipment, piping, and structures; and 3) response analyses of nuclear power plant systems. The effort under discussion focuses its attention on the validation of methods and data which are used to determine plant response and fragility. Failure data for equipment are best addressed in separate effects laboratory testing; piping fragility requires both system and component testing; failure data for structures is difficult to obtain because it is not practical to test as-built structures. Validation of response analyses requires extensive comparisons with experimental data from complex site-structure-component systems

  3. Laser: a Tool for Optimization and Enhancement of Analytical Methods

    Energy Technology Data Exchange (ETDEWEB)

    Preisler, Jan

    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

  4. A CT-based analytical dose calculation method for HDR 192Ir brachytherapy

    International Nuclear Information System (INIS)

    Purpose: This article presents an analytical dose calculation method for high-dose-rate 192Ir brachytherapy, taking into account the effects of inhomogeneities and reduced photon backscatter near the skin. The adequacy of the Task Group 43 (TG-43) two-dimensional formalism for treatment planning is also assessed. Methods: The proposed method uses material composition and density data derived from computed tomography images. The primary and scatter dose distributions for each dwell position are calculated first as if the patient is an infinite water phantom. This is done using either TG-43 or a database of Monte Carlo (MC) dose distributions. The latter can be used to account for the effects of shielding in water. Subsequently, corrections for photon attenuation, scatter, and spectral variations along medium- or low-Z inhomogeneities are made according to the radiological paths determined by ray tracing. The scatter dose is then scaled by a correction factor that depends on the distances between the point of interest, the body contour, and the source position. Dose calculations are done for phantoms with tissue and lead inserts, as well as patient plans for head-and-neck, esophagus, and MammoSite balloon breast brachytherapy treatments. Gamma indices are evaluated using a dose-difference criterion of 3% and a distance-to-agreement criterion of 2 mm. PTRANCT MC calculations are used as the reference dose distributions. Results: For the phantom with tissue and lead inserts, the percentages of the voxels of interest passing the gamma criteria (Pγ≥1) are 100% for the analytical calculation and 91% for TG-43. For the breast patient plan, TG-43 overestimates the target volume receiving the prescribed dose by 4% and the dose to the hottest 0.1 cm3 of the skin by 9%, whereas the analytical and MC results agree within 0.4%. Pγ≥1 are 100% and 48% for the analytical and TG-43 calculations, respectively. For the head-and-neck and esophagus patient plans, Pγ≥1 are ≥99

  5. Analytical modeling and experimental validation of a V-shape piezoelectric ultrasonic transducer

    Science.gov (United States)

    Li, Xiaoniu; Yao, Zhiyuan

    2016-07-01

    In this paper, an analytical model of a V-shape piezoelectric ultrasonic transducer is presented. The V-shape piezoelectric ultrasonic transducer has been widely applied to the piezoelectric actuator (ultrasonic motor), ultrasonic aided fabrication, sensor, and energy harvesting device. The V-shape piezoelectric ultrasonic transducer consists of two Langevin-type transducers connected together through a coupling point with a certain coupling angle. Considering the longitudinal and lateral movements of a single beam, the symmetrical and asymmetrical modals of the V-shape piezoelectric ultrasonic transducer are calculated. By using Hamilton–Lagrange equations, the electromechanical coupling model of the V-shape piezoelectric ultrasonic transducer is proposed. The influence of the coupling angle and cross-section on modal characteristics and electromechanical coupling coefficient are analyzed by the analytical model. A prototype of the V-shape piezoelectric ultrasonic transducer is fabricated, and the results of the experiments are in good agreement with the analytical model.

  6. 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.

  7. 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.

  8. Validation of a method to determine methylmercury in fish tissues using gas chromatography

    International Nuclear Information System (INIS)

    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%

  9. Determination of Al in cake mix: Method validation and estimation of measurement uncertainty

    Science.gov (United States)

    Andrade, G.; Rocha, O.; Junqueira, R.

    2016-07-01

    An analytical method for the determination of Al in cake mix was developed. Acceptable values were obtained for the following parameters: linearity, detection limit - LOD (5.00 mg-kg-1) quantification limit - LOQ (12.5 mg-kg-1), the recovery assays values (between 91 and 102%), the relative standard deviation under repeatability and within-reproducibility conditions (<20.0%) and measurement uncertainty tests (<10.0%) The results of the validation process showed that the proposed method is fitness for purpose.

  10. A brief introduction to analytical methods in nuclear forensics

    International Nuclear Information System (INIS)

    Nuclear forensic (NF) techniques are critical in responding to both environmental releases of nuclear materials and illicit trafficking activities involving both nuclear and counterfeit materials. Despite rising need, however, significant barriers exist to the future success of such research. This subset of analytical chemistry contains unique concerns (e.g. chronometry and impurity signatures), a wide variety of preparatory/instrumental approaches, and is in need of innovative solutions to current problems both in and out of the lab. The present work introduces existing NF research, development challenges and notes potential areas for advancement by highlighting several key analytical approaches. Examples of concerns and techniques discussed in this review include: chronometry, reference materials, separations, counting spectrometry, mass spectrometry and more. (author)

  11. Validation of a chromatographic method for quantitation of 50 μg/mL Latanoprost in a Cuban eye drops

    International Nuclear Information System (INIS)

    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

  12. Validação de método analítico para determinar a migração de ε-caprolactama das embalagens para alimentos gordurosos Validation of analytical method to determine ε-caprolactam migration from packagings to fatty food

    OpenAIRE

    Marcus Vinicius Justo Bomfim; Shirley de Mello Pereira Abrantes; Helena Pereira da Silva Zamith

    2010-01-01

    ε-Caprolactam (CAP) is a monomer of nylon 6 used as food packaging for bologna sausage, turkey blanquettes, fowl breast, pâtés and ham luncheon meat. After polymerization a part of the monomer can remain in the packaging and migrate into the food. The aim of this work was develop and validate a single laboratory method to determine CAP in ethanol 95% that simulates fatty food characteristics. Thus, linear range was 2 to 32 mg/L of CAP, detection and quantification limits were 0.83 and 1....

  13. Recent applications of nuclear analytical methods to the certification of elemental content in NIST standard reference materials

    International Nuclear Information System (INIS)

    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

  14. Analytical methods of heat transfer compared with numerical methods as related to nuclear waste repositories

    International Nuclear Information System (INIS)

    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

  15. Validation of different soft tissue simulation methods for breast augmentation

    OpenAIRE

    Roose, Liesbet; De Maerteleire, Wim; Mollemans, Wouter; Suetens, Paul

    2005-01-01

    Roose L., De Maerteleire W., Mollemans W., Suetens P., ''Validation of different soft tissue simulation methods for breast augmentation'', International congress series 19th international congress and exhibition on computer assisted radiology and surgery - CARS 2005, vol. 1281, pp. 485-490, June 22-25, 2005, Berlin, Germany.

  16. An experimental method for validating compressor valve vibration theory

    NARCIS (Netherlands)

    Habing, R.A.; Peters, M.C.A.M.

    2006-01-01

    This paper presents an experimental method for validating traditional compressor valve theory for unsteady flow conditions. Traditional valve theory considers the flow force acting on the plate and the flow rate as quasi-steady variables. These variables are related via semi-empirical coefficients w

  17. ePortfolios: The Method of Choice for Validation

    Science.gov (United States)

    Scott, Ken; Kim, Jichul

    2015-01-01

    Community colleges have long been institutions of higher education in the arenas of technical education and training, as well as preparing students for transfer to universities. While students are engaged in their student learning outcomes, projects, research, and community service, how have these students validated their work? One method of…

  18. Recommendations on biomarker bioanalytical method validation by GCC.

    Science.gov (United States)

    Hougton, Richard; Gouty, Dominique; Allinson, John; Green, Rachel; Losauro, Mike; Lowes, Steve; LeLacheur, Richard; Garofolo, Fabio; Couerbe, Philippe; Bronner, Stéphane; Struwe, Petra; Schiebl, Christine; Sangster, Timothy; Pattison, Colin; Islam, Rafiq; Garofolo, Wei; Pawula, Maria; Buonarati, Mike; Hayes, Roger; Cameron, Mark; Nicholson, Robert; Harman, Jake; Wieling, Jaap; De Boer, Theo; Reuschel, Scott; Cojocaru, Laura; Harter, Tammy; Malone, Michele; Nowatzke, William

    2012-10-01

    The 5th GCC in Barcelona (Spain) and 6th GCC in San Antonio (TX, USA) events provided a unique opportunity for CRO leaders to openly share opinions and perspectives, and to agree upon recommendations on biomarker bioanalytical method validation. PMID:23157353

  19. Simplified Analytical Method for Estimating the Resistance of Lock Gates to Ship Impacts

    Directory of Open Access Journals (Sweden)

    Loïc Buldgen

    2012-01-01

    Full Text Available The present paper is concerned with the design of lock gates submitted to ship impacts. In this paper, a simplified analytical method is presented to evaluate the resistance of such structures under collision. The basic idea is to assume that the resistance is first provided through a local deforming mode, corresponding to a localized crushing of some impacted structural elements. For consecutive larger deformations, the resistance is then mostly provided through a global deforming mode, corresponding to an overall movement of the entire gate. For assessing the resistance in the case of the local deforming mode, the structure is divided into a given number of large structural entities called “superelements.” For each of them, a relation between the resistance of the gate and the penetration of the striking ship is established. However, as some results are already available in the literature, this subject is not treated extensively in this paper. On the contrary, the calculation of the resistance of the gate provided through the global mode is detailed and the strategy to switch from local to global deformation is highlighted. Finally, we propose to validate our developments by making a comparison between results obtained numerically and those predicted by the present analytical approach.

  20. MULTIPLE CRITERA METHODS WITH FOCUS ON ANALYTIC HIERARCHY PROCESS AND GROUP DECISION MAKING

    OpenAIRE

    Lidija Zadnik-Stirn; Petra Grošelj

    2010-01-01

    Managing natural resources is a group multiple criteria decision making problem. In this paper the analytic hierarchy process is the chosen method for handling the natural resource problems. The one decision maker problem is discussed and, three methods: the eigenvector method, data envelopment analysis method, and logarithmic least squares method are presented for the derivation of the priority vector. Further, the group analytic hierarchy process is discussed and six methods for the aggrega...

  1. Validation of the analytical procedure for the determination of the neurotoxin β-N-methylamino-L-alanine in complex environmental samples.

    Science.gov (United States)

    Combes, Audrey; El Abdellaoui, Saïda; Sarazin, Cédric; Vial, Jérome; Mejean, Annick; Ploux, Olivier; Pichon, Valérie

    2013-04-10

    The neurotoxic l-2-amino-3-methylaminopropionic acid (BMAA) was hypothesized to be involved in sporadic cases of amyotrophic lateral sclerosis (ALS). Studies highlighting a possible implication of environmental factors in the incidence of sporadic ALS have become more numerous over recent years. Over the past years, the most widely used method for quantifying BMAA was based on the derivatization of this polar and basic molecule with a fluorescent compound (6-aminoquinolonyl-N-hydroxysuccinimidyl, 6-AQC). This derivatization allows the retention of the conjugate by reversed-phase liquid chromatography and its detection by fluorescence. Nevertheless, recent findings have shown that this method applied to complex samples may cause false positive responses. We therefore developed an analytical procedure for the determination of underivatized BMAA at trace level in complex environmental matrices (river water, cyanobacteria and biofilm) using solid-phase extraction (SPE) based on mixed mode sorbent to concentrate and clean up real samples. Analyzes were performed by hydrophilic interaction chromatography (HILIC) coupled to electrospray ionization and tandem mass spectrometry used in multiple reaction monitoring scan mode. Analytical procedures were validated for the different natural samples using the total error approach. BMAA can be quantified by these reliable and highly selective analytical methods in a range of only a few ng mL(-1) in river water and a few ng mg(-1) dry weight in cyanobacteria and biofilm matrices. PMID:23522111

  2. Chemical analysis of solid residue from liquid and solid fuel combustion: Method development and validation

    Energy Technology Data Exchange (ETDEWEB)

    Trkmic, M. [University of Zagreb, Faculty of Mechanical Engineering and Naval Architecturek Zagreb (Croatia); Curkovic, L. [University of Zagreb, Faculty of Chemical Engineering and Technology, Zagreb (Croatia); Asperger, D. [HEP-Proizvodnja, Thermal Power Plant Department, Zagreb (Croatia)

    2012-06-15

    This paper deals with the development and validation of methods for identifying the composition of solid residue after liquid and solid fuel combustion in thermal power plant furnaces. The methods were developed for energy dispersive X-ray fluorescence (EDXRF) spectrometer analysis. Due to the fuels used, the different composition and the location of creation of solid residue, it was necessary to develop two methods. The first method is used for identifying solid residue composition after fuel oil combustion (Method 1), while the second method is used for identifying solid residue composition after the combustion of solid fuels, i. e. coal (Method 2). Method calibration was performed on sets of 12 (Method 1) and 6 (Method 2) certified reference materials (CRM). CRMs and analysis test samples were prepared in pellet form using hydraulic press. For the purpose of method validation the linearity, accuracy, precision and specificity were determined, and the measurement uncertainty of methods for each analyte separately was assessed. The methods were applied in the analysis of real furnace residue samples. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  3. Analytical validation of operator actions based on SAMG for VVER 1000 with ASTECv2r3 computer code

    International Nuclear Information System (INIS)

    Highlights: • Performing of analytical validation of operator action based SAMG. • Simulation of base calculation of SBO scenario without operator action for VVER 1000. • Simulation of SBO scenario with investigation of operator actions based on SAMG for VVER 1000. - Abstract: This paper presents the analytical validation of operator action based on severe accident management guidelines (SAMG) for Kozloduy NPP VVER1000 with severe accident computer code ASTECv2r3. The work is oriented on investigation of plant behavior during total loss of power and the operator actions performed based on strategies considered in severe accident management guidelines (SAMG) in Kozloduy nuclear power plant (KNPP). Using the SAMG strategies the operator depressurize primary circuit by gas removing system (YR) and try to cool down the reactor core by high pressure injection system (HPIS). The purpose of these analyses is to examine the possibility of keeping the core from further damage during a severe accident and to assess the likelihood of additional generation of hydrogen by additional flooding of the heated core. For this purpose it have been simulated a SBO scenario with injection of cold water by a high pressure pump (HPP) in cold leg at different core exit temperatures at 923 K and 1253 K. The selection of investigated analyses was based on severe accident management strategy of KNPP VVER1000. The presented work is important for analytical validation, verification, and further improvements of SAMG as well as for assessment of Level 2 probabilistic safety analyses (L2 PSA). The work was performed at the Institute for Nuclear Research and Nuclear Energy (INRNE) in the frame of severe accident research

  4. Analytical validation of operator actions based on SAMG for VVER 1000 with ASTECv2r3 computer code

    Energy Technology Data Exchange (ETDEWEB)

    Stefanova, Antoaneta Emilova, E-mail: antoanet@inrne.bas.bg; Gencheva, Rositsa Veselinova, E-mail: roseh@mail.bg; Groudev, Pavlin Petkov, E-mail: pavlinpg@inrne.bas.bg

    2015-01-15

    Highlights: • Performing of analytical validation of operator action based SAMG. • Simulation of base calculation of SBO scenario without operator action for VVER 1000. • Simulation of SBO scenario with investigation of operator actions based on SAMG for VVER 1000. - Abstract: This paper presents the analytical validation of operator action based on severe accident management guidelines (SAMG) for Kozloduy NPP VVER1000 with severe accident computer code ASTECv2r3. The work is oriented on investigation of plant behavior during total loss of power and the operator actions performed based on strategies considered in severe accident management guidelines (SAMG) in Kozloduy nuclear power plant (KNPP). Using the SAMG strategies the operator depressurize primary circuit by gas removing system (YR) and try to cool down the reactor core by high pressure injection system (HPIS). The purpose of these analyses is to examine the possibility of keeping the core from further damage during a severe accident and to assess the likelihood of additional generation of hydrogen by additional flooding of the heated core. For this purpose it have been simulated a SBO scenario with injection of cold water by a high pressure pump (HPP) in cold leg at different core exit temperatures at 923 K and 1253 K. The selection of investigated analyses was based on severe accident management strategy of KNPP VVER1000. The presented work is important for analytical validation, verification, and further improvements of SAMG as well as for assessment of Level 2 probabilistic safety analyses (L2 PSA). The work was performed at the Institute for Nuclear Research and Nuclear Energy (INRNE) in the frame of severe accident research.

  5. 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

  6. A Rapid Gas Chromatography Method for Simultaneous Quantification of Ornidazole and Miconazole from Cream Formulations: Development, Validation and Application

    Directory of Open Access Journals (Sweden)

    Hetal M. Phatak

    2016-02-01

    Full Text Available Combination drug formulations are better in terms of effectiveness and hence are used many times for treatment of diseases. The physico-chemical properties of the different API used in a formulation have a significant impact in the development of a single method for the analysis of such drugs. In the current research a rapid analytical method employing GC-FID has been developed and validated for simultaneous quantification of the active ingredients Ornidazole and Miconazole from the cream formulation. The analytes were extracted from cream base and filtered. Adimethyl polysiloxane column is used for the separation of the analytes. The method involves simple temperature gradient and FID detection. Validation of the method showed response was a linear function of concentration in the range 50-150 µg mL−1 for both Ornidazole and Miconazole. The method was suitably validated and was found to be precise and robust, with recoveries for both the analytes being consistent and complete. The method has been successfully applied for the analysis of samples from marketed cream formulations.

  7. Refinement and extension of AOAC Method 2005.06 to include additional toxins in mussels: single-laboratory validation.

    Science.gov (United States)

    Turner, Andrew D; Norton, Deirdre M; Hatfield, Robert G; Morris, Steven; Reese, Allan R; Algoet, Myriam; Lees, David N

    2009-01-01

    A single-laboratory validation study was undertaken for the analysis of paralytic shellfish poisoning (PSP) toxins in common mussels, extending AOAC Official Method 2005.06 to include the additional toxins dcNEO and dcGTX2,3. The method was refined to improve toxin oxidation product stability, analytical sensitivity of N-hydroxylated toxins, and throughput. Validation was performed to characterize the method for selectivity, sensitivity, linearity, precision, repeatability, recovery, ruggedness, and uncertainty. Parallel testing of naturally contaminated mussels enabled comparison of sample toxicities obtained using mouse bioassay (MBA) and high-performance liquid chromatographic (HPLC) methodologies. Performance characteristics of the method are reported for all commercially available certified reference toxins. Results from the MBA and HPLC methods were well correlated, and the analytical method has been instigated as the sole monitoring tool for UK official control surveillance of PSP toxins in common mussels. PMID:19382578

  8. Validação de método analítico para determinar a migração de ε-caprolactama das embalagens para alimentos gordurosos Validation of analytical method to determine ε-caprolactam migration from packagings to fatty food

    Directory of Open Access Journals (Sweden)

    Marcus Vinicius Justo Bomfim

    2010-01-01

    Full Text Available ε-Caprolactam (CAP is a monomer of nylon 6 used as food packaging for bologna sausage, turkey blanquettes, fowl breast, pâtés and ham luncheon meat. After polymerization a part of the monomer can remain in the packaging and migrate into the food. The aim of this work was develop and validate a single laboratory method to determine CAP in ethanol 95% that simulates fatty food characteristics. Thus, linear range was 2 to 32 mg/L of CAP, detection and quantification limits were 0.83 and 1.63 mg/L, respectively. Repeatability showed Hor Rat values lower than 2 while recovery range was 97.5 to 106.5%. The method was considered adequate for purpose.

  9. Development Rapid Analytical Methods for Inositol as a Trace Component by HPLC and LC-MS/MS in Infant Formula.

    Science.gov (United States)

    Shin, Jin-Ho; Park, Jung-Min; Kim, Ha-Jung; Ahn, Jang-Hyuk; Kwak, Byung-Man; Kim, Jin-Man

    2015-01-01

    A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor. PMID:26761867

  10. Parametric validations of analytical lifetime estimates for radiation belt electron diffusion by whistler waves

    Directory of Open Access Journals (Sweden)

    A. V. Artemyev

    2013-04-01

    Full Text Available The lifetimes of electrons trapped in Earth's radiation belts can be calculated from quasi-linear pitch-angle diffusion by whistler-mode waves, provided that their frequency spectrum is broad enough and/or their average amplitude is not too large. Extensive comparisons between improved analytical lifetime estimates and full numerical calculations have been performed in a broad parameter range representative of a large part of the magnetosphere from L ~ 2 to 6. The effects of observed very oblique whistler waves are taken into account in both numerical and analytical calculations. Analytical lifetimes (and pitch-angle diffusion coefficients are found to be in good agreement with full numerical calculations based on CRRES and Cluster hiss and lightning-generated wave measurements inside the plasmasphere and Cluster lower-band chorus waves measurements in the outer belt for electron energies ranging from 100 keV to 5 MeV. Comparisons with lifetimes recently obtained from electron flux measurements on SAMPEX, SCATHA, SAC-C and DEMETER also show reasonable agreement.

  11. Parametric validations of analytical lifetime estimates for radiation belt electron diffusion by whistler waves

    International Nuclear Information System (INIS)

    The lifetimes of electrons trapped in Earth's radiation belts can be calculated from quasi-linear pitch-angle diffusion by whistler-mode waves, provided that their frequency spectrum is broad enough and/or their average amplitude is not too large. Extensive comparisons between improved analytical lifetime estimates and full numerical calculations have been performed in a broad parameter range representative of a large part of the magnetosphere from L ∼ 2 to 6. The effects of observed very oblique whistler waves are taken into account in both numerical and analytical calculations. Analytical lifetimes (and pitch-angle diffusion coefficients) are found to be in good agreement with full numerical calculations based on CRRES and Cluster hiss and lightning-generated wave measurements inside the plasmasphere and Cluster lower-band chorus waves measurements in the outer belt for electron energies ranging from 100 keV to 5 MeV. Comparisons with lifetimes recently obtained from electron flux measurements on SAMPEX, SCATHA, SAC-C and DEMETER also show reasonable agreement. (authors)

  12. Analytical model for temperature distribution of an end diode-pumped laser slab with Robin boundary conditions by Green’s function method

    Science.gov (United States)

    Moghtader Dindarlu, M. H.; Kavosh Tehrani, M.; Saghafifar, H.; Maleki, A.

    2016-05-01

    In this paper, an analytical model is introduced for temperature distribution of an end diode-pumped laser slab by Green’s function method. To solve the heat equation, Robin boundary conditions are considered because four lateral faces of the slab are cooled by water. An analytical model is extracted for single and dual end-pumping configuration. For an example, the 2D and 3D temperature distributions are plotted and our analytical model is validated by numerical solution based on the finite element method (FEM). The results show that our model has very good agreement with numerical solution. Furthermore, dependence of the temperature distribution on absorbed pump power is shown.

  13. Factor Analytic Validation of the Ford, Wolvin, and Chung Listening Competence Scale

    Science.gov (United States)

    Mickelson, William T.; Welch, S. A.

    2012-01-01

    This research begins to independently and quantitatively validate the Ford, Wolvin, and Chung (2000) Listening Competency Scale. Reliability and Confirmatory Factor analyses were conducted on two independent samples. The reliability estimates were found to be below those reported by Ford, Wolvin, and Chung (2000) and below acceptable levels for…

  14. Development and Validation of a Path Analytic Model of Students' Performance in Chemistry.

    Science.gov (United States)

    Anamuah-Mensah, Jophus; And Others

    1987-01-01

    Reported the development and validation of an integrated model of performance on chemical concept-volumetric analysis. Model was tested on 265 chemistry students in eight schools.Results indicated that for subjects using algorithms without understanding, performance on volumetric analysis problems was not influenced by proportional reasoning…

  15. 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 < 0.05), further indicating the robustness of the model. PMID:24327168

  16. Exact travelling wave solutions of the symmetric regularized long wave (SRLW using analytical methods

    Directory of Open Access Journals (Sweden)

    Jalil Manafian Heris

    2014-02-01

    Full Text Available In this article, we establish exact travelling wave solutions of the symmetric regularized long wave (SRLW by using analytical methods. The analytical methods are: the tanh-coth method and the sech^2 method which used to construct solitary wave solutions of nonlinear evolution equations. With the help of symbolic computation, we show that aforementioned methods provide a straightforward and powerful mathematical tool for solving nonlinear partial differential equations.

  17. 40 CFR 141.402 - Ground water source microbial monitoring and analytical methods.

    Science.gov (United States)

    2010-07-01

    ... by reference of the documents listed in footnotes 2-11 in accordance with 5 U.S.C. 552(a) and 1 CFR... monitoring and analytical methods. 141.402 Section 141.402 Protection of Environment ENVIRONMENTAL PROTECTION... Rule § 141.402 Ground water source microbial monitoring and analytical methods. (a) Triggered...

  18. 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

    tested 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. The method parameters: extraction temperature, sample weight, flush volume and solvent type were optimised, and a clean-up step was integrated in the PLE procedure by in-cell addition of C18-material to the extraction cells, which slightly improved the recovery and reproducibility of the......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...

  19. 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.

  20. Gas chromatographic validated method for quantification of ayurvedic polyherbal formulation

    Directory of Open Access Journals (Sweden)

    Navdeep Saini

    2015-01-01

    Full Text Available A new gas chromatographic-flame ionization detector (GC-FID method was developed for quantification of ayurvedic polyherbal formulation. The GC-FID method was found highly accurate, sensitive, simple and precise. This method was validated as per international conference on harmonization (ICH guidelines. Experimental work was performed by nonpolar capillary column (Zb-5, 5%-Phenyl-95%-dimethylpolysiloxane. Film thickness of capillary column (Zb-5 was (0.25 μm and length 30 m × 0.25 mm i.d. The temperature of the oven, injector and detector were 200, 210 and 280°C respectively. Data processing system was applied to obtain data. The standards and test samples were prepared in absolute ethanol. The principle constituents t-Anethol, d-Limonene, cuminaldehyde and thymol were found in ayurvedic polyherbal formulation. The ICH validation parameters for the proposed procedure, recovery (limit 98.85-100.76%, precision (<1.00%, limits of detection, limits of quantification and linearity (r2 = 0.995 ± 0.002 were observed under acceptance limit. Validation results were statistically calculated. The result shows that method is selective and reproducible for quantification of ayurvedic polyherbal formulation. The presented GC method can be applied for the routine analysis of principle constituents as well as ayurvedic polyherbal formulation.

  1. Analytical Quality by Design Approach in RP-HPLC Method Development for the Assay of Etofenamate in Dosage Forms.

    Science.gov (United States)

    Peraman, R; Bhadraya, K; Reddy, Y Padmanabha; Reddy, C Surayaprakash; Lokesh, T

    2015-01-01

    By considering the current regulatory requirement for an analytical method development, a reversed phase high performance liquid chromatographic method for routine analysis of etofenamate in dosage form has been optimized using analytical quality by design approach. Unlike routine approach, the present study was initiated with understanding of quality target product profile, analytical target profile and risk assessment for method variables that affect the method response. A liquid chromatography system equipped with a C18 column (250×4.6 mm, 5 μ), a binary pump and photodiode array detector were used in this work. The experiments were conducted based on plan by central composite design, which could save time, reagents and other resources. Sigma Tech software was used to plan and analyses the experimental observations and obtain quadratic process model. The process model was used for predictive solution for retention time. The predicted data from contour diagram for retention time were verified actually and it satisfied with actual experimental data. The optimized method was achieved at 1.2 ml/min flow rate of using mobile phase composition of methanol and 0.2% triethylamine in water at 85:15, % v/v, pH adjusted to 6.5. The method was validated and verified for targeted method performances, robustness and system suitability during method transfer. PMID:26997704

  2. A manual of analytical methods used at MINTEK

    International Nuclear Information System (INIS)

    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

  3. Determination of paraquat and diquat: LC-MS method optimization and validation.

    Science.gov (United States)

    Pizzutti, Ionara R; Vela, Giovana M E; de Kok, André; Scholten, Jos M; Dias, Jonatan V; Cardoso, Carmem D; Concenço, Germani; Vivian, Rafael

    2016-10-15

    This study describes the optimization and single-laboratory validation of a single residue method for determination of two bipyridylium herbicides, paraquat and diquat, in cowpeas by UPLC-MS/MS in a total run time of 9.3min. The method is based on extraction with an acidified methanol-water mixture. Different extraction parameters (extraction solvent composition, temperature, sample extract filtration, and pre-treatment of the laboratory sample) were evaluated in order to optimize the extraction method efficiency. Isotopically labeled internal standards, Paraquat-D6 and Diquat-D4, were used and added to the test portions prior to extraction. The method validation was performed by analyzing spiked samples at three concentrations (10, 20 and 50μgkg(-1)), with seven replicates (n=7) for each concentration. Linearity (r(2)) of analytical curves, accuracy (trueness as recovery % and precision as RSD%), instrument and method limits of detection and quantification (LOD and LOQ) and matrix effects were determined. Average recoveries obtained for diquat were between 77 and 85% with RSD values ⩽20%, for all spike levels studied. On the other hand, paraquat showed average recoveries between 68 and 103% with RSDs in the range 14.4-25.4%. The method LOQ was 10 and 20μgkg(-1) for diquat and paraquat, respectively. The matrix effect was significant for both pesticides. Consequently, matrix-matched calibration standards and using isotopically labeled (IL) analogues as internal standards for the target analytes are required for application in routine analysis. The validated method was successfully applied for cowpea samples obtained from various field studies. PMID:27173559

  4. 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...

  5. Validation of ascorbic acid tablets of national production by igh-performance liquid chromatography method

    International Nuclear Information System (INIS)

    We validate an analytical method by high-performance liquid chromatography to determine ascorbic acid proportion in vitamin C tablets, which was designed as an alternative method to quality control and to follow-up of active principle chemical stability, since official techniques to quality control of ascorbic acid in tablets are not selective with degradation products. Method was modified according to that reported in USP 28, 2005 for analysis of injectable product. We used a RP-18 column of 250 x 4.6 mm 5 μm with a UV detector to 245 nm. Its validation was necessary for both objectives, considering parameters required for methods of I and II categories. This method was enough linear, exact, and precise in the rank of 100-300 μg/mL. Also, it was selective with remaining components of matrix and with the possible degradation products achieved in stressing conditions. Detection and quantification limits were estimated. When method was validated it was applied to ascorbic acid quantification in two batches of expired tablets and we detected a marked influence of container in active degradation principle after 12 months at room temperature. (Author)

  6. A Validated HPLC-DAD Method for Simultaneous Determination of Etodolac and Pantoprazole in Rat Plasma

    Directory of Open Access Journals (Sweden)

    Ali S. Abdelhameed

    2014-01-01

    Full Text Available A simple, sensitive, and accurate HPLC-DAD method has been developed and validated for the simultaneous determination of pantoprazole and etodolac in rat plasma as a tool for therapeutic drug monitoring. Optimal chromatographic separation of the analytes was achieved on a Waters Symmetry C18 column using a mobile phase that consisted of phosphate buffer pH~4.0 as eluent A and acetonitrile as eluent B in a ratio of A : B, 55 : 45 v/v for 6 min, pumped isocratically at a flow rate of 0.8 mL min−1. The eluted analytes were monitored using photodiode array detector set to quantify samples at 254 nm. The method was linear with r2=0.9999 for PTZ and r2=0.9995 for ETD at a concentration range of 0.1–15 and 5–50 μgmL−1 for PTZ and ETD, respectively. The limits of detection were found to be 0.033 and 0.918 μgmL−1 for PTZ and ETD, respectively. The method was statistically validated for linearity, accuracy, precision, and selectivity following the International Conference for Harmonization (ICH guidelines. The reproducibility of the method was reliable with the intra- and interday precision (% RSD <7.76% for PTZ and <7.58 % for ETD.

  7. Probability of identification: a statistical model for the validation of qualitative botanical identification methods.

    Science.gov (United States)

    LaBudde, Robert A; Harnly, James M

    2012-01-01

    A qualitative botanical identification method (BIM) is an analytical procedure that returns a binary result (1 = Identified, 0 = Not Identified). A BIM may be used by a buyer, manufacturer, or regulator to determine whether a botanical material being tested is the same as the target (desired) material, or whether it contains excessive nontarget (undesirable) material. The report describes the development and validation of studies for a BIM based on the proportion of replicates identified, or probability of identification (POI), as the basic observed statistic. The statistical procedures proposed for data analysis follow closely those of the probability of detection, and harmonize the statistical concepts and parameters between quantitative and qualitative method validation. Use of POI statistics also harmonizes statistical concepts for botanical, microbiological, toxin, and other analyte identification methods that produce binary results. The POI statistical model provides a tool for graphical representation of response curves for qualitative methods, reporting of descriptive statistics, and application of performance requirements. Single collaborator and multicollaborative study examples are given. PMID:22468371

  8. Improvement and validation of the method to determine neutral detergent fiber in feed.

    Science.gov (United States)

    Hiraoka, Hisaaki; Fukunaka, Rie; Ishikuro, Eiichi; Enishi, Osamu; Goto, Tetsuhisa

    2012-10-01

    To improve the performance of the analytical method for neutral detergent fiber in feed with heat-stable α-amylase treatment (aNDFom), the process of adding heat-stable α-amylase, as well as other analytical conditions, were examined. In this new process, the starch in the samples was removed by adding amylase to neutral detergent (ND) solution twice, just after the start of heating and immediately after refluxing. We also examined the effects of the use of sodium sulfite, and drying and ashing conditions for aNDFom analysis by this modified amylase addition method. A collaborative study to validate this new method was carried out with 15 laboratories. These laboratories analyzed two samples, alfalfa pellet and dairy mixed feed, with blind duplicates. Ten laboratories used a conventional apparatus and five used a Fibertec(®) type apparatus. There were no significant differences in aNDFom values between these two refluxing apparatuses. The aNDFom values in alfalfa pellet and dairy mixed feed were 388 g/kg and 145 g/kg, the coefficients of variation for the repeatability and reproducibility (CV(r) and CV(R) ) were 1.3% and 2.9%, and the HorRat values were 0.8 and 1.1, respectively. This new method was validated with 5.8% uncertainty (k = 2) from the collaborative study. PMID:23035708

  9. Analytical method to accurately predict LMFBR core flow distribution

    International Nuclear Information System (INIS)

    An accurate and detailed representation of the flow distribution in LMFBR cores is very important as the starting point and basis of the thermal and structural core design. Previous experience indicated that the steady state and transient core design is as good as the core orificing; thus, a new orificing philosophy satisfying a priori all design constraints was developd. However, optimized orificing is a necessary, but not sufficient condition for achieving the optimum core flow distribution, which is affected by the hydraulic characteristics of the remainder of the primary system. Consequently, an analytical model of the overall primary system was developed, resulting in the CATFISH computer code, which, even though specifically written for LMFBRs, can be used for any reactor employing ducted assemblies

  10. Sterigmatocystin: occurrence in foodstuffs and analytical methods--an overview.

    Science.gov (United States)

    Versilovskis, Aleksandrs; De Saeger, Sarah

    2010-01-01

    Sterigmatocystin (STC) is a mycotoxin produced by fungi of many different Aspergillus species. Other species such as Bipolaris, Chaetomium, Emiricella are also able to produce STC. STC producing fungi were frequently isolated from different foodstuffs, while STC was regularly detected in grains, corn, bread, cheese, spices, coffee beans, soybeans, pistachio nuts, animal feed and silage. STC shows different toxicological, mutagenic and carcinogenic effects in animals and has been recognized as a 2B carcinogen (possible human carcinogen) by International Agency for Research on Cancer. There are more than 775 publications available in Scopus (and more than 505 in PubMed) mentioning STC, but there is no summary information available about STC occurrence and analysis in food. This review presents an overview of the worldwide information on the occurrence of STC in different foodstuffs during the last 40 years, and describes the progress made in analytical methodology for the determination of STC in food. PMID:19998385

  11. An analytic method for sensitivity analysis of complex systems

    CERN Document Server

    Zhu, Yueying; Li, Wei; Cai, Xu

    2016-01-01

    Sensitivity analysis is concerned with understanding how the model output depends on uncertainties (variances) in inputs and then identifies which inputs are important in contributing to the prediction imprecision. Uncertainty determination in output is the most crucial step in sensitivity analysis. In the present paper, an analytic expression, which can exactly evaluate the uncertainty in output as a function of the output's derivatives and inputs' central moments, is firstly deduced for general multivariate models with given relationship between output and inputs in terms of Taylor series expansion. A $\\gamma$-order relative uncertainty for output, denoted by $\\mathrm{R^{\\gamma}_v}$, is introduced to quantify the contributions of input uncertainty of different orders. On this basis, it is shown that the widely used approximation considering the first order contribution from the variance of input variable can satisfactorily express the output uncertainty only when the input variance is very small or the inpu...

  12. Intercalibration of analytical methods on marine environmental samples

    International Nuclear Information System (INIS)

    The analytical results reported by the 55 laboratories from 29 countries participating in this intercomparison have enabled to certify the concentration of 16 elements (As, Br, Ca, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Na, Rb, Se, Sr, Zn) in the mussel homogenate MA-M-2/TM. Information values could be established for 6 additional elements (Ag, Au, Cl, Pb, Sb, Sc). The atomic absorption spectroscopy was predominantly used in this intercomparison (45% of all determinations). It was followed by neutron activation analysis (28%), atomic emission spectroscopy (15%) and X-ray fluorescence (5%). The total number of outliers was moderate: 11.7% of all results. The number of outlying results by participating laboratories varied between 0 and 6

  13. Potential of accuracy profile for method validation in inductively coupled plasma spectrochemistry

    Science.gov (United States)

    Mermet, J. M.; Granier, G.

    2012-10-01

    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.

  14. Transformational and transactional leadership: a meta-analytic test of their relative validity.

    Science.gov (United States)

    Judge, Timothy A; Piccolo, Ronald F

    2004-10-01

    This study provided a comprehensive examination of the full range of transformational, transactional, and laissez-faire leadership. Results (based on 626 correlations from 87 sources) revealed an overall validity of .44 for transformational leadership, and this validity generalized over longitudinal and multisource designs. Contingent reward (.39) and laissez-faire (-.37) leadership had the next highest overall relations; management by exception (active and passive) was inconsistently related to the criteria. Surprisingly, there were several criteria for which contingent reward leadership had stronger relations than did transformational leadership. Furthermore, transformational leadership was strongly correlated with contingent reward (.80) and laissez-faire (-.65) leadership. Transformational and contingent reward leadership generally predicted criteria controlling for the other leadership dimensions, although transformational leadership failed to predict leader job performance. PMID:15506858

  15. Survey of Technetium Analytical Production Methods Supporting Hanford Nuclear Materials Processing

    International Nuclear Information System (INIS)

    This document provides a historical survey of analytical methods used for measuring 99Tc in nuclear fuel reprocessing materials and wastes at Hanford. Method challenges including special sludge matrices tested are discussed. Special problems and recommendations are presented

  16. Analytic Matrix Method for the Study of Propagation Characteristics of a Bent Planar Waveguide

    Institute of Scientific and Technical Information of China (English)

    LIU Qing; CAO Zhuang-Qi; SHEN Qi-Shun; DOU Xiao-Ming; CHEN Ying-Li

    2000-01-01

    An analytic matrix method is used to analyze and accurately calculate the propagation constant and bendinglosses of a bent planar waveguide. This method gives not only a dispersion equation with explicit physical insight,but also accurate complex propagation constants.

  17. Methods for Geometric Data Validation of 3d City Models

    Science.gov (United States)

    Wagner, D.; Alam, N.; Wewetzer, M.; Pries, M.; Coors, V.

    2015-12-01

    Geometric quality of 3D city models is crucial for data analysis and simulation tasks, which are part of modern applications of the data (e.g. potential heating energy consumption of city quarters, solar potential, etc.). Geometric quality in these contexts is however a different concept as it is for 2D maps. In the latter case, aspects such as positional or temporal accuracy and correctness represent typical quality metrics of the data. They are defined in ISO 19157 and should be mentioned as part of the metadata. 3D data has a far wider range of aspects which influence their quality, plus the idea of quality itself is application dependent. Thus, concepts for definition of quality are needed, including methods to validate these definitions. Quality on this sense means internal validation and detection of inconsistent or wrong geometry according to a predefined set of rules. A useful starting point would be to have correct geometry in accordance with ISO 19107. A valid solid should consist of planar faces which touch their neighbours exclusively in defined corner points and edges. No gaps between them are allowed, and the whole feature must be 2-manifold. In this paper, we present methods to validate common geometric requirements for building geometry. Different checks based on several algorithms have been implemented to validate a set of rules derived from the solid definition mentioned above (e.g. water tightness of the solid or planarity of its polygons), as they were developed for the software tool CityDoctor. The method of each check is specified, with a special focus on the discussion of tolerance values where they are necessary. The checks include polygon level checks to validate the correctness of each polygon, i.e. closeness of the bounding linear ring and planarity. On the solid level, which is only validated if the polygons have passed validation, correct polygon orientation is checked, after self-intersections outside of defined corner points and edges

  18. Development and Validation of an HPLC Method for the Analysis of Sirolimus in Drug Products

    Directory of Open Access Journals (Sweden)

    Hadi Valizadeh

    2012-05-01

    Full Text Available Purpose: The aim of this study was to develop a simple, rapid and sensitive reverse phase high performance liquid chromatography (RP-HPLC method for quantification of sirolimus (SRL in pharmaceutical dosage forms. Methods: The chromatographic system employs isocratic elution using a Knauer- C18, 5 mm, 4.6 × 150 mm. Mobile phase consisting of acetonitril and ammonium acetate buffer set at flow rate 1.5 ml/min. The analyte was detected and quantified at 278nm using ultraviolet detector. The method was validated as per ICH guidelines. Results: The standard curve was found to have a linear relationship (r2 > 0.99 over the analytical range of 125–2000ng/ml. For all quality control (QC standards in intraday and interday assay, accuracy and precision range were -0.96 to 6.30 and 0.86 to 13.74 respectively, demonstrating the precision and accuracy over the analytical range. Samples were stable during preparation and analysis procedure. Conclusion: Therefore the rapid and sensitive developed method can be used for the routine analysis of sirolimus such as dissolution and stability assays of pre- and post-marketed dosage forms.

  19. 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.

  20. Potential data used for validation of concentration statistics obtained using analytical model for conservative transport in an estuary

    Science.gov (United States)

    Galesic, Morena; Andricevic, Roko; Divic, Vladimir; Mateus, Marcos; Pinto, Ligia

    2016-04-01

    Coastal areas worldwide are important and sensitive ecosystems. Rivers are considered to be one of the most influential hydrological pathways for the waterborne transport and therefore estuaries are critical areas for a pollution hazard. To describe that hazard, the risk of exceeding the allowed concentration values of the pollution substance in such environment is often used. The analytical model calculates concentration statistics directly from the fundamental advective-diffusion equation for the case of continuous, steady conservative transport with the dominant stream flow mean velocity such is the case of low tide estuaries. Similar analytical models were previously proposed in atmosphere (Sullivan, 2004) and in groundwater (Andricevic, 2008). Knowing the main velocity and initial mass coming from the river, this kind of approach enables one a direct prediction of one-point concentration probability density function (pdf) which is then used to define the risk of exceeding the allowed concentration for certain water body. In this work we investigate how different data can be used for validation of the developed analytical model for conservative transport in an estuary. Two different types of measurement are being conducted at the local river Zrnovnica near city of Split, one measuring velocity and the other measuring salinity and temperature. Velocity data are used as an input to a numerical random walk particle tracking model to calculate the concentration moments. The salinity data are used as inverse proxy substance, hence the concentration moments are calculated directly from the inverse measured values. The results are highly affected by the scale effect, as the analytical model is developed at the point, while both numerical and measured values are smoothed over the grid size and over the sampling volume, respectively. However, the measured salinity, as concentration proxy, proved more resemblance to the concentration moment's shape, while numerical model

  1. An experimental and analytical method for approximate determination of the tilt rotor research aircraft rotor/wing download

    Science.gov (United States)

    Jordon, D. E.; Patterson, W.; Sandlin, D. R.

    1985-01-01

    The XV-15 Tilt Rotor Research Aircraft download phenomenon was analyzed. This phenomenon is a direct result of the two rotor wakes impinging on the wing upper surface when the aircraft is in the hover configuration. For this study the analysis proceeded along tow lines. First was a method whereby results from actual hover tests of the XV-15 aircraft were combined with drag coefficient results from wind tunnel tests of a wing that was representative of the aircraft wing. Second, an analytical method was used that modeled that airflow caused gy the two rotors. Formulas were developed in such a way that acomputer program could be used to calculate the axial velocities were then used in conjunction with the aforementioned wind tunnel drag coefficinet results to produce download values. An attempt was made to validate the analytical results by modeling a model rotor system for which direct download values were determinrd..

  2. Prognostics of Power Electronics, Methods and Validation Experiments

    Science.gov (United States)

    Kulkarni, Chetan S.; Celaya, Jose R.; Biswas, Gautam; Goebel, Kai

    2012-01-01

    Abstract Failure of electronic devices is a concern for future electric aircrafts that will see an increase of electronics to drive and control safety-critical equipment throughout the aircraft. As a result, investigation of precursors to failure in electronics and prediction of remaining life of electronic components is of key importance. DC-DC power converters are power electronics systems employed typically as sourcing elements for avionics equipment. Current research efforts in prognostics for these power systems focuses on the identification of failure mechanisms and the development of accelerated aging methodologies and systems to accelerate the aging process of test devices, while continuously measuring key electrical and thermal parameters. Preliminary model-based prognostics algorithms have been developed making use of empirical degradation models and physics-inspired degradation model with focus on key components like electrolytic capacitors and power MOSFETs (metal-oxide-semiconductor-field-effect-transistor). This paper presents current results on the development of validation methods for prognostics algorithms of power electrolytic capacitors. Particularly, in the use of accelerated aging systems for algorithm validation. Validation of prognostics algorithms present difficulties in practice due to the lack of run-to-failure experiments in deployed systems. By using accelerated experiments, we circumvent this problem in order to define initial validation activities.

  3. Experimental and analytical validation of a modular acetabular prosthesis in total hip arthroplasty

    Directory of Open Access Journals (Sweden)

    Aram Luke

    2007-05-01

    Full Text Available Abstract A finite element model has been developed to predict in vivo micro motion between a modular acetabular cup and liner after cement less total hip arthroplasty. The purpose of this study is to experimentally validate the model. Six LVDT sensors were used to monitor the micromotion of the liner when subjected to loading conditions ranging from 250 N to 5000 N. Deformations at points of interest for both the experiment and FEM were compared. Results of the FEM with different coefficient of friction between the liner and the cup were investigated to correlate with the experimental results.

  4. Validated HPTLC method for the simultaneous determination of cinnarizine and dimenhydrinate in their combined dosage form

    Directory of Open Access Journals (Sweden)

    Dina S. El-Kafrawy

    2016-02-01

    Full Text Available A simple, rapid and selective high performance thin layer chromatography (HPTLC method was developed for the simultaneous determination of cinnarizine (CNZ and dimenhydrinate (DMH in pure form and in their combined dosage form. Reviewing the literature revealed that there are no reports for the use of TLC for the assay of this mixture. Effective separation was achieved using Fluka HPTLC aluminum sheets of silica gel 60 F254 using chloroform–n-hexane–methanol (8.5:0.8:0.7, by volume as mobile phase, followed by densitometric measurement of CNZ and DMH spots at 254 and 279 nm, respectively. The reliability and analytical performance of the proposed HPTLC method were statistically validated with respect to linearity, ranges, precision, accuracy, selectivity, robustness and detection and quantification limits. Calibration curves were linear in the ranges of 50–400 and 50–500 ng/spot for CNZ and DMH, respectively with correlation coefficients >0.9998. The limits of detection were 8.1 and 8.0 ng/spot for CNZ and DMH respectively. The validated HPTLC method was applied to the simultaneous analysis of CNZ and DMH in laboratory-prepared tablets. Both analytes were successfully quantified with good recovery values, and no interference was encountered from the inactive ingredients.

  5. Method for Pre-Conditioning a Measured Surface Height Map for Model Validation

    Science.gov (United States)

    Sidick, Erkin

    2012-01-01

    This software allows one to up-sample or down-sample a measured surface map for model validation, not only without introducing any re-sampling errors, but also eliminating the existing measurement noise and measurement errors. Because the re-sampling of a surface map is accomplished based on the analytical expressions of Zernike-polynomials and a power spectral density model, such re-sampling does not introduce any aliasing and interpolation errors as is done by the conventional interpolation and FFT-based (fast-Fourier-transform-based) spatial-filtering method. Also, this new method automatically eliminates the measurement noise and other measurement errors such as artificial discontinuity. The developmental cycle of an optical system, such as a space telescope, includes, but is not limited to, the following two steps: (1) deriving requirements or specs on the optical quality of individual optics before they are fabricated through optical modeling and simulations, and (2) validating the optical model using the measured surface height maps after all optics are fabricated. There are a number of computational issues related to model validation, one of which is the "pre-conditioning" or pre-processing of the measured surface maps before using them in a model validation software tool. This software addresses the following issues: (1) up- or down-sampling a measured surface map to match it with the gridded data format of a model validation tool, and (2) eliminating the surface measurement noise or measurement errors such that the resulted surface height map is continuous or smoothly-varying. So far, the preferred method used for re-sampling a surface map is two-dimensional interpolation. The main problem of this method is that the same pixel can take different values when the method of interpolation is changed among the different methods such as the "nearest," "linear," "cubic," and "spline" fitting in Matlab. The conventional, FFT-based spatial filtering method used to

  6. Development and validation of analytical methodology for determination of polycyclic aromatic hydrocarbons (PAHS) in sediments. Assesment of Pedroso Park dam, Santo Andre, SP

    International Nuclear Information System (INIS)

    The polycyclic aromatic hydrocarbons (PAHs), by being considered persistent contaminants, by their ubiquity in the environment and by the recognition of their genotoxicity, have stimulated research activities in order to determine and evaluate their sources, transport, processing, biological effects and accumulation in compartments of aquatic and terrestrial ecosystems. In this work, the matrix studied was sediment collected at Pedroso Park's dam at Santo Andre, SP. The analytical technique employed was liquid chromatography in reverse phase with a UV/Vis detector. Statistics treatment of the data was established during the process of developing the methodology for which there was reliable results. The steps involved were evaluated using the concept of Validation of Chemical Testing. The parameters selected for the analytical validation were selectivity, linearity, Working Range, Sensitivity, Accuracy, Precision, Limit of Detection, Limit of quantification and robustness. These parameters showed satisfactory results, allowing the application of the methodology, and is a simple method that allows the minimization of contamination and loss of compounds by over-handling. For the PAHs tested were no found positive results, above the limit of detection, in any of the samples collected in the first phase. But, at the second collection, were found small changes mainly acenaphthylene, fluorene and benzo[a]anthracene. Although the area is preserved, it is possible to realize little signs of contamination. (author)

  7. An analytical model for heat transfer in a pin-bundle presentation and first validation

    International Nuclear Information System (INIS)

    The ANACONDA mathematical model presented here is aimed at calculating the three dimensional temperature field inside a LMFBR rod-bundle cooled by forced convection. In this thermal model the cross section of the rod bundle is discretized into a number of fluid and solid regions (pin heating zones, claddings, hexagonal duct). The lateral operators representing transverse energy transport inside the rod bundle (i.e. at a given cross-section) are approximated so as to enable an integration by hand of the thermal balance set of equations without any discrete representation of the axial space or time operators. The first validation of the model was done through calculating the three dimensional enthalpy field inside a 19 pin bundle, which had been experimentally investigated by the CEA in GRENOBLE (GR 19/sup I/ bundle). The model was then used for the preparation of the SCARLET II local porous blockage experiments to the run by EDF at CHATOU. Both sets of calculations were run rapidly on a pocket programmable calculator, and their results bring a good confidence in the validity of the model

  8. OWL-based reasoning methods for validating archetypes.

    Science.gov (United States)

    Menárguez-Tortosa, Marcos; Fernández-Breis, Jesualdo Tomás

    2013-04-01

    Some modern Electronic Healthcare Record (EHR) architectures and standards are based on the dual model-based architecture, which defines two conceptual levels: reference model and archetype model. Such architectures represent EHR domain knowledge by means of archetypes, which are considered by many researchers to play a fundamental role for the achievement of semantic interoperability in healthcare. Consequently, formal methods for validating archetypes are necessary. In recent years, there has been an increasing interest in exploring how semantic web technologies in general, and ontologies in particular, can facilitate the representation and management of archetypes, including binding to terminologies, but no solution based on such technologies has been provided to date to validate archetypes. Our approach represents archetypes by means of OWL ontologies. This permits to combine the two levels of the dual model-based architecture in one modeling framework which can also integrate terminologies available in OWL format. The validation method consists of reasoning on those ontologies to find modeling errors in archetypes: incorrect restrictions over the reference model, non-conformant archetype specializations and inconsistent terminological bindings. The archetypes available in the repositories supported by the openEHR Foundation and the NHS Connecting for Health Program, which are the two largest publicly available ones, have been analyzed with our validation method. For such purpose, we have implemented a software tool called Archeck. Our results show that around 1/5 of archetype specializations contain modeling errors, the most common mistakes being related to coded terms and terminological bindings. The analysis of each repository reveals that different patterns of errors are found in both repositories. This result reinforces the need for making serious efforts in improving archetype design processes. PMID:23246613

  9. Formal methods and digital systems validation for airborne systems

    Science.gov (United States)

    Rushby, John

    1993-01-01

    This report has been prepared to supplement a forthcoming chapter on formal methods in the FAA Digital Systems Validation Handbook. Its purpose is as follows: to outline the technical basis for formal methods in computer science; to explain the use of formal methods in the specification and verification of software and hardware requirements, designs, and implementations; to identify the benefits, weaknesses, and difficulties in applying these methods to digital systems used on board aircraft; and to suggest factors for consideration when formal methods are offered in support of certification. These latter factors assume the context for software development and assurance described in RTCA document DO-178B, 'Software Considerations in Airborne Systems and Equipment Certification,' Dec. 1992.

  10. Stepwise Procedure for Development and Validation of a Multipesticide Method

    International Nuclear Information System (INIS)

    The stepwise procedure for development and the validation of so called multi-pesticide methods are described. Principles, preliminary actions, criteria for the selection of chromatographic separation, detection and performance verification of multi-pesticide methods are outlined. Also the long term repeatability and reproducibility, as well as the necessity for the documentation of laboratory work are highlighted. Appendix I hereof describes in detail the calculation of calibration parameters, whereas Appendix II focuses on the calculation of the significance of differences of concentrations obtained on two different separation columns. (author)

  11. Description of JNC's analytical method and its performance for FBR cores

    International Nuclear Information System (INIS)

    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 keff, 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

  12. 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.

  13. 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.

  14. Manual of analytical methods for the Industrial Hygiene Chemistry Laboratory

    International Nuclear Information System (INIS)

    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

  15. Analytical Methods and Perturbation Theory for the Elliptic Restricted Three-Body Problem of Astrodynamics

    Science.gov (United States)

    Duffy, Brenton

    The distinguishing characteristic of the elliptic restricted three-body problem from that of the circular case is a pulsating potential field resulting in non-autonomous and non-integrable spacecraft dynamics, which are difficult to model using classical methods of analysis. The purpose of this study is to harness modern methods of analytical perturbation theory to normalize the system dynamics about the circular restricted three-body problem and about one of the triangular Lagrange points. The normalization is achieved through a canonical transformation of the system Hamiltonian function based on the Lie transform method introduced by Hori and Deprit in the 1960s. The classic method derives a near-identity transformation of a Hamiltonian function expanded about a single parameter such that the transformed system possesses ideal properties of integrability. One of the major contributions of this study is to extend the normalization method to two-parameter expansions and to non-autonomous Hamiltonian systems. The two-parameter extension is used to normalize the system dynamics of the elliptic restricted three-body problem such that the stability of the triangular Lagrange points may be determined using the Kolmogorov-Arnold-Moser theorem. Further dynamical analysis is performed in the transformed phase space in terms of local integrals of motion akin to Jacobi's integral of the circular restricted three-body problem. The local phase space around the Lagrange point is foliated by invariant tori that effectively separate the planar dynamics into qualitative regions of motion. Additional analysis is presented for the incorporation of control into the normalization routine with the goal of eliminating the non-circular secular perturbations. The control method is validated on a test case and applied to the elliptic restricted three-body problem for the purposes of stabilizing the motion around the triangular Lagrange points.

  16. Gas Chromatography Method of Cleaning Validation Process for 2-Propanol Residue Determination in Pharmaceutical Manufacturing Equipment

    Directory of Open Access Journals (Sweden)

    Łukasz Czubak

    2014-07-01

    Full Text Available Cleaning validation is an integral operation of good manufacturing practice in pharmaceutical industry. The aim of this study was to validate simple analytical method for detection of 2-propanol residue in equipment, which is likely contaminated with 2-propanol, usually used in the production area. The gas chromatography with flame ionization detection (GC-FID method was validated on a GC system using DB-FFAP capillary column at the flow rate of 4.9 mL/min. The calibration curve was linear over concentration range from 2.8µg/mL to 110.7µg/mL with a correlation coefficient equal to 0.99981. The detection limit (LOD and quantitation limit (LOQ were 1.1µg/mL and 2.8µg/mL, respectively. The simplicity of gas chromatography method makes it useful for routine analysis of 2-propanol residue and is an alternative to corresponding methods.

  17. Analytical method for promoting process capability of shock absorption steel

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Mechanical properties and low cycle fatigue are two factors that must be considered in developing new type steel for shock absorption. Process capability and process control are significant factors in achieving the purpose of research and development programs. Often-used evaluation methods failed to measure process yield and process centering; so this paper uses Taguchi loss function as basis to establish an evaluation method and the steps for assessing the quality of mechanical properties and process control of an iron and steel manufacturer. The establishment of this method can serve the research and development and manufacturing industry and lay a foundation in enhancing its process control ability to select better manufacturing processes that are more reliable than decision making by using the other commonly used methods.

  18. Elasto-plastic strain analysis by a semi-analytical method

    Indian Academy of Sciences (India)

    Debabrata Das; Prasanta Sahoo; Kashinath Saha

    2008-08-01

    The aim of this paper is to develop a simulation model of large deformation problems following a semi-analytical method, incorporating the complications of geometric and material non-linearity in the formulation. The solution algorithm is based on the method of energy principle in structural mechanics, as applicable for conservative systems. A one-dimensional solid circular bar problem has been solved in post-elastic range assuming linear elastic, linear strain hardening material behaviour. Type of loading includes uniform uniaxial loading and gravity loading due to body force, whereas the geometry of the bar is considered to be non-uniformly taper. Results are validated successfully with benchmark solution and some new results have also been reported. The location of initiation of elasto-plastic front and its growth are found to be functions of geometry of the bar and loading conditions. Some indicative results have been presented for static and dynamic problems and the solution methodology developed for one-dimension has been extended to the elasto-plastic analysis of two-dimensional strain field problems of a rotating disk.

  19. Analytic fitting and simulation methods for characteristic X-ray peaks from Si-PIN detector

    International Nuclear Information System (INIS)

    A semi-empirical detector response function (DRF) model is established to fit characteristic X-ray peaks recorded in Si-PIN spectra, which is mainly composed of four components: a truncated step function, a Gaussian-shaped full-energy peak, a Gaussian-shaped Si escape peak and an exponential tail. A simple but useful statistical distribution-based analytic method (SDA) is proposed to achieve accurate values of standard deviation for characteristic X-ray peaks. And the values of the model parameters except for the standard deviation are obtained by weighted least-squares fitting of the pulse-height spectra from a number of pure-element samples. A Monte Carlo model is also established to simulate the X-ray measurement setup. The simulated flux spectrum can be transformed by Si-PIN detector response function to real pulse height spectrum as studied in this work. Finally, the fitting result for a copper alloy sample was compared with experimental spectra, and the validity of the present method was demonstrated. (authors)

  20. Base flow separation: A comparison of analytical and mass balance methods

    Science.gov (United States)

    Lott, Darline A.; Stewart, Mark T.

    2016-04-01

    Base flow is the ground water contribution to stream flow. Many activities, such as water resource management, calibrating hydrological and climate models, and studies of basin hydrology, require good estimates of base flow. The base flow component of stream flow is usually determined by separating a stream hydrograph into two components, base flow and runoff. Analytical methods, mathematical functions or algorithms used to calculate base flow directly from discharge, are the most widely used base flow separation methods and are often used without calibration to basin or gage-specific parameters other than basin area. In this study, six analytical methods are compared to a mass balance method, the conductivity mass-balance (CMB) method. The base flow index (BFI) values for 35 stream gages are obtained from each of the seven methods with each gage having at least two consecutive years of specific conductance data and 30 years of continuous discharge data. BFI is cumulative base flow divided by cumulative total discharge over the period of record of analysis. The BFI value is dimensionless, and always varies from 0 to 1. Areas of basins used in this study range from 27 km2 to 68,117 km2. BFI was first determined for the uncalibrated analytical methods. The parameters of each analytical method were then calibrated to produce BFI values as close to the CMB derived BFI values as possible. One of the methods, the power function (aQb + cQ) method, is inherently calibrated and was not recalibrated. The uncalibrated analytical methods have an average correlation coefficient of 0.43 when compared to CMB-derived values, and an average correlation coefficient of 0.93 when calibrated with the CMB method. Once calibrated, the analytical methods can closely reproduce the base flow values of a mass balance method. Therefore, it is recommended that analytical methods be calibrated against tracer or mass balance methods.

  1. LOX/hydrocarbon rocket engine analytical design methodology development and validation. Volume 2: Appendices

    Science.gov (United States)

    Niiya, Karen E.; Walker, Richard E.; Pieper, Jerry L.; Nguyen, Thong V.

    1993-01-01

    This final report includes a discussion of the work accomplished during the period from Dec. 1988 through Nov. 1991. The objective of the program was to assemble existing performance and combustion stability models into a usable design methodology capable of designing and analyzing high-performance and stable LOX/hydrocarbon booster engines. The methodology was then used to design a validation engine. The capabilities and validity of the methodology were demonstrated using this engine in an extensive hot fire test program. The engine used LOX/RP-1 propellants and was tested over a range of mixture ratios, chamber pressures, and acoustic damping device configurations. This volume contains time domain and frequency domain stability plots which indicate the pressure perturbation amplitudes and frequencies from approximately 30 tests of a 50K thrust rocket engine using LOX/RP-1 propellants over a range of chamber pressures from 240 to 1750 psia with mixture ratios of from 1.2 to 7.5. The data is from test configurations which used both bitune and monotune acoustic cavities and from tests with no acoustic cavities. The engine had a length of 14 inches and a contraction ratio of 2.0 using a 7.68 inch diameter injector. The data was taken from both stable and unstable tests. All combustion instabilities were spontaneous in the first tangential mode. Although stability bombs were used and generated overpressures of approximately 20 percent, no tests were driven unstable by the bombs. The stability instrumentation included six high-frequency Kistler transducers in the combustion chamber, a high-frequency Kistler transducer in each propellant manifold, and tri-axial accelerometers. Performance data is presented, both characteristic velocity efficiencies and energy release efficiencies, for those tests of sufficient duration to record steady state values.

  2. An Efficient Certificate Status Validation Method for Mobile Communication

    Institute of Scientific and Technical Information of China (English)

    ZHOUYongbin; QINGSihan; ZHANGZhenfeng; JIQingguang

    2004-01-01

    The huge success of mobile telephone and such other wireless digital devices have transformed business and the Inter'net. In order to protect the security of mobile commerce transaction, WAP forum specified the WAP security protocol and defined WPKI architecture. Certificate status checking is one of the challenging issues of PKI in wired settings~ and it is more challenging in the wireless world (that is WPKI here) due to the limitations of mobile devices. In this paper, several mechanisms for certificate status validation are summarized and compared, and a new efficient certificate status validation method for WPKI is presented based on commutative hashing and a variation of dynamic Merkle hash tree. The newly proposed scheme has the advantages of being efficient and secure. The computation of the tree is independent of the nodes’ relative location in the hash tree, thus simplifying the computation and verification process. The proposed scheme is compatible with both X.509 certificate and WTLS certificate.

  3. Validation of analytical measurement and generation of quality data related to post Fukushima coastal marine assessment

    International Nuclear Information System (INIS)

    The present report gives the brief summary of the participation of Environmental Radioactivity Measurement Section, Health Physics Division in the proficiency test organized in the frame of the IAEA Technical Cooperation project RAS/7/021. The objective of the proficiency test was to check performances, analytical capabilities and comparability of results of radiological measurements. This proficiency test has deviated from normal exercise as additional conditions were imposed by IAEA. The extraction efficiency of cesium isotopes on copper ferrocyanide filter cartridge used for in-situ pre concentration for large volume of sea water was found in the range of 85 to 90 %. Our country reported 134Cs and 137Cs activity levels of 0.0707±0.0043 Bg.kg-1 and 0.1027±0.0064 Bg.kg-1. The approach discussed for low level measurement in high volume of sea water resulted in a precision of 3.2%. The relative bias for 134Cs and 137Cs was - 4% and 2% respectively which was well below the criteria of maximum acceptable bias fixed by IAEA at 25% for both radionuclides. The results also ensure that our laboratory is producing data that is accurate, precise and reliable. Our results passed the evaluation criteria required by IAEA. This report describes a detailed methodology and approach to carry out low level measurement in the marine environment. (author)

  4. Validity of the CT to attenuation coefficient map conversion methods

    International Nuclear Information System (INIS)

    The most important commercialized methods of attenuation correction in SPECT are based on attenuation coefficient map from a transmission imaging method. The transmission imaging system can be the linear source of radioelement or a X-ray CT system. The image of transmission imaging system is not useful unless to replacement of the attenuation coefficient or CT number with the attenuation coefficient in SPECT energy. In this paper we essay to evaluate the validity and estimate the error of the most used method of this transformation. The final result shows that the methods which use a linear or multi-linear curve accept a error in their estimation. The value of mA is not important but the patient thickness is very important and it can introduce a error more than 10 percent in the final result

  5. A valid method of calculating virtual scene depth

    Institute of Scientific and Technical Information of China (English)

    QUAN Hong-yan; ZHANG Tian-wen; LIN Xiang-hong

    2005-01-01

    A valid method of virtual scene depth calculating is put forward. In this method cameras rotate in three different viewpoints in the plane and we calculate the depth of panorama using three stitching cylinder panoramas. In the investigation, the column of panorama is regarded as a slot image. Using the conic intersected by the epipolar plane and the cylinder, we can obtain the perpendicularity disparity. In order to obtain dense correspondence fast and accurately, a new method of obtaining horizontal disparity using depth continuity is also put forward. It converts the problem of panorama dense correspondence to the problem of searching points in the conic. The occlusion problem is dealt with using three cylinders in the depth calculation. It is verified that this method is convenient, useful and efficient in calculating the depth of a virtual scene.

  6. Analytical Model Analysis Of Distributed Cooperative Spectrum Sensing Method

    Directory of Open Access Journals (Sweden)

    Ravi Prakash Shukla

    2012-05-01

    Full Text Available Spectrum sensing is a key function of cognitive radio to prevent the harmful interference with licensed users and identify the available spectrum for improving the spectrum’s utilization. Various methods for spectrum sensing control, such as deciding which sensors should perform sensing simultaneously and finding the appropriate trade-off between probability of misdetection and false alarm rate, are described. However, detection performance in practice is often compromised with multipath fading, shadowing and receiver uncertainty issues. To mitigate the impact of these issues, cooperative spectrum sensing has been shown to be an effective method to improve the detection performance by exploiting spatial diversity.

  7. Validated spectrophotometric methods for determination of some oral hypoglycemic drugs.

    Science.gov (United States)

    Farouk, M; Abdel-Satar, O; Abdel-Aziz, O; Shaaban, M

    2011-02-01

    Four accurate, precise, rapid, reproducible, and simple spectrophotometric methods were validated for determination of repaglinide (RPG), pioglitazone hydrochloride (PGL) and rosiglitazone maleate (RGL). The first two methods were based on the formation of a charge-transfer purple-colored complex of chloranilic acid with RPG and RGL with a molar absorptivity 1.23 × 103 and 8.67 × 102 l•mol-1•cm-1 and a Sandell's sensitivity of 0.367 and 0.412 μg•cm-2, respectively, and an ion-pair yellow-colored complex of bromophenol blue with RPG, PGL and RGL with molar absorptivity 8.86 × 103, 6.95 × 103, and 7.06 × 103 l•mol-1•cm-1, respectively, and a Sandell's sensitivity of 0.051 μg•cm-2 for all ion-pair complexes. The influence of different parameters on color formation was studied to determine optimum conditions for the visible spectrophotometric methods. The other spectrophotometric methods were adopted for demtermination of the studied drugs in the presence of their acid-, alkaline- and oxidative-degradates by computing derivative and pH-induced difference spectrophotometry, as stability-indicating techniques. All the proposed methods were validated according to the International Conference on Harmonization guidelines and successfully applied for determination of the studied drugs in pure form and in pharmaceutical preparations with good extraction recovery ranges between 98.7-101.4%, 98.2-101.3%, and 99.9-101.4% for RPG, PGL, and RGL, respectively. Results of relative standard deviations did not exceed 1.6%, indicating that the proposed methods having good repeatability and reproducibility. All the obtained results were statistically compared to the official method used for RPG analysis and the manufacturers methods used for PGL and RGL analysis, respectively, where no significant differences were found. PMID:22466095

  8. Validation of an Impedance Education Method in Flow

    Science.gov (United States)

    Watson, Willie R.; Jones, Michael G.; Parrott, Tony L.

    2004-01-01

    This paper reports results of a research effort to validate a method for educing the normal incidence impedance of a locally reacting liner, located in a grazing incidence, nonprogressive acoustic wave environment with flow. The results presented in this paper test the ability of the method to reproduce the measured normal incidence impedance of a solid steel plate and two soft test liners in a uniform flow. The test liners are known to be locally react- ing and exhibit no measurable amplitude-dependent impedance nonlinearities or flow effects. Baseline impedance spectra for these liners were therefore established from measurements in a conventional normal incidence impedance tube. A key feature of the method is the expansion of the unknown impedance function as a piecewise continuous polynomial with undetermined coefficients. Stewart's adaptation of the Davidon-Fletcher-Powell optimization algorithm is used to educe the normal incidence impedance at each Mach number by optimizing an objective function. The method is shown to reproduce the measured normal incidence impedance spectrum for each of the test liners, thus validating its usefulness for determining the normal incidence impedance of test liners for a broad range of source frequencies and flow Mach numbers. Nomenclature

  9. Development and validation of a high performance liquid chromatography method for oligodeoxynucleotides determination in a novel coagel-based formulation

    Directory of Open Access Journals (Sweden)

    Gabriela V. Ullio-Gamboa

    2015-06-01

    However, due to inter-assay variability and accuracy problems associated with the afore mentioned methods, we have developed and validated an isocratic high performance liquid chromatographic (HPLC for analytical determination of PS-ODN containing unmethylated CpG motifs (CpG-ODN. Validation under Food and Drug Administration (FDA guidelines of the analytical parameters include: linearity (r2 0.9996, LOD (0.86 μg/ml and LOQ (6.25 μg/ml, intra (0.19–3.37% and inter-day precision (0.63–3.75% expressed as relative standard deviation (RSD, and robustness parameters (less than 2.80%. Using this method, recoveries ranging from 89.9% to 99.9% were obtained. Thus, this method provides a simple, sensitive, precise and reproducible examination which can be readily adapted for the assessment of CpG-ODN in different pharmaceutical preparations.

  10. A new robust method for the treatment of analytical data

    International Nuclear Information System (INIS)

    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

  11. Analytical Methods for Determination of the Oxidative Status in Oils

    OpenAIRE

    Semb, Thea Norveel

    2012-01-01

    In industry today standard oxidative quality parameters are based on measurements of primary and secondary oxidation products, measured by PV and AV respectively. These methods are all prone to limitations and weaknesses, and their suitability for application on marine oils is not well documented. An increase in fish oil products with added flavor, color compounds, antioxidants and vitamins has entered the market in recent years. However, no documentation on the effect of these additives on t...

  12. A Vocal-Based Analytical Method for Goose Behaviour Recognition

    OpenAIRE

    Henrik Karstoft; Ole Green; Kim Arild Steen; Ole Roland Therkildsen

    2012-01-01

    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...

  13. The analytic method for calculating the control rod worth

    International Nuclear Information System (INIS)

    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

  14. Brazilian Center for the Validation of Alternative Methods (BraCVAM) and the process of validation in Brazil.

    Science.gov (United States)

    Presgrave, Octavio; Moura, Wlamir; Caldeira, Cristiane; Pereira, Elisabete; Bôas, Maria H Villas; Eskes, Chantra

    2016-03-01

    The need for the creation of a Brazilian centre for the validation of alternative methods was recognised in 2008, and members of academia, industry and existing international validation centres immediately engaged with the idea. In 2012, co-operation between the Oswaldo Cruz Foundation (FIOCRUZ) and the Brazilian Health Surveillance Agency (ANVISA) instigated the establishment of the Brazilian Center for the Validation of Alternative Methods (BraCVAM), which was officially launched in 2013. The Brazilian validation process follows OECD Guidance Document No. 34, where BraCVAM functions as the focal point to identify and/or receive requests from parties interested in submitting tests for validation. BraCVAM then informs the Brazilian National Network on Alternative Methods (RENaMA) of promising assays, which helps with prioritisation and contributes to the validation studies of selected assays. A Validation Management Group supervises the validation study, and the results obtained are peer-reviewed by an ad hoc Scientific Review Committee, organised under the auspices of BraCVAM. Based on the peer-review outcome, BraCVAM will prepare recommendations on the validated test method, which will be sent to the National Council for the Control of Animal Experimentation (CONCEA). CONCEA is in charge of the regulatory adoption of all validated test methods in Brazil, following an open public consultation. PMID:27031604

  15. The MRBT model: an analytical dispersion model in a finite mixing layer. Sensitivity analysis and validation against tracer measurements

    Science.gov (United States)

    Andretta, Massimo; Bianconi, Roberto; Flospergher, Walter; Tamponi, Matteo

    This paper describes the characteristics of the MRBT model for studying the dispersion of a pollutant in the lower atmosphere under conditions of spatial homogeneity. The MRBT is shown to be a simple and efficient model based upon a non-stationary analytical solution of the atmospheric dispersion equation in a finite mixing layer. The results of the sensitivity analysis and of validation testing, made with field measurements of tracers carried out at the Nuclear Research Centre in Karlsruhe (Germany), demonstrate the superiority of MRBT with respect to traditional Gaussian models. The model is currently implemented in FORTRAN 77 for the personal computer and is suitable for an initial assessment of short-term atmospheric dispersion with limited computing resources.

  16. Testing of analytical and purification methods for HTR helium coolant

    International Nuclear Information System (INIS)

    The paper describes a method of determination of gaseous impurities (H2, O2, N2, CO, CH4, CO2) in high purity helium as well as the methods of gaseous impurities removal. A device used for the determination was the Master GC type gas chromatograph with a helium detection unit and a ShinCarbon ST column. A temperature program was used to improve the conditions of separation and to reach maximum response of the detector. The obtained limits of detection defined as three times the standard deviation of the background value of tested components are H2 0.3 vppm, O2 0.4 vppm, N2 0.2 vppm, CO 2 vppm, CH4 3 vppm, CO2 2 vppm. Analysis time is less than 20 min. The developed method will be used for checking the purity of helium environment in the experimental loop to model experimental conditions in the high temperature gas cooled reactor (HTGR). Within the scope of the proposal of the helium purification system, the efficiency of removing selected impurities (CO, CO2, CH4) on adsorbents (based on zeolites and active carbon) was tested. A laboratory scale apparatus and an FTIR spectrometer were used for experiments.

  17. An improved analytical method for plate-fluid frequency determination

    International Nuclear Information System (INIS)

    The rectangular thin elastic plates are broadly used as structural components of different thin-walled parallelepiped tanks, containing an acoustic liquid and subjected to dynamic loads. The important problem - to determine the basic natural frequencies of the plate, taking into account its interaction with the internal fluid, has been considered by A.I. Pretlove and A. Craggs (1970) suggested an original approximate method. The philosophy of the method proposed is to take into account only some harmonics (but the most essential ones) in the motion equation of the plate, considering in the same time in original manner the R.H. Sides which describe the plate-fluid interaction. The plate considered is free supported. Following their suggestion, only the main co-ordinates q11(t) and q31(t), has to be considered presupposing with this, that the plate size along the x-direction always has to be considerably longer. This preference over the x-direction brakes the geometric symmetry, and as a consequence, their smart method loses its generality. As it is well known (from the plate stability/dynamics theory) the wave forming has its own law, which in the article under discussion possibly are not quite well observed. From another side, in connection with the assumption that the fluid-structure interaction (FSI) will be adiabatic process, they express some suspect on the results obtained

  18. Validation of finite element and boundary element methods for predicting structural vibration and radiated noise

    Science.gov (United States)

    Seybert, A. F.; Wu, X. F.; Oswald, Fred B.

    1992-01-01

    Analytical and experimental validation of methods to predict structural vibration and radiated noise are presented. A rectangular box excited by a mechanical shaker was used as a vibrating structure. Combined finite element method (FEM) and boundary element method (BEM) models of the apparatus were used to predict the noise radiated from the box. The FEM was used to predict the vibration, and the surface vibration was used as input to the BEM to predict the sound intensity and sound power. Vibration predicted by the FEM model was validated by experimental modal analysis. Noise predicted by the BEM was validated by sound intensity measurements. Three types of results are presented for the total radiated sound power: (1) sound power predicted by the BEM modeling using vibration data measured on the surface of the box; (2) sound power predicted by the FEM/BEM model; and (3) sound power measured by a sound intensity scan. The sound power predicted from the BEM model using measured vibration data yields an excellent prediction of radiated noise. The sound power predicted by the combined FEM/BEM model also gives a good prediction of radiated noise except for a shift of the natural frequencies that are due to limitations in the FEM model.

  19. Validação de método analítico espectrofotométrico UV para determinação de ácido úsnico em lipossomas Validation of a UV-spectrophotometric analytical method for the determination of usnic acid in liposomes

    Directory of Open Access Journals (Sweden)

    Marigilson Pontes de Siqueira-Moura

    2008-12-01

    Full Text Available O ácido úsnico (AU é um composto de origem liquênica e tem demonstrado importantes atividades biológicas, tais como: antitumoral, antimicrobiano, antiviral, antiproliferativo e antiinflamatório. Os lipossomas são vesículas lipídicas contendo espaço aquoso interno e têm sido utilizados como carreadores coloidais de fármacos, principalmente na terapêutica de câncer e infecções bacterianas e fúngicas. O objetivo desse trabalho foi desenvolver e validar um método espectrofotométrico UV para determinação de ácido úsnico em lipossomas. Os parâmetros de validação linearidade, precisão, exatidão, robustez, limites de detecção e quantificação foram determinados segundo diretrizes internacionais de padronização e Farmacopéia Americana. A faixa de linearidade foi de 3 a 15 µg.mL-1, a equação de regressão: absorbância = 0,070 x [AU] (µg.mL-1 + 0,013 e r = 0,9997. A repetibilidade (coeficiente de variação do método foi 1,96% e a precisão intermediária indicou que a diferença entre as médias foi estatisticamente insignificante (P The secondary lichen metabolite usnic acid [2,6-diacetyl-7,9-dihydroxy-8,9b-dimethyl-1,3(2H,9bH-dibenzofuran] has demonstrated pharmacological potential activities such as antitumor, antimicrobial, antiviral, antiproliferative, and anti-inflammatory. Liposomes are vesicles composed of phospholipid bilayers surrounding aqueous compartments and they have been used as colloidal drug carriers. The aim of this study was to develop and validate a quantitative UV spectrophotometric method for determination of usnic acid in liposomal formulations. The validation parameters were assessed according to The International Conference on Harmonization (ICH and American Pharmacopoeia guidelines. The linearity range was of 3-15 µg.mL-1, regression equation: absorbance = 0.070 x UA concentration (µg.mL-1 + 0.013, and r = 0.9997. The repeatability (relative standard deviation of the method was 1.96% and

  20. Analytical methods in heavy quark physics and the case of $\\tau_{1/2}(w)$

    OpenAIRE

    Yaouanc, A. Le

    2004-01-01

    Analytical methods in heavy quark physics are shortly reviewed, with emphasis on the problems of dynamical calculations. Then, attention is attracted to the various difficulties raised by a tentative experimental determination of $\\tau_{1/2}$

  1. 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.

  2. Some considerations to quality control and method validation in EDXRF analysis

    International Nuclear Information System (INIS)

    The x-ray laboratories face an urgent need for Quality Assurance System implementation, due to the demands from the society for reliable / certified results. The implemented Quality Assurance System should comply with the general requirements for the competence of testing and calibration laboratories of the latest approved quality assurance ISO standard, in particular with the ISO/IEC 17025:2005. The specific features of energy dispersive x-ray fluorescence techniques require of a careful interpretation of some concepts related to quality control of the results and to method validation. This contribution presents some thoughts on how to assess the traceability of the results, as well as to evaluate the characteristics of performance of the methods, in particular linearity, working range, precision, trueness and detection limits providing some typical examples of EDXRF analytical methods for illustration. Recommendations are provided to quantify the uncertainty of the results. (Full Text)

  3. Validation of a residue method to determine pesticide residues in cucumber by using nuclear techniques

    International Nuclear Information System (INIS)

    In this study, a multi-residue method using ethyl acetate for extraction and gel permeation chromatography for clean-up was validated to determine chlorpyrifos, malathion and dichlorvos in cucumber by gas chromatography. For this purpose, homogenized cucumber samples were fortified with pesticides at 0.02 0.2, 0.8 and 1 mg/kg levels. The efficiency and repeatability of the method in extraction and cleanup steps were performed using 14C-carbaryl by radioisotope tracer technique. 14C-carbaryl recoveries after the extraction and cleanup steps were between 92.63-111.73 % with a repeatability of 4.85% (CV) and 74.83-102.22 % with a repeatability of 7.19% (CV), respectively. The homogeneity of analytical samples and the stability of pesticides during homogenization were determined using radio tracer technique and chromatographic methods, respectively.

  4. Method validation and stability study of quercetin in topical emulsions

    Directory of Open Access Journals (Sweden)

    Rúbia Casagrande

    2009-01-01

    Full Text Available This study validated a high performance liquid chromatography (HPLC method for the quantitative evaluation of quercetin in topical emulsions. The method was linear within 0.05 - 200 μg/mL range with a correlation coefficient of 0.9997, and without interference in the quercetin peak. The detection and quantitation limits were 18 and 29 ng/mL, respectively. The intra- and inter-assay precisions presented R.S.D. values lower than 2%. An average of 93% and 94% of quercetin was recovered for non-ionic and anionic emulsions, respectively. The raw material and anionic emulsion, but not non-ionic emulsion, were stable in all storage conditions for one year. The method reported is a fast and reliable HPLC technique useful for quercetin determination in topical emulsions.

  5. Validation of screening method for determination of methyltestosterone in fish

    Directory of Open Access Journals (Sweden)

    Stojkovski Velimir

    2013-07-01

    Full Text Available Anabolic androgenic steroids are synthetic derivatives of testosterone, which is the primary male sex hormone. These anabolic agents are used to increase the weight gain, to improve the food efficiency, storing proteins and to decrease fatness. However, depending on the use of anabolic agent in animal feed, anabolic residues that may occur in meat and meat products present risks to human health. The aim of this study was the validation of screening ELISA method for determination of methyltestoterone anabolic steroid in fish. The validation process was carried out according to Commission Decision 2002/657/EC criteria. The detection limit for methyltestosterone was 140.95 ng/kg and the detection capability was 564.43 ng/kg. The overall recoveries and the coefficients of variation (CV were in the range of 82.4%-97.4% and 1.5%-6.9%, respectively, a working range between 50 to 4050 ng/kg, and the regression equation of the final inhibition curve was: y= -0,1741x + 1,5082, R2 = 0.9927. Because of the good recovery and precision, and satisfactory detection capability, this method is applicable in official control laboratories as a rapid screening method for determination of methyltestosterone in fish.

  6. Simulation Methods and Validation Criteria for Modeling Cardiac Ventricular Electrophysiology.

    Directory of Open Access Journals (Sweden)

    Shankarjee Krishnamoorthi

    Full Text Available We describe a sequence of methods to produce a partial differential equation model of the electrical activation of the ventricles. In our framework, we incorporate the anatomy and cardiac microstructure obtained from magnetic resonance imaging and diffusion tensor imaging of a New Zealand White rabbit, the Purkinje structure and the Purkinje-muscle junctions, and an electrophysiologically accurate model of the ventricular myocytes and tissue, which includes transmural and apex-to-base gradients of action potential characteristics. We solve the electrophysiology governing equations using the finite element method and compute both a 6-lead precordial electrocardiogram (ECG and the activation wavefronts over time. We are particularly concerned with the validation of the various methods used in our model and, in this regard, propose a series of validation criteria that we consider essential. These include producing a physiologically accurate ECG, a correct ventricular activation sequence, and the inducibility of ventricular fibrillation. Among other components, we conclude that a Purkinje geometry with a high density of Purkinje muscle junctions covering the right and left ventricular endocardial surfaces as well as transmural and apex-to-base gradients in action potential characteristics are necessary to produce ECGs and time activation plots that agree with physiological observations.

  7. A General Method of Empirical Q-matrix Validation.

    Science.gov (United States)

    de la Torre, Jimmy; Chiu, Chia-Yi

    2016-06-01

    In contrast to unidimensional item response models that postulate a single underlying proficiency, cognitive diagnosis models (CDMs) posit multiple, discrete skills or attributes, thus allowing CDMs to provide a finer-grained assessment of examinees' test performance. A common component of CDMs for specifying the attributes required for each item is the Q-matrix. Although construction of Q-matrix is typically performed by domain experts, it nonetheless, to a large extent, remains a subjective process, and misspecifications in the Q-matrix, if left unchecked, can have important practical implications. To address this concern, this paper proposes a discrimination index that can be used with a wide class of CDM subsumed by the generalized deterministic input, noisy "and" gate model to empirically validate the Q-matrix specifications by identifying and replacing misspecified entries in the Q-matrix. The rationale for using the index as the basis for a proposed validation method is provided in the form of mathematical proofs to several relevant lemmas and a theorem. The feasibility of the proposed method was examined using simulated data generated under various conditions. The proposed method is illustrated using fraction subtraction data. PMID:25943366

  8. 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.

  9. A vocal-based analytical method for goose behaviour recognition.

    Science.gov (United States)

    Steen, Kim Arild; Therkildsen, Ole Roland; Karstoft, Henrik; Green, Ole

    2012-01-01

    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-linear capabilities 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 a wildlife management system. PMID:22737037

  10. Development and validation of mass spectrometry-based methods for food quality and food safety assessment

    OpenAIRE

    Bignardi, Chiara

    2014-01-01

    In this PhD thesis, analytical chemistry plays a significant role in the assessment of food quality and safety; in particular, three different topics have been addressed to and they are presented into three chapters in which different analytical methodologies have been developed, validated and applied successfully in different topics of food chemistry research. The first chapter is focused on an innovative analytical technique, capillary zone electrophoresis coupled to tandem mass spectrom...

  11. Laboratory diagnostic methods, system of quality and validation

    Directory of Open Access Journals (Sweden)

    Ašanin Ružica

    2005-01-01

    Full Text Available It is known that laboratory investigations secure safe and reliable results that provide a final confirmation of the quality of work. Ideas, planning, knowledge, skills, experience, and environment, along with good laboratory practice, quality control and reliability of quality, make the area of biological investigations very complex. In recent years, quality control, including the control of work in the laboratory, is based on international standards and is used at that level. The implementation of widely recognized international standards, such as the International Standard ISO/IEC 17025 (1 and the implementing of the quality system series ISO/IEC 9000 (2 have become the imperative on the grounds of which laboratories have a formal, visible and corresponding system of quality. The diagnostic methods that are used must constantly yield results which identify the animal as positive or negative, and the precise status of the animal is determined with a predefined degree of statistical significance. Methods applied on a selected population reduce the risk of obtaining falsely positive or falsely negative results. A condition for this are well conceived and documented methods, with the application of the corresponding reagents, and work with professional and skilled staff. This process requires also a consistent implementation of the most rigorous experimental plans, epidemiological and statistical data and estimations, with constant monitoring of the validity of the applied methods. Such an approach is necessary in order to cut down the number of misconceptions and accidental mistakes, for a referent population of animals on which the validity of a method is tested. Once a valid method is included in daily routine investigations, it is necessary to apply constant monitoring for the purpose of internal quality control, in order adequately to evaluate its reproducibility and reliability. Consequently, it is necessary at least twice yearly to conduct

  12. A two-dimensional analytical model and experimental validation of garter stitch knitted shape memory alloy actuator architecture

    International Nuclear Information System (INIS)

    Active knits are a unique architectural approach to meeting emerging smart structure needs for distributed high strain actuation with simultaneous force generation. This paper presents an analytical state-based model for predicting the actuation response of a shape memory alloy (SMA) garter knit textile. Garter knits generate significant contraction against moderate to large loads when heated, due to the continuous interlocked network of loops of SMA wire. For this knit architecture, the states of operation are defined on the basis of the thermal and mechanical loading of the textile, the resulting phase change of the SMA, and the load path followed to that state. Transitions between these operational states induce either stick or slip frictional forces depending upon the state and path, which affect the actuation response. A load–extension model of the textile is derived for each operational state using elastica theory and Euler–Bernoulli beam bending for the large deformations within a loop of wire based on the stress–strain behavior of the SMA material. This provides kinematic and kinetic relations which scale to form analytical transcendental expressions for the net actuation motion against an external load. This model was validated experimentally for an SMA garter knit textile over a range of applied forces with good correlation for both the load–extension behavior in each state as well as the net motion produced during the actuation cycle (250% recoverable strain and over 50% actuation). The two-dimensional analytical model of the garter stitch active knit provides the ability to predict the kinetic actuation performance, providing the basis for the design and synthesis of large stroke, large force distributed actuators that employ this novel architecture. (paper)

  13. Analytical Methods for Environmental Risk Assessment of Acid Sulfate Soils: A Review

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Assessment of acid sulfate soil risk is an important step for acid sulfate soil management and its reliability depends very much on the suitability and accuracy of various analytical methods for estimating sulfide-derived potential acidity, actual acidity and acid-neutralizing capacity in acid sulfate soils. This paper critically reviews various analytical methods that are currently used for determination of the above parameters, as well as their implications for environmental risk assessment of acid sulfate soils.

  14. 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)

  15. Critical node treatment in the analytic function expansion method for Pin Power Reconstruction

    International Nuclear Information System (INIS)

    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)

  16. Joint Monitoring Programme (JMP). Overview of analytical methods employed by JMP in Norway 1981-1987

    OpenAIRE

    Green, N.

    1988-01-01

    Brief descriptions are given of the analytical methods employed by Norway under the Joint Monitoring Programme (JMP) and in cooperation with the International Council for the exploration of the Sea (ICES). Methods concern determination of trace metals and chlorinated hydrocarbons in sea water, sea bed sediment and marine organisms. Included are the detection limits, analytical laborator- ies, and references to the intercalibration exercises that applied to samples collected 1981-86.

  17. Determination of formaldehyde in food and feed by an in-house validated HPLC method.

    Science.gov (United States)

    Wahed, P; Razzaq, Md A; Dharmapuri, S; Corrales, M

    2016-07-01

    Formalin is carcinogenic and is detrimental to public health. The illegal addition of formalin (37% formaldehyde and 14% methanol) to foods to extend their shelf-life is considered to be a common practice in Bangladesh. The lack of accurate methods and the ubiquitous presence of formaldehyde in foods make the detection of illegally added formalin challenging. With the aim of helping regulatory authorities, a sensitive high performance liquid chromatography method was validated for the quantitative determination of formaldehyde in mango, fish and milk. The method was fit-for-purpose and showed good analytical performance in terms of specificity, linearity, precision, recovery and robustness. The expanded uncertainty was <35%. The validated method was applied to screen samples of fruits, vegetables, fresh fish, milk and fish feed collected from different local markets in Dhaka, Bangladesh. Levels of formaldehyde in food samples were compared with published data. The applicability of the method in different food matrices might mean it has potential as a reference standard method. PMID:26920321

  18. Development and validation of HPLC method for quantitative analysis of triamcinolone in biodegradable microparticles

    Directory of Open Access Journals (Sweden)

    A. A. Silva-Júnior

    2009-01-01

    Full Text Available

    A simple, rapid, selective and specific high performance liquid chromatographic (HPLC method for quantitative analysis of the triamcinolone in polylactide-co-glycolide acid (PLGA microparticles was developed. The chromatographic parameters were reversed-phase C18 column, 250mm x 4.6mm, with particle size 5 m. The column oven was thermostated at 35 ºC ± 2 ºC. The mobile phase was methanol/water 45:55 (v/v and elution was isocratic at a flow-rate of 1mL.mL-1. The determinations were performed using a UV-Vis detector at 239 nm. The injected sample volume was 10 µL. The standard curve was linear (r2 > 0.999 in the concentration range 100-2500 ng.mL-1. The method showed adequate precision, with a relative standard deviation (RSD was smaller than 3%. The accuracy was analyzed by adding a standard drug and good recovery values were obtained for all drug concentrations used. The method showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for quantitation of triamcinolone in PLGA microparticles. Keywords: triamcinolone; HPLC analytical method; PLGA microparticles; analytical method validation.

  19. Rapid And Accurate Technique For Measuring N-15 Of Nitrate Method Development, Calibration And Validation

    International Nuclear Information System (INIS)

    A precise and simplified procedure for measuring nitrogen-15 of nitrate in water with moderate ionic strength and moderate to high organic loads is presented. The modified analytical train consists of two main steps: (a) extraction and purification of nitrate from liquid matrix and (b) pyrolysis of purified potassium nitrate. The presented method was evaluated with simulated solutions containing constant amounts of inter-laboratory nitrate standard salt (KNO3 , δ15N = -4.34 ± 0.32 % AirN2) and potentially interfering anions (SO42-, Cl- and HCO3-) as well as dissolved organic carbon (DOC) load. Dowex 1X8 anion exchange resin proved to be a suitable mean and provide accurate and reproducible δ15N values (SD: ± 0.48%).It tolerates high concentrations of chloride and sulfate ions for samples of small volumes (100 ml) of about four folds of the amounts enough to fully saturate the resin column. Rapid, accurate, precise, low-priced and less labour intensive activated graphite based offline pyrolysis technique for measuring N-15 content of nitrate has been developed and implemented. This involves combusting nitrate salt with activated graphite at 550oC for 30 minutes. Dramatic reduction in processing times needed for the analysis of N-15 of nitrate at natural abundance level was achieved. Performance characteristics of the modified analytical cascade showed that 1 to 2 hrs/sample/set of 5 samples processing time is required. The pyrolysis step of the developed method was validated using internationally distributed nitrate stable isotope reference materials. N-15 content of some selected nitrate salts, namely calcium nitrate, sodium nitrate, potassium nitrate and ammonium nitrate fertilizer, was measured using the modified technique, vacuum distillation method, modified ammonia diffusion method, microbial denitrifier method and EA-CF IRMS method at two different laboratories in Egypt and Germany. The results proved the validity and applicability of the modified

  20. Analytic method for geometrical parameter correction of planar HPGe detector

    International Nuclear Information System (INIS)

    A numerical integration formula was introduced to calculate the response of planar HPGe detector to photons emitted from point source. Then the formula was used to correct the geometrical parameter of planar HPGe detector. 241Am and 137Cs point sources were placed at a certain distance (1-20 cm) away from entrance window to get the corresponding detection efficiency. The detection parameters were calculated in weighted least square fitting using the formula with the experimental efficiencies as formula results. This correction method was accurate and timesaving. The simulation result from MCNP using the corrected parameters shows that the relative deviations between simulation and experimental efficiencies are less than 1% for 59.5 and 661.6 keV photons with the distance of 1-20 cm. (authors)