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Sample records for analytical methods validation

  1. 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 ...

  2. 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.

  3. 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.

  4. 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

  5. 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)

  6. 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

  7. Analytical Quality by Design Approach to Test Method Development and Validation in Drug Substance Manufacturing

    Directory of Open Access Journals (Sweden)

    N. V. V. S. S. Raman

    2015-01-01

    Full Text Available Pharmaceutical industry has been emerging rapidly for the last decade by focusing on product Quality, Safety, and Efficacy. Pharmaceutical firms increased the number of product development by using scientific tools such as QbD (Quality by Design and PAT (Process Analytical Technology. ICH guidelines Q8 to Q11 have discussed QbD implementation in API synthetic process and formulation development. ICH Q11 guidelines clearly discussed QbD approach for API synthesis with examples. Generic companies are implementing QbD approach in formulation development and even it is mandatory for USFDA perspective. As of now there is no specific requirements for AQbD (Analytical Quality by Design and PAT in analytical development from all regulatory agencies. In this review, authors have discussed the implementation of QbD and AQbD simultaneously for API synthetic process and analytical methods development. AQbD key tools are identification of ATP (Analytical Target Profile, CQA (Critical Quality Attributes with risk assessment, Method Optimization and Development with DoE, MODR (method operable design region, Control Strategy, AQbD Method Validation, and Continuous Method Monitoring (CMM. Simultaneous implementation of QbD activities in synthetic and analytical development will provide the highest quality product by minimizing the risks and even it is very good input for PAT approach.

  8. 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

  9. 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

  10. 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

  11. 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.

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

    NARCIS (Netherlands)

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

    2016-01-01

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

  13. 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

  14. 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...

  15. 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.

  16. 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.

  17. 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...

  18. 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

  19. 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%.

  20. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR ESTIMATION OF DICLOFENAC SODIUM IN SWAB SAMPLES

    Directory of Open Access Journals (Sweden)

    P.P. Goti, J.J. Savsani and P.B. Patel

    2013-02-01

    Full Text Available The objective of the current study was to develop and validate simple and precise UV Spectrophotometric method for estimation of Diclofenac Sodium in the swab samples to validate cleaning procedure. The swabbing procedure was optimized in order to obtain a suitable recovery from stainless steel surface using Tex wipe polyurethane swab stick. Detection wavelength selected was 267 nm. The proposed method was validated in terms of Linearity, precision, accuracy, limit of detection and limit of quantitation. Linearity was studied over concentration range of 0.5 -3 μg / ml and correlation coefficient was found to be 0.999 for regression line. A recovery obtained was 94.58 %. LOD and LOQ for developed method were found to be 0.014715 µg/ml and 0.044592 µg/ml respectively.

  1. 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.

  2. Development and validation of the analytical method by high performance liquid chromatography (HPLC for Lamotrigine raw material Development and validation of the analytical method by high performance liquid chromatography (HPLC for Lamotrigine raw material

    Directory of Open Access Journals (Sweden)

    Hisao Nishijo

    2011-09-01

    Full Text Available Currently when all roads lead to the pursuit of total quality in production of drugs, it is essential to fully understand each phase of a production process. In this case, validation is the appropriate tool to ensure reliability of a production process involving new equipment and the analytical methodology, either in the pharmaceutical, food, computer, microelectronics area or any other area where the quality of the manufactured product is one of the main reasons for the existence of a given company. This study aimed to analyze the main aspects of the validation of analytical methods for Lamotrigine, new drug for bipolar disorder with wide use today. In conclusion, the proposed analytical method for determination of the lamotrigine content in raw materials is adequate, effective and capable of reproducing reliable results during analysis. This method is fast (running time of 10 minutes, selective, accurate, precise and robust for the determination of the drug, with no observed interfering substances in the optimum wavelength. It could be concluded that this may be a routine method for quality control laboratories to certify the quality of Lamotrigine.Currently when all roads lead to the pursuit of total quality in production of drugs, it is essential to fully understand each phase of a production process. In this case, validation is the appropriate tool to ensure reliability of a production process involving new equipment and the analytical methodology, either in the pharmaceutical, food, computer, microelectronics area or any other area where the quality of the manufactured product is one of the main reasons for the existence of a given company. This study aimed to analyze the main aspects of the validation of analytical methods for Lamotrigine, new drug for bipolar disorder with wide use today. In conclusion, the proposed analytical method for determination of the lamotrigine content in raw materials is adequate, effective and capable of

  3. 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.

  4. 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...

  5. 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.

  6. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR PALM OIL DETERMINATION IN MICROCAPSULES PRODUCED BY COMPLEX COACERVATION

    Directory of Open Access Journals (Sweden)

    Paulo H. M. Marfil

    2016-01-01

    Full Text Available The microencapsulation of palm oil may be a mechanism for protecting and promoting the controlled release of its bioactive compounds. To optimize the microencapsulation process, it is necessary to accurately quantify the palm oil present both external and internal to the microcapsules. In this study, we developed and validated a spectrophotometric method to determine the microencapsulation efficiency of palm oil by complex coacervation. We used gelatin and gum arabic (1:1 as wall material in a 5% concentration (w/v and palm oil in the same concentration. The coacervates were obtained at pH 4.0 ± 0.01, decanted for 24 h, frozen (−40 ºC, and lyophilized for 72 h. Morphological analyzes were then performed. We standardized the extraction of the external palm oil through five successive washes with an organic solvent. We then explored the best method for rupturing the microcapsules. After successive extractions with hexane, we determined the amount of palm oil contained in the microcapsules using a spectrophotometer. The proposed method was shown to be of low cost, fast, and easy to implement. In addition, in the validation step, we confirmed the method to be safe and reliable, as it proved to be specific, accurate, precise, and robust.

  7. 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.

  8. 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

  9. 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.

  10. 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

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

    Science.gov (United States)

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

    2012-08-31

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

  12. Validation of an HPLC analytical method coupled to a multifunctional clean-up column for the determination of deoxynivalenol.

    Science.gov (United States)

    Sugita-Konsihi, Yoshiko; Tanaka, Toshitsugu; Tabata, Setsuko; Nakajima, Masahiro; Nouno, Masanori; Nakaie, Yoko; Chonan, Takao; Aoyagi, Mitsutoshi; Kibune, Nobuyuki; Mizuno, Kazutoshi; Ishikuro, Eiichi; Kanamaru, Naoki; Minamisawa, Masatoshi; Aita, Norio; Kushiro, Masayo; Tanaka, Kenji; Takatori, Kosuke

    2006-04-01

    To evaluate a method using a multifunctional clean-up column coupled with high performance liquid chromatography as an official analytical method for the determination of deoxynivalenol in wheat used as food or feed, an inter-laboratory study was performed in 12 laboratories using four naturally contaminated wheat samples and one spiked sample. The relative standard deviations for repeatability (RSDr) and reproducibility (RSDR) of naturally contaminated wheat were in the range 5.8-11.3% and 12.0-20.7%, respectively. The HORRAT was less than 1.0 in each sample. From the spiking test, the recovery rate, RSDr, RSDR and HORRAT value were 100.0%, 11.2%, 10.3% and 0.5, respectively. The limit of quantification is 0.10 mg/kg from the range obtained in a linear calibration. Thus, it should be useful as a sensitive and validated analytical method for the determination of deoxynivalenol in wheat intended for use in food and feed.

  13. 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

  14. 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)

  15. 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...

  16. Validation of selected analytical methods using accuracy profiles to assess the impact of a Tobacco Heating System on indoor air quality.

    Science.gov (United States)

    Mottier, Nicolas; Tharin, Manuel; Cluse, Camille; Crudo, Jean-René; Lueso, María Gómez; Goujon-Ginglinger, Catherine G; Jaquier, Anne; Mitova, Maya I; Rouget, Emmanuel G R; Schaller, Mathieu; Solioz, Jennifer

    2016-09-01

    Studies in environmentally controlled rooms have been used over the years to assess the impact of environmental tobacco smoke on indoor air quality. As new tobacco products are developed, it is important to determine their impact on air quality when used indoors. Before such an assessment can take place it is essential that the analytical methods used to assess indoor air quality are validated and shown to be fit for their intended purpose. Consequently, for this assessment, an environmentally controlled room was built and seven analytical methods, representing eighteen analytes, were validated. The validations were carried out with smoking machines using a matrix-based approach applying the accuracy profile procedure. The performances of the methods were compared for all three matrices under investigation: background air samples, the environmental aerosol of Tobacco Heating System THS 2.2, a heat-not-burn tobacco product developed by Philip Morris International, and the environmental tobacco smoke of a cigarette. The environmental aerosol generated by the THS 2.2 device did not have any appreciable impact on the performances of the methods. The comparison between the background and THS 2.2 environmental aerosol samples generated by smoking machines showed that only five compounds were higher when THS 2.2 was used in the environmentally controlled room. Regarding environmental tobacco smoke from cigarettes, the yields of all analytes were clearly above those obtained with the other two air sample types.

  17. Validation of a UV-spectrophotometric analytical method for determination of LPSF/AC04 from inclusion complex and liposomes

    Directory of Open Access Journals (Sweden)

    Rafaela Siqueira Ferraz

    2015-03-01

    Full Text Available The aim of this study was to develop and validate a UV spectrophotometric method for determination of LPSF/AC04 from inclusion complex and encapsulated into liposomes. The validation parameters were determined according to the International Conference on Harmonisation (ICH and National Health Surveillance Agency (ANVISA guidelines. LPSF/AC04 was determined at 250 nm in methanol by a UV spectrophotometric method, exhibiting linearity in the range from 0.3 to 2 µg.mL−1 (Absorbance=0.18068 x [LPSF/AC04 µg.mL-1] + 0.00348, (r2=0.9995. The limits of detection and quantification were 0.047µg.mL−1 and 0.143µg.mL−1, respectively. The method was accurate, precise, reproducible and robust since all the samples analyzed had coefficient of variation of less than 5% and no statistically significant difference between theoretical and practical concentrations was detected. Thus, a rapid, simple, low cost and sensitive spectrophotometric method was developed and validated for determining the content of inclusion complex and liposomes containing LPSF/AC04.

  18. 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

  19. 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)

  20. 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.

  1. Occupational exposure to polycyclic aromatic hydrocarbons in airborne particulate matter: validation and application of a gas chromatography-mass spectrometry analytical method.

    Science.gov (United States)

    Fioretti, Marzia; Catrambone, Tamara; Gordiani, Andrea; Cabella, Renato

    2010-12-01

    This study concerns the validation of an analytical method for the measurement of occupational exposure to trace levels of polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matter (APM). Personal exposure to selected PAHs of five workers occupationally exposed to urban pollution in Rome, Italy, was evaluated. The samples were collected over 10 days evenly distributed during winter and summer of 2008. Polycyclic aromatic hydrocarbons were collected by a sampling pump and trapped in polytetrafluoroethylene filters; ultrasonic extraction was applied to extract PAH species from the matrix with toluene, and the concentrated extract was quantitatively analyzed by GC/MS. The analytical method was optimized and validated using a standard reference material of urban dust (SRM 1649a). Detection limits ranged from 0.8 ng per sample for indeno [1,2,3-cd] pyrene to 20.4 ng for sample for anthracene. Experimental results of the 50 personal samples collected showed that phenanthrene was the predominant polycyclic aromatic hydrocarbon [95% CI (32.42-41.13 ng m(-3))]; the highest benzo[a]pyrene concentration was 2.58 ng m(-3), approximately 2-fold higher than European annual target values (1 ng m(-3)). Seasonal variations of personal exposure to selected PAHs suggested higher emissions and reduced atmospheric reactivity of PAH compounds in winter. The analytical method was a suitable procedure for the determination of 13 of the 16 priority PAHs in APM personal samples and can be considered a useful tool to evaluate occupational exposure to low PAH levels.

  2. An evaluation of 25B-, 25C-, 25D-, 25H-, 25I- and 25T2-NBOMe via LC-MS-MS: method validation and analyte stability.

    Science.gov (United States)

    Johnson, Robert D; Botch-Jones, Sabra R; Flowers, Tiffany; Lewis, Connie A

    2014-10-01

    As potent serotonin (5-HT2A) receptor agonists, the NBOMe class of drugs including 25B-, 25C-, 25D-, 25H-, 25I- and 25T2-NBOMe is frequently abused due to the intense hallucinations that they induce. From the limited literature available, the concentration of these NBOMe compounds reported in postmortem cases is exceedingly low. In most instances, published concentrations are NBOMe, evaluation of 25B-, 25C-, 25D-, 25H and 25T2- in whole blood, plasma and urine was conducted. This publication presents the data obtained from the validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of these six NBOMe analogs. The method utilizes ultra-performance liquid chromatography technology for the separation followed by positive electrospray ionization of each analog. Limits of quantification for these analogs ranged from 0.01 to 0.02 ng/mL (10-20 pg/mL) with typical linear dynamic ranges of 0.01-20 ng/mL. Data for recovery, intraday control accuracy and precision, matrix effects, ion suppression/enhancement and analyte stability are included. Validation was completed in whole blood, plasma and urine. Short run times and high sensitivity afforded by this newly validated analytical method that allows for the detection of these six analogs in the most common toxicological matrices and can be applied to both ante- and postmortem specimens.

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

    Directory of Open Access Journals (Sweden)

    Gunetti Monica

    2012-05-01

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

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

    Science.gov (United States)

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

    2015-09-01

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

  5. 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.

  6. RP-HPLC Analytical Method Development and Validation for Simultaneous Estimation of Three Drugs: Glimepiride, Pioglitazone, and Metformin and Its Pharmaceutical Dosage Forms

    Directory of Open Access Journals (Sweden)

    Gadapa Nirupa

    2013-01-01

    Full Text Available Developing a single analytical method for estimation of individual drug from a multidrug composition is a very challenging task. A simple, rapid, precise, and reliable reverse phase HPLC method was developed for the separation and estimation of three drugs glimepiride, pioglitazone and metformin in bulk drug mix and pharmaceutical dosage forms. The estimation was carried out using Inertsil ODS-3V (250 mm × 4.6 mm, 5 μm column; mobile phase consisting of acetonitrile, tetrahydrofuran, and buffer at pH 5; the flow rate of 1.7 mL/min and ultraviolet detection at 228 nm. All the three drugs were properly resolved having run time of 5 minutes, 3.9 minutes and 1.3 minutes for glimepiride, pioglitazone, and metformin, respectively. The method was validated as a final verification of method development with respect to precision, linearity, accuracy, ruggedness, and robustness. The validated method was successfully applied to the commercially available pharmaceutical dosage form, yielding very good and reproducible result.

  7. Development and validation of an HPLC-MS/MS method to quantify clopidogrel acyl glucuronide, clopidogrel acid metabolite, and clopidogrel in plasma samples avoiding analyte back-conversion.

    Science.gov (United States)

    Silvestro, Luigi; Gheorghe, Mihaela; Iordachescu, Adriana; Ciuca, Valentin; Tudoroniu, Ariana; Rizea Savu, Simona; Tarcomnicu, Isabela

    2011-08-01

    A new sensitive and fast quantitative analytical method for the simultaneous determination of clopidogrel, its main metabolite clopidogrel carboxylic acid, and the newly described acyl glucuronide metabolite, in human plasma samples, is presented. The analytical procedures (plasma storage, handling, and extract storage in the autosampler) were optimized in order to avoid back-conversion; a known drawback in measurements of clopidogrel. Clopidogrel acyl glucuronide was confirmed as a major source of back-conversion to the parent drug in the presence of methanol, and thorough stability experiments were carried out to find the most appropriate conditions for an accurate analysis of clopidogrel and the two metabolites. The method was validated by assessing selectivity, sensitivity, linearity, accuracy, and precision for all three analytes, in accordance to Food and Drug Administration guidelines. Spiked quality controls in plasma as well as incurred samples were used to verify back-conversion in the selected conditions, with results meeting European Medicines Agency acceptance criteria (concentrations within 80-120% of the first reading). The method was then applied to a pharmacokinetic study, and for the first time, a pharmacokinetic curve of clopidogrel acyl glucuronide in human plasma is presented. The concentrations ranged up to 1,048.684 ng/mL, with a mean of 470.268 ng/mL, while clopidogrel had a mean C(max) of 1.348 ng/mL; these orders of magnitude show how much the back-conversion of this metabolite may influence clopidogrel quantification if it is not properly controlled.

  8. 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

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

    Science.gov (United States)

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

    2015-01-05

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

  10. 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

  11. 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

  12. 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- ...

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. 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

  18. 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)

  19. 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...

  20. 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...

  1. 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.

  2. 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.

  3. 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...

  4. 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...

  5. 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

  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. 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...

  8. Validation of an Analytical Method for Determination of Benzo[a]pyrene Bread using QuEChERS Method by GC-MS.

    Science.gov (United States)

    Eslamizad, Samira; Yazdanpanah, Hassan; Javidnia, Katayon; Sadeghi, Ramezan; Bayat, Mitra; Shahabipour, Sara; Khalighian, Najmeh; Kobarfard, Farzad

    2016-01-01

    A fast and simple modified QuEChERS (quick, easy, cheap, rugged and safe) extraction method based on spiked calibration curves and direct sample introduction was developed for determination of Benzo [a] pyrene (BaP) in bread by gas chromatography-mass spectrometry single quadrupole selected ion monitoring (GC/MS-SQ-SIM). Sample preparation includes: extraction of BaP into acetone followed by cleanup with dispersive solid phase extraction. The use of spiked samples for constructing the calibration curve substantially reduced adverse matrix-related effects. The average recovery of BaP at 6 concentration levels was in range of 95-120%. The method was proved to be reproducible with relative standard deviation less than 14.5% for all of the concentration levels. The limit of detection and limit of quantification were 0.3 ng/g and 0.5 ng/g, respectively. Correlation coefficient of 0.997 was obtained for spiked calibration standards over the concentration range of 0.5-20 ng/g. To the best of our knowledge, this is the first time that a QuEChERS method is used for the analysis of BaP in breads. The developed method was used for determination of BaP in 29 traditional (Sangak) and industrial (Senan) bread samples collected from Tehran in 2014. These results showed that two Sangak samples were contaminated with BaP. Therefore, a comprehensive survey for monitoring of BaP in Sangak bread samples seems to be needed. This is the first report concerning contamination of bread samples with BaP in Iran. PMID:27642317

  9. 7 CFR 98.4 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to.... Army Individual Protection Directorate's Military Specifications, approved analytical test...

  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. 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

  12. 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...

  13. 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

  14. Implementation of QbD Approach to the Analytical Method Development and Validation for the Estimation of Propafenone Hydrochloride in Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    Monika L. Jadhav

    2013-01-01

    Full Text Available Chromatographic and spectrophotometric methods were developed according to Quality by Design (QbD approach as per ICH Q8(R2 guidelines for estimation of propafenone hydrochloride in tablet dosage form. QbD approach was carried out by varying various parameters and these variable parameters were designed into Ishikawa diagram. The critical parameters were determined by using principal component analysis as well as by observation. Estimated critical parameters in HPTLC method include solvent methanol, mode of detection absorbance, precoated aluminium backed TLC plate (10 cm 10 cm, wavelength: 250 nm, saturation time: 20 min, band length: 8 mm, solvent front: 70 mm, volume of mobile phase: 5 mL, type of chamber: 10 cm 10 cm, scanning time: 10 min, and mobile phase methanol : ethyl acetate : triethylamine (1.5 : 3.5 : 0.4 v/v/v. Estimated critical parameters in zero order spectrophotometric method were solvent methanol, sample preparation tablet, wavelength: 247.4 nm, slit width: 1.0, scan speed medium, and sampling interval: 0.2, and for first order derivative spectrophotometric method it was scaling factor: 5 and delta lambda 4. The above methods were validated according to ICH Q2(R1 guidelines. Proposed methods can be used for routine analysis of propafenone hydrochloride in tablet dosage form as they were found to be robust and specific.

  15. 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... Analytical Methods Manual, American Spice Trade Association (ASTA), 560 Sylvan Avenue, P.O. Box...

  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. 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

  18. 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 Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Standards... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical...

  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 ESI-LC-MS/MS method for simultaneous identification and quantification of 24 analytes of forensic relevance in vitreous humour, whole blood and plasma.

    Science.gov (United States)

    Arora, Beauty; Velpandian, Thirumurthy; Saxena, Rohit; Lalwani, Sanjeev; Dogra, T D; Ghose, Supriyo

    2016-01-01

    Detection and quantification of drugs from various biological matrices are of immense importance in forensic toxicological analysis. Despite the various reported methods, development of a new method for the detection and quantification of drugs is still an active area of research. However, every method and biological matrix has its own limitation, which further encourage forensic toxicologists to develop new methods and to explore new matrices for the analysis of drugs. In this study, an electrospray ionization-liquid chromatograph-tandem mass spectrometry (ESI-LC-MS/MS) method is developed and validated for simultaneous identification and quantification of 24 drugs of forensic relevance in various body fluids, namely, whole blood, plasma and vitreous humour. The newly developed method has been validated for intra-day and inter-day accuracy, precision, selectivity and sensitivity. Absolute recovery shows a mean of 84.5, 86.2, and 103% in the vitreous humour, whole blood and plasma respectively, which is suitable for the screening procedure. Further, the absolute matrix effect (AME) shows a mean of 105, 96.5, and 109% in the vitreous humour, whole blood and plasma, respectively. In addition, to examine the practical utility of this method, it has been applied for screening of drugs in post-mortem samples of the vitreous humour, whole blood and plasma collected at autopsy from ten cadavers. Experimental results show that the newly developed method is well applicable for screening of analytes in all the three matrices.

  1. 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

  2. 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.

  3. 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.

  4. 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...... of severity. In an example, the results of traditional FMEA of a Near Infrared (NIR) analytical procedure used for the screening of suspected counterfeited tablets are re-interpretated by this probabilistic modification of FMEA. Using this probabilistic modification of FMEA, the frequency of occurrence...... of undetected failure mode(s) can be estimated quantitatively, for each individual failure mode, for a set of failure modes, and the full analytical procedure....

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

    Science.gov (United States)

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

    2015-08-15

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

  6. 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 ...

  7. 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 Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Standards... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The...

  8. 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...

  9. 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 141.89 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Control of Lead and Copper § 141.89 Analytical methods....

  10. 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

  11. 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.

  12. 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.

  13. 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

  14. A New Method to Study Analytic Inequalities

    Directory of Open Access Journals (Sweden)

    Xiao-Ming Zhang

    2010-01-01

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

  15. Determination of total iodine in serum and urine samples by ion chromatography with pulsed amperometric detection - studies on analyte loss, optimization of sample preparation procedures, and validation of analytical method.

    Science.gov (United States)

    Błażewicz, Anna; Klatka, Maria; Dolliver, Wojciech; Kocjan, Ryszard

    2014-07-01

    A fast, accurate and precise ion chromatography method with pulsed amperometric detection was applied to evaluate a variety of parameters affecting the determination of total iodine in serum and urine of 81 subjects, including 56 obese and 25 healthy Polish children. The sample pretreatment methods were carried out in a closed system and with the assistance of microwaves. Both alkaline and acidic digestion procedures were developed and optimized to find the simplest combination of reagents and the appropriate parameters for digestion that would allow for the fastest, least time consuming and most cost-effective way of analysis. A good correlation between the certified and the measured concentrations was achieved. The best recoveries (96.8% for urine and 98.8% for serum samples) were achieved using 1ml of 25% tetramethylammonium hydroxide solution within 6min for 0.1ml of serum/urine samples. Using 0.5ml of 65% nitric acid solution the best recovery (95.3%) was obtained when 7min of effective digestion time was used. Freeze-thaw stability and long-term stability were checked. After 24 weeks 14.7% loss of iodine in urine, and 10.9% in serum samples occurred. For urine samples, better correlation (R(2)=0.9891) of various sample preparation procedures (alkaline digestion and application of OnGuard RP cartidges) was obtained. Significantly lower iodide content was found in samples taken from obese children. Serum iodine content in obese children was markedly variable in comparison with the healthy group, whereas the difference was less evident when urine samples were analyzed. The mean content in serum was 59.12±8.86μg/L, and in urine 98.26±25.93 for obese children when samples were prepared by the use of optimized alkaline digestion reinforced by microwaves. In healthy children the mean content in serum was 82.58±6.01μg/L, and in urine 145.76±31.44μg/L.

  16. Prioritizing pesticide compounds for analytical methods development

    Science.gov (United States)

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

    2012-01-01

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

  17. 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.

  18. 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.

  19. Analytical and computational methods in electromagnetics

    CERN Document Server

    Garg, Ramesh

    2008-01-01

    This authoritative resource offers you clear and complete explanation of this essential electromagnetics knowledge, providing you with the analytical background you need to understand such key approaches as MoM (method of moments), FDTD (Finite Difference Time Domain) and FEM (Finite Element Method), and Green's functions. This comprehensive book includes all math necessary to master the material.

  20. 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

  1. 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.

  2. An inverse and analytic lens design method

    OpenAIRE

    Lu, Yang; Lakshminarayanan, Vasudevan

    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 ...

  3. 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

  4. 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

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

    Science.gov (United States)

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

    2013-08-01

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

  6. 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...

  7. 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

  8. 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.

  9. On Analytical Methods in Neuroblastoma Detection

    Directory of Open Access Journals (Sweden)

    R. Martínez-Díaz

    2013-01-01

    quantitative and consistent methods of evaluation are needed to assess reponse to patient therapy. Whole-body I123-metaiodobenzylguanidine (mIBG scintigraphy is used as primary medical image modality to detect neuroblastoma tumours due to its high specificity and sensitivity. However, current oncological guidelines are based on qualitative observer-dependent analysis. This fact makes it difficult to compare results of scintigraphies taken at different moments during therapy or at different institutions. In this paper, we review analytical methods used in neuroblastoma detection and propose an observer-independent method to quantitatively analyse a I123-mIBG scintigraphy.

  10. Algorithmic and analytical methods in network biology.

    Science.gov (United States)

    Koyutürk, Mehmet

    2010-01-01

    During the genomic revolution, algorithmic and analytical methods for organizing, integrating, analyzing, and querying biological sequence data proved invaluable. Today, increasing availability of high-throughput data pertaining to functional states of biomolecules, as well as their interactions, enables genome-scale studies of the cell from a systems perspective. The past decade witnessed significant efforts on the development of computational infrastructure for large-scale modeling and analysis of biological systems, commonly using network models. Such efforts lead to novel insights into the complexity of living systems, through development of sophisticated abstractions, algorithms, and analytical techniques that address a broad range of problems, including the following: (1) inference and reconstruction of complex cellular networks; (2) identification of common and coherent patterns in cellular networks, with a view to understanding the organizing principles and building blocks of cellular signaling, regulation, and metabolism; and (3) characterization of cellular mechanisms that underlie the differences between living systems, in terms of evolutionary diversity, development and differentiation, and complex phenotypes, including human disease. These problems pose significant algorithmic and analytical challenges because of the inherent complexity of the systems being studied; limitations of data in terms of availability, scope, and scale; intractability of resulting computational problems; and limitations of reference models for reliable statistical inference. This article provides a broad overview of existing algorithmic and analytical approaches to these problems, highlights key biological insights provided by these approaches, and outlines emerging opportunities and challenges in computational systems biology.

  11. 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...

  12. 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.

  13. 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

  14. Pioglitazone:A review of analytical methods

    Institute of Scientific and Technical Information of China (English)

    N. Satheeshkumar; S. Shantikumar; R. Srinivas

    2014-01-01

    Pioglitazone is an oral anti-hyperglycemic agent. It is used for the treatment of diabetes mellitus type 2. It selectively stimulates nuclear receptor peroxisome proliferator-activated receptor gamma (PPAR-gamma). It was the tenth-best-selling drug in the U.S. in 2008. This article examines published analytical methods reported so far in the literature for the determination of pioglitazone in biological samples and pharmaceutical formulations. They include various techniques like electrochemical methods, spectrophotometry, capillary electrophoresis, high-performance liquid chromatography, liquid chromatography-electrospray ionization-tandem mass spectrometry and high-performance thin layer chromatography.

  15. 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.

  16. Big data analytics methods and applications

    CERN Document Server

    Rao, BLS; Rao, SB

    2016-01-01

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

  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

    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

  19. 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.

  20. 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.

  1. 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

  2. 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.)

  3. 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.

  4. 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

  5. 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...

  6. 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.

  7. Youden test application in robustness assays during method validation.

    Science.gov (United States)

    Karageorgou, Eftichia; Samanidou, Victoria

    2014-08-01

    Analytical method validation is a vital step following method development for ensuring reliable and accurate method performance. Among examined figures of merit, robustness/ruggedness study allows us to test performance characteristics of the analytical process when operating conditions are altered either deliberately or not. This study yields useful information, being a fundamental part of method validation. Since many experiments are required, this step is high demanding in time and consumables. In order to avoid the difficult task of performing too many experiments the Youden test which makes use of fractional factorial designs and has been proved to be a very effective approach. The main advantage of Youden test is the fact that it keeps the required time and effort to a minimum, since only a limited number of determinations have to be made, using combinations of the chosen investigated factors. Typical applications of this robustness test found in literature covering a wide variety of sample matrices are briefly discussed in this review.

  8. 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...

  9. 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...

  10. 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...... above the 90th percentile of RPN values as failure modes needing urgent corrective action; failure modes falling between the 75th and 90th percentile of RPN values were identified as failure modes needing necessary corrective action, respectively. Team 1 and Team 2 identified five and six failure modes...

  11. 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.

  12. 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

  13. 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

  14. 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.

  15. 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...

  16. 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.

  17. 清洁效果验证中硫酸卷曲霉素残留量分析方法建立%Establishment of Analytical Method of Capreomycin Sulfate Residual in Cleaning Effect validation

    Institute of Scientific and Technical Information of China (English)

    韦翠; 彭志兴

    2013-01-01

    The cleaning effect of packaging machine needed essential validation in the sterile separation packed process of capreo-mycin sulfate for injection. The residue of the active substance in final rinse water of cleaning validation were determined by HPLC on the column C18 with elution (flow rate: 1.0mL/min), 0.016mol/L hexane sodium solution-methanol-acetonitrile-acetic acid (70∶25∶25∶2,v/v) mixture as mobile phase, UV detection at 254nm. The results showed that suitability, linearity and precision of cleaning validation systemmeet met the analysis demand of the active substance. The method could be applied to the detection of ca-preomycin cleaning effect validation of neomycin residues.%  注射用硫酸卷曲霉素无菌分装过程需要对分装机清洁效果进行验证,本文利用高效液相色谱法对清洁验证最终淋洗水中硫酸卷曲霉素残留量进行检测。色谱条件:以C18色谱柱为固定相,以0.016mol·L-1己烷磺酸钠溶液-甲醇-乙腈-冰醋酸(70∶25∶25∶2,v/v)为流动相,流速为1mL·min-1,紫外检测波长254nm,柱温为常温。结果表明,该方法系统适用性、线性、精密度均符合清洁验证活性物质检测方法要求,可用于清洁效果验证中硫酸卷曲霉素残留量的检测。

  18. 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.)

  19. 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.

  20. Numerical-Analytical Method for Magnetic Field Computation in Rotational Electric Machines

    Institute of Scientific and Technical Information of China (English)

    章跃进; 江建中; 屠关镇

    2003-01-01

    A numerical-analytical method is applied for the two-dimensional magnetic field computation in rotational electric machines in this paper. The analytical expressions for air gap magnetic field axe derived. The pole pairs in the expressions are taken into account so that the solution region can be reduced within one periodic range. The numerical and analytical magnetic field equations are linked with equal vector magnetic potential boundary conditions. The magnetic field of a brushless permanent magnet machine is computed by the proposed method. The result is compared to that obtained by finite element method so as to validate the correction of th method.

  1. 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...

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Analytical methods for heat transfer and fluid flow problems

    CERN Document Server

    Weigand, Bernhard

    2015-01-01

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

  7. 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

  8. 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...

  9. 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...

  10. 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...

  11. 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

  12. 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

  13. Some analytical methods for explosives: Part 2

    Energy Technology Data Exchange (ETDEWEB)

    Selig, W.

    1965-12-08

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

  14. 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

  15. 7 CFR 91.23 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... are used. The manuals of standard methods most often used by the Science and Technology laboratories... Identification of Enterobacteriaceae, Elsevier Science, Inc., Regional Sales Office, 655 Avenue of the Americas... Methods for the Examination of Dairy Products, American Public Health Association, 1015 Fifteenth...

  16. Learner Language Analytic Methods and Pedagogical Implications

    Science.gov (United States)

    Dyson, Bronwen

    2010-01-01

    Methods for analysing interlanguage have long aimed to capture learner language in its own right. By surveying the cognitive methods of Error Analysis, Obligatory Occasion Analysis and Frequency Analysis, this paper traces reformulations to attain this goal. The paper then focuses on Emergence Analysis, which fine-tunes learner language analysis…

  17. 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 ...

  18. 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

  19. 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

  20. 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.

  1. 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)...

  2. 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

  3. 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)

  4. 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

  5. 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

  6. 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.

  7. 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)

  8. 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.

  9. Assessment of Two Analytical Methods in Solving the Linear and Nonlinear Elastic Beam Deformation Problems

    DEFF Research Database (Denmark)

    Barari, Amin; Ganjavi, B.; Jeloudar, M. Ghanbari;

    2010-01-01

    boundary value problems, but also are used as mathematical models in viscoelastic and inelastic flows. The purpose of this paper is to present the application of the homotopy-perturbation method (HPM) and variational iteration method (VIM) to solve some boundary value problems in structural engineering...... and fluid mechanics. Design/methodology/approach – Two new but powerful analytical methods, namely, He's VIM and HPM, are introduced to solve some boundary value problems in structural engineering and fluid mechanics. Findings – Analytical solutions often fit under classical perturbation methods. However....... Furthermore, the approximate solutions solved by the perturbation methods are valid, in most cases, only for the small values of the parameters. In the present study, two powerful analytical methods HPM and VIM have been employed to solve the linear and nonlinear elastic beam deformation problems. The results...

  10. Relativistic mirrors in laser plasmas (analytical methods)

    Science.gov (United States)

    Bulanov, S. V.; Esirkepov, T. Zh; Kando, M.; Koga, J.

    2016-10-01

    Relativistic flying mirrors in plasmas are realized as thin dense electron (or electron-ion) layers accelerated by high-intensity electromagnetic waves to velocities close to the speed of light in vacuum. The reflection of an electromagnetic wave from the relativistic mirror results in its energy and frequency changing. In a counter-propagation configuration, the frequency of the reflected wave is multiplied by the factor proportional to the Lorentz factor squared. This scientific area promises the development of sources of ultrashort x-ray pulses in the attosecond range. The expected intensity will reach the level at which the effects predicted by nonlinear quantum electrodynamics start to play a key role. We present an overview of theoretical methods used to describe relativistic flying, accelerating, oscillating mirrors emerging in intense laser-plasma interactions.

  11. Analysis of selected prioritization methods in the analytic hierarchy process

    Science.gov (United States)

    Jablonsky, J.

    2015-06-01

    A crucial problem in the analytic hierarchy process (or its extension analytic network process) deriving priorities form pairwise comparison matrices. The most popular methods for deriving priorities are eigenvector method, which is originally proposed by Saaty[5], logarithmic least square method, and least square method. The paper deals with other alternative approaches using goal programming methodology - one of them is based on minimization of sum of absolute or relative deviations and the other one on minimization of maximum deviation. The results of methods are compared on a set of randomly generated matrices of different sizes and consistency levels.

  12. 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.

  13. 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

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

    Science.gov (United States)

    Anubala, S; Sekar, R; Nagaiah, K

    2014-06-01

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

  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. 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...

  17. 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)

  18. Analytical methods for quantitation of prenylated flavonoids from hops.

    Science.gov (United States)

    Nikolić, Dejan; van Breemen, Richard B

    2013-01-01

    The female flowers of hops (Humulus lupulus L.) are used as a flavoring agent in the brewing industry. There is growing interest in possible health benefits of hops, particularly as estrogenic and chemopreventive agents. Among the possible active constituents, most of the attention has focused on prenylated flavonoids, which can chemically be classified as prenylated chalcones and prenylated flavanones. Among chalcones, xanthohumol (XN) and desmethylxanthohumol (DMX) have been the most studied, while among flavanones, 8-prenylnaringenin (8-PN) and 6-prenylnaringenin (6-PN) have received the most attention. Because of the interest in medicinal properties of prenylated flavonoids, there is demand for accurate, reproducible and sensitive analytical methods to quantify these compounds in various matrices. Such methods are needed, for example, for quality control and standardization of hop extracts, measurement of the content of prenylated flavonoids in beer, and to determine pharmacokinetic properties of prenylated flavonoids in animals and humans. This review summarizes currently available analytical methods for quantitative analysis of the major prenylated flavonoids, with an emphasis on the LC-MS and LC-MS-MS methods and their recent applications to biomedical research on hops. This review covers all methods in which prenylated flavonoids have been measured, either as the primary analytes or as a part of a larger group of analytes. The review also discusses methodological issues relating to the quantitative analysis of these compounds regardless of the chosen analytical approach. PMID:24077106

  19. 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

  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;

    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. 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

  2. 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 ...

  3. 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.

  4. 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.

  5. Space Suit Joint Torque Measurement Method Validation

    Science.gov (United States)

    Valish, Dana; Eversley, Karina

    2012-01-01

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

  6. 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

  7. 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

  8. 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.

  9. 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.

  10. Analytical chemistry methods for metallic core components: Revision March 1985

    Energy Technology Data Exchange (ETDEWEB)

    1985-03-01

    This standard provides analytical chemistry methods for the analysis of alloys used to fabricate core components. These alloys are 302, 308, 316, 316-Ti, and 321 stainless steels and 600 and 718 Inconels and they may include other 300-series stainless steels.

  11. 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.

  12. 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 ...

  13. 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

  14. 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.

  15. Recent developments in detection methods for microfabricated analytical devices.

    Science.gov (United States)

    Schwarz, M A; Hauser, P C

    2001-09-01

    Sensitive detection in microfluidic analytical devices is a challenge because of the extremely small detection volumes available. Considerable efforts have been made lately to further address this aspect and to investigate techniques other than fluorescence. Among the newly introduced techniques are the optical methods of chemiluminescence, refraction and thermooptics, as well as the electrochemical methods of amperometry, conductimetry and potentiometry. Developments are also in progress to create miniaturized plasma-emission spectrometers and sensitive detectors for gas-chromatographic separations.

  16. 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...

  17. Development and validation of the analytical method by high performance liquid chromatography (HPLC for Lamotrigine raw material = Desenvolvimento e validação do método analítico por cromatografia líquida de alta eficiência (CLAE para a matéria prima Lamotrigina

    Directory of Open Access Journals (Sweden)

    Guilherme Nobre Lima do Nascimento

    2011-07-01

    Full Text Available Currently when all roads lead to the pursuit of total quality in production of drugs, it is essential to fully understand each phase of a production process. In this case, validation is the appropriate tool to ensure reliability of a production process involving new equipment and the analytical methodology, either in the pharmaceutical, food, computer, microelectronics area or any other area where the quality of the manufactured product is one of the main reasons for the existence of a given company. This study aimed to analyze the main aspects of the validation of analytical methods for Lamotrigine, new drug for bipolar disorder with wide use today. In conclusion, the proposed analytical method for determination of the lamotrigine content in raw materials is adequate, effective and capable of reproducing reliable results during analysis. This method is fast (running time of 10 minutes, selective, accurate, precise and robust for the determination of the drug, with no observedinterfering substances in the optimum wavelength. It could be concluded that this may be a routine method for quality control laboratories to certify the quality of Lamotrigine. Atualmente quando todos os caminhos levam à busca da qualidade total na produção de medicamentos, 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 novo e, inclusive, da metodologia analítica, seja do setor farmacêutico, alimentício, informática microeletrônico ou qualquer outra área onde a qualidade do produto fabricado é uma das principais razões da existência da empresa. O presente trabalho teve por objetivo analisar os principais aspectos da validação de métodos analíticos para Lamotrigina, fármaco novo para transtorno bipolar com amplo usoatualmente. Em conclusão, o método analítico proposto para determina

  18. 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.

  19. 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

  20. 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.

  1. 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...

  2. 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.

  3. Dynamic buckling analysis of delaminated composite plates using semi-analytical finite strip method

    Science.gov (United States)

    Ovesy, H. R.; Totounferoush, A.; Ghannadpour, S. A. M.

    2015-05-01

    The delamination phenomena can become of paramount importance when the design of the composite plates is concerned. In the current study, the effect of through-the-width delamination on dynamic buckling behavior of a composite plate is studied by implementing semi-analytical finite strip method. In this method, the energy and work integrations are computed analytically due to the implementation of trigonometric functions. Moreover, the method can lead to converged results with comparatively small number of degrees of freedom. These features have made the method quite efficient. To account for delamination effects, displacement field is enriched by adding appropriate terms. Also, the penetration of the delamination surfaces is prevented by incorporating an appropriate contact scheme into the time response analysis. Some selected results are validated against those available in the literature.

  4. 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...

  5. 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.

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

    Institute of Scientific and Technical Information of China (English)

    Basavaiah Kanakapura n; Vamsi Krishna Penmatsa

    2016-01-01

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

  7. 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.

  8. Customizing computational methods for visual analytics with big data.

    Science.gov (United States)

    Choo, Jaegul; Park, Haesun

    2013-01-01

    The volume of available data has been growing exponentially, increasing data problem's complexity and obscurity. In response, visual analytics (VA) has gained attention, yet its solutions haven't scaled well for big data. Computational methods can improve VA's scalability by giving users compact, meaningful information about the input data. However, the significant computation time these methods require hinders real-time interactive visualization of big data. By addressing crucial discrepancies between these methods and VA regarding precision and convergence, researchers have proposed ways to customize them for VA. These approaches, which include low-precision computation and iteration-level interactive visualization, ensure real-time interactive VA for big data.

  9. Validation of methods for the detection and quantification of engineered nanoparticles in food

    DEFF Research Database (Denmark)

    Linsinger, T.P.J.; Chaudhry, Q.; Dehalu, V.;

    2013-01-01

    The potential impact of nanomaterials on the environment and on human health has already triggered legislation requiring labelling of products containing nanoparticles. However, so far, no validated analytical methods for the implementation of this legislation exist. This paper outlines a generic...... approach for the validation of methods for detection and quantification of nanoparticles in food samples. It proposes validation of identity, selectivity, precision, working range, limit of detection and robustness, bearing in mind that each “result” must include information about the chemical identity...

  10. 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

  11. 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 ...

  12. 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.

  13. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Ferrell, Jack R. [National Renewable Energy Laboratory (NREL), Golden CO USA; Olarte, Mariefel V. [Pacific Northwest National Laboratory (PNNL), Richland WA USA; Christensen, Earl D. [National Renewable Energy Laboratory (NREL), Golden CO USA; Padmaperuma, Asanga B. [Pacific Northwest National Laboratory (PNNL), Richland WA USA; Connatser, Raynella M. [Oak Ridge National Laboratory (ORNL), Oak Ridge TN USA; Stankovikj, Filip [Washington State University (WSU), Pullman WA USA; Meier, Dietrich [Thünen Institute of Wood Research (TI), Hamburg Germany; Paasikallio, Ville [VTT Technical Research Centre of Finland Ltd (VTT), Espoo Finland

    2016-07-05

    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.

  15. 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

  16. 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.

  17. An Analytical Method for Positioning Drag Anchors in Seabed Soils

    Institute of Scientific and Technical Information of China (English)

    张炜; 刘海笑; 李新仲; 李清平; 曹静

    2015-01-01

    Positioning drag anchors in seabed soils are strongly influenced not only by the properties of the anchor and soil, but also by the characteristics of the installation line. The investigation on the previous prediction methods related to anchor positioning demonstrates that the prediction of the anchor position during dragging has inevitably introduced some key and unsubstantiated hypotheses and the applicability of these methods is limited. In the present study, the interactional system between the drag anchor and installation line is firstly introduced for the analysis of anchor positioning. Based on the two mechanical models for embedded lines and drag anchors, the positioning equations for drag anchors have been derived both for cohesive and noncohesive soils. Since the drag angle at the shackle is the most important parameter in the positioning equations, a novel analytical method that can predict both the variation and the exact value of the drag angle at the shackle is proposed. The analytical method for positioning drag anchors which combines the interactional system between the drag anchor and the installation line has provided a reasonable theoretic approach to investigate the anchor behaviors in soils. By comparing with the model flume experiments, the sensitivity, effectiveness and veracity of the positioning method are well verified.

  18. Comparison of analytical methods for calculation of wind loads

    Science.gov (United States)

    Minderman, Donald J.; Schultz, Larry L.

    1989-01-01

    The following analysis is a comparison of analytical methods for calculation of wind load pressures. The analytical methods specified in ASCE Paper No. 3269, ANSI A58.1-1982, the Standard Building Code, and the Uniform Building Code were analyzed using various hurricane speeds to determine the differences in the calculated results. The winds used for the analysis ranged from 100 mph to 125 mph and applied inland from the shoreline of a large open body of water (i.e., an enormous lake or the ocean) a distance of 1500 feet or ten times the height of the building or structure considered. For a building or structure less than or equal to 250 feet in height acted upon by a wind greater than or equal to 115 mph, it was determined that the method specified in ANSI A58.1-1982 calculates a larger wind load pressure than the other methods. For a building or structure between 250 feet and 500 feet tall acted upon by a wind rangind from 100 mph to 110 mph, there is no clear choice of which method to use; for these cases, factors that must be considered are the steady-state or peak wind velocity, the geographic location, the distance from a large open body of water, and the expected design life and its risk factor.

  19. An Analytic Method for Measuring Accurate Fundamental Frequency Components

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Soon Ryul; Park Jong Keun [Seoul National University, Seoul(Korea); Kang, Sang Hee [Myongji University, Seoul (Korea)

    2002-04-01

    This paper proposes an analytic method for measuring the accurate fundamental frequency component of a fault current signal distorted with a DC-offset, a characteristic frequency component, and harmonics. The proposed algorithm is composed of four stages: sine filer, linear filter, Prony's method, and measurement. The sine filter and the linear filter eliminate harmonics and the fundamental frequency component, respectively. Then Prony's method is used to estimate the parameters of the DC-offset and the characteristic frequency component. Finally, the fundamental frequency component is measured by compensating the sine-filtered signal with the estimated parameters. The performance evaluation of the proposed method is presented for a-phase to ground faults on a 345 kV 200 km overhead transmission line. The EMTP is used to generate fault current signals under different fault locations and fault inception angles. It is shown that the analytic method accurately measures the fundamental frequency component regardless of the characteristic frequency component as well as the DC-offset.(author). 19 refs., 4 figs., 4 tabs.

  20. 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.

  1. Effective method for calculation of the analytic QCD coupling constant

    CERN Document Server

    Alekseev, A Yu

    2002-01-01

    The analytic running coupling of strong interaction alpha sub a sub n for initial standard perturbative approximations up to three-loop order is studied. The nonperturbative contributions to alpha sub a sub n are obtained in an explicit form. They are shown to be represented in the form of the expansion in the inverse powers of Euclidean momentum squared. It is shown that two-loop and three-loop-order corrections result in partial compensation of one-loop-order leading in the ultraviolet region nonperturbative contribution of the form 1/q sup 2. On basis of the stated expansion the effective method for calculation of the analytic running coupling is developed for all q > LAMBDA. The comparative analysis of the perturbative and nonperturbative contributions is carried out in the momentum dependence of alpha sub a sub n and its perturbative component for one - three-loop cases leads to a conclusion on higher loop stability of the analytic running coupling and its low dependence on the n sub f -threshold matchin...

  2. Selectivity in analytical chemistry: two interpretations for univariate methods.

    Science.gov (United States)

    Dorkó, Zsanett; Verbić, Tatjana; Horvai, George

    2015-01-01

    Selectivity is extremely important in analytical chemistry but its definition is elusive despite continued efforts by professional organizations and individual scientists. This paper shows that the existing selectivity concepts for univariate analytical methods broadly fall in two classes: selectivity concepts based on measurement error and concepts based on response surfaces (the response surface being the 3D plot of the univariate signal as a function of analyte and interferent concentration, respectively). The strengths and weaknesses of the different definitions are analyzed and contradictions between them unveiled. The error based selectivity is very general and very safe but its application to a range of samples (as opposed to a single sample) requires the knowledge of some constraint about the possible sample compositions. The selectivity concepts based on the response surface are easily applied to linear response surfaces but may lead to difficulties and counterintuitive results when applied to nonlinear response surfaces. A particular advantage of this class of selectivity is that with linear response surfaces it can provide a concentration independent measure of selectivity. In contrast, the error based selectivity concept allows only yes/no type decision about selectivity.

  3. Comparison of analytical methods for HULIS measurements in atmospheric particles

    Directory of Open Access Journals (Sweden)

    C. Baduel

    2009-03-01

    Full Text Available Humic-Like Substances (HULIS are a major contributor to the organic carbon in atmospheric aerosol. It would be necessary to standardise an analytical method that could be easily and routinely used for HULIS measurements. We present one of the first comparisons of two of the main methods in use to extract HULIS, using i a weak anion exchanger (DEAE and ii the combination of two separation steps, one according to polarity (on C18 and the second according to acidity (with a strong anion exchanger SAX. The quantification is performed with a DOC analyzer, complemented by an investigation of the chemical structure of the extracted fractions by UV-Visible spectroscopy. The analytical performances of each method are determined and compared for humic substances standards. These methods are further applied to determine the water extractable HULIS (HULISWS and the 0.1M NaOH alkaline extractable HULIS (HULIST in atmospheric aerosol collected in an Alpine Valley during winter time. This comparison shows that the simpler DEAE isolation procedure leads to higher recoveries and better reproducibility and should therefore be recommended.

  4. 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.

  5. 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.

  6. 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.

  7. 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)

  8. 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.

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

    Directory of Open Access Journals (Sweden)

    Elaheh Hooshmand

    2015-10-01

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

  10. 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.

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

    CERN Document Server

    Woods, Frederick S

    2005-01-01

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

  12. 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

  13. 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

  14. Method of Analytic Evolution of Flat Distribution Amplitudes in QCD

    CERN Document Server

    Tandogan, Asli

    2011-01-01

    A new analytical method of performing ERBL evolution is described. The main goal is to develop an approach that works for distribution amplitudes that do not vanish at the end points, for which the standard method of expansion in Gegenbauer polynomials is inefficient. Two cases of the initial DA are considered: a purely flat DA, given by the same constant for all x, and an antisymmetric DA given by opposite constants for x 1/2. For a purely flat DA, the evolution is governed by an overall (x (1-x))^t dependence on the evolution parameter t times a factor that was calculated as an expansion in t. For an antisymmetric flat DA, an extra overall factor |1-2x|^{2t} appears due to a jump at x=1/2. A good convergence was observed in the t < 1/2 region. For larger t, one can use the standard method of the Gegenbauer expansion.

  15. 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

  16. 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.

  17. 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

  18. 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.

  19. THERE IS NO MATHEMATICAL VALIDITY FOR USING FUZZY NUMBER CRUNCHING IN THE ANALYTIC HIERARCHY PROCESS

    Institute of Scientific and Technical Information of China (English)

    Thomas L. SAATY

    2006-01-01

    Fuzzy logic has difficulty producing valid answers in decision-making. Absent are theorems to prove that it works to produce results already known that are being estimated with judgments by transforming such judgments numerically. The numerical representation of judgments in the AHP is already fuzzy. Making fuzzy judgments more fuzzy does not lead to a better more valid outcome and it often leads to a worse one. The compatibility index of the AHP is used to illustrate how the answers obtained by fuzzifying AHP judgments do not produce better results than direct derivation of the principal eigenvector. Other authors who did experiments with given data in decision making quoted in the conclusions section of the paper, have observed that fuzzy sets gives the poorest answers among all methods used to derive best decisions.

  20. 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.

  1. 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.

  2. 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 ...

  3. 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...

  4. 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.

  5. 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)

  6. Validation of an analytical compressed elastic tube model for acoustic wave propagation

    Science.gov (United States)

    Van Hirtum, A.; Blandin, R.; Pelorson, X.

    2015-12-01

    Acoustic wave propagation through a compressed elastic tube is a recurrent problem in engineering. Compression of the tube is achieved by pinching it between two parallel bars so that the pinching effort as well as the longitudinal position of pinching can be controlled. A stadium-based geometrical tube model is combined with a plane wave acoustic model in order to estimate acoustic wave propagation through the elastic tube as a function of pinching effort, pinching position, and outlet termination (flanged or unflanged). The model outcome is validated against experimental data obtained in a frequency range from 3.5 kHz up to 10 kHz by displacing an acoustic probe along the tube's centerline. Due to plane wave model assumptions and the decrease of the lowest higher order mode cut-on frequency with increasing pinching effort, the difference between modeled and measured data is analysed in three frequency bands, up to 5 kHz, 8 kHz, and 9.5 kHz, respectively. It is seen that the mean and standard error within each frequency band do not significantly vary with pinching effort, pinching position, or outlet termination. Therefore, it is concluded that the analytical tube model is suitable to approximate the elastic tube geometry when modeling acoustic wave propagation through the pinched elastic tube with either flanged or unflanged termination.

  7. An analytical validation for the attenuation of lateral propagating light in sea ice

    Institute of Scientific and Technical Information of China (English)

    ZHAO Jinping; LI Tao; EHN Jens; BARBER David

    2015-01-01

    The attenuation of lateral propagating light (LPL) in sea ice was measured using an artificial light source in the Canadian Arctic during the 2007/2008 winter. The apparent attenuation coefficientμ(λ)for lateral prop-agating light was obtained from the measured logarithmic relative variation rate. In this study an analytical solution based on the strict optical theories is developed to validate the measured result. There is a good consistency between theoretical solution and measured data, by which a quite simple but very rigorous relationship among the light source, measurement geometry, and measured irradiance is established. The attenuation coefficients acquired by measurement and theory are the diffusion attenuation as an apparent optical property of ice, independent of the light source and shining condition. The attenuation ability of sea ice should be caused by the microstructure of sea ice, such as crystal size, ice density, brine volume, air inclusion, etc. It also includes the leak from both interfaces by directional scattering. It is verified that the measuring approach is operational and accurate to measure the attenuation of the LPL. The solution from this study did not tell the connection among the extinction and the inclusions of sea ice theoretically be-cause of insufficient understanding.

  8. An analytic method to compute star cluster luminosity statistics

    Science.gov (United States)

    da Silva, Robert L.; Krumholz, Mark R.; Fumagalli, Michele; Fall, S. Michael

    2014-03-01

    The luminosity distribution of the brightest star clusters in a population of galaxies encodes critical pieces of information about how clusters form, evolve and disperse, and whether and how these processes depend on the large-scale galactic environment. However, extracting constraints on models from these data is challenging, in part because comparisons between theory and observation have traditionally required computationally intensive Monte Carlo methods to generate mock data that can be compared to observations. We introduce a new method that circumvents this limitation by allowing analytic computation of cluster order statistics, i.e. the luminosity distribution of the Nth most luminous cluster in a population. Our method is flexible and requires few assumptions, allowing for parametrized variations in the initial cluster mass function and its upper and lower cutoffs, variations in the cluster age distribution, stellar evolution and dust extinction, as well as observational uncertainties in both the properties of star clusters and their underlying host galaxies. The method is fast enough to make it feasible for the first time to use Markov chain Monte Carlo methods to search parameter space to find best-fitting values for the parameters describing cluster formation and disruption, and to obtain rigorous confidence intervals on the inferred values. We implement our method in a software package called the Cluster Luminosity Order-Statistic Code, which we have made publicly available.

  9. Analytical validation for the HRMS detection of organochlorines in living marine mammals from biopsy microsamples

    Energy Technology Data Exchange (ETDEWEB)

    Ikonomou, M.G.; Crewe, N.F.; Fischer, M.; Smith, T.G. [Dept. of Fisheries and Oceans, Sidney, British Columbia (Canada)

    1995-12-31

    It has been demonstrated that marine mammals accumulate high concentrations of lipophilic organochlorine contaminants in blubber. As predators of the high trophic level they have also been used to evaluate contamination in the marine environment. Sampling of living marine mammals using a microsample (100 to 200 mg) biopsy dart technique offers a potentially invaluable chronicle in assessing levels and types of persistent environmental pollutants from a sample in which age, sex and other genetic information can additionally be ascertained. The authors have explored analytical methodology based on a high sensitivity detection system (HRGC/HRMS) which provides multi-residue determinations from biopsy dart microsamples. Lipid content and the concentrations of PCDDs, PCDFs and non-ortho and mono-ortho substituted PCBs were measured in 100 mg biopsy dart replicates taken from a killer whale carcass and in three strata of the blubber of that carcass. Statistically acceptable results were obtained from the dart replicates which compared very well with those of the blubber strata. Analytical data from 100 mg extractions from an established in house blubber CRM also compared well against a series of 2.5 g extractions of that CRM. The extraction and cleanup procedures used also allow for the determination of other organohalogen contaminants such as DDT and other pesticides, all the remaining PCBs, polychlorinated diphenylethers and brominated residues. The strengths and limitations of the analytical methodology and the biopsy dart as a sampling tool and pollution predicator will be illustrated in terms of method accuracy and precision, glassware and procedural blanks associated with each extraction batch, and the incorporation of an in house micro reference standard.

  10. 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.

  11. 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 ...

  12. 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.

  13. 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.

  14. Application of analytical methods in authentication and adulteration of honey.

    Science.gov (United States)

    Siddiqui, Amna Jabbar; Musharraf, Syed Ghulam; Choudhary, M Iqbal; Rahman, Atta-Ur-

    2017-02-15

    Honey is synthesized from flower nectar and it is famous for its tremendous therapeutic potential since ancient times. Many factors influence the basic properties of honey including the nectar-providing plant species, bee species, geographic area, and harvesting conditions. Quality and composition of honey is also affected by many other factors, such as overfeeding of bees with sucrose, harvesting prior to maturity, and adulteration with sugar syrups. Due to the complex nature of honey, it is often challenging to authenticate the purity and quality by using common methods such as physicochemical parameters and more specialized procedures need to be developed. This article reviews the literature (between 2000 and 2016) on the use of analytical techniques, mainly NMR spectroscopy, for authentication of honey, its botanical and geographical origin, and adulteration by sugar syrups. NMR is a powerful technique and can be used as a fingerprinting technique to compare various samples. PMID:27664687

  15. Polymeric vehicles for topical delivery and related analytical methods.

    Science.gov (United States)

    Cho, Heui Kyoung; Cho, Jin Hun; Jeong, Seong Hoon; Cho, Dong Chul; Yeum, Jeong Hyun; Cheong, In Woo

    2014-04-01

    Recently a variety of polymeric vehicles, such as micelles, nanoparticles, and polymersomes, have been explored and some of them are clinically used to deliver therapeutic drugs through skin. In topical delivery, the polymeric vehicles as drug carrier should guarantee non-toxicity, long-term stability, and permeation efficacy for drugs, etc. For the development of the successful topical delivery system, it is of importance to develop the polymeric vehicles of well-defined intrinsic properties, such as molecular weights, HLB, chemical composition, topology, specific ligand conjugation and to investigate the effects of the properties on drug permeation behavior. In addition, the role of polymeric vehicles must be elucidated in in vitro and in vivo analyses. This article describes some important features of polymeric vehicles and corresponding analytical methods in topical delivery even though the application span of polymers has been truly broad in the pharmaceutical fields.

  16. Modelling of packet traffic with matrix analytic methods

    DEFF Research Database (Denmark)

    Andersen, Allan T.

    1995-01-01

    Network (B-ISDN). As a case study of packet switched networks Common Channel Signalling System No. 7(SS7) has been used. SS7 is the packet switched network currently employed to command/control the public switched telephone network i.e. the setup and teardown of trunks and the basis for intelligent......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...

  17. 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.

  18. Validation of qualitative microbiological test methods

    NARCIS (Netherlands)

    IJzerman-Boon, Pieta C.; van den Heuvel, Edwin R.

    2015-01-01

    This paper considers a statistical model for the detection mechanism of qualitative microbiological test methods with a parameter for the detection proportion (the probability to detect a single organism) and a parameter for the false positive rate. It is demonstrated that the detection proportion a

  19. 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.

  20. 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

  1. Analytical methods for thorium determination: A journey from conventional methods to novel applications

    Energy Technology Data Exchange (ETDEWEB)

    Mayer, K.; Ottmar, H.; Tamborini, G.; Ray, I.; Thiele, H

    2001-07-01

    Thorium may be determined using a variety of analytical methods. These may be based on chemical or physical principles or may make use of the radioactive decay of the individual thorium isotopes. The method to be used for a certain analytical purpose is selected as a function of the matrix of the sample and of the concentration of thorium. The present paper describes different methodologies, their range of application and discusses selected results. The methods described cover a concentration range of more than twelve orders of magnitude, i.e. from concentrated solutions to micrometre-sized particles. Emphasis is given to active radiometric techniques, chemical and instrumental analysis. (author)

  2. 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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Kanda, Tomonori [Department of Radiology, Kobe University Graduate School of Medicine, 7-5-2 Kusunokicho, Chuoku, Kobe 650-0017 (Japan); Yoshikawa, Takeshi, E-mail: yoshikawa0816@aol.com [Department of Radiology, Kobe University Graduate School of Medicine, 7-5-2 Kusunokicho, Chuoku, Kobe 650-0017 (Japan); Ohno, Yoshiharu; Kanata, Naoki; Koyama, Hisanobu; Takenaka, Daisuke; Sugimura, Kazuro [Department of Radiology, Kobe University Graduate School of Medicine, 7-5-2 Kusunokicho, Chuoku, Kobe 650-0017 (Japan)

    2012-09-15

    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.

  4. 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

  5. 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)

  6. 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...

  7. 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...

  8. 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:...

  9. RETROSPECTIVE METHOD VALIDATION AND UNCERTAINTY ESTIMATION FOR ACTINIDES DETERMINATION IN EXCRETA BY ALPHA SPECTROMETRY.

    Science.gov (United States)

    Hernández, C; Sierra, I

    2016-09-01

    Two essential technical requirements of ISO 17025 guide for accreditation of testing and calibration laboratories are the validation of methods and the estimation of all sources of uncertainty that may affect the analytical result. Bioelimination Laboratory from Radiation Dosimetry Service of CIEMAT (Spain) uses alpha spectrometry to quantify alpha emitters (Pu, Am, Th, U and Cm isotopes) in urine and faecal samples from workers exposed to internal radiation. Therefore and as a step previous to achieving the ISO 17025 accreditation, the laboratory has performed retrospective studies based on the obtained results in the past few years to validate the analytical method. Uncertainty estimation was done identifying and quantifying all the contributions, and finally the overall combined standard uncertainty was calculated. PMID:26424133

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

    Institute of Scientific and Technical Information of China (English)

    Lu Jie; Zheng Longxi; Wang Zhiwu; Peng Changxin; Chen Xinggu

    2014-01-01

    In order to test the feasibility of a new thrust stand system based on impulse thrust mea-surement method, a liquid-fueled pulse detonation engine (PDE) is designed and built. Thrust per-formance 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 ignor-ing 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. 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.

  12. 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

  13. ON A GENERALIZED TAYLOR THEOREM: A RATIONAL PROOF OF THE VALIDITY OF THE HOMOTOPY ANALYSIS METHOD

    Institute of Scientific and Technical Information of China (English)

    廖世俊

    2003-01-01

    A generalized Taylor series of a complex function was derived and some relatedtheorems about its convergence region were given. The generalized Taylor theorem can beapplied to greatly enlarge convergence regions of approximation series given by othertraditional techniques. The rigorous proof of the generalized Taylor theorem also provides uswith a rational base of the validity of a new kind of powerful analytic technique for nonlinearproblems, namely the homotopy analysis method.

  14. 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)

  15. 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.

  16. Pesticides in honey: A review on chromatographic analytical methods.

    Science.gov (United States)

    Tette, Patrícia Amaral Souza; Rocha Guidi, Letícia; Glória, Maria Beatriz de Abreu; Fernandes, Christian

    2016-01-01

    Honey is a product of high consumption due to its nutritional and antimicrobial properties. However, residues of pesticides, used in plagues' treatment in the hive or in crop fields in the neighborhoods, can compromise its quality. Therefore, determination of these contaminants in honey is essential, since the use of pesticides has increased significantly in recent decades because of the growing demand for food production. Furthermore, pesticides in honey can be an indicator of environmental contamination. As the concentration of these compounds in honey is usually at trace levels and several pesticides can be found simultaneously, the use of highly sensitive and selective techniques is required. In this context, miniaturized sample preparation approaches and liquid or gas chromatography coupled to mass spectrometry became the most important analytical techniques. In this review we present and discuss recent studies dealing with pesticide determination in honey, focusing on sample preparation and separation/detection methods as well as application of the developed methods worldwide. Furthermore, trends and future perspectives are presented.

  17. 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.

  18. 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 %.

  19. 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.

  20. Validação em métodos cromatográficos e eletroforéticos Validation for chromatographic and electrophoretic methods

    Directory of Open Access Journals (Sweden)

    Marcelo Ribani

    2004-10-01

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

  1. 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.

  2. 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.

  3. 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…

  4. 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.

  5. 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.

  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. 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

  8. 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.

  9. 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.

  10. 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)

  11. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-07-01

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

  13. Desenvolvimento e validação de método analítico por cromatografia líquida de alta eficiência (CLAE para determinação de associação de ampicilinas em pó liofilizado para injeção Development and validation of analytical method for determination of an association of ampicillins in lyophilized powder for injection by HPLC

    Directory of Open Access Journals (Sweden)

    Ana Paola Prata Cione

    2010-01-01

    Full Text Available An analytical method has been developed and validated for the determination of an association of ampicillins in a lyophilized powder for injection by HPLC. The advantage of chromatographic method other than the microbiological one is that, it is possible to monitor precisely, out-of-specification results in quality control processes and also during stability studies, in which an association of ampicillins is present. The proposed HPLC method was developed by using forced degraded samples, in order to reach a selective analysis of ampicillins when in the presence of their degradation products. It was possible to detect benzatine and through indirect calculation, to determine the ampicillin sodium in the drug sample. The method showed to be selective, accurate, precise, robust and linear (from 45.92 to 36.04 μg mL-1 of total ampicillin and from 14.53 to 43.28 μg mL-1 of benzatine. The accuracy determined from recovery test, gave results in the range of 99.41% of total ampicillin to 100.31% of benzatine. Hence, it can be concluded that the proposed HPLC method is applicable for ampicillins determination.

  14. 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.

  15. 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...

  16. 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

  17. 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

  18. 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.

  19. 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

  20. 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...

  1. 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…

  2. Predictive validity of the Hand Arm Risk assessment Method (HARM)

    NARCIS (Netherlands)

    Douwes, M.; Boocock, M.; Coenen, P.; Heuvel, S. van den; Bosch, T.

    2014-01-01

    The Hand Arm Risk assessment Method (HARM) is a simplified risk assessment method for determining musculoskeletal symptoms to the arm, neck and/or shoulder posed by hand-arm tasks of the upper body. The purpose of this study was to evaluate the predictive validity of HARM using data collected from a

  3. 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

  4. ANALYTICAL METHODS IN ARCHAEOMETRY: STUDY OF SUPPORT MATERIAL

    Directory of Open Access Journals (Sweden)

    Rodica Mariana Ion

    2011-02-01

    Full Text Available The application of some analytical techniques developed initially in materials science (techniques based on physical-chemical phenomena in the study of art and archaeological objects offers the historian and archaeologist quantitative information that can prove useful in order to better understanding of ancient society. The preservation of material culture for future generations with the best possible fidelity requires in-depth knowledge, to aid the most suitable restoration, conservation, storage, and eventual museum display. The use of analytical techniques often proves useful for the specialists in conservation and/or restoration due to the valuable information given (composition, state of degradation, and so on. This paper describes the use of some analytical techniques (X-ray fluorescence - XRF, inductively coupled plasma - atomic emission spectrometry - ICP-AES, Fourier transformed - infrared spectroscopy - FTIR for analyzing compositions of artifacts.

  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. 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

  7. 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...

  8. 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

  9. A new and consistent parameter for measuring the quality of multivariate analytical methods: Generalized analytical sensitivity.

    Science.gov (United States)

    Fragoso, Wallace; Allegrini, Franco; Olivieri, Alejandro C

    2016-08-24

    Generalized analytical sensitivity (γ) is proposed as a new figure of merit, which can be estimated from a multivariate calibration data set. It can be confidently applied to compare different calibration methodologies, and helps to solve literature inconsistencies on the relationship between classical sensitivity and prediction error. In contrast to the classical plain sensitivity, γ incorporates the noise properties in its definition, and its inverse is well correlated with root mean square errors of prediction in the presence of general noise structures. The proposal is supported by studying simulated and experimental first-order multivariate calibration systems with various models, namely multiple linear regression, principal component regression (PCR) and maximum likelihood PCR (MLPCR). The simulations included instrumental noise of different types: independently and identically distributed (iid), correlated (pink) and proportional noise, while the experimental data carried noise which is clearly non-iid. PMID:27496995

  10. A new and consistent parameter for measuring the quality of multivariate analytical methods: Generalized analytical sensitivity.

    Science.gov (United States)

    Fragoso, Wallace; Allegrini, Franco; Olivieri, Alejandro C

    2016-08-24

    Generalized analytical sensitivity (γ) is proposed as a new figure of merit, which can be estimated from a multivariate calibration data set. It can be confidently applied to compare different calibration methodologies, and helps to solve literature inconsistencies on the relationship between classical sensitivity and prediction error. In contrast to the classical plain sensitivity, γ incorporates the noise properties in its definition, and its inverse is well correlated with root mean square errors of prediction in the presence of general noise structures. The proposal is supported by studying simulated and experimental first-order multivariate calibration systems with various models, namely multiple linear regression, principal component regression (PCR) and maximum likelihood PCR (MLPCR). The simulations included instrumental noise of different types: independently and identically distributed (iid), correlated (pink) and proportional noise, while the experimental data carried noise which is clearly non-iid.

  11. 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

  12. 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%

  13. 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.

  14. 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.

  15. 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)

  16. 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.

  17. 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

  18. 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

  19. 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

  20. 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.

  1. 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.

  2. 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

  3. 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)

  4. 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.

  5. Derivation of gravity anomalies from airborne gravimeter and IMU recordings - Validation with regional analytic models using ground and satellite gravity data

    OpenAIRE

    Juergen Neumeyer; Schäfer, U.; Kremer, J; Hartmut Pflug; Guochang Xu;  

    2009-01-01

    Derivation of gravity anomalies from Airborne Gravimeter, IMU recordings - validation with regional analytic models using ground and satellite gravity data GERMANY (Neumeyer, Jurgen) GERMANY Received: 2008-03-31 Revised: 2008-08-01 Accepted: 2008-08-21

  6. Preliminary Validation of High Performance Liquid Chromatography Method for Detection of Methyltestosterone Residue in Carp Muscle

    Institute of Scientific and Technical Information of China (English)

    JIANG Jie; LIN Hong; FU Xiaoting; LI Mingming

    2005-01-01

    The use of synthetic anabolic steroid methyltestosterone (MT) as growth promoter is prohibited in China. Validations of analytical methods for MT residue in food and the results obtained have become indispensable. The high performance liquid chromatography (HPLC) method for the detection of MT with liquid-liquid extraction by trichloromethanemethanol in carp muscle tissue was preliminarily validated with reference to the following parameters: recovery (accuracy)at the 1, 5 and 10 mgkg-1 level, between-run and within-run CV values (repeatability, also called relative standard deviation(RSD)) and limit of detection. The recoveries were above 80% and the between-run and within-run CV values below 10%for muscle tissue. The limit of detection was 0.05 mgkg-1.

  7. 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

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

    DEFF Research Database (Denmark)

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

    2009-01-01

    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...

  9. Development of analytical methods for polycyclic aromatic hydrocarbons (PAHs) in airborne particulates:A review

    Institute of Scientific and Technical Information of China (English)

    LIU Li-bin; LIU Yan; LIN Jin-ming; TANG Ning; HAYAKAWA Kazuichi; MAEDA Tsuneaki

    2007-01-01

    In the present work,the different sample collection, pretreatment and analytical methods for polycyclic aromatic hydrocarbons (PAHs) in airborne particulates is systematacially reviewed, and the applications of these pretreatment and analytical methods for PAHs are compared in detail. Some comments on the future expectation are also presented.

  10. 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...

  11. 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.

  12. 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

  13. 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.

  14. 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...

  15. 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

  16. 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

  17. 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.

  18. 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

  19. In-house validation and quality control of real-time PCR methods for GMO detection: a practical approach.

    Science.gov (United States)

    Ciabatti, I; Froiio, A; Gatto, F; Amaddeo, D; Marchesi, U

    2006-01-01

    GMO detection and quantification methods in the EU are mainly based on real-time PCR. The analytical methods in use must be validated, first on an intra-laboratory scale and through a collaborative trial thereafter. Since a consensual protocol for intra-laboratory validation of real-time PCR methods is lacking, we provide a practical approach for the in-house validation of quantitative real-time PCR methods, establishing acceptability criteria and quality controls for PCR runs. Parameters such as limit of detection, limit of quantification, precision, trueness, linear dynamic range, PCR efficiency, robustness and specificity are considered. The protocol is sufficiently detailed to be directly applicable, increases the reliability of results and their harmonization among different laboratories, and represents a necessary preliminary step before proceeding to a time-consuming and costly full validation study.

  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. 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

  2. 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

  3. 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...

  4. 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

  5. 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.

  6. Analysis of Carbamate Pesticides: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS666

    Energy Technology Data Exchange (ETDEWEB)

    Owens, J; Koester, C

    2008-05-14

    The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method for analysis of aldicarb, bromadiolone, carbofuran, oxamyl, and methomyl in water by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), titled Method EPA MS666. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures described in MS666 for analysis of carbamate pesticides in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of Method EPA MS666 can be determined.

  7. 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.

  8. Analytical Method for Designing Grating Compensated Dispersion-Managed Soliton Systems

    Institute of Scientific and Technical Information of China (English)

    Y. H. C. Kwan; K. Nakkeeran; P. K. A. Wai

    2003-01-01

    We show a useful analytical method to design grating compensated dispersion-managed systems. Our method is in good agreement with the numerical results even in the presence of group delay ripples in the chirped fiber gratings.

  9. 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.

  10. Determination of chloramphenicol in bovine urine, meat and shrimp by GC-MS. Method validation according to Commission Decision 2002/657/EC

    NARCIS (Netherlands)

    Rossum HJ van; Kootstra PR; Sterk SS; ARO

    2004-01-01

    This report describes the validation of the quantification and the identification of an analytical method for the determination of low concentrations (0.1-1.0 micro g/kg) of chloramphenicol in samples of urine, shrimps and meat. The validation study was based on the criteria described in Decision 20

  11. 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.

  12. 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)

  13. 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.

  14. 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.

  15. 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..

  16. Analytical method for assessing potential dermal exposure to captan, using whole body dosimetry, in small vegetable production units in Argentina.

    Science.gov (United States)

    Hughes, Enrique A; Zalts, Anita; Ojeda, Javier J; Flores, Andrea P; Glass, Richard C; Montserrat, Javier M

    2006-09-01

    An analytical method has been developed that can be used to determine the potential dermal exposure (PDE) of workers to the pesticide captan in small-scale horticultural production units. The methodology is based on the whole body dosimetry technique, using a cotton coverall and cotton gloves as sampling media, with protective clothing worn beneath the cotton media to protect the operator. The quantitative determination of captan was done by gas chromatography-electron capture detector (GC-ECD), with the analytical method validated by measuring limits of detection and quantification, linear ranges, sample recovery and precision. Special emphasis is placed on factors that affected the stability of captan during chromatographic determination. The data generated for potential dermal exposure are presented separately for mixing/loading and application activities. These data are compared with values obtained with visible tracers using a similar field technique. Margin of safety (MOS) values are also calculated for the agricultural procedures studied.

  17. Analytical Evaluation of Beam Deformation Problem Using Approximate Methods

    DEFF Research Database (Denmark)

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

    2010-01-01

    The beam deformation equation has very wide applications in structural engineering. As a differential equation, it has its own problem concerning existence, uniqueness and methods of solutions. Often, original forms of governing differential equations used in engineering problems are simplified, ...... 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....

  18. Team mental models: techniques, methods, and analytic approaches.

    Science.gov (United States)

    Langan-Fox, J; Code, S; Langfield-Smith, K

    2000-01-01

    Effective team functioning requires the existence of a shared or team mental model among members of a team. However, the best method for measuring team mental models is unclear. Methods reported vary in terms of how mental model content is elicited and analyzed or represented. We review the strengths and weaknesses of vatrious methods that have been used to elicit, represent, and analyze individual and team mental models and provide recommendations for method selection and development. We describe the nature of mental models and review techniques that have been used to elicit and represent them. We focus on a case study on selecting a method to examine team mental models in industry. The processes involved in the selection and development of an appropriate method for eliciting, representing, and analyzing team mental models are described. The criteria for method selection were (a) applicability to the problem under investigation; (b) practical considerations - suitability for collecting data from the targeted research sample; and (c) theoretical rationale - the assumption that associative networks in memory are a basis for the development of mental models. We provide an evaluation of the method matched to the research problem and make recommendations for future research. The practical applications of this research include the provision of a technique for analyzing team mental models in organizations, the development of methods and processes for eliciting a mental model from research participants in their normal work environment, and a survey of available methodologies for mental model research.

  19. 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.

  20. 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.

  1. 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)

  2. Application of an analytical method for solution of thermal hydraulic conservation equations

    Energy Technology Data Exchange (ETDEWEB)

    Fakory, M.R. [Simulation, Systems & Services Technologies Company (S3 Technologies), Columbia, MD (United States)

    1995-09-01

    An analytical method has been developed and applied for solution of two-phase flow conservation equations. The test results for application of the model for simulation of BWR transients are presented and compared with the results obtained from application of the explicit method for integration of conservation equations. The test results show that with application of the analytical method for integration of conservation equations, the Courant limitation associated with explicit Euler method of integration was eliminated. The results obtained from application of the analytical method (with large time steps) agreed well with the results obtained from application of explicit method of integration (with time steps smaller than the size imposed by Courant limitation). The results demonstrate that application of the analytical approach significantly improves the numerical stability and computational efficiency.

  3. 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.

  4. Hybrid analytic-numeric calculation method for light through a bounded planar dielectric

    NARCIS (Netherlands)

    Nicolau, J.B.; Groesen, van E.

    2005-01-01

    We present a hybrid analytic-numeric method to calculate the transmission and reflection of light that is fluxed into a bounded complicated optical structure surrounded by air. The solution is obtained by numerical calculations inside a square containing the structure and by analytical calculations

  5. 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.

  6. VALUE - Validating and Integrating Downscaling Methods for Climate Change Research

    Science.gov (United States)

    Maraun, Douglas; Widmann, Martin; Benestad, Rasmus; Kotlarski, Sven; Huth, Radan; Hertig, Elke; Wibig, Joanna; Gutierrez, Jose

    2013-04-01

    Our understanding of global climate change is mainly based on General Circulation Models (GCMs) with a relatively coarse resolution. Since climate change impacts are mainly experienced on regional scales, high-resolution climate change scenarios need to be derived from GCM simulations by downscaling. Several projects have been carried out over the last years to validate the performance of statistical and dynamical downscaling, yet several aspects have not been systematically addressed: variability on sub-daily, decadal and longer time-scales, extreme events, spatial variability and inter-variable relationships. Different downscaling approaches such as dynamical downscaling, statistical downscaling and bias correction approaches have not been systematically compared. Furthermore, collaboration between different communities, in particular regional climate modellers, statistical downscalers and statisticians has been limited. To address these gaps, the EU Cooperation in Science and Technology (COST) action VALUE (www.value-cost.eu) has been brought into life. VALUE is a research network with participants from currently 23 European countries running from 2012 to 2015. Its main aim is to systematically validate and develop downscaling methods for climate change research in order to improve regional climate change scenarios for use in climate impact studies. Inspired by the co-design idea of the international research initiative "future earth", stakeholders of climate change information have been involved in the definition of research questions to be addressed and are actively participating in the network. The key idea of VALUE is to identify the relevant weather and climate characteristics required as input for a wide range of impact models and to define an open framework to systematically validate these characteristics. Based on a range of benchmark data sets, in principle every downscaling method can be validated and compared with competing methods. The results of

  7. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Greulich, K.A.; Gray, C.E. (comp.)

    1991-08-01

    This Manual is compiled from techniques used in the Industrial Hygiene Chemistry Laboratory of Sandia National Laboratories in Albuquerque, New Mexico. The procedures are similar to those used in other laboratories devoted to industrial hygiene practices. Some of the methods are standard; some, modified to suit our needs; and still others, developed at Sandia. The authors have attempted to present all methods in a simple and concise manner but in sufficient detail to make them readily usable. It is not to be inferred that these methods are universal for any type of sample, but they have been found very reliable for the types of samples mentioned.

  9. 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.

  10. 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.

  11. 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)

  12. 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.

  13. 40 CFR 136.6 - Method modifications and analytical requirements.

    Science.gov (United States)

    2010-07-01

    ..., oil and grease, total suspended solids, total phenolics, turbidity, chemical oxygen demand, and..., an analyst may not modify an approved method if the modification would result in measurement of...

  14. 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.

  15. Temperature based validation of the analytical model for the estimation of the amount of heat generated during friction stir welding

    Directory of Open Access Journals (Sweden)

    Milčić Dragan S.

    2012-01-01

    Full Text Available Friction stir welding is a solid-state welding technique that utilizes thermomechanical influence of the rotating welding tool on parent material resulting in a monolith joint - weld. On the contact of welding tool and parent material, significant stirring and deformation of parent material appears, and during this process, mechanical energy is partially transformed into heat. Generated heat affects the temperature of the welding tool and parent material, thus the proposed analytical model for the estimation of the amount of generated heat can be verified by temperature: analytically determined heat is used for numerical estimation of the temperature of parent material and this temperature is compared to the experimentally determined temperature. Numerical solution is estimated using the finite difference method - explicit scheme with adaptive grid, considering influence of temperature on material's conductivity, contact conditions between welding tool and parent material, material flow around welding tool, etc. The analytical model shows that 60-100% of mechanical power given to the welding tool is transformed into heat, while the comparison of results shows the maximal relative difference between the analytical and experimental temperature of about 10%.

  16. 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.

  17. Analytical validation considerations of multiplex mass-spectrometry-based proteomic platforms for measuring protein biomarkers.

    Science.gov (United States)

    Boja, Emily S; Fehniger, Thomas E; Baker, Mark S; Marko-Varga, György; Rodriguez, Henry

    2014-12-01

    Protein biomarker discovery and validation in current omics era are vital for healthcare professionals to improve diagnosis, detect cancers at an early stage, identify the likelihood of cancer recurrence, stratify stages with differential survival outcomes, and monitor therapeutic responses. The success of such biomarkers would have a huge impact on how we improve the diagnosis and treatment of patients and alleviate the financial burden of healthcare systems. In the past, the genomics community (mostly through large-scale, deep genomic sequencing technologies) has been steadily improving our understanding of the molecular basis of disease, with a number of biomarker panels already authorized by the U.S. Food and Drug Administration (FDA) for clinical use (e.g., MammaPrint, two recently cleared devices using next-generation sequencing platforms to detect DNA changes in the cystic fibrosis transmembrane conductance regulator (CFTR) gene). Clinical proteomics, on the other hand, albeit its ability to delineate the functional units of a cell, more likely driving the phenotypic differences of a disease (i.e., proteins and protein-protein interaction networks and signaling pathways underlying the disease), "staggers" to make a significant impact with only an average ∼ 1.5 protein biomarkers per year approved by the FDA over the past 15-20 years. This statistic itself raises the concern that major roadblocks have been impeding an efficient transition of protein marker candidates in biomarker development despite major technological advances in proteomics in recent years.

  18. 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.

  19. 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

  20. Solving Burger's equation by semi-analytical and implicit method

    Directory of Open Access Journals (Sweden)

    Jalil Manafian Heris

    2014-08-01

    Full Text Available In this work, the modified Laplace Adomian decomposition method (LADM is applied to solve the Burgers’ equation. In addition, example that illustrate the pertinent features of this method is presented, and the results of the study is discussed. We prove the convergence of LADM applied to the Burgers’ equation. Also, Burgers’ equation has some discontinuous solutions because of effects of viscosity term. These discontinuities raise phenomenon of shock waves. Some explicit and implicit numerical methods have been experimented on Burgers’ equation but these schemes have not been seen proper in this case because of their conditional stability and existence of viscosity term. We consider two types of box schemes and implement on Burgers’ equation to get better results with no artificial wiggles.

  1. Comparison of analytical and predictive methods for water, protein, fat, sugar, and gross energy in marine mammal milk.

    Science.gov (United States)

    Oftedal, O T; Eisert, R; Barrell, G K

    2014-01-01

    sugar methods for total sugar-appear likely to produce substantial error in marine mammal milks. It is important that alternative analytical methods be properly validated against a reference method before being used, especially for mammalian milks that differ greatly from cow milk in analyte characteristics and concentrations.

  2. 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.

  3. 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.

  4. Development and validation of methods for the trace determination of phthalates in sludge and vegetables.

    Science.gov (United States)

    Sablayrolles, Caroline; Montréjaud-Vignoles, Mireille; Benanou, David; Patria, Lucie; Treilhou, Michel

    2005-04-29

    A routine method which is simple, quick and precise has been set up and validated for phthalate analysis in environmental samples (tomato plants and sewage sludges). Six phthalates have been studied simultaneously: dimethylphthalate, diethylphthalate, di-n-butylphthalate, n-butylbenzylphthalate, di-2-ethyl-hexyl phthalate (DEHP) and di-n-octylphthalate. Optimization of sample, solvent extraction uses a Soxtec apparatus and extract purification with an a solid-phase extraction cartridge allows between 90 and 110% recovery of phthalates. Precise, sensitive and selective identification and quantifying of analytes is by GC-MS in the single ion monitoring mode. This protocol allows analytes with concentrations as low as 10 microg/kg dry matter (DM) to be determined from small (1-2 g DM) samples. This analytical method has been applied to the phthalate transfer study for agricultural recycling of sludges, where phthalate bioavailability has been studied in aquiculture using two types of experiments. Tomatoes have been grown in containers where the trace organics have been directly introduced as pure substances, and in a second experiment under the same growth conditions, sewage sludge has replaced the pure substances. Transfer of these trace organics has been followed into the various parts of the tomato plant and in general only the DEHP is worthy of note although its percentage transfer remains very low even in an experiment designed to maximize this.

  5. Study on Fluorescence Analytical Method of Micro Th in Pu

    Institute of Scientific and Technical Information of China (English)

    QIAN; Hong-juan; ZHANG; Li-hua; LIU; Huan-liang; FAN; De-jun

    2013-01-01

    As one of impurities,Th is needed to be determined for control quality of Pu product.Due to the high radioactivity and fatal toxicity of Pu,it is very difficult to measure the micro Th in Pu product.It is necessary to develop a sensitive method for determining the micro Th in Pu under the described harsh condition.

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

    Science.gov (United States)

    Abel, Julianna; Luntz, Jonathan; Brei, Diann

    2012-08-01

    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.

  7. 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

  8. 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

  9. 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...

  10. 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...

  11. 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

  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. 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.

  14. An Other Perspective on Personality: Meta-Analytic Integration of Observers' Accuracy and Predictive Validity

    Science.gov (United States)

    Connelly, Brian S.; Ones, Deniz S.

    2010-01-01

    The bulk of personality research has been built from self-report measures of personality. However, collecting personality ratings from other-raters, such as family, friends, and even strangers, is a dramatically underutilized method that allows better explanation and prediction of personality's role in many domains of psychology. Drawing…

  15. Analytical solution and experimental validation of the energy management problem for fuel cell hybrid vehicles

    NARCIS (Netherlands)

    Hoppenbrouwers, Stijn; Grimminck, M.; Bosch, P.P.J. van den; Veenhuizen, Bram; Tazelaar, Edwin

    2011-01-01

    The objective of an energy management strategy for fuel cell hybrid propulsion systems is to minimize the fuel needed to provide the required power demand. This minimization is defined as an optimization problem. Methods such as dynamic programming numerically solve this optimization problem. Strate

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. 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.

  1. Approximation analytical solutions for a unified plasma sheath model by double decomposition method

    Institute of Scientific and Technical Information of China (English)

    FangJin-Qing

    1998-01-01

    A unified plasma sheath model and its potential equation are proposed.Any higher-order approximation analytical solutions for the unified plasma sheath potential equation are derived by double decomposition method.

  2. 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

  3. 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.

  4. 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.

  5. 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

  6. 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

  7. 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.

  8. 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.

  9. 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)

  10. 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)

  11. SEMI-ANALYTICAL FINITE ELEMENT METHOD FOR FICTITIOUS CRACK MODEL IN FRACTURE MECHANICS OF CONCRETE

    Institute of Scientific and Technical Information of China (English)

    王承强; 郑长良

    2004-01-01

    Based on the Hamiltonian governing equations of plane elasticity for sectorial domain, the variable separation and eigenfunction expansion techniques were employed to develop a novel analytical finite element for the fictitious crack model in fracture mechanics of concrete. The new analytical element can be implemented into FEM program systems to solve fictitious crack propagation problems for concrete cracked plates with arbitrary shapes and loads. Numerical results indicate that the method is more efficient and accurate than ordinary finite element method.

  12. 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.

  13. Analytical validation of whole exome and whole genome sequencing for clinical applications

    OpenAIRE

    Linderman, Michael D.; Brandt, Tracy; Edelmann, Lisa; Jabado, Omar; Kasai, Yumi; Kornreich, Ruth; Mahajan, Milind; Shah, Hardik; Kasarskis, Andrew; Eric E Schadt

    2014-01-01

    Background Whole exome and genome sequencing (WES/WGS) is now routinely offered as a clinical test by a growing number of laboratories. As part of the test design process each laboratory must determine the performance characteristics of the platform, test and informatics pipeline. This report documents one such characterization of WES/WGS. Methods Whole exome and whole genome sequencing was performed on multiple technical replicates of five reference samples using the Illumina HiSeq 2000/2500...

  14. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina para espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

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

  15. 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)

  16. Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 4, Organic methods

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    This interim notice covers the following: extractable organic halides in solids, total organic halides, analysis by gas chromatography/Fourier transform-infrared spectroscopy, hexadecane extracts for volatile organic compounds, GC/MS analysis of VOCs, GC/MS analysis of methanol extracts of cryogenic vapor samples, screening of semivolatile organic extracts, GPC cleanup for semivolatiles, sample preparation for GC/MS for semi-VOCs, analysis for pesticides/PCBs by GC with electron capture detection, sample preparation for pesticides/PCBs in water and soil sediment, report preparation, Florisil column cleanup for pesticide/PCBs, silica gel and acid-base partition cleanup of samples for semi-VOCs, concentrate acid wash cleanup, carbon determination in solids using Coulometrics` CO{sub 2} coulometer, determination of total carbon/total organic carbon/total inorganic carbon in radioactive liquids/soils/sludges by hot persulfate method, analysis of solids for carbonates using Coulometrics` Model 5011 coulometer, and soxhlet extraction.

  17. Zinco eritrocitário (validação de um método de análise e zinco dietético na avaliação do estado nutricional de mulheres adultas Erythrocytic zinc (validation of an analytical method and dietetic in nutriture evaluation of adult women

    Directory of Open Access Journals (Sweden)

    Hosana Gonçalves dos Santos

    2005-06-01

    Full Text Available O objetivo deste estudo foi validar um método de determinação de zinco eritrocitário (ZnER por espectrofotometria de absorção atômica (EAA, avaliar com esse parâmetro o estado nutricional em Zn de mulheres adultas, relacioná-lo com a ingestão dietética diária, identificando os alimentos fonte do mineral. O método foi validado com limites de detecção e de quantificação de 0,006 e 0,045(0,013 migZn/mL, respectivamente, e níveis de exatidão e de imprecisão intra-ensaio e inter-ensaio de 95 (0,4% , 3,6% e 5,3%, respectivamente. A ingestão média de Zn do grupo (n=21 foi de 9,7(3mgZn/dia e 15 desses resultados estão acima da RDA de 8 mg/d e 4 abaixo da EAR de 6,8 mg/d (Institute of Medicine/2000b. A concentração média de ZnER foi de 38,2(5 mgZn/gHb, valor menor do que o encontrado por outros autores para o mesmo gênero e estágio de vida. As fontes de Zn da dieta do grupo (>1,2 mg Zn/100 g foram: carnes bovina e suína, fígado bovino, linguiça, queijos dos tipos prato, branco, gouda e mussarela e amendoim.The aim of this study was to validate a method for determining erythrocytic Zn (ZnER by atomic absorption spectrophotometry (AAS, in order to evaluate, with this parameter, the Zn nutriture of adult women (n=21, and to relate it with the dietary daily Zn ingestion by the group. The method was validated with limits of detection and quantification of 0.006 and 0.045(0.013mgZn/mL, respectively, and accuracy and intra and inter-assay coefficients of variation of 95(0.4%, 3.6% and 5.3%, respectively. The average daily ingestion of Zn by the adult women was 9.7(3mgZn/d, 15 of them had intake levels above the Recommended Dietary Allowance of 8 mg/d (RDA/2001 and 4 below the Estimated Average Requirement of 6,8 mg/d (EAR /2001. The average concentration of ZnER was 38.2(5 mgZn/gHb, a value lower than that found by other authors for the same age and gender group. Food sources of Zn in their diets (>1.2 mg Zn/serving were: bovine

  18. Validation study of core analysis methods for full MOX BWR

    International Nuclear Information System (INIS)

    JNES has been developing a technical database used in reviewing validation of core analysis methods of LWRs in the coming occasions: (1) confirming the core safety parameters of the initial core (one-third MOX core) through a full MOX core in Oma Nuclear Power Plant, which is under the construction, (2) licensing high-burnup MOX cores in the future and (3) reviewing topical reports on core analysis codes for safety design and evaluation. Based on the technical database, JNES will issue a guide of reviewing the core analysis methods used for safety design and evaluation of LWRs. The database will be also used for validation and improving of core analysis codes developed by JNES. JNES has progressed with the projects: (1) improving a Doppler reactivity analysis model in a Monte Carlo calculation code MVP, (2) sensitivity study of nuclear cross section date on reactivity calculation of experimental cores composed of UO2 and MOX fuel rods, (3) analysis of isotopic composition data for UO2 and MOX fuels and (4) the guide of reviewing the core analysis codes and others. (author)

  19. Validation study of core analysis methods for full MOX BWR

    International Nuclear Information System (INIS)

    JNES has been developing a technical data base used in reviewing validation of core analysis methods of LWRs in the occasions: (1) confirming core safety parameters of the initial core (one-third MOX core) through a full MOX core in Oma Nuclear Power Plant, which is under the construction, (2) licensing high-burnup MOX cores in the future and (3) reviewing topical reports on core analysis codes for safety design and evaluation. Based on the technical data base, JNES will issue a guide of reviewing the core analysis methods used for safety design and evaluation of LWRs. The data base will be also used for validation and improving of core analysis codes developed by JNES. JNES has progressed with the projects (1) measurements of Doppler reactivity in experimental MOX core simulating LWR cores, (2) measurement of isotopic compositions of fission product nuclides on high-burn up BWR UO2 fuels and (3) neutronics analysis of the experimental data that has been obtained in the international joint programs such as FUBILA and REBUS. (author)

  20. Validation study of core analysis methods for full MOX BWR

    International Nuclear Information System (INIS)

    JNES has been developing a technical data base used in reviewing validation of core analysis methods of LWRs in the coming occasions: (1) confirming the core safety parameters of the initial core (one-third MOX core) through a full MOX core in Oma Nuclear Power Plant, which is under the construction, (2) licensing high-burnup MOX cores in the future and (3) reviewing topical reports on core analysis codes for safety design and evaluation. Based on the technical data base, JNES will issue a guide of reviewing the core analysis methods used for safety design and evaluation of LWRs. The data base will be also used for validation and improving of core analysis codes developed by JNES. JNES has progressed with the projects (1) analysis of the measurement data of Doppler reactivity in experimental MOX core simulating LWR cores, (2) measurements of isotopic compositions of fission product nuclides on high-burnup BWR UO2 fuels and the analysis of the measurement data, and (3) neutronics analysis of the experimental data that has been obtained in the international joint programs such as FUBILA and REBUS. (author)

  1. Spectrophotometric validation of assay method for selected medicinal plant extracts

    Directory of Open Access Journals (Sweden)

    Matthew Arhewoh

    2014-09-01

    Full Text Available Objective: To develop UV spectrophotometric assay validation methods for some selected medicinal plant extracts.Methods: Dried, powdered leaves of Annona muricata (AM and Andrographis paniculata (AP as well as seeds of Garcinia kola (GK and Hunteria umbellata (HU were separately subjected to maceration using distilled water. Different concentrations of the extracts were scanned spectrophotometrically to obtain wavelengths of maximum absorbance. The different extracts were then subjected to validation studies following international guidelines at the respective wavelengths obtained.Results: The results showed linearity at peak wavelengths of maximum absorbance of 292, 280, 274 and 230 nm for GK, HU, AM and AP, respectively. The calibration curves for the different concentrations of the extract gave R2 values ranging from 0.9831 for AM to 0.9996 for AP the inter-day and intra-day precision study showed that the relative standard deviation (% was ≤ 10% for all the extracts.Conclusion: The aqueous extracts and isolates of these plants can be assayed and monitored using these wavelengths.

  2. Analytical methods for 2,4-D (Dichlorophenoxyacetic acid) determination

    International Nuclear Information System (INIS)

    The 2,4-D herbicide is one of the main pesticides for controlling the bad grass in crops such as the water undergrowth. In Mexico the allowed bound of this pesticide is 0.05 mg/l in water of 2,4-D so it is required to have methods trusts and exacts, which can used in order to detected low concentration of it. In this work we show some for the conventional techniques and for establishing the 2,4-D concentrations. The UV-Vis spectrometer and liquids chromatography due that they are the most common used nowadays. Beside, we introduce a now developed technique, which is based on the neutronic activation analysis. Though use of the UV-Vis spectrometer technique it was possible target the concentrations interval between 1 and 200 mg/l. In the liquids chromatography interval was between 0.1 and 0.9, and by the neutronic activation analysis the interval was between 0.01 and 200 mg/l. (Author)

  3. An analytical method of estimating Value-at-Risk on the Belgrade Stock Exchange

    Directory of Open Access Journals (Sweden)

    Obadović Milica D.

    2009-01-01

    Full Text Available This paper presents market risk evaluation for a portfolio consisting of shares that are continuously traded on the Belgrade Stock Exchange, by applying the Value-at-Risk model - the analytical method. It describes the manner of analytical method application and compares the results obtained by implementing this method at different confidence levels. Method verification was carried out on the basis of the failure rate that demonstrated the confidence level for which this method was acceptable in view of the given conditions.

  4. Analytical validation of the Roche 25-OH Vitamin D Total assay

    DEFF Research Database (Denmark)

    Knudsen, Cindy Soendersoe; Nexo, Ebba; Højskov, Carsten Schriver;

    2012-01-01

    evaluated the 25-OH Vitamin D Total assay in comparison to our in-house liquid chromatography tandem mass spectrometry (LC-MS/MS) method [194 patient samples without 25-hydroxy vitamin D2 (25OHD2) and 23 patient samples containing 25OHD2]. Results: At concentrations of 34 and 56 nmol/L within-run CVs were 4.......8% and 1.9% and total CVs were 8.3% and 6.1%. We verified that the limit of quantification was 22.5 nmol/L, as stated by the manufacturer. No significant difference was observed between serum and plasma samples (Li-heparin). Comparison with LC-MS/MS using 194 samples containing 25OHD3 only (no 25OHD2...

  5. A retrieval and validation method for shelterbelt vegetation fraction

    Institute of Scientific and Technical Information of China (English)

    DENG Rong-xin; WANG Wen-juan; LI Ying; ZHAO Dong-bao

    2013-01-01

    Shelterbelts are important in defending against natural disaster and maintaining ecological balances in farmland.Understanding of the shelterbelt vegetation fraction is fundamental to regional research of shelterbelts using remote sensing.We used SPOT5 imagery with 10×10m spatial resolution in combination with knowledge of the characteristics of shelterbelts to develop a method for retrieval of the vegetation fraction of shelterbelts by the pixel un-mixing model.We then used the method to retrieve values for shelterbelts in study area.By combining the parameters of photographic images with characteristics of shelterbelts,we developed a method for measuring the vegetation fraction of shelterbelts based on an advanced photographic method.We then measured the actual values to validate the retrieval result.The multiple correlation coefficients between the retrieved and measured values were 0.715.Our retrieval and measuring methods presented in this paper accurately reflect field conditions.We suggest that this method is useful to describe shelterbelt structure using remote sensing.

  6. Validation of structural analysis methods using burner liner cyclic rig test data

    Science.gov (United States)

    Thompson, R.

    1983-01-01

    The objectives of the hot section technology (HOST) burner liner cyclic rig test program are basically threefold: (1) to assist in developing predictive tools needed to improve design analyses and procedures for the efficient and accurate prediction of burner liner structural response; (2) to calibrate, evaluate and validate these predictive tools by comparing the predicted results with the experimental data generated in the tests; and (3) to evaluate existing as well as advanced temperature and strain measurement instrumentation, both contact and noncontact, in a simulated engine cycle environment. The data generated will include measurements of the thermal environment (metal surface temperatures) as well as structural (strain) and life (fatigue) responses of simulated burner liners and specimens under controlled boundary and operating conditions. These data will be used to calibrate, compare and validate analytical theories, methodologies and design procedures, as well as improvements in them, for predicting liner temperatures, stress-strain responses and cycles to failure. Comparison of predicted results with experimental data will be used to show where the predictive theories, etc. need improvements. In addition, as the predictive tools, as well as the tests, test methods, and data acquisition and reduction techniques, are developed and validated, a proven, integrated analysis/experiment method will be developed to determine the cyclic life of a simulated burner liner.

  7. Chlorophenols in tap water from wells and surface sources in Rio de Janeiro, Brazil: method validation and analysis

    Directory of Open Access Journals (Sweden)

    André Victor Sartori

    2012-01-01

    Full Text Available Two analytical methods were validated for determination of trichlorophenols, tetrachlorophenols and pentachlorophenol in drinking water. Limits of quantification were at least ten times lower than maximum permissible levels set by the Brazilian legislation, which are 200 ng mL-1 for 2,4,6-trichlorophenol and 9 ng mL-1 for pentachlorophenol. Chlorophenol levels were determined in tap water collected in the Municipality of Rio de Janeiro. 2,4,6-Trichlorophenol residues were detected in 36% of the samples, varying from 0.008 to 0.238 ng mL-1. All other analytes were below the limit of quantification. The validated methods showed to be suitable for application in routine quality control.

  8. Experimental validation of finite element and boundary element methods for predicting structural vibration and radiated noise

    Science.gov (United States)

    Seybert, A. F.; Wu, T. W.; Wu, X. F.

    1994-01-01

    This research report is presented in three parts. In the first part, acoustical analyses were performed on modes of vibration of the housing of a transmission of a gear test rig developed by NASA. The modes of vibration of the transmission housing were measured using experimental modal analysis. The boundary element method (BEM) was used to calculate the sound pressure and sound intensity on the surface of the housing and the radiation efficiency of each mode. The radiation efficiency of each of the transmission housing modes was then compared to theoretical results for a finite baffled plate. In the second part, 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 level radiated from the box. The FEM was used to predict the vibration, while the BEM was used to predict the sound intensity and total radiated sound power using surface vibration as the input data. Vibration predicted by the FEM model was validated by experimental modal analysis; noise predicted by the BEM was validated by measurements of sound intensity. Three types of results are presented for the total radiated sound power: sound power predicted by the BEM model using vibration data measured on the surface of the box; sound power predicted by the FEM/BEM model; and sound power measured by an acoustic intensity scan. In the third part, the structure used in part two was modified. A rib was attached to the top plate of the structure. The FEM and BEM were then used to predict structural vibration and radiated noise respectively. The predicted vibration and radiated noise were then validated through experimentation.

  9. An introduction to clinical microeconomic analysis: purposes and analytic methods.

    Science.gov (United States)

    Weintraub, W S; Mauldin, P D; Becker, E R

    1994-06-01

    The recent concern with health care economics has fostered the development of a new discipline that is generally called clinical microeconomics. This is a discipline in which microeconomic methods are used to study the economics of specific medical therapies. It is possible to perform stand alone cost analyses, but more profound insight into the medical decision making process may be accomplished by combining cost studies with measures of outcome. This is most often accomplished with cost-effectiveness or cost-utility studies. In cost-effectiveness studies there is one measure of outcome, often death. In cost-utility studies there are multiple measures of outcome, which must be grouped together to give an overall picture of outcome or utility. There are theoretical limitations to the determination of utility that must be accepted to perform this type of analysis. A summary statement of outcome is quality adjusted life years (QALYs), which is utility time socially discounted survival. Discounting is used because people value a year of future life less than a year of present life. Costs are made up of in-hospital direct, professional, follow-up direct, and follow-up indirect costs. Direct costs are for medical services. Indirect costs reflect opportunity costs such as lost time at work. Cost estimates are often based on marginal costs, or the cost for one additional procedure of the same type. Finally an overall statistic may be generated as cost per unit increase in effectiveness, such as dollars per QALY.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:10151059

  10. Analytical and Clinical Validation of a Digital Sequencing Panel for Quantitative, Highly Accurate Evaluation of Cell-Free Circulating Tumor DNA.

    Directory of Open Access Journals (Sweden)

    Richard B Lanman

    Full Text Available Next-generation sequencing of cell-free circulating solid tumor DNA addresses two challenges in contemporary cancer care. First this method of massively parallel and deep sequencing enables assessment of a comprehensive panel of genomic targets from a single sample, and second, it obviates the need for repeat invasive tissue biopsies. Digital Sequencing™ is a novel method for high-quality sequencing of circulating tumor DNA simultaneously across a comprehensive panel of over 50 cancer-related genes with a simple blood test. Here we report the analytic and clinical validation of the gene panel. Analytic sensitivity down to 0.1% mutant allele fraction is demonstrated via serial dilution studies of known samples. Near-perfect analytic specificity (> 99.9999% enables complete coverage of many genes without the false positives typically seen with traditional sequencing assays at mutant allele frequencies or fractions below 5%. We compared digital sequencing of plasma-derived cell-free DNA to tissue-based sequencing on 165 consecutive matched samples from five outside centers in patients with stage III-IV solid tumor cancers. Clinical sensitivity of plasma-derived NGS was 85.0%, comparable to 80.7% sensitivity for tissue. The assay success rate on 1,000 consecutive samples in clinical practice was 99.8%. Digital sequencing of plasma-derived DNA is indicated in advanced cancer patients to prevent repeated invasive biopsies when the initial biopsy is inadequate, unobtainable for genomic testing, or uninformative, or when the patient's cancer has progressed despite treatment. Its clinical utility is derived from reduction in the costs, complications and delays associated with invasive tissue biopsies for genomic testing.

  11. Analytical and Clinical Validation of a Digital Sequencing Panel for Quantitative, Highly Accurate Evaluation of Cell-Free Circulating Tumor DNA

    Science.gov (United States)

    Zill, Oliver A.; Sebisanovic, Dragan; Lopez, Rene; Blau, Sibel; Collisson, Eric A.; Divers, Stephen G.; Hoon, Dave S. B.; Kopetz, E. Scott; Lee, Jeeyun; Nikolinakos, Petros G.; Baca, Arthur M.; Kermani, Bahram G.; Eltoukhy, Helmy; Talasaz, AmirAli

    2015-01-01

    Next-generation sequencing of cell-free circulating solid tumor DNA addresses two challenges in contemporary cancer care. First this method of massively parallel and deep sequencing enables assessment of a comprehensive panel of genomic targets from a single sample, and second, it obviates the need for repeat invasive tissue biopsies. Digital SequencingTM is a novel method for high-quality sequencing of circulating tumor DNA simultaneously across a comprehensive panel of over 50 cancer-related genes with a simple blood test. Here we report the analytic and clinical validation of the gene panel. Analytic sensitivity down to 0.1% mutant allele fraction is demonstrated via serial dilution studies of known samples. Near-perfect analytic specificity (> 99.9999%) enables complete coverage of many genes without the false positives typically seen with traditional sequencing assays at mutant allele frequencies or fractions below 5%. We compared digital sequencing of plasma-derived cell-free DNA to tissue-based sequencing on 165 consecutive matched samples from five outside centers in patients with stage III-IV solid tumor cancers. Clinical sensitivity of plasma-derived NGS was 85.0%, comparable to 80.7% sensitivity for tissue. The assay success rate on 1,000 consecutive samples in clinical practice was 99.8%. Digital sequencing of plasma-derived DNA is indicated in advanced cancer patients to prevent repeated invasive biopsies when the initial biopsy is inadequate, unobtainable for genomic testing, or uninformative, or when the patient’s cancer has progressed despite treatment. Its clinical utility is derived from reduction in the costs, complications and delays associated with invasive tissue biopsies for genomic testing. PMID:26474073

  12. Video quality experts group: the quest for valid objective methods

    Science.gov (United States)

    Corriveau, Philip J.; Webster, Arthur A.; Rohaly, Ann M.; Libert, John M.

    2000-06-01

    Subjective assessment methods have been used reliably for many years to evaluate video quality. They continue to provide the most reliable assessments compared to objective methods. Some issues that arise with subjective assessment include the cost of conducting the evaluations and the fact that these methods cannot easily be used to monitor video quality in real time. Furthermore, traditional, analog objective methods, while still necessary, are not sufficient to measure the quality of digitally compressed video systems. Thus, there is a need to develop new objective methods utilizing the characteristics of the human visual system. While several new objective methods have been developed, there is to date no internationally standardized method. The Video Quality Experts Group (VQEG) was formed in October 1997 to address video quality issues. The group is composed of experts from various backgrounds and affiliations, including participants from several internationally recognized organizations working in the field of video quality assessment. The majority of participants are active in the International Telecommunications Union (ITU) and VQEG combines the expertise and resources found in several ITU Study Groups to work towards a common goal. The first task undertaken by VQEG was to provide a validation of objective video quality measurement methods leading to Recommendations in both the Telecommunications (ITU-T) and Radiocommunication (ITU-R) sectors of the ITU. To this end, VQEG designed and executed a test program to compare subjective video quality evaluations to the predictions of a number of proposed objective measurement methods for video quality in the bit rate range of 768 kb/s to 50 Mb/s. The results of this test show that there is no objective measurement system that is currently able to replace subjective testing. Depending on the metric used for evaluation, the performance of eight or nine models was found to be statistically equivalent, leading to the

  13. Validation of thermodesorption method for analysis of semi-volatile organic compounds adsorbed on wafer surface.

    Science.gov (United States)

    Hayeck, Nathalie; Gligorovski, Sasho; Poulet, Irène; Wortham, Henri

    2014-05-01

    To prevent the degradation of the device characteristics it is important to detect the organic contaminants adsorbed on the wafers. In this respect, a reliable qualitative and quantitative analytical method for analysis of semi-volatile organic compounds which can adsorb on wafer surfaces is of paramount importance. Here, we present a new analytical method based on Wafer Outgassing System (WOS) coupled to Automated Thermal Desorber-Gas chromatography-Mass spectrometry (ATD-GC-MS) to identify and quantify volatile and semi-volatile organic compounds from 6", 8" and 12" wafers. WOS technique allows the desorption of organic compounds from one side of the wafers. This method was tested on three important airborne contaminants in cleanroom i.e. tris-(2-chloroethyl) phosphate (TCEP), tris-(2-chloroisopropyl) phosphate (TCPP) and diethyl phthalate (DEP). In addition, we validated this method for the analysis and quantification of DEP, TCEP and TCPP and we estimated the backside organic contamination which may contribute to the front side of the contaminated wafers. We are demonstrating that WOS/ATD-GC-MS is a suitable and highly efficient technique for desorption and quantitative analysis of organophosphorous compounds and phthalate ester which could be found on the wafer surface.

  14. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina por espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

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

  15. Analytical recovery of protozoan enumeration methods: have drinking water QMRA models corrected or created bias?

    Science.gov (United States)

    Schmidt, P J; Emelko, M B; Thompson, M E

    2013-05-01

    Quantitative microbial risk assessment (QMRA) is a tool to evaluate the potential implications of pathogens in a water supply or other media and is of increasing interest to regulators. In the case of potentially pathogenic protozoa (e.g. Cryptosporidium oocysts and Giardia cysts), it is well known that the methods used to enumerate (oo)cysts in samples of water and other media can have low and highly variable analytical recovery. In these applications, QMRA has evolved from ignoring analytical recovery to addressing it in point-estimates of risk, and then to addressing variation of analytical recovery in Monte Carlo risk assessments. Often, variation of analytical recovery is addressed in exposure assessment by dividing concentration values that were obtained without consideration of analytical recovery by random beta-distributed recovery values. A simple mathematical proof is provided to demonstrate that this conventional approach to address non-constant analytical recovery in drinking water QMRA will lead to overestimation of mean pathogen concentrations. The bias, which can exceed an order of magnitude, is greatest when low analytical recovery values are common. A simulated dataset is analyzed using a diverse set of approaches to obtain distributions representing temporal variation in the oocyst concentration, and mean annual risk is then computed from each concentration distribution using a simple risk model. This illustrative example demonstrates that the bias associated with mishandling non-constant analytical recovery and non-detect samples can cause drinking water systems to be erroneously classified as surpassing risk thresholds.

  16. Development of an Analytical System for Determination of Free Acid via a Joint Method Combining Density and Conductivity Measurement

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    Determination of free acid plays an important role in spent nuclear fuel reprocessing. It is necessary to develop a rapid analytical device and method for measuring free acid. A novel analytical system and method was studied to monitor the acidity

  17. Validated Spectrophotometric Methods for the Determination of Mycophenolate: An Anti-Neoplastic Agent in Bulk and Pharmaceutical Dosage Forms

    Directory of Open Access Journals (Sweden)

    A. Narendra

    2013-01-01

    Full Text Available Three simple, precise and cost-effective spectrophotometric methods have been developed for the determination of Mycophenolate in bulk and its pharmaceutical formulations. Mycophenolate shows max at 250.0 nm in zero-derivative spectrum (method A, 258.0 nm in first-derivative spectrum (method B and method C is based on the calculation of area under curve (AUC for analysis of Mycophenolate in the wavelength range of 240.0–260.0 nm. The drug follows the Beer-Lambert's law in the concentration range of 1.0–150.0 μg/mL for all the methods. The methods were validated by following the analytical performance parameters suggested by the International Conference on Harmonization. All validation parameters were within the acceptable range. The developed methods were successfully applied to estimate the amount of Mycophenolate in bulk and pharmaceutical dosage forms.

  18. Validation of internal dosimetry protocols based on stochastic method

    Energy Technology Data Exchange (ETDEWEB)

    Mendes, Bruno M.; Fonseca, Telma C.F., E-mail: bmm@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Almeida, Iassudara G.; Trindade, Bruno M.; Campos, Tarcisio P.R., E-mail: tprcampos@yahoo.com.br [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Departamento de Engenharia Nuclear

    2015-07-01

    Computational phantoms adapted to Monte Carlo codes have been applied successfully in radiation dosimetry fields. NRI research group has been developing Internal Dosimetry Protocols - IDPs, addressing distinct methodologies, software and computational human-simulators, to perform internal dosimetry, especially for new radiopharmaceuticals. Validation of the IDPs is critical to ensure the reliability of the simulations results. Inter comparisons of data from literature with those produced by our IDPs is a suitable method for validation. The aim of this study was to validate the IDPs following such inter comparison procedure. The Golem phantom has been reconfigured to run on MCNP5. The specific absorbed fractions (SAF) for photon at 30, 100 and 1000 keV energies were simulated based on the IDPs and compared with reference values (RV) published by Zankl and Petoussi-Henss, 1998. The SAF average differences from RV and those obtained in IDP simulations was 2.3 %. The SAF largest differences were found in situations involving low energy photons at 30 keV. The Adrenals and thyroid, i.e. the lowest mass organs, had the highest SAF discrepancies towards RV as 7.2 % and 3.8 %, respectively. The statistic differences of SAF applying our IDPs from reference values were considered acceptable at the 30, 100 and 1000 keV spectra. We believe that the main reason for the discrepancies in IDPs run, found in lower masses organs, was due to our source definition methodology. Improvements of source spatial distribution in the voxels may provide outputs more consistent with reference values for lower masses organs. (author)

  19. Subsidence modelling with analytic elements.

    NARCIS (Netherlands)

    Fokker, P.A.; Orlic, B.

    2000-01-01

    The method of Analytic Elements has been extended to enable elasticity calculations, to evaluate subsidence at the surface as resulting from extraction of oil or gas. Validation has been achieved by comparison with more limited analytical methods and with a comprehensive finite-element simulator. Th

  20. Validated spectrofluorometric methods for determination of amlodipine besylate in tablets

    Science.gov (United States)

    Abdel-Wadood, Hanaa M.; Mohamed, Niveen A.; Mahmoud, Ashraf M.

    2008-08-01

    Two simple and sensitive spectrofluorometric methods have been developed and validated for determination of amlodipine besylate (AML) in tablets. The first method was based on the condensation reaction of AML with ninhydrin and phenylacetaldehyde in buffered medium (pH 7.0) resulting in formation of a green fluorescent product, which exhibits excitation and emission maxima at 375 and 480 nm, respectively. The second method was based on the reaction of AML with 7-chloro-4-nitro-2,1,3-benzoxadiazole (NBD-Cl) in a buffered medium (pH 8.6) resulting in formation of a highly fluorescent product, which was measured fluorometrically at 535 nm ( λex, 480 nm). The factors affecting the reactions were studied and optimized. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.9949-0.9997) were found between the fluorescence intensity and the concentrations of AML in the concentration range of 0.35-1.8 and 0.55-3.0 μg ml -1 for ninhydrin and NBD-Cl methods, respectively. The limits of assays detection were 0.09 and 0.16 μg ml -1 for the first and second method, respectively. The precisions of the methods were satisfactory; the relative standard deviations were ranged from 1.69 to 1.98%. The proposed methods were successfully applied to the analysis of AML in pure and pharmaceutical dosage forms with good accuracy; the recovery percentages ranged from 100.4-100.8 ± 1.70-2.32%. The results were compared favorably with those of the reported method.

  1. Protein structure validation using a semi-empirical method

    Science.gov (United States)

    Lahiri, Tapobrata; Singh, Kalpana; Pal, Manoj Kumar; Verma, Gaurav

    2012-01-01

    Current practice of validating predicted protein structural model is knowledge-based where scoring parameters are derived from already known structures to obtain decision on validation out of this structure information. For example, the scoring parameter, Ramachandran Score gives percentage conformity with steric-property higher value of which implies higher acceptability. On the other hand, Force-Field Energy Score gives conformity with energy-wise stability higher value of which implies lower acceptability. Naturally, setting these two scoring parameters as target objectives sometimes yields a set of multiple models for the same protein for which acceptance based on a particular parameter, say, Ramachandran score, may not satisfy well with the acceptance of the same model based on other parameter, say, energy score. The confusion set of such models can further be resolved by introducing some parameters value of which are easily obtainable through experiment on the same protein. In this piece of work it was found that the confusion regarding final acceptance of a model out of multiple models of the same protein can be removed using a parameter Surface Rough Index which can be obtained through semi-empirical method from the ordinary microscopic image of heat denatured protein. PMID:23275692

  2. Indentation Measurements to Validate Dynamic Elasticity Imaging Methods.

    Science.gov (United States)

    Altahhan, Khaldoon N; Wang, Yue; Sobh, Nahil; Insana, Michael F

    2016-09-01

    We describe macro-indentation techniques for estimating the elastic modulus of soft hydrogels. Our study describes (a) conditions under which quasi-static indentation can validate dynamic shear-wave imaging estimates and (b) how each of these techniques uniquely biases modulus estimates as they couple to the sample geometry. Harmonic shear waves between 25 and 400 Hz were imaged using ultrasonic Doppler and optical coherence tomography methods to estimate shear dispersion. From the shear-wave speed of sound, average elastic moduli of homogeneous samples were estimated. These results are compared directly with macroscopic indentation measurements measured two ways. One set of measurements applied Hertzian theory to the loading phase of the force-displacement curves using samples treated to minimize surface adhesion forces. A second set of measurements applied Johnson-Kendall-Roberts theory to the unloading phase of the force-displacement curve when surface adhesions were significant. All measurements were made using gelatin hydrogel samples of different sizes and concentrations. Agreement within 5% among elastic modulus estimates was achieved for a range of experimental conditions. Consequently, a simple quasi-static indentation measurement using a common gel can provide elastic modulus measurements that help validate dynamic shear-wave imaging estimates. PMID:26376923

  3. Analytical chemistry in semiconductor manufacturing: Techniques, role of nuclear methods and need for quality control

    International Nuclear Information System (INIS)

    This report is the result of a consultants meeting held in Gaithersburg, USA, 2-3 October 1987. The meeting was hosted by the National Bureau of Standards and Technology, and it was attended by 18 participants from Denmark, Finland, India, Japan, Norway, People's Republic of China and the USA. The purpose of the meeting was to assess the present status of analytical chemistry in semiconductor manufacturing, the role of nuclear analytical methods and the need for internationally organized quality control of the chemical analysis. The report contains the three presentations in full and a summary report of the discussions. Thus, it gives an overview of the need of analytical chemistry in manufacturing of silicon based devices, the use of nuclear analytical methods, and discusses the need for quality control. Refs, figs and tabs

  4. LC-MS/MS multi-analyte method for mycotoxin determination in food supplements

    OpenAIRE

    Diana Di Mavungu, José; Monbaliu, Sofie; Scippo, Marie-Louise; Maghuin-Rogister, Guy; Schneider, Yves-Jacques; Larondelle, Yvan; Callebaut, Alfons; Robbens, Johan; Van Peteghem, Carlos; De Saeger, Sarah

    2009-01-01

    Abstract A multi-analyte method for the liquid chromatography-tandem mass spectrometric determination of mycotoxins in food supplements is presented. The analytes included A and B trichothecenes (nivalenol, deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, neosolaniol, fusarenon-X, diacetoxyscirpenol, HT-2 toxin and T-2 toxin), aflatoxins (aflatoxin-B1, aflatoxin-B2, aflatoxin-G1 and aflatoxin-G2), Alternaria toxins (alternariol, alternariol methyl ether and altenuen...

  5. Application of Statistical Methods to Activation Analytical Results near the Limit of Detection

    DEFF Research Database (Denmark)

    Heydorn, Kaj; Wanscher, B.

    1978-01-01

    Reporting actual numbers instead of upper limits for analytical results at or below the detection limit may produce reliable data when these numbers are subjected to appropriate statistical processing. Particularly in radiometric methods, such as activation analysis, where individual standard...... deviations of analytical results may be estimated, improved discrimination may be based on the Analysis of Precision. Actual experimental results from a study of the concentrations of arsenic in human skin demonstrate the power of this principle....

  6. Analytic Continuation in the Coupling Constant Method for the Dirac Equation

    Institute of Scientific and Technical Information of China (English)

    张时声; 郭建友; 张双全; 孟杰

    2004-01-01

    On the basis of the Dirac equation, the analytic continuation in the coupling constant method is employed to investigate the energies and widths of single-particle resonant in square-well, harmonic-oscillator, and Woodsconvergent energies and widths of single-particle resonant states can be obtained, which makes the application of the analytic continuation in the coupling constant for the relativistic mean field theory possible.

  7. Exploring valid and reliable assessment methods for care management education.

    Science.gov (United States)

    Gennissen, Lokke; Stammen, Lorette; Bueno-de-Mesquita, Jolien; Wieringa, Sietse; Busari, Jamiu

    2016-07-01

    Purpose It is assumed that the use of valid and reliable assessment methods can facilitate the development of medical residents' management and leadership competencies. To justify this assertion, the perceptions of an expert panel of health care leaders were explored on assessment methods used for evaluating care management (CM) development in Dutch residency programs. This paper aims to investigate how assessors and trainees value these methods and examine for any inherent benefits or shortcomings when they are applied in practice. Design/methodology/approach A Delphi survey was conducted among members of the platform for medical leadership in The Netherlands. This panel of experts was made up of clinical educators, practitioners and residents interested in CM education. Findings Of the respondents, 40 (55.6 per cent) and 31 (43 per cent) participated in the first and second rounds of the Delphi survey, respectively. The respondents agreed that assessment methods currently being used to measure residents' CM competencies were weak, though feasible for use in many residency programs. Multi-source feedback (MSF, 92.1 per cent), portfolio/e-portfolio (86.8 per cent) and knowledge testing (76.3 per cent) were identified as the most commonly known assessment methods with familiarity rates exceeding 75 per cent. Practical implications The findings suggested that an "assessment framework" comprising MSF, portfolios, individual process improvement projects or self-reflections and observations in clinical practice should be used to measure CM competencies in residents. Originality/value This study reaffirms the need for objective methods to assess CM skills in post-graduate medical education, as there was not a single assessment method that stood out as the best instrument. PMID:27397747

  8. Validation of a liquid chromatographic method for the pharmaceutical quality control of products containing elacridar

    Directory of Open Access Journals (Sweden)

    Emilia Sawicki

    2016-08-01

    Full Text Available Many anticancer drugs have an impaired bioavailability and poor brain penetration because they are substrates to drug efflux pumps such as P-glycoprotein and Breast Cancer Resistance Protein. Elacridar is a strong inhibitor of these two drug efflux pumps and therefore has great potential to improve oral absorption and brain penetration of many anticancer drugs. Currently, a clinical formulation of elacridar is unavailable and therefore the pharmaceutical development of a drug product is highly warranted. This also necessitates the availability of an analytical method for its quality control. A reverse-phase high-performance liquid chromatographic method with ultraviolet detection was developed for the pharmaceutical quality control of products containing elacridar as the active pharmaceutical ingredient. The analytical method was validated for linearity, accuracy, precision, selectivity, carry-over, stability of stock and reference solutions, stability of the final extract, stability-indicating capability and impurity testing. We found that elacridar is unstable in aqueous solutions that are exposed to light because a hydroxylation product of elacridar is formed. Therefore, sample solutions with elacridar must be protected from light.

  9. Validation of a liquid chromatographic method for the pharmaceutical quality control of products containing elacridar$

    Institute of Scientific and Technical Information of China (English)

    Emilia Sawicki; Michel J. Hillebrand; Hilde Rosing; Jan H.M. Schellens; Bastiaan Nuijen; Jos H. Beijnen

    2016-01-01

    Many anticancer drugs have an impaired bioavailability and poor brain penetration because they are sub-strates to drug efflux pumps such as P-glycoprotein and Breast Cancer Resistance Protein. Elacridar is a strong inhibitor of these two drug efflux pumps and therefore has great potential to improve oral absorption and brain penetration of many anticancer drugs. Currently, a clinical formulation of elacridar is unavailable and therefore the pharmaceutical development of a drug product is highly warranted. This also necessitates the availability of an analytical method for its quality control. A reverse-phase high-performance liquid chro-matographic method with ultraviolet detection was developed for the pharmaceutical quality control of products containing elacridar as the active pharmaceutical ingredient. The analytical method was validated for linearity, accuracy, precision, selectivity, carry-over, stability of stock and reference solutions, stability of the final extract, stability-indicating capability and impurity testing. We found that elacridar is unstable in aqueous solutions that are exposed to light because a hydroxylation product of elacridar is formed. Therefore, sample solutions with elacridar must be protected from light.

  10. Validation of a method for the targeted analysis of 96 drugs in hair by UPLC-MS/MS

    DEFF Research Database (Denmark)

    Montesano, Camilla; Johansen, Sys Stybe; Nielsen, Marie Katrine Klose

    2014-01-01

    in drug facilitated assaults (DFA); however, chronic use (compliance) can also be examined. The method has been fully validated for the drugs included in the study. The accuracy of the method was demonstrated by the analysis of certified authentic hair samples containing common drugs of abuse. The hair......-method has broad potential as the measuring range is wide for the target analytes and new drugs can easily be added to the method due to the versatility of the extraction procedure and chromatographic system....

  11. Validating for Use and Interpretation: A Mixed Methods Contribution Illustrated

    Science.gov (United States)

    Morell, Linda; Tan, Rachael Jin Bee

    2009-01-01

    Researchers in the areas of psychology and education strive to understand the intersections among validity, educational measurement, and cognitive theory. Guided by a mixed model conceptual framework, this study investigates how respondents' opinions inform the validation argument. Validity evidence for a science assessment was collected through…

  12. DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC ESTIMATION OF EBASTINE IN BULK AND TABLET DOSAGE FORM USING AREA UNDER CURVE METHOD

    Directory of Open Access Journals (Sweden)

    Dahivadkar Manish Sudhakar

    2013-06-01

    Full Text Available The aim of this work is to develop a simple, accurate, reproducible and cost effective spectrophotometric method for determination of Ebastine in bulk and pharmaceutical dosage form. This method is basedon area under curve (AUC in wavelength range of 247-257nm and method has followed linearity in the concentration range of 5-30μg/ml. Methanol was used as a solvent. The developed analytical method was validated as per International Conference on Harmonization (ICH guidelines. The value of correlation coefficient (R2 was 0.999. Limit of Detection and Limit of Quantitation were calculated as 0.78µg/ml and 2.37µg/ml, respectively. Results of the recovery studies showed good accuracy of the method. Validation results suggest that the developed method can be used for routine quality control studies for assay of Ebastine in bulk and tablet dosage form.

  13. Validação de um método analítico para a determinação de substâncias ativas em formulações farmacêuticas empregadas em "peelings" químicos Validation of analytical methods for the determination of active substances in pharmaceutical preparations used in chemical peelings

    Directory of Open Access Journals (Sweden)

    Tatiane Rodrigues Ramos

    2005-06-01

    Full Text Available Nos "peelings" químicos utilizam-se formulações esfoliantes, empregadas na terapêutica de queratoses actínicas, rugas, discromias pigmentares, acne vulgar e rosácea. Na presente pesquisa, foram empregadas como amostras, a solução de Jessner (SJ composta por resorcinol (RS 14%, ácido salicílico (AS 14% e ácido láctico (AL 14% em solução alcoólica e géis de AS a 20% e RS a 30%. As técnicas utilizadas foram a espectrofotometria derivada no UV de primeira e segunda ordens em etanol absoluto para o AS e RS, respectivamente na SJ, e a espectrofotometria derivada no UV de primeira ordem em ácido sulfúrico 0,1 N para o AS e RS nos géis. Para o AS na SJ, o coeficiente de correlação (r foi de 0,9999, a precisão expressa pela média dos desvios padrão relativos (DPR de 0,68% e a exatidão expressa pela recuperação média de 100,5%. Para o RS na SJ o r foi de 0,9999, a média dos DPR de 0,83% e a recuperação média de 100,3%. No gel de AS, o r foi de 0,9999, a média dos DPR de 0,28 e a recuperação média de 99,3%. No gel de RS, o r foi de 0,9998, a média dos DPR de 0,34 e a recuperação média de 99,9%.Chemical peeling is obtained with exfoliating formulations and is used in the treatment of actinic keratosis, wrinkles, dyschromies, acne vulgaris and rosacea acne. In this research we selected the Jessner Solution (JS, a pharmaceutical preparation composed of resorcinol (RS (14%, salicylic acid (SA (14% and lactic acid (LA (14% in alcoholic solution and two gel samples composed of RS (30% and SA (20%, respectively. First and second derivative UV spectrophotometric methods were developed and validated for determination of SA and RS, respectively in JS alcoholic solution, ethanol was used as background. A first derivative UV spectrophotometric method was developed for determination of these active substances in gel samples using 0.1N sulfuric acid as background. For SA in the JS, the correlation coefficient (r was 0.9999, the

  14. [Methods for quantifying phasic skin conductance amplitudes: threats to validity?].

    Science.gov (United States)

    Zimmer, H; Vossel, G

    1993-01-01

    Two methods of determining the event-related skin conductance response (SCR) amplitude are in common use. In one of these, the difference in conductance between the point of onset and the peak level of a single wave is measured (method 1). The second approach is to determine the difference between two measures, one characterizing the prestimulus level, the other the highest conductance point of the SCR reached within a fixed period following the stimulus (method 2). A problem with quantifying the SCR amplitude occurs when a SCR is elicited before an immediately preceding response has had time to recover, because in this case the two methods lead to quite different values. If the amplitude of each response is measured from its own individual deflection point, the measurable amplitude of the second response will be smaller when it occurs immediately after or in the ascending limb of the first response. The problem is most evident in situations with a high probability of response superimposition, such as when a large number of nonspecific responses occur at the same time as the SCRs. This is found in individuals with a high degree of electrodermal lability. Electrodermal lability refers to a psychophysiological construct that is operationally defined by the frequency of spontaneous electrodermal fluctuations. In the present study, we therefore systematically investigated the effects of the two score methods on SCR amplitude in relation to lability by analyzing electrodermal data from two habituation studies. As expected, several method-specific effects which were related to lability emerged. Results and questions concerning the relevance of the findings are discussed, with special emphasis on the validity of psychophysiological investigations.

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

    Directory of Open Access Journals (Sweden)

    Lidija Zadnik-Stirn

    2010-12-01

    Full Text Available 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 aggregation of individual judgments or priorities: weighted arithmetic mean method, weighted geometric mean method, and four methods based on data envelopment analysis are compared. The case study on land use in Slovenia is applied. The conclusions review consistency, sensitivity analyses, and some future directions of research.

  16. OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

    Directory of Open Access Journals (Sweden)

    Maja Vrkljan

    2004-12-01

    Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

  17. Analytical methods for vancomycin determination in biological fluids and in pharmaceuticals

    Directory of Open Access Journals (Sweden)

    Marta Maria Duarte Carvalho Vila

    2007-04-01

    Full Text Available Vancomycin is a glycopeptide antibiotic employed in the treatment of infections caused by certain methicillin-resistant staphylococci. It is indicated also for patients allergic to penicillin or when there is no response to penicillins or cephalosporins. The adequate vancomycin concentration levels in blood serum lies between 5 and 10 mg/L. Higher values are toxic, causing mainly nephrotoxicity and ototoxicity. Various analytical methods are described in the literature: spectrophotometric, immunologic, biologic and chromatographic methods. This paper reviews the main analytical methods for vancomycin determination in biological fluids and in pharmaceutical preparations.

  18. A method based on stochastic resonance for the detection of weak analytical signal.

    Science.gov (United States)

    Wu, Xiaojing; Guo, Weiming; Cai, Wensheng; Shao, Xueguang; Pan, Zhongxiao

    2003-12-23

    An effective method for detection of weak analytical signals with strong noise background is proposed based on the theory of stochastic resonance (SR). Compared with the conventional SR-based algorithms, the proposed algorithm is simplified by changing only one parameter to realize the weak signal detection. Simulation studies revealed that the method performs well in detection of analytical signals in very high level of noise background and is suitable for detecting signals with the different noise level by changing the parameter. Applications of the method to experimental weak signals of X-ray diffraction and Raman spectrum are also investigated. It is found that reliable results can be obtained.

  19. Determination of nifuroxazide and drotaverine hydrochloride in pharmaceutical preparations by three independent analytical methods.

    Science.gov (United States)

    Metwally, Fadia H; Abdelkawy, Mohammed; Naguib, Ibrahim A

    2006-01-01

    Three new, different, simple, sensitive, and accurate methods were developed for quantitative determination of nifuroxazide (I) and drotaverine hydrochloride (II) in a binary mixture. The first method was spectrophotometry, which allowed determination of I in the presence of II using a zero-order spectrum with an analytically useful maximum at 364.5 nm that obeyed Beer's law over a concentration range of 2-10 microg/mL with mean percentage recovery of 100.08 +/- 0.61. Determination of II in presence of I was obtained by second derivative spectrophotometry at 243.6 nm, which obeyed Beer's law over a concentration range of 2-10 microg/mL with mean recovery of 99.82 +/- 1.46%. The second method was spectrodensitometry, with which both drugs were separated on a silica gel plate using chloroform-acetone-methanol-glacial acetic acid (6 + 3 + 0.9 + 0.1) as the mobile phase and ultraviolet (UV) detection at 365 nm over a concentration range of 0.2-1 microg/band for both drugs, with mean recoveries of 99.99 +/- 0.15 and 100.00 +/- 0.34% for I and II, respectively. The third method was reversed-phase liquid chromatography using acetonitrile-water (40 + 60, v/v; adjusted to pH 2.55 with orthophosphoric acid) as the mobile phase and pentoxifylline as the internal standard at a flow rate of 1 mU/min with UV detection at 285 nm at ambient temperature over a concentration range of 2-10 microg/mL for both drugs, with mean recoveries of 100.24 +/- 1.51 and 100.08 +/- 0.78% for I and II, respectively. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulations containing the above drugs with no interference from other dosage form additives. The validity of the suggested procedures was further assessed by applying the standard addition technique which was found to be satisfactory, and the percentage recoveries obtained were in accordance with those given by the EVA Pharma reference

  20. Rapid and alternative fabrication method for microfluidic paper based analytical devices.

    Science.gov (United States)

    Malekghasemi, Soheil; Kahveci, Enver; Duman, Memed

    2016-10-01

    A major application of microfluidic paper-based analytical devices (µPADs) includes the field of point-of-care (POC) diagnostics. It is important for POC diagnostics to possess properties such as ease-of-use and low cost. However, µPADs need multiple instruments and fabrication steps. In this study, two different chemicals (Hexamethyldisilazane and Tetra-ethylorthosilicate) were used, and three different methods (heating, plasma treatment, and microwave irradiation) were compared to develop µPADs. Additionally, an inkjet-printing technique was used for generating a hydrophilic channel and printing certain chemical agents on different regions of a modified filter paper. A rapid and effective fabrication method to develop µPADs within 10min was introduced using an inkjet-printing technique in conjunction with a microwave irradiation method. Environmental scanning electron microscope (ESEM) and x-ray photoelectron spectroscopy (XPS) were used for morphology characterization and determining the surface chemical compositions of the modified filter paper, respectively. Contact angle measurements were used to fulfill the hydrophobicity of the treated filter paper. The highest contact angle value (141°±1) was obtained using the microwave irradiation method over a period of 7min, when the filter paper was modified by TEOS. Furthermore, by using this method, the XPS results of TEOS-modified filter paper revealed Si2p (23%) and Si-O bounds (81.55%) indicating the presence of Si-O-Si bridges and Si(OEt) groups, respectively. The ESEM results revealed changes in the porous structures of the papers and decreases in the pore sizes. Washburn assay measurements tested the efficiency of the generated hydrophilic channels in which similar water penetration rates were observed in the TEOS-modified filter paper and unmodified (plain) filter paper. The validation of the developed µPADs was performed by utilizing the rapid urease test as a model test system. The detection limit of

  1. Validation of uranium determination by ICP-SMS from QC samples from the IAEA Safeguards Analytical Laboratory

    International Nuclear Information System (INIS)

    The IAEA Safeguards Analytical Laboratory (SAL) recently installed a high-resolution inductively coupled plasma sector-field mass spectrometer (ICP-SMS) for determination of uranium concentration down to environmental levels, with the goal of enhancing the efficiency of the analysis of quality control samples at the IAEA Clean Laboratory for Safeguards. The most challenging samples from the Clean Laboratory are room blanks, which commonly have uranium contents of 0.1 to 5 pg. The location of the instrument in the nuclear area of SAL poses challenges regarding the realistic lower working detection and quantification limits of uranium. A systematic experimental study was implemented to validate the performance of the ICP-SMS under routine operational conditions. The results demonstrate that reliable, precise determinations of uranium can be made at concentrations of ≥200 ppq with a standard uncertainty down to ∼1%, assuming proper precautions against contamination are taken and the unknown sample is well bounded by fresh calibration curves. At this performance level, the ICP-SMS at SAL is capable of reliably detecting and measuring uranium for the purposes of the Clean Laboratory. (author)

  2. Contextual and Analytic Qualities of Research Methods Exemplified in Research on Teaching

    Science.gov (United States)

    Svensson, Lennart; Doumas, Kyriaki

    2013-01-01

    The aim of the present article is to discuss contextual and analytic qualities of research methods. The arguments are specified in relation to research on teaching. A specific investigation is used as an example to illustrate the general methodological approach. It is argued that research methods should be carefully grounded in an understanding of…

  3. Flammable gas safety program. Analytical methods development: FY 1994 progress report

    International Nuclear Information System (INIS)

    This report describes the status of developing analytical methods to account for the organic components in Hanford waste tanks, with particular focus 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-101 (Tank 101-SY)

  4. Application of the analytic hierarchy process method in the selection of optimal tactical radio communication systems

    Directory of Open Access Journals (Sweden)

    Saša M. Devetak

    2011-07-01

    Full Text Available This article deals with the analytic hierarchy process method in selecting an optimal tactic radio communication system. The problem has been defined, followed by the description of the AHP method procedure as well as the criteria and alternatives for radio communication systems. The problem was solved using the mathematical model and the presented software.

  5. Application of the analytic hierarchy process method in the selection of optimal tactical radio communication systems

    OpenAIRE

    Saša M. Devetak; Miroslav R. Terzić

    2011-01-01

    This article deals with the analytic hierarchy process method in selecting an optimal tactic radio communication system. The problem has been defined, followed by the description of the AHP method procedure as well as the criteria and alternatives for radio communication systems. The problem was solved using the mathematical model and the presented software.

  6. System and Method for Providing a Climate Data Analytic Services Application Programming Interface Distribution Package

    Science.gov (United States)

    Schnase, John L. (Inventor); Duffy, Daniel Q. (Inventor); Tamkin, Glenn S. (Inventor)

    2016-01-01

    A system, method and computer-readable storage devices for providing a climate data analytic services application programming interface distribution package. The example system can provide various components. The system provides a climate data analytic services application programming interface library that enables software applications running on a client device to invoke the capabilities of a climate data analytic service. The system provides a command-line interface that provides a means of interacting with a climate data analytic service by issuing commands directly to the system's server interface. The system provides sample programs that call on the capabilities of the application programming interface library and can be used as templates for the construction of new client applications. The system can also provide test utilities, build utilities, service integration utilities, and documentation.

  7. Analytical solution of population balance equation involving aggregation and breakage in terms of auxiliary equation method

    Indian Academy of Sciences (India)

    Zehra Pinar; Abhishek Dutta; Guido Bény; Turgut Öziş

    2015-01-01

    This paper presents an effective analytical simulation to solve population balance equation (PBE), involving particulate aggregation and breakage, by making use of appropriate solution(s) of associated complementary equation via auxiliary equation method (AEM). Travelling wave solutions of the complementary equation of a nonlinear PBE with appropriately chosen parameters is taken to be analogous to the description of the dynamic behaviour of the particulate processes. For an initial proof-of-concept, a general case when the number of particles varies with respect to time is chosen. Three cases, i.e. (1) balanced aggregation and breakage, (2) when aggregation can dominate and (3) breakage can dominate, are selected and solved for their corresponding analytical solutions. The results are then compared with the available analytical solution, based on Laplace transform obtained from literature. In this communication, it is shown that the solution approach proposed via AEM is flexible and therefore more efficient than the analytical approach used in the literature.

  8. Analysis of Thiodiglycol: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS777

    Energy Technology Data Exchange (ETDEWEB)

    Owens, J; Koester, C

    2008-07-24

    The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method for the analysis of thiodiglycol, the breakdown product of the sulfur mustard HD, in water by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), titled Method EPA MS777 (hereafter referred to as EPA CRL SOP MS777). This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to verify the analytical procedures described in MS777 for analysis of thiodiglycol in aqueous samples. The gathered data from this study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of Method EPA MS777 can be determined.

  9. An Analytical Investigation of Three General Methods of Calculating Chemical-Equilibrium Compositions

    Science.gov (United States)

    Zeleznik, Frank J.; Gordon, Sanford

    1960-01-01

    The Brinkley, Huff, and White methods for chemical-equilibrium calculations were modified and extended in order to permit an analytical comparison. The extended forms of these methods permit condensed species as reaction products, include temperature as a variable in the iteration, and permit arbitrary estimates for the variables. It is analytically shown that the three extended methods can be placed in a form that is independent of components. In this form the Brinkley iteration is identical computationally to the White method, while the modified Huff method differs only'slightly from these two. The convergence rates of the modified Brinkley and White methods are identical; and, further, all three methods are guaranteed to converge and will ultimately converge quadratically. It is concluded that no one of the three methods offers any significant computational advantages over the other two.

  10. Validation of an HPLC method for the simultaneous determination of eletriptan and UK 120.413

    Directory of Open Access Journals (Sweden)

    LJILJANA ZIVANOVIC

    2006-11-01

    Full Text Available Arapid and sensitive RPHPLCmethod was developed for the routine control analysis of eletriptan hydrobromide and its organic impurity UK 120.413 in Relpax® tablets. The chromatography was performed at 20 °Cusing a C18 XTerraTM (5 m, 150 × 4,6 mm column at a flow rate 1.0 ml/min. The drug and its impurity were detected at 225 nm. The mobile phase consisted of TEA (1 % – methanol (67.2:32.8 v/v, the pH of which was adjusted to 6.8 with 85 % orthophosphoric acid. Quantification was accomplished by the internal standard method. The developed RP HPLC method was validated by testing: accuracy, precision, repeatibility, specificity, detection limit, quantification limit, linearity, robustness and sensitivity. High linearity of the analytical procedure was confirmed over the concentration range of 0.05 – 1.00 mg/ml for eletriptan hydrobromide and from 0.10 – 1.50 µg/ml for UK 120.413, with correlation coefficients greater than r = 0.995. The low value of the RSD expressed the good repeatability and precision of the method. Experimental design and a response surface method were used to test robustness of the analytical procedure and to evaluate the effect of variation of the method parameters, namely the mobile phase composition, pH and temperature. They showed small deviations from the method setting. The good recovery and low RSD confirm the suitability of the proposed RP HPLC method for the routine determination of eletriptan hydrobromide and its impurity UK 120.413 in Relpax® tables.

  11. Analytical Method in Solving Flow of Viscoelastic Fluid in a Porous Converging Channel

    OpenAIRE

    M. Esmaeilpour; Naeem Roshan; Negar Roshan; D.D. Ganji

    2011-01-01

    An analytical method, called homotopy perturbation method (HPM), is used to compute an approximation to the solution of the nonlinear differential equation governing the problem of two-dimensional and steady flow of a second-grade fluid in a converging channel. The table and figures are presented for influencing various parameters on the velocity field. The results compare well with those obtained by the numerical method. The method is straightforward and concise, and it can also be applied t...

  12. The importance of 1H-nuclear magnetic resonance spectroscopy for reference standard validation in analytical sciences.

    Directory of Open Access Journals (Sweden)

    Dovi Kelman

    Full Text Available This paper highlights the importance of recording at least a (1H nuclear magnetic resonance (NMR spectrum to verify identity of standards used in analyses of organic materials irrespective of source. We show the importance of this approach with an example of a quantitative high-performance liquid chromatography (HPLC study undertaken with green tea extracts that required the use of several polyphenols as standards. In the course of the study one of these standards [(--epigallocatechin, EGC], although having the physical appearance and appropriate HPLC chromatographic behavior of EGC, proved by (1H-NMR to be a completely different class of molecule. For us, this raised significant questions concerning validity of many published pieces of research that used quantitative HPLC methods without first performing rigorous validation of the employed standards prior to their use. This paper clearly illustrates the importance of validation of all standards used in analysis of organic materials by recording at least a (1H-NMR spectrum of them prior to their use.

  13. Development of CAD implementing the algorithm of boundary elements’ numerical analytical method

    Directory of Open Access Journals (Sweden)

    Yulia V. Korniyenko

    2015-03-01

    Full Text Available Up to recent days the algorithms for numerical-analytical boundary elements method had been implemented with programs written in MATLAB environment language. Each program had a local character, i.e. used to solve a particular problem: calculation of beam, frame, arch, etc. Constructing matrices in these programs was carried out “manually” therefore being time-consuming. The research was purposed onto a reasoned choice of programming language for new CAD development, allows to implement algorithm of numerical analytical boundary elements method and to create visualization tools for initial objects and calculation results. Research conducted shows that among wide variety of programming languages the most efficient one for CAD development, employing the numerical analytical boundary elements method algorithm, is the Java language. This language provides tools not only for development of calculating CAD part, but also to build the graphic interface for geometrical models construction and calculated results interpretation.

  14. Review of Properties and Analytical Methods for the Determination of Norfloxacin.

    Science.gov (United States)

    Chierentin, Lucas; Salgado, Hérida Regina Nunes

    2016-01-01

    The first-generation quinolones have their greatest potency against Gram-negative bacteria, but newly developed molecules have exhibited increased potency against Gram-positive bacteria, and existing agents are available with additional activity against anaerobic microorganisms. Norfloxacin is a broad-spectrum antimicrobial fluoroquinolone used against Gram-positive and Gram-negative organisms (aerobic organisms). There are different analytical methods available to determine norfloxacin applied in quality control of this medicine in order to ensure its effectiveness and safety. The authors present an overview of the fourth generation of quinolones, followed by the properties, applications, and analytical methods of norfloxacin. These results show several existing analytical techniques that are flexible and broad-based methods of analysis in different matrices. This article focuses on bionalytical and pharmaceutical quality-control applications, such as thin-layer chromatography, microbiological assay, spectrophotometry, capillary electrophoresis (CE), and high-performance liquid chromatography (HPLC).

  15. DISCRIMINATORY DISSOLUTION METHOD DEVELOPMENT AND VALIDATION FOR CEPHALEXIN OD TABLETS

    Directory of Open Access Journals (Sweden)

    S. Ramachandran et al.

    2011-11-01

    Full Text Available In this study, a discriminative dissolution method was developed for Cephalexin OD (orally disintegrating tablets 750mg. The solubility and stability of the cephalexin API was determined in ten different solutions. In that 0.01N HCl, glycine buffer pH 3-0, acetate buffer pH 4.5 and water gave good stability and the solubility. Dissolution profiling of cephalexin OD tablets 750mg of single batch was done with the selected media containing varying concentration of surfactants (tween 80 and Sodium lauryl sulphate- SLS. The release profile is compared with that of the control media. The media that gave discriminately faster release than that of the control were found to be 0.01N HCl with 0.75% of tween 80, 0.01N HCl with 0.5% of SLS, acetate buffer with 1% of tween 80 and water with 0.5% of SLS. With the selected media, dissolution profile was done on the three different batches of cephalexin OD tablets one with lesser polymer ratio and other with higher polymer ratio that that of the test batch. Only 0.01N HCl with 0.75% of tween 80 as dissolution medium was found to show good discrimination in the release profile with change in the formulation conditions. The discriminative dissolution method developed was validated for its specificity, accuracy, stability, linearity and precision and it passes all the parameters.

  16. Development of a solvent-free analytical method for paracetamol quantitative determination in Blood Brain Barrier in vitro model.

    Science.gov (United States)

    Langlois, Marie-Hélène; Vekris, Antonios; Bousses, Christine; Mordelet, Elodie; Buhannic, Nathalie; Séguard, Céline; Couraud, Pierre-Olivier; Weksler, Babette B; Petry, Klaus G; Gaudin, Karen

    2015-04-15

    A Reversed Phase-High Performance Liquid Chromatography/Diode Array Detection method was developed and validated for paracetamol quantification in cell culture fluid from an in vitro Blood Brain Barrier model. The chromatographic method and sample preparation were developed using only aqueous solvents. The column was a XTerra RP18 150 × 4.6mm, 3.5 μm with a guard column XTerra RP18 20 × 4.6 mm, 3.5 μm at 35 °C and the mobile phase was composed by 100% formate buffer 20 mM at pH 4 and flow rate was set at 1 mL/min. The detection was at 242 nm. The sample was injected at 10 μL. Validation was performed using the accuracy profile approach. The analytical procedure was validated with the acceptance limits at ± 10% over a range of concentration from 1 to 58 mg L(-1). The procedure was then used in routine to determine paracetamol concentration in a brain blood barrier in vitro model. Application of the Unither paracetamol formulation in Blood Brain Barrier model allowed the determination and comparison of the transcellular passage of paracetamol at 37 °C and 4 °C, that excludes paracellular or non specific leakage.

  17. HPLC method validated for the simultaneous analysis of cichoric acid and alkamides in Echinacea purpurea plants and products

    DEFF Research Database (Denmark)

    Mølgaard, Per; Johnsen, Søren; Christensen, Peter;

    2003-01-01

    A reversed-phase high-performance liquid chromatography (HPLC) method has been developed to determine caffeic acid derivatives, for example, cichoric acid, and alkamides in plant parts and herbal products of Echinacea purpurea. The method consists of an extraction procedure whereby the hydrophilic...... phenolics as well as the lipophilic alkamides are released from the samples, followed by the analytical HPLC procedure for quantitative determination of these compounds. The method is the first one validated for the determination of these two groups of compounds in the same procedure. Naringenin has been...

  18. Harvesting energy from the sloshing motion of ferrofluids in an externally excited container: Analytical modeling and experimental validation

    Science.gov (United States)

    Alazmi, S.; Xu, Y.; Daqaq, M. F.

    2016-07-01

    When a container carrying a magnetized ferrofluid is subjected to external mechanical stimuli, the sloshing motion of the magnetized ferrofluid generates a time-varying magnetic flux, which can be used to induce an electromotive force in a coil placed adjacent to the container. This process generates an electric current in the coil, and therewith, can be used to transduce external vibrations into electric energy. In this article, we develop a nonlinear analytical model, which governs the electro-magneto-hydrodynamics of an electromagnetic ferrofluid-based vibratory energy harvester. Using perturbation methods, we obtain an approximate analytical solution of the model for a case involving primary resonance excitation of the first mode and a two-to-one internal resonance between the first two modes. This occurs when the external excitation is harmonic with a frequency close to the fundamental sloshing frequency and when the second modal frequency is nearly twice the first modal frequency. Theoretical results are compared to experimental findings illustrating very good qualitative agreement.

  19. Subsonic Indicial Aerodynamics for Aerofoil's Unsteady Loads via Numerical and Analytical Methods

    CERN Document Server

    Berci, Marco

    2016-01-01

    This study deals with generating aerodynamic indicial-admittance functions for predicting the unsteady lift of two-dimensional aerofoils in subsonic flow, using approximate numerical and analytical formulations. Both a step-change in the angle of attack and a sharp-edge gust are suitably considered as small perturbations. Novel contributions concern both a systematic analysis of the computational simulations process and an effective theoretical synthesis of its outcome, providing with sound cross-validation. Good practice for generating the indicial-admittance functions via computational fluid dynamics is first investigated for several Mach numbers, angles of attack and aerofoil profiles. Convenient analytical approximations of such indicial functions are then obtained by generalising those available for incompressible flow, taking advantage of acoustic wave theory for the non-circulatory airload and Prandtl-Glauert's scalability rule for the circulatory airload. An explicit parametric formula is newly propos...

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

    Science.gov (United States)

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

    2016-06-01

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

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

    Science.gov (United States)

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

    2016-06-01

    This paper deals with the development of hydrophilic interaction liquid chromatographic (HILIC) method for the analysis of bilastine and its degradation impurities following Analytical Quality by Design approach. It is the first time that the method for bilastine and its impurities is proposed. The main objective was to identify the conditions where an adequate separation in minimal analysis duration could be achieved within a robust region. Critical process parameters which have the most influence on method performance were defined as acetonitrile content in the mobile phase, pH of the aqueous phase and ammonium acetate concentration in the aqueous phase. Box-Behnken design was applied for establishing a relationship between critical process parameters and critical quality attributes. The defined mathematical models and Monte Carlo simulations were used to identify the design space. Fractional factorial design was applied for experimental robustness testing and the method is validated to verify the adequacy of selected optimal conditions: the analytical column Luna(®) HILIC (100mm×4.6mm, 5μm particle size); mobile phase consisted of acetonitrile-aqueous phase (50mM ammonium acetate, pH adjusted to 5.3 with glacial acetic acid) (90.5:9.5, v/v); column temperature 30°C, mobile phase flow rate 1mLmin(-1), wavelength of detection 275nm. PMID:27131148

  2. Possibilities of Utilizing the Method of Analytical Hierarchy Process Within the Strategy of Corporate Social Business

    Science.gov (United States)

    Drieniková, Katarína; Hrdinová, Gabriela; Naňo, Tomáš; Sakál, Peter

    2010-01-01

    The paper deals with the analysis of the theory of corporate social responsibility, risk management and the exact method of analytic hierarchic process that is used in the decision-making processes. The Chapters 2 and 3 focus on presentation of the experience with the application of the method in formulating the stakeholders' strategic goals within the Corporate Social Responsibility (CSR) and simultaneously its utilization in minimizing the environmental risks. The major benefit of this paper is the application of Analytical Hierarchy Process (AHP).

  3. Advantages of Analytical Transformations in Monte Carlo Methods for Radiation Transport

    International Nuclear Information System (INIS)

    Monte Carlo methods for radiation transport typically attempt to solve an integral by directly sampling analog or weighted particles, which are treated as physical entities. Improvements to the methods involve better sampling, probability games or physical intuition about the problem. We show that significant improvements can be achieved by recasting the equations with an analytical transform to solve for new, non-physical entities or fields. This paper looks at one such transform, the difference formulation for thermal photon transport, showing a significant advantage for Monte Carlo solution of the equations for time dependent transport. Other related areas are discussed that may also realize significant benefits from similar analytical transformations

  4. [Behavioral therapy, cognitive behavioral therapy and cognitive-analytic methods in treatment of anorexia].

    Science.gov (United States)

    Schmidt, U

    1997-01-01

    This paper describes the current state of behavioural, cognitive-behavioural and cognitive-analytical treatments of anorexia nervosa and the underlying theoretical models. Purely behavioural treatment methods have been evaluated in a number of single case studies. Although effective in terms of increasing body weight, these methods are obsolete in view of their unpleasant side-effects. Cognitive-behavioural and cognitive-analytical therapies are much more appropriate for these patients given their complex symptomatology and frequently ambivalent attitude to treatment. However, so far evaluations of these treatments are rare. The reasons for this are discussed. PMID:9411461

  5. 2D Stabilised analytic signal method in DC pole-pole potential data interpretation

    Indian Academy of Sciences (India)

    Paras R Pujari; Rambhatla G Sastry

    2003-03-01

    Using analytic signal method, interpretation of pole-pole secondary electric potentials due to 2D conductive/resistive prisms is presented. The estimated parameters are the location, lateral extent or width and depth to top surface of the prism. Forward modelling is attempted by 2D-Finite Difference method. The proposed stabilised analytic signal algorithm (RES2AS) uses Tikhonov's regularization scheme and FFT routines. The algorithm is tested on three theoretical examples and field data from the campus of Roorkee University. The stability of RES2AS is also tested on synthetic error prone secondary pole-pole potential data.

  6. Analytical Method to Calculate the DC Link Current Stress in Voltage Source Converters

    DEFF Research Database (Denmark)

    Gohil, Ghanshyamsinh Vijaysinh; Bede, Lorand; Teodorescu, Remus;

    2014-01-01

    for the applications with high line current ripple. The effect of the pulsewidth modulation (PWM) scheme on the rms value of the dc-link current is also studied and the analysis for continuous PWM and discontinuous PWM (DPWM) schemes is presented. The proposed analytical method is also verified experimentally....... of the current flowing through the dc-link capacitor. A simple analytical method to calculate the rms value of the dc-link capacitor current is presented in this paper. The effect of the line current ripple on the rms value of the dc-link capacitor current is considered. This yields accurate results, especially...

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

    Directory of Open Access Journals (Sweden)

    Kranti P. Musmade

    2014-01-01

    Full Text Available 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 employing a C18 (250.0 × 4.6 mm, 5 μm column at ambient temperature in isocratic conditions using phosphate buffer pH 3.5: acetonitrile (75 : 25% v/v as mobile phase pumped at a flow rate of 1.0 mL/min. UV detection was carried out at 282 nm. The developed method was validated according to ICH guidelines Q2(R1. The method was found to be precise and accurate on statistical evaluation with a linearity range of 0.1 to 20.0 μg/mL for NAR. The intra- and interday precision studies showed good reproducibility with coefficients of variation (CV less than 1.0%. The mean recovery of NAR was found to be 99.33 ± 0.16%. The proposed method was found to be highly accurate, sensitive, and robust. The proposed liquid chromatographic method was successfully employed for the routine analysis of said compound in developed novel nanopharmaceuticals. The presence of excipients did not show any interference on the determination of NAR, indicating method specificity.

  8. RP-HPLC Method Development and Validation of Abacavir Sulphate in Bulk and Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    S. LAVANYA

    2014-11-01

    Full Text Available RP-HPLC method was developed for the estimation of abacavir sulphate in bulk and pharmaceutical dosage form (tablets by using INERTSIL ODS 3V column, C18 (250x4.6 ID mobile phase consisting of a mixture of 10mM phosphate buffer: ACN (60:40 v/v % PH: 4.0 with detection of 287 nm. The retention time was found to be 2.430min and linearity was observed in the range 60-140μg /ml. Still now there were a number of analytical methods were developed for the estimation of abacavir in pharmaceutical dosage form and also in biological samples like spectroscopic methods, chromatographic methods, etc. But the present method was met the validation parameters according ICH guidelines like accuracy, precision, linearity, range, robustness, ruggedness, limit of detection and limit of quantitation, etc. with a short around time. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2.

  9. Research on the simultaneous multi-components analytical method for polluted soil

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Kang Sup; Song, Duk Young; Choi, Byung In; Kim, Kun Han; Eum, Chul Hun; Jeon, Chi Wan; Lee, Jung Hwa [Korea Institute of Geology Mining and Materials, Taejon (Korea)

    1998-12-01

    Dissolution properties for the several inorganic pollutants in soils have been studied and simultaneous multi-components analytical method has been established with using ICP/MS for 13 monitoring elements in order to protect water and soil environments. And addition, more effective new analytical methods have been studied for TPH(total petroleum hydrocarbon) and organophosphorus compounds in soils. Several inorganic pollutants were spiked to 3 kinds of fresh soils which were sand, clay, loam. The dissolution properties of the prepared samples were investigated under the various extracting conditions such as extracting time, acid concentration, particle size, etc. in order to take basic information about the process of extraction test and improvement of related analytical methods. As the results, dissolution properties were affected mainly by acid concentration in extraction procedure and mineral composition of soils. On the other hand, extracting time, sort of acids and particle size of soils has a little influence on the dissolution properties. Cd revealed very high dissolving efficiency and As was very low in whole extracting test. Current analytical methods for the determination of soils are based on the purge and trap for volatiles such as gasoline and solvent extraction for semivolatiles such as kerosene and diesel oils. These methods are not proper in cost and time. In addition to, there are potential for analyte contamination and some problems in pretreatment procedure. In this study , we have discussed simultaneous determination of TPH containing gasoline, kerosene, diesel oils and etc. And determination of Organophosphorus compounds in soils has studied. In this procedure, the application of ultrasonication methods and several extraction methods were compared. In the results of this study, we could take very low practical detection limit and good precision. Approved methods were suitable for the determination of oils and pesticides in soil at high and low

  10. Analytical calculation of spectral phase of grism pairs by the geometrical ray tracing method

    Science.gov (United States)

    Rahimi, L.; Askari, A. A.; Saghafifar, H.

    2016-07-01

    The most optimum operation of a grism pair is practically approachable when an analytical expression of its spectral phase is in hand. In this paper, we have employed the accurate geometrical ray tracing method to calculate the analytical phase shift of a grism pair, at transmission and reflection configurations. As shown by the results, for a great variety of complicated configurations, the spectral phase of a grism pair is in the same form of that of a prism pair. The only exception is when the light enters into and exits from different facets of a reflection grism. The analytical result has been used to calculate the second-order dispersions of several examples of grism pairs in various possible configurations. All results are in complete agreement with those from ray tracing method. The result of this work can be very helpful in the optimal design and application of grism pairs at various configurations.

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

    Science.gov (United States)

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

    2015-10-15

    Control of chemotherapies preparations are now an obligation in France, though analytical control is compulsory. Several methods are available and none of them is presumed as ideal. We wanted to compare them so as to determine which one could be the best choice. We compared non analytical (visual and video-assisted, gravimetric) and analytical (HPLC/FIA, UV/FT-IR, UV/Raman, Raman) methods thanks to our experience and a SWOT analysis. The results of the analysis show great differences between the techniques, but as expected none us them is without defects. However they can probably be used in synergy. Overall for the pharmacist willing to get involved, the implementation of the control for chemotherapies preparations must be widely anticipated, with the listing of every parameter, and remains according to us an analyst's job. PMID:26299761

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

    Science.gov (United States)

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

    2015-10-15

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

  13. Experimental design and multiple response optimization. Using the desirability function in analytical methods development.

    Science.gov (United States)

    Candioti, Luciana Vera; De Zan, María M; Cámara, María S; Goicoechea, Héctor C

    2014-06-01

    A review about the application of response surface methodology (RSM) when several responses have to be simultaneously optimized in the field of analytical methods development is presented. Several critical issues like response transformation, multiple response optimization and modeling with least squares and artificial neural networks are discussed. Most recent analytical applications are presented in the context of analytLaboratorio de Control de Calidad de Medicamentos (LCCM), Facultad de Bioquímica y Ciencias Biológicas, Universidad Nacional del Litoral, C.C. 242, S3000ZAA Santa Fe, ArgentinaLaboratorio de Control de Calidad de Medicamentos (LCCM), Facultad de Bioquímica y Ciencias Biológicas, Universidad Nacional del Litoral, C.C. 242, S3000ZAA Santa Fe, Argentinaical methods development, especially in multiple response optimization procedures using the desirability function.

  14. METHODS TO VALIDATE TOOTH-SUPPORTING REGENERATIVE THERAPIES

    Science.gov (United States)

    Padial-Molina, Miguel; Marchesan, Julie T.; Taut, Andrei D.; Jin, Qiming; Giannobile, William V.; Rios, Hector F.

    2012-01-01

    SUMMARY In humans, microbially-induced inflammatory periodontal diseases are the primary initiators that disrupt the functional and structural integrity of the periodontium (i.e., the alveolar bone, the periodontal ligament, and the cementum). The re-establishment of its original structure, properties and function constitutes a significant challenge in the development of new therapies to regenerate tooth-supporting defects. Preclinical models represent an important in vivo tool to critically evaluate and analyze key aspects of novel regenerative therapies including: 1) Safety, 2) Effectiveness, 3) Practicality, and 4) Functional and structural stability over time. Therefore, these models provide foundational data that supports the clinical validation and the development of novel innovative regenerative periodontal technologies. Steps are provided on the use of the root fenestration animal model for the proper evaluation of periodontal outcome measures using the following parameters: descriptive histology, histomorphometry, immunostaining techniques, three-dimensional imaging, electron microscopy, gene expression analyses and safety assessments. These methods will prepare investigators and assist them in identifying key endpoints that can then be adapted to later stage human clinical trials. PMID:22566053

  15. Modifications of spectrophotometric methods for antioxidative vitamins determination convenient in analytic practice

    OpenAIRE

    Maciej Rutkowski; Krzysztof Grzegorczyk

    2007-01-01

    Although there are numerous methods for quantitative determination of antioxidative vitamins: C, E, and A, there are no methods favourable for the broadly understood analytic practice – they have various faults and limitations or require expensive apparatus. Therefore, we have elaborated modifications of valuable spectrophotometric methods for determination each of those vitamins, which originally could not be applied for laboratory practice from various regards. They are based on: ...

  16. Analytical methods used at IPR (Instituto de Pesquisas Radioativas - Minas Gerais, Brazil)

    International Nuclear Information System (INIS)

    The analytical methods available at IPR (MG-Brazil) for the routine determination of uranium are described. These methods are: gravimetric analysis; fluorescence spectroscopy, voltametry, polarography, absorption spectroscopy, beta-and gamma-radiometric analysis, gamma spectroscopy, activation analysis, X-rays fluorescence analysis and delayed neutron analysis. Some additional methods for the study of mineral ores, such as X-rays diffractometry, emmission spectroscopy, thermal analysis, etc, are also discussed

  17. Determination of methylmercury in marine sediment samples: Method validation and occurrence data

    Energy Technology Data Exchange (ETDEWEB)

    Carrasco, Luis; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    Highlights: • A method for MeHg determination at trace level in marine sediments is completely validated. • Validation is performed according to ISO-17025 and Eurachem guidelines. • The extraction efficiency of four sample preparation procedures is evaluated. • The uncertainty budget is used as a tool for evaluation of main uncertainty contributors. • Comparison with independent methods yields good agreement within stated uncertainty. - Abstract: The determination of methylmercury (MeHg) in sediment samples is a difficult task due to the extremely low MeHg/THg (total mercury) ratio and species interconversion. Here, we present the method validation of a cost-effective fit-for-purpose analytical procedure for the measurement of MeHg in sediments, which is based on aqueous phase ethylation, followed by purge and trap and hyphenated gas chromatography–pyrolysis–atomic fluorescence spectrometry (GC–Py–AFS) separation and detection. Four different extraction techniques, namely acid and alkaline leaching followed by solvent extraction and evaporation, microwave-assisted extraction with 2-mercaptoethanol, and acid leaching, solvent extraction and back extraction into sodium thiosulfate, were examined regarding their potential to selectively extract MeHg from estuarine sediment IAEA-405 certified reference material (CRM). The procedure based on acid leaching with HNO{sub 3}/CuSO{sub 4}, solvent extraction and back extraction into Na{sub 2}S{sub 2}O{sub 3} yielded the highest extraction recovery, i.e., 94 ± 3% and offered the possibility to perform the extraction of a large number of samples in a short time, by eliminating the evaporation step. The artifact formation of MeHg was evaluated by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC–ICP–MS), using isotopically enriched Me{sup 201}Hg and {sup 202}Hg and it was found to be nonexistent. A full validation approach in line with ISO 17025 and

  18. Fisk-based criteria to support validation of detection methods for drinking water and air.

    Energy Technology Data Exchange (ETDEWEB)

    MacDonell, M.; Bhattacharyya, M.; Finster, M.; Williams, M.; Picel, K.; Chang, Y.-S.; Peterson, J.; Adeshina, F.; Sonich-Mullin, C.; Environmental Science Division; EPA

    2009-02-18

    This report was prepared to support the validation of analytical methods for threat contaminants under the U.S. Environmental Protection Agency (EPA) National Homeland Security Research Center (NHSRC) program. It is designed to serve as a resource for certain applications of benchmark and fate information for homeland security threat contaminants. The report identifies risk-based criteria from existing health benchmarks for drinking water and air for potential use as validation targets. The focus is on benchmarks for chronic public exposures. The priority sources are standard EPA concentration limits for drinking water and air, along with oral and inhalation toxicity values. Many contaminants identified as homeland security threats to drinking water or air would convert to other chemicals within minutes to hours of being released. For this reason, a fate analysis has been performed to identify potential transformation products and removal half-lives in air and water so appropriate forms can be targeted for detection over time. The risk-based criteria presented in this report to frame method validation are expected to be lower than actual operational targets based on realistic exposures following a release. Note that many target criteria provided in this report are taken from available benchmarks without assessing the underlying toxicological details. That is, although the relevance of the chemical form and analogues are evaluated, the toxicological interpretations and extrapolations conducted by the authoring organizations are not. It is also important to emphasize that such targets in the current analysis are not health-based advisory levels to guide homeland security responses. This integrated evaluation of chronic public benchmarks and contaminant fate has identified more than 200 risk-based criteria as method validation targets across numerous contaminants and fate products in drinking water and air combined. The gap in directly applicable values is

  19. A platform analytical quality by design (AQbD) approach for multiple UHPLC-UV and UHPLC-MS methods development for protein analysis.

    Science.gov (United States)

    Kochling, Jianmei; Wu, Wei; Hua, Yimin; Guan, Qian; Castaneda-Merced, Juan

    2016-06-01

    A platform analytical quality by design approach for methods development is presented in this paper. This approach is not limited just to method development following the same logical Analytical quality by design (AQbD) process, it is also exploited across a range of applications in methods development with commonality in equipment and procedures. As demonstrated by the development process of 3 methods, the systematic approach strategy offers a thorough understanding of the method scientific strength. The knowledge gained from the UHPLC-UV peptide mapping method can be easily transferred to the UHPLC-MS oxidation method and the UHPLC-UV C-terminal heterogeneity methods of the same protein. In addition, the platform AQbD method development strategy ensures method robustness is built in during development. In early phases, a good method can generate reliable data for product development allowing confident decision making. Methods generated following the AQbD approach have great potential for avoiding extensive post-approval analytical method change. While in the commercial phase, high quality data ensures timely data release, reduced regulatory risk, and lowered lab operational cost. Moreover, large, reliable database and knowledge gained during AQbD method development provide strong justifications during regulatory filling for the selection of important parameters or parameter change needs for method validation, and help to justify for removal of unnecessary tests used for product specifications.

  20. A platform analytical quality by design (AQbD) approach for multiple UHPLC-UV and UHPLC-MS methods development for protein analysis.

    Science.gov (United States)

    Kochling, Jianmei; Wu, Wei; Hua, Yimin; Guan, Qian; Castaneda-Merced, Juan

    2016-06-01

    A platform analytical quality by design approach for methods development is presented in this paper. This approach is not limited just to method development following the same logical Analytical quality by design (AQbD) process, it is also exploited across a range of applications in methods development with commonality in equipment and procedures. As demonstrated by the development process of 3 methods, the systematic approach strategy offers a thorough understanding of the method scientific strength. The knowledge gained from the UHPLC-UV peptide mapping method can be easily transferred to the UHPLC-MS oxidation method and the UHPLC-UV C-terminal heterogeneity methods of the same protein. In addition, the platform AQbD method development strategy ensures method robustness is built in during development. In early phases, a good method can generate reliable data for product development allowing confident decision making. Methods generated following the AQbD approach have great potential for avoiding extensive post-approval analytical method change. While in the commercial phase, high quality data ensures timely data release, reduced regulatory risk, and lowered lab operational cost. Moreover, large, reliable database and knowledge gained during AQbD method development provide strong justifications during regulatory filling for the selection of important parameters or parameter change needs for method validation, and help to justify for removal of unnecessary tests used for product specifications. PMID:27017571