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Sample records for acid determination metodos

  1. A method for the determination of ascorbic acid using the iron(II)-pyridine-dimethylglyoxime complex

    Energy Technology Data Exchange (ETDEWEB)

    Arya, S. P.; Mahajan, M. [Haryana, Kurukshetra Univ. (India). Dept. of Chemistry

    1998-05-01

    A simple and rapid spectrophotometric method for the determination of ascorbic acid is proposed. Ascorbic acid reduces iron (III) to iron (II) which forms a red colored complex with dimethylglyoxime in the presence of pyridine. The absorbance of the resulting solution is measured at 514 nm and a linear relationship between absorbance and concentration of ascorbic acid is observed up to 14 {mu}g ml{sup -1}. Studies on the interference of substances usually associated with ascorbic acid have been carried out and the applicability of the method has been tested by analysing pharmaceutical preparations of vitamin C. [Italiano] Si propone un rapido e semplice metodo spettrofotometrico per la determinazione dell`acido ascorbico. L`acido ascorbico riduce il ferro(III) a ferro(II) che forma con la dimetilgliossima, in presenza di piridina, un complesso colorato in rosso. L`assorbanza della soluzione risultante e` misurata a 514 nm e si ottiene una relazione lineare tra assorbanza e concentrazione dell`acido ascorbico fino a 14 {mu}g ml{sup -1}. Si sono condotti studi sugli interferenti usualmente associati all`acido ascorbico ed e` stata valutata l`applicabilita` del metodo all`analisi di preparati farmaceutici di vitamina C.

  2. LE «SOTTIGLIEZZE DI CERTA DIDATTICA SUPERLATIVA» DELLA GRAMMATICA ELEMENTARE: STORIA (ATTESTATA DEL METODO RAFFORZISTA (1814-1914

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    Michela Dota

    2018-03-01

    Full Text Available Il contributo ripercorre la storia e le peculiarità del metodo rafforzista, metodo glottodidattico per l’insegnamento della lettura e della scrittura. Il metodo, nato in Italia nel primo Ottocento, nell’epoca postunitaria era praticato nelle scuole elementari soprattutto dell’Italia meridionale, nonché nelle scuole reggimentali e in alcuni istituti per sordomuti. Le sue fondamenta, aberranti rispetto alla norma ortografica e ortoepica tradizionale, lo resero obiettivo di un tenace ostracismo da parte del Ministero dell’Istruzione pubblica, sostenuto per questa occasione da due tra i più eminenti glottologi dell’epoca: Graziadio Isaia Ascoli e Francesco Lorenzo Pullè. Il metodo finì per estinguersi nel secondo decennio del Novecento.   The history of the “metodo rafforzista” for teaching Italian (1814-1914 This article retraces the history and peculiarities of the “metodo rafforzista”, a language teaching method developed in Italy during the first part of 1800s. In the post-Unitarian period, it was used in elementary schools, especially in Southern Italy, and also in military schools and in some institutes for the Deaf and Dumb. Orthographic and orthoepic models proposed by the “metodo rafforzista” diverged from rules of traditional Italian grammar. The method, supported by Graziadio Isaia Ascoli and Francesco Lorenzo Pullè, two of the most distinguished Italian linguists at that time, was subsequently rejected by the Ministry of Public Education, and it vanished during the second half of 1900s.

  3. Scienza e conoscenza: sul valore del metodo scientifico

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    Riccardo Luciano Appolloni

    2014-05-01

    Full Text Available L’antico problema di riconoscere una forma di conoscenza oggettivae fondata è ancora vivo; in questo scritto cercheremo di capire se la scienza moderna possa essere una forma di conoscenza tale e, quindi, privilegiata. A tal fine ci serviremo del pensiero di alcuni epistemologi e scienziati. In particolare, nel trattare il problema del valore epistemologico del metodo scientifico, non potremo esimerci dal fare i conti con l’anarchismo metodologico di Paul K. Feyerabend, verso il quale l’esito del presente articolo sarà fondamentalmente critico. A partire dai fecondi spunti di questo filosofo, tenteremo dapprima di analizzare i caratteri distintivi della scienza e del suo metodo rispetto ad altre forme di sapere; quindi, cercheremo di individuare alcuni limiti della conoscenza razionale.

  4. The need of alkalinity determination in the characterization of rain; Necesidad de la determinacion de la alcalinidad en la caracterizacion de la lluvia

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    Pal Verma, Mahendra [Instituto de Investigaciones Electricas, Cuernavaca (Mexico)

    1998-01-01

    In this paper is presented the alkalinity determination of the carbonic species in the rain waters by the Gran titration method. The alkalinity values obtained by this method in low electric conductivity waters are fairly reliable. Also, the existing studies on the characterization of acid rains, are discussed. [Espanol] En este trabajo se presenta la medicion de la alcalinidad y la determinacion de las especies carbonicas en las aguas de lluvia por el metodo de la titulacion de Gran. Los valores de alcalinidad obtenidos por este metodo en las aguas de baja conductividad electrica son bastante confiables. Asimismo, se discuten los estudios existentes sobre la caracterizacion de la lluvia acida en la republica mexicana.

  5. Microscale adaptation of the potentiometric method with ion-selective electrode for the quantification of fluoride; Adaptacion a microescala del metodo potenciometrico con electrodo ion selectivo para la cuantificacion de fluoruro

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    Guevara Ruiz, Paulina; Ortiz Perez, Maria Deogracias [Laboratorio de Bioquimica, Facultad de de Medicina, Universidad Autonoma de San Luis Potosi, San Luis Potosi, San Luis Potosi, (Mexico)]. E-mail: mdortiz@uaslp.mx

    2009-05-15

    Similarly to other countries, ground water from Mexico is naturally polluted by fluoride. The main effects of fluoride at typical ground water concentrations are dental fluorosis, neurological deficits and reproductive disorders. In order to verify that the fluoride concentration is within the allowed guideline in Mexico (NOM 127 and 201), it is important to monitor fluoride levels in water and commercial beverages. The aim of this work is to develop a modification of the standard potentiometric method for fluoride determination in water, in order to reduce costs and amount of potentially toxic waste substances. Both methods were validated, the standard potentiometric method with the ion selective electrode and the microscale modification proposed in this paper. The methods were compared using statistic tests and graphics, followed by the comparison of 125 samples of commercial bottled water sold in the city of San Luis Potosi. Optimal results were obtained for the validation of both methods, and the microscale modification showed statistically identical results to those obtained with the standard method in all samples of bottled water. The microscale modification is a good alternative for fluoride assessment in water and beverages, and it represents a 95 % reduction of costs and chemical waste. [Spanish] En varios paises, incluido Mexico se presenta una contaminacion natural con fluoruro en agua subterranea; los principales efectos en la salud observados en poblacion expuesta a concentraciones mayores al valor permisible (que en Mexico es de 1.5 mg/L) son la fluorosis dental y esqueletica, asi como dano reproductivo y neurologico. En varios estados de la republica Mexicana, este problema es aun desconocido, de ahi la necesidad de evaluar las concentraciones de fluoruro en agua de consumo en varias comunidades. Asi, el objetivo de este trabajo es desarrollar un metodo a microescala para la determinacion de fluoruro en agua, que al reducir la cantidad de reactivo y

  6. Estudio numerico y experimental del proceso de soldeo MIG sobre la aleacion 6063--T5 utilizando el metodo de Taguchi

    Science.gov (United States)

    Meseguer Valdenebro, Jose Luis

    improvement on mechanical properties in aluminum metal joint. Los procesos de soldadura por arco electrico representan unas de las tecnicas mas utilizadas en los procesos de fabricacion de componentes mecanicos en la industria moderna. Los procesos de soldeo por arco se han adaptado a las necesidades actuales, haciendose un modo de fabricacion flexible y versatil. Los resultados obtenidos numericamente en el proceso de soldadura son validados experimentalmente. Los principales metodos numericos mas empleados en la actualidad son tres, metodo por diferencias finitas, metodos por elementos finitos y metodo por volumenes finitos. El metodo numerico mas empleado para el modelado de uniones soldadas, es el metodo por elementos finitos, debido a que presenta una buena adaptacion a las condiciones geometricas y de contorno ademas de que existe una diversidad de programas comerciales que utilizan el metodo por elementos finitos como base de calculo. Este trabajo de investigacion presenta un estudio experimental de una union soldada mediante el proceso MIG de la aleacion de aluminio 6063-T5. El metodo numerico se valida experimentalmente aplicando el metodo de los elementos finitos con el programa de calculo ANSYS. Los resultados experimentales obtenidos son: las curvas de enfriamiento, el tiempo critico de enfriamiento t4/3, geometria del cordon, microdurezas obtenidas en la union soldada, zona afectada termicamente y metal base, dilucion del proceso, areas criticas intersecadas entre las curvas de enfriamiento y la curva TTP. Los resultados numericos son: las curvas del ciclo termico, que representan tanto el calentamiento hasta alcanzar la temperatura maxima y un posterior enfriamiento. Se calculan el tiempo critico de enfriamiento t4/3, el rendimiento termico y se representa la geometria del cordon obtenida experimentalmente. La zona afectada termicamente se obtiene diferenciando las zonas que se encuentran a diferentes temperaturas, las areas criticas intersecadas entre las

  7. Osservazioni sul principio di legalità come idea e come metodo nell’esperienza giuridica della Chiesa

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    Beatrice Serra

    2012-10-01

    SOMMARIO: 1. Introduzione - 2. – La struttura essenziale del concetto di legalità e la sua realizzazione radicale nel diritto della Chiesa. - 3. L’idea di legalità come “regola che sta prima” nel ius commune e la sua coesistenza con un approccio empirico, essenzialmente giurisprudenziale e dottrinale, di costruzione del diritto. Il principio di legalità come metodo di produzione del diritto nel pensiero giuridico moderno- 4. Il legame storico-concettuale fra il principio di legalità e i Codici moderni - 5. Il Codex iuris canonici del 1917 e il principio di legalità come metodo di costruzione del ius ecclesiae in funzione della certezza del diritto - 6. (segueUlteriori riflessi della prima codificazione canonica sul principio di legalità.:

  8. Subsurface microbial ecology. Epi fluorescence direct counts; Ecologia microbica del sottosuolo: metodo di conta diretta in epifluorescenza

    Energy Technology Data Exchange (ETDEWEB)

    Barra Caracciolo, A.; Silvestri, C.; Creo, C.; Izzo, G. [ENEA, Centro Ricerche Casaccia, Rome (Italy). Dipt. Ambiente

    1998-07-01

    To the aim of recognize the importance of microorganisms in affecting or even determining the fate of xenobiotics in the subsurface environment evaluating bacteria concentration in a subsurface ecosystem, the report discusses a soil sample treatment method which has been developed for epi fluorescence direct counting with DAPI. [Italian] Lo studio discute un metodo di trattamento del campione per la conta diretta in epifluorescenza con un marcatore selettivo per il DNA, il DAPI, al fine di quantificare la concentrazione batterica del sottosuolo e studiare il ruolo dei microrganismi nella biodegradazione delle molecole esogene, ancora poco indagato.

  9. DOLOČITEV POVRŠINSKE NAPETOSTI Z METODO KAPILARNEGA DVIGA DVOFAZNIH SISTEMOV

    OpenAIRE

    Kravanja, Gregor

    2014-01-01

    Namen magistrske naloge je bil postavitev merilne naprave in razvoj nove metode merjenja površinske napetosti s kapilarnim dvigom dvofaznih sistemov v okolici kritične točke. Za pridobitev natančnih in primerljivih meritev je bilo potrebno poznati natančni notranji premer tankih kapilar. Določili smo ga z metodo laserskega tipanja na nemški koordinatni merilni napravi ZEISS tipa UMC-850 s pomočjo merilne programske opreme CALYPSO 5.1.4. Za merjenje ravnotežne višine smo uporabili računalniški...

  10. Development of an analytic method for arsenic's determination in lime and tortilla; Desarrollo de un metodo analitico para determinacion de arsenico en cal y tortilla

    Energy Technology Data Exchange (ETDEWEB)

    Huato Soberanis, Julio; Ogura, Tetsuya [Universidad Autonoma de Guadalajara, Guadalajara, Jalisco (Mexico)

    1995-02-01

    A spectrophotometric method to determine As in tortilla and lime has been optimized, modifying the AsH{sub 3} generator. The reaction between arsin (AsH{sub 3}){sub 4} and diethyldithiocarbamate of Ag (AgDDC); was followed spectrophotometrically. The conditions under which the As remains in the ash during the calcination of the tortillas were studied. It was found that when they were heated in a quartz tube with a careful control of the air flow and oxygen, as well as the heating temperature, the arsenic loss in minimized. [Spanish] Se ha optimizado el metodo para determinar As en la tortilla y cal mediante espectrometria en el visible del color producido en la reaccion entre Arsina (AsH{sub 3}){sub 4} y dietilditiocarbamato de plata (AgDDC); modificando el generador de AsH{sub 3}. Se han buscado las condiciones en las que el arsenico permanece en las cenizas de la calcinacion de las tortillas; encontrandose que las tortillas deben calentarse en un tubo de cuarzo con control del flujo de aire y oxigeno asi como de la temperatura de calentamiento.

  11. Torque calculation in the induction motor with the finite element method; Calculo del par en el motor de induccion con el metodo del elemento finito

    Energy Technology Data Exchange (ETDEWEB)

    Castillo Diaz, Ramon

    2002-06-15

    In this work the method of the finite element is applied to the bi-dimensional analysis of the induction motor in operation in steady state, excited by sine sources of laminar currents and sine sources of voltage. The analysis is focused mainly in the calculation of the electromagnetic torque. The topics of electromagnetic theory are covered and in an idealized model of the induction motor, analytically and numerically with the method of the finite element, in the variant method of Galerkin, the vectorial potential and the torque are calculated. The results obtained with the analytical and numerical methods are compared. Three formulations are developed to calculate the torque with the method of the finite element, using triangular elements of first order, based in the equation of force of Lorentz, the Maxwell tensor and the principle of the virtual work. Finally, a motor of induction of real characteristics is simulated, assuming it is connected to a three-phase voltage source. In this motor it is analyzed the convergence and the evolution in the results obtained of the torque with different discretions, and the torque-velocity performance curve is calculated. [Spanish] En este trabajo se aplica el metodo del elemento finito al analisis bidimensional del motor de induccion en operacion en estado estable, excitado por fuentes de corriente laminar senoidales y fuentes de voltaje senoidales. El analisis se enfoca principalmente en el calculo del par electromagnetico. Se tratan los topicos de teoria electromagnetica involucrados y en un modelo idealizado del motor de induccion, se calculan analitica y numericamente con el metodo del elemento finito, en la variante metodo de Galerkin, el potencial vectorial y el par. Se comparan resultados obtenidos con los metodos analiticos y numericos. Se desarrollan tres formulaciones para calcular el par con el metodo del elemento finito, utilizando elementos triangulares de primer orden, basadas en la ecuacion de fuerza de

  12. Sequential injection redox or acid-base titration for determination of ascorbic acid or acetic acid.

    Science.gov (United States)

    Lenghor, Narong; Jakmunee, Jaroon; Vilen, Michael; Sara, Rolf; Christian, Gary D; Grudpan, Kate

    2002-12-06

    Two sequential injection titration systems with spectrophotometric detection have been developed. The first system for determination of ascorbic acid was based on redox reaction between ascorbic acid and permanganate in an acidic medium and lead to a decrease in color intensity of permanganate, monitored at 525 nm. A linear dependence of peak area obtained with ascorbic acid concentration up to 1200 mg l(-1) was achieved. The relative standard deviation for 11 replicate determinations of 400 mg l(-1) ascorbic acid was 2.9%. The second system, for acetic acid determination, was based on acid-base titration of acetic acid with sodium hydroxide using phenolphthalein as an indicator. The decrease in color intensity of the indicator was proportional to the acid content. A linear calibration graph in the range of 2-8% w v(-1) of acetic acid with a relative standard deviation of 4.8% (5.0% w v(-1) acetic acid, n=11) was obtained. Sample throughputs of 60 h(-1) were achieved for both systems. The systems were successfully applied for the assays of ascorbic acid in vitamin C tablets and acetic acid content in vinegars, respectively.

  13. Correlacion entre metodos de analisis de Zn disponible en cuatro ordenes de suelos de Costa Rica

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    Eloy Molina

    2001-01-01

    Full Text Available Se realizo una comparación entre métodos analisis del Zn disponible en 4 ordenes de sue- Analytilos de Costa Rica (Ultisoles, Vertisoles, Andisoles Inceptisoles, 25 de c/u, utilizando las siguientes soluciones extractoras: Olsen Modificado, Meh- lich 3, Morgan Modificado, DTPA y HC1. Las cantidades de Zn extrafdas dependieron de la natu- raleza qufmica de la solucion extractora. El HCl presento los contenidos mas altos de Zn en los chasuelos, excepto en Vertisoles. Las soluciones que hicontienen el agente quelante EDTA (Olsen Modi- ficado y Mehlich`3, extrajeron niveles interme- Modidios de Zn, en tanto que los metodos que contie- Den el quelato DTPA (Morgan Modificado y DT - PA, obtuvieron los valores mas bajos. Las corre- laciones de Zn extrafble entre los 5 metodos fue- signifirOD significativas en la mayona de los casos, tanto nivel de orden de suelos como en el conjunto de indivilos 100 suelos analizados. Los coeficientes de co- rrelacion mas altos, se presentaron entre Mehlich Morgan Modificado y DTPA. Las correlaciones Modifueron consistentes en los 4 ordenes, 10 que indica que estas soluciones poseen un amplio margen de adaptacion a diferentes tipos de suelo, siendo una caractenstica ventajosa para la selección de un metodo de analisis. El Olsen Modificado fue mas slighteficiente para la extraccion de Zn en suelos de pH ligeramente acido 0 neutro (Vertisoles e Inceptiso- les, que en suelos acidos (Ultisoles y Andisoles. EI HCI extrajo cantidades muy aItas de Zn que Moraparentementestan relacionadas con formas no disponibles para lag plantas. Se concluye que lag soluciones Mehlich 3, Morgan Modificado y DT - PA son semejantes en la forma de extraer Zn dispo- Dible, y podrian seT una altemativa para sustituir el metoda tradicional de Olsen Modificado utilizado en Costa Rica. Sin embargo,la eficiencia de ellas no puede seT establecida sino a traves de log estudios de correlacion contra rendimiento en invernadero y campo.

  14. Method to allow the estimation of heat transfer coefficients in solar stills; Metodo para determinar coeficientes locales de transferencia de calor en destiladores solares

    Energy Technology Data Exchange (ETDEWEB)

    Rubio Cerda, Eduardo; Porta Gandara, Miguel A [CIBNOR, Mexico D.F (Mexico); Fernandez Zayas, Jose Luis [UNAM Mexico, D.F. (Mexico)

    2000-07-01

    This work reports an experimental method that allows to estimate the heat transfer coefficients in the neighborhood of walls or flat plates subject to convective transport phenomena. This method can be applied to a great variety of thermal systems since it is based on the knowledge of the border condition for the temperature at the surface of the plate, and the temperature profile that characterize the dimensionless coefficient of heat transfer in the fluid, according to its definition given by the Nusselt number. The approach of this work are the foundations of the method and the system that has been developed to apply it, that incorporates automatic acquisition equipment for continuos monitoring of the information and elements to control the parameters of interest. In addition, the experimental cavities on which the method will be evaluated are discussed, considering two different scales, as well as experiments in cavities filled with air, and with a mixture of air and steam water, as is the case for solar distillation. [Spanish] En este trabajo se presenta un metodo que permite determinar de manera experimental coeficientes de transferencia de calor por conveccion. Este metodo puede ser aplicado a una gran variedad de sistemas termicos ya que se fundamenta en el conocimiento de la condicion de frontera para la temperatura en la superficie de la placa, y del perfil de temperaturas que caracteriza el coeficiente adimensional de transferencia de calor en el fluido, de acuerdo a la definicion de este, dada por el numero de Nusselt. El trabajo que aqui se reporta esta enfocado a la fundamentacion del metodo y al equipamiento que se ha desarrollado para instrumentarlo, que incorpora equipos automaticos de adquisicion continua de informacion y elementos de control para los parametros de interes. Se presentan ademas, las cavidades experimentales sobre las que sera evaluado el metodo, que considera dos escalas diferentes, asi como experimentos en cavidades llenas de aire

  15. Flow measurement in a 170-MW hydraulic turbine using the Gibson method; Medicion del flujo de una turbina hidraulica de 170 MW utilizando el metodo Gibson

    Energy Technology Data Exchange (ETDEWEB)

    Urquiza, Gustavo [Universidad Autonoma del Estado de Morelos (Mexico); Adamkowski, Adam [The Szewalski Institute of Fluid-Flow Machinery (Poland); Kubiak, Janusz; Sierra, Fernando [Universidad Autonoma del Estado de Morelos (Mexico); Janicki, Waldemar [The Szewalski Institute of Fluid-Flow Machinery (Poland); Fernandez, J. Manuel [Comision Federal de Electricidad (Mexico)

    2007-07-15

    This paper describes the methodology applied for measuring water flow through a 170-MW hydraulic turbine. The flow rate was measured using the pressure-time method, also known as the Gibson method. This method uses the well-known water hammer phenomenon in pipelines; in turbine penstocks, for instance. The version of this method used here is based on measuring, during total stop of the water stream, the time-history of pressure change in one section of the turbine penstock and relate it to the pressure in the upper reservoir to which the penstock is connected. The volumetric flow rate is determined from the relevant integration of the measured temporary pressure rise. Flow measurement was possible this way because the influence of the penstock inlet was negligible as far as an error of the measurement is concerned. The length of the penstock was 300 m. Previous experience and a standard IEC-41-1991 were the criteria adopted and applied. A fast and efficient acquisition system, including a 16 bit card, was used. The flow rate was calculated using a computer program developed and tested on several cases. The results obtained with the Gibson method were used for calibration of the on-line flow measuring system based on the Winter-Kennedy method as one of the index methods. This method is very often used for continuous monitoring of the flow rate through hydraulic turbines, when the calibration has been done on site by using the results of measurements obtained by the absolute method. Having measured the flow rate and output power, the efficiency was calculated for any operating conditions. A curve showing the best operating conditions based on the highest efficiency is presented and discussed. The details of the instrumentation, its installation, and the results obtained are discussed in the paper. [Spanish] Este articulo describe la metodologia aplicada para la medicion del flujo en una turbina hidraulica de 170 MW. El flujo se midio utilizando el metodo de presion

  16. Method of identifying the friction of rotors using the wavelet transform; Metodo para identificar el rozamiento de rotores utilizado la transformada wavelet

    Energy Technology Data Exchange (ETDEWEB)

    Jauregui Correa, Juan Carlos; Rubio Cerda, Eduardo; Gonzalez Brambila, Oscar [CIATEQ, A.C., Queretaro (Mexico)

    2007-11-15

    The modern processes of signal analysis that measure mechanical vibrations are based on the fast transform of Fourier (FFT), nevertheless, this method is not able to identify transient phenomena nor of nonlinear nature. Although many efforts have been made to try to identify these phenomena in the frequency spectra, it is not possible to correlate the spectra with the physical characteristics of this type of phenomena. Within these phenomena on the rubbing of a rotor against the housing or trunnion of a bearing, this phenomenon has a nonlinear behavior, as it is demonstrated in this paper. In the first part a method based on the of signal analysis type wavelets is presented and how this technique can be used to predict transient and nonlinear phenomena. Once defined the method, its application in the identification of the friction of rotors is demonstrated. With this, one demonstrates that the method presented in this paper allows to also identifying in real time the rubbing phenomenon and also that it can be used as an of analysis technique in the preventive maintenance systems. [Spanish] Los procesos modernos de analisis de senales que miden vibraciones mecanicas se basan en la transformada rapida de Fourier (FFT por sus siglas en ingles), sin embargo, este metodo no es capaz de identificar fenomenos transitorios ni de naturaleza no lineal. A pesar de que se han hecho muchos esfuerzos para tratar de identificar estos fenomenos en los espectros de frecuencia, no es posible correlacionar el espectro con las caracteristicas fisicas de este tipo de fenomenos. Dentro de estos fenomenos sobre el rozamiento de un rotor contra la carcasa o munon de una chumacera, este fenomeno tiene un comportamiento no lineal, como se demuestra en este trabajo. En la primera parte se presenta un metodo basado en el analisis de senales tipo wavelets y como esta tecnica puede utilizarse para predecir fenomenos transitorios y no lineales. Una vez definido el metodo, se demuestra su

  17. Determination of Acidity and Alkalinity of Food Materials

    OpenAIRE

    三浦,芳助; 福永,祐子; 瀧川,裕里子; 津田,真美; 渡辺,陽子; 瀨山,一正

    2006-01-01

    The acidity and alkalinity of food materials in various menus was determined to clarify the influence of food on physiological functions. Menus mainly containing alkaline food materials (alkaline menu) and acid ones (acid menu) were compared. Determination of acidity and alkalinity was performed for each food material in the alkaline menu and acid menu, and acidity and alkalinity of one meal and a day's one were estimated. 1. Most of food materials in acid menu were assessed to be...

  18. Flow in potential cascades by means of the finite element method; Flujo en cascadas potenciales mediante el metodo del elemento finito

    Energy Technology Data Exchange (ETDEWEB)

    Sosa Cordero, Rodolfo; Fernandez Valencia, Gonzalo [Instituto de Investigaciones Electricas, Cuernavaca (Mexico)

    1987-12-31

    This article presents a mathematical model and its solution by means of the finite element method with approximate Garlekin formulation, for the flow analysis in a circular cascade, in a surface of revolution current of a turbo- machine, that can be axial, mixed or radial. To the revolution surface an agreed transformation is applied to obtain a plane, eliminating in this form one term in the equation succeeding in avoiding an iterative solution. Likewise, the finite element method allows to solve the equation in partial derivatives of the elliptical type in its quasi-harmonic form. Additionally, the method followed to introduce the contour conditions is presented; specially, the Kutta-Joukowsky conditions and the one of periodicity, which distinguishes this problem from the classical problems of ideal flows evaluated in the contour. [Espanol] En este articulo se presenta un modelo matematico y su solucion mediante el empleo del metodo del elemento finito con formulacion aproximada de Galerkin, para el analisis del flujo en una cascada circular, en una superficie de corriente de revolucion de una turbomaquina, que puede ser axial, mixta o radial. A la superficie de revolucion se le aplica una transformacion conforme para obtener un plano, eliminando de esta forma un termino en la ecuacion logrando evitar la solucion iterativa. Asimismo, el metodo del elemento finito permite resolver la ecuacion en derivadas parciales del tipo eliptico en su forma cuasiarmonica. Se presenta, ademas, el metodo seguido para introducir las condiciones de contorno; en especial, las condiciones de Kutta-Joukowsky y la de periodicidad, que distinguen a este problema de los problemas clasicos de flujos ideales valuados en el contorno.

  19. Flow in potential cascades by means of the finite element method; Flujo en cascadas potenciales mediante el metodo del elemento finito

    Energy Technology Data Exchange (ETDEWEB)

    Sosa Cordero, Rodolfo; Fernandez Valencia, Gonzalo [Instituto de Investigaciones Electricas, Cuernavaca (Mexico)

    1986-12-31

    This article presents a mathematical model and its solution by means of the finite element method with approximate Garlekin formulation, for the flow analysis in a circular cascade, in a surface of revolution current of a turbo- machine, that can be axial, mixed or radial. To the revolution surface an agreed transformation is applied to obtain a plane, eliminating in this form one term in the equation succeeding in avoiding an iterative solution. Likewise, the finite element method allows to solve the equation in partial derivatives of the elliptical type in its quasi-harmonic form. Additionally, the method followed to introduce the contour conditions is presented; specially, the Kutta-Joukowsky conditions and the one of periodicity, which distinguishes this problem from the classical problems of ideal flows evaluated in the contour. [Espanol] En este articulo se presenta un modelo matematico y su solucion mediante el empleo del metodo del elemento finito con formulacion aproximada de Galerkin, para el analisis del flujo en una cascada circular, en una superficie de corriente de revolucion de una turbomaquina, que puede ser axial, mixta o radial. A la superficie de revolucion se le aplica una transformacion conforme para obtener un plano, eliminando de esta forma un termino en la ecuacion logrando evitar la solucion iterativa. Asimismo, el metodo del elemento finito permite resolver la ecuacion en derivadas parciales del tipo eliptico en su forma cuasiarmonica. Se presenta, ademas, el metodo seguido para introducir las condiciones de contorno; en especial, las condiciones de Kutta-Joukowsky y la de periodicidad, que distinguen a este problema de los problemas clasicos de flujos ideales valuados en el contorno.

  20. Determination of acetylsalicylic acid and salicylic acid in foods, using HPLC with fluorescence detection.

    NARCIS (Netherlands)

    Venema, D.P.; Hollman, P.C.H.; Janssen, P.L.T.M.K.; Katan, M.B.

    1996-01-01

    We developed a specific and sensitive HPLC method with fluorescence detection for the determination of free acetylsalicylic acid, free salicylic acid, and free salicylic acid plus salicylic acid after alkaline hydrolysis (free-plus-bound) in foods. Acetylsalicylic acid was detected after postcolumn

  1. Fluorometric determination of uric acid in bovine milk

    DEFF Research Database (Denmark)

    Larsen, Torben; Moyes, Kasey

    2010-01-01

    The primary objective of this study is to validate a new fast method for determination of uric acid in milk. The method is based on an enzymatic-fluorometric technique that requires minimal pre-treatment of milk samples. The present determination of uric acid is based on the enzymatic oxidation o...

  2. Determination of peracetic acid and hydrogen peroxide in the mixture

    Directory of Open Access Journals (Sweden)

    Bodiroga Milanka

    2002-01-01

    Full Text Available Iodometric and permanganometric titrations were used for determination of peracetic acid and hydrogen peroxide (H2O2 in the mixture. Two procedures were described and compared. Titrations could be done in only one vessel, in the same reaction mixture, when iodometric titration of peracetic acid was continued after the permanganometric titration of H2O2, (procedure A. Peracetic acid and H2O2, as oxidizing agents, reacted with potassium iodide in an acid medium, evolving iodine. This reaction was used for the quantitative iodometric determination of total peroxide in procedure B. H2O2 reacted with potassium permanganate in acid medium, but peracetic acid did not react under the same conditions. That made possible the selective permanganometric determination of H2O2 in the presence of peracetic acid. The procedure B was performed in two titration vessels (KV=3.4% for peracetic acid, 0.6% for H2O2. The procedure A for iodometric determination of peracetic acid in one titration vessel after permanganometric titration of H2O2 was recommended (KV=2,5% for peracetic acid, 0,45% for H2O2.

  3. [Determination of glutamic acid in biological material by capillary electrophoresis].

    Science.gov (United States)

    Narezhnaya, E; Krukier, I; Avrutskaya, V; Degtyareva, A; Igumnova, E A

    2015-01-01

    The conditions for the identification and determination of Glutamic acid by capillary zone electrophoresis without their preliminary derivatization have been optimized. The effect of concentration of buffer electrolyte and pH on determination of Glutamic acid has been investigated. It is shown that the 5 Mm borate buffer concentration and a pH 9.15 are optimal. Quantitative determination of glutamic acid has been carried out using a linear dependence between the concentration of the analyte and the area of the peak. The accuracy and reproducibility of the determination are confirmed by the method "introduced - found". Glutamic acid has been determined in the placenta homogenate. The duration of analysis doesn't exceed 30 minutes. The results showed a decrease in the level of glutamic acid in cases of pregnancy complicated by placental insufficiency compared with the physiological, and this fact allows to consider the level of glutamic acid as a possible marker of complicated pregnancy.

  4. Specific bile acid radioimmunoassays for separate determinations of unconjugated cholic acid, conjugated cholic acid and conjugated deoxycholic acid in serum and their clinical application

    International Nuclear Information System (INIS)

    Matern, S.; Gerok, W.

    1977-01-01

    Specific radioimmunoassays for separate determinations of serum unconjugated cholic, conjugated cholic and conjugated deoxycholic acids have been developed. Prior to the radioimmunoassay, extraction of serum bile acids was performed with Amberlite XAD-2. Unconjugated cholic acid was separated from glyco- and taurocholic acids by thin-layer chromatography. At 50% displacement of bound labeled glyco[ 3 H]cholic acid using antiserum obtained after immunization with cholic acid-bovine serum albumin-conjugate the cross-reactivity of taurocholic acid was 100%, cholic acid 80%, glycochenodeoxycholic acid 10%, chenodeoxycholic acid 7%, conjugated deoxycholic acid 3%, and conjugated lithocholic acid 3 H]cholic acid was linear on a logit-log plot from 5 to 80 pmol of unlabeled glycocholic acid. Fasting serum conjugated cholic acid in healthy subjects was 0.68 +- 0.34 μmol/l. Unconjugated cholic acid was determined by a solid phase radioimmunoassay using the cholic acid antibody chemically bound to Sepharose. The displacement curve of [ 3 H]cholic acid in the solid phase radioimmunoassay was linear on a logit-log plot from 5 to 200 pmol of unlabeled cholic acid. The coefficient of variation between samples was 5%. Fasting serum conjugated deoxycholic acid concentrations in 10 healthy subjects ranged from 0.18 to 0.92 μmol/l determined by a radioimmunoassay using antiserum obtained after immunization with deoxycholic acid-bovine serum albumin-conjugate. The clinical application of these bile acid radioimmunoassays is shown by an 'oral cholate tolerance test' as a sensitive indicator of liver function and by an 'oral cholyglycine tolerance test' as a useful test for bile acid absorption. (orig.) [de

  5. Study of free acidity determinations in aqueous solution

    International Nuclear Information System (INIS)

    Kergreis, A.

    1966-04-01

    The object of this work is the study of the principal methods which can be applied to the measurement of 'free' acidity. In the first part, we define the various types of acidity which can exist in aqueous solution; then, after having studied some hydrolysis reactions, we compare the value of the neutralisation pH of the hydrated cation and that of the precipitation of the hydroxide. In the second part we have started to study the determination of the acidity of an aqueous solution. After having rapidly considered the 'total' acidity determination, we deal with the problem of the 'free' acidity titration. We have considered in particular certain methods: extrapolation of the equivalent point, colorimetric titrations with or without a complexing agent, and finally the use of ion-exchange resins with mixed aqueous and solvent solutions. (author) [fr

  6. Vitamin B2 content determination in liver paste by using acid and acid-enzyme hydrolysis

    Directory of Open Access Journals (Sweden)

    Basić Zorica

    2007-01-01

    Full Text Available Background/Aim. Vitamin B2 is available in foodstuff in the form of coenzyme and in free form. For its content determination a few procedures should be performed (deliberation from a complex, extraction of free and deliberated form and detection, identification and quantification. There is a particular problem in determination of vitamin B2 in the meat products. For a determination of total vitamin B2 content in liver paste two preparation procedures are compared: acid and acid-enzymatic hydrolysis. The aim of this study thus, was to compare the effectiveness of these two different procedures for vitamin B2 content determination in liver paste. Methods. High pressure liquid chromatography (HPLC method with fluorescence detector, as specific and adequately sensitive for the foodstuff of a complex composition with a natural vitamin content, was used for determination of vitamin B2 in liver paste. Acid hydrolysis was performed with the application 0.1 M hydrochloric acid in a pressure cooker, and enzymatic hydrolysis was performed with the 10% takadiastase on 45 ºC within four hours. Ten samples of liver paste from the supply of the Serbian Army were examined. Separation was performed on the analytical column Nucleosil 50−5 C18 with mobile phase 450 ml CH3OH + 20 ml 5 mM CH3COONH4, and detection on the fluorescent detector with the variable wave length. Both methods were validated: examining a detection limit, quantification limit, specificity (because of a possible B2 vitamin interference with reagents, linearity of a peak area and standard concentration of B2 vitamin ratio in the range from 0.05 μg/ml to 2 μg/ml, precision for the 0.05 μg/ml concentration and recovery. Results. All the previously examined parameters validated both methods as specific, precise and reproductive, with a high recovery (98.5% for acid and 98.2% for acid - enzymatic hydrolysis, as well as linearity in a range that significantly superseded the expected content in

  7. The method of quantitative determination of iodine in acetic acid

    International Nuclear Information System (INIS)

    Sukhomlinov, A.B.; Kalinchenko, N.B.

    1988-01-01

    Method for separate determination of J 2 and J - concentrations in acetic acid is suggested. Iodine concentration in acetic acid is determined by measuring potential of iodine-selective electrode first in the initial solution of acetic acid, where molecular iodine dissociation equals 0.5, and then in acetic acid, with alkali (NaOH) addition up to pH > 3, where molecular iodine dissociation equals 1. Determination is conducted in 5x10 -7 -5x10 -6 mol/l concentration range with relative standard deviation not more than 0.1. 1 fig

  8. Spectrophotometric determination of boric acid in boron powder with curcumin

    International Nuclear Information System (INIS)

    Grotheer, E.W.

    1979-01-01

    A rapid and accurate method was needed to determine trace amounts of boric acid for quality control and specification testing of elemental boron. The reaction between boric acid and curcumin occurs at a measurable rate only when the curcumin molecule is protonated. Protonation takes place at the carbonyl groups in the presence of a strong acid and occurs completely and rapidly when sulfuric acid is added to a solution of curcumin in acetic acid. Spectrophotometric measurements were made. The extraction of boric acid from boron powder was found to be complete within 2h when either water or the diol solution was used. Whatman No. 40 cr 42 filter paper was used to obtain diol samples free of boron particles. The extraction efficiency of 2-ethyl-1,3-hexanediol was evaluated by adding 1 ml of 500 ppM aqueous boric acid and 1 drop of 10% NaOH to accurately weighed samples of boron powder. The water then was evaporated at room temperature and the samples were extracted with diol solution. The data obtained are included. The extraction efficiency also was evaluated by determining the boric acid content of boron which had been recovered from a previous extraction and boric acid determination. The determination of boric acid using curcumin is unaffected by the presence of other compounds, except for fluoride and nitrate ions. 2 tables

  9. Determination of the seasonal changes on total fatty acid ...

    African Journals Online (AJOL)

    Total fatty acid compositions and seasonal variations of Oncorhynchus mykiss in Ivriz Dam Lake, Turkey were investigated using gas chromatographic method. A total of 38 different fatty acids were determined in the fatty acid composition of rainbow trout. Polyunsaturated fatty acids (PUFAs) were found to be higher than ...

  10. Determination of amino acids in grape-derived products: a review.

    Science.gov (United States)

    Callejón, R M; Troncoso, A M; Morales, M L

    2010-06-15

    The amino acids present in foods and beverages affect the quality of these products and they play an important role in enology. Amino acids are consumed by yeasts as a source of nitrogen during alcoholic fermentation and are precursors of aroma compounds. In this review various chromatographic methodologies for the determination of amino acids are described, and specific applications for the analysis of amino acid content are discussed. Amino acids usually need to be derivatized to make them more detectable. Several derivatizing reagents have been employed for the determination of amino acids in enological applications, and each has its advantages and disadvantages.

  11. Comparison of bile acid synthesis determined by isotope dilution versus fecal acidic sterol output in human subjects

    International Nuclear Information System (INIS)

    Duane, W.C.; Holloway, D.E.; Hutton, S.W.; Corcoran, P.J.; Haas, N.A.

    1982-01-01

    Fecal acidic sterol output has been found to be much lower than bile acid synthesis determined by isotope dilution. Because of this confusing discrepancy, we compared these 2 measurements done simultaneously on 13 occasions in 5 normal volunteers. In contrast to previous findings, bile acid synthesis by the Lindstedt isotope dilution method averaged 16.3% lower than synthesis simultaneously determined by fecal acidic sterol output (95% confidence limit for the difference - 22.2 to -10.4%). When one-sample determinations of bile acid pools were substituted for Lindstedt pools, bile acid synthesis by isotope dilution averaged 5.6% higher than synthesis by fecal acidic sterol output (95% confidence limits -4.9 to 16.1%). These data indicate that the 2 methods yield values in reasonably close agreement with one another. If anything, fecal acidic sterol outputs are slightly higher than synthesis by isotope dilution

  12. Rapid Methods of Determining Internal Radioactive Contamination; Methodes Rapides Permettant d'Evaluer la Contamination Radioactive Interne; 0411 042b 0414 ; Metodos Rapidos para Determinar la Contaminacion Radiactiva Interna

    Energy Technology Data Exchange (ETDEWEB)

    Sedlet, J.; Fairman, W. D.; Robinson, J. J. [Industrial Hygiene and Safety Division, Argonne National Laboratory, Argonne, IL (United States)

    1965-06-15

    , il est possible de l'atteindre. Les emetteurs alpha et les emetteurs beta purs de faible energie presentent la plus grande difficulte du fait que les charges corporelles de ces nucleides doivent ordinairement etre evaluees par une analyse radiochimique du sang ou des excreta. Les auteurs decrivent les separations radiochimiques qui ont ete mises au point et appliquees au Laboratoire national d*Argonne pour doser rapidement ces emetteurs. Le memoire examine d'autre part certains problemes que pose l'obtention de charges corporelles a partir des taux d'excretion, peu apres l'absorption. Pendant ce laps de temps, l'excretion se modifie rapidement et, pour beaucoup de nucleides importants en l'occurrence, a un taux inconnu. Pour les taux d'absorption tres eleves ou tres bas, il n'est pas necessaire de connaitre immediatement la mesure precise des charges corporelles. Cependant, il existe pour chaque radionucleide une dose d'absorption intermediaire pour laquelle il faut pouvoir -determiner sans trop tarder la charge corporelle avec une precision relative, ce qui permet de decider ou non le traitement. Les auteurs examinent les proprietes et les facteurs qui rendent le dosage des elements osteotropes particulierement difficile dans les cas d'accident. (author) [Spanish] Los metodos aplicables en casos de accidente o en situaciones excepcionales tienen que ser suficientemente rapidos y sensibles para proporcionar resultados en plazos que faciliten el tratamiento eficaz de las personas sobreexpuestas. Los plazos disponibles dependeran, en parte, del numero de individuos irradiados. Si se logra obtener en pocas horas resultados utiles, se habra cumplido la funcion primaria de las mediciones rapidas de la carga corporal, que es la de contribuir en toda la medida de lo posible a reducir los danos debidos .a radionuclidos depositados internamente. Los metodos que se citan a continuacion pueden servir para evaluar la contaminacion interna en casos de accidente: recuento gamma y

  13. Critical load of acid precipitations. Mapping of Italian regions; Mappa dei carichi critici di acidita' totale riferita al territorio italiano

    Energy Technology Data Exchange (ETDEWEB)

    Bonanni, P.; Brini, S.; Delmonaco, G.; Liburdi, R.; Trocciola, A.; Vetrella, G. [ENEA Centro Ricerche Casaccia, S. Maria di Galeria, RM (Italy). Dipt. Ambiente

    1999-07-01

    In this report the mapping of critical loads of acidity for the Italian terrestrial ecosystems is presented. The level O method (Stockholm Environment Institute) has been used to determine sensitivity to acid deposition; this semi-quantitative method has been modified to address some Italian characteristics. The results show that the sensitivity of the Italian soils to acidification is not particularly elevated: there are really only few small areas with poor tolerance to acid depositions. These areas are in the north-east of Italy, in Alpine and Prealpine region. [Italian] Nel rapporto vengono riportati i risultati della mappatura, riferita agli ecosistemi terrestri del territorio italiano, dei carichi critici per l'acidita' totale. Il calcolo dei carichi critici e' stato eseguito sulla base della metodologia messa a punto dallo Stokholm Environment Institute; a questo metodo semi-quantitativo sono state apportate alcune modifiche per meglio adattarlo alle caratteristiche del territorio italiano. Dall'analisi dei risultati ottenuti, si evince come la sensibilita' dei suoli italiani all'acidificazione non sia particolarmente elevata: sono state riscontrate infatti solo alcune aree, peraltro con superficie limitata, con una scarsa tolleranza alle deposizioni acide. Tali aree sono localizzate nell'Italia nord-orientale, in zona alpina e prealpina.

  14. Determination of concentration and molar absorptivity of hypochlorous acid and hypobromous acid species by hydrogen peroxide titration

    Science.gov (United States)

    Uehara, H.; Arakaki, T.

    2017-12-01

    Hypochlorous acid and hypobromous acid (abbreviated as "HypoX acids") are the main ingredients of bleaching and bactericides. The HypoX acids change their chemical forms depending on environmental factors such as pH and various chemical reactions. For example, it has been reported that hypobromite ion in water changes to carcinogenic bromate by photochemical reaction with ultraviolet light. In this study, concentrations of HypoX acids were determined by UV-VIS absorbance measurement utilizing the fact that HypoX acids react with hydrogen peroxide and do not co-exist in the solution. The method for determining the concentration by titration with hydrogen peroxide can be carried out simpler and more efficiently than the DPD method or the current titration method generally used for chlorine concentration measurement. Molar absorptivity between 250 - 500 nm of HypoX acids, including their conjugate base species, was determined by solving theoretical acid-base formula including molar fraction of each chemical species at various pHs. Molar absorptivity of OCl- and OBr- between 250 - 500 nm was determined based on the concentrations obtained from titration with hydrogen peroxide and absorbance at pH > 10, where OCl- and OBr- dominate. Furthermore, the HypoX acids solutions were irradiated with a solar simulator, and the photolysis rate constants were obtained. Based on those values, the half-lives were calculated and the behavior of HypoX acids in the environment was elucidated.

  15. A novel fusidic acid resistance determinant, fusF, in Staphylococcus cohnii.

    Science.gov (United States)

    Chen, Hsiao-Jan; Hung, Wei-Chun; Lin, Yu-Tzu; Tsai, Jui-Chang; Chiu, Hao-Chieh; Hsueh, Po-Ren; Teng, Lee-Jene

    2015-02-01

    To determine MICs of fusidic acid for and identify genetic determinants of resistance in Staphylococcus cohnii isolates. Susceptibility to fusidic acid was determined by the standard agar dilution method in 24 S. cohnii subsp. urealyticus clinical isolates, 7 S. cohnii subsp. cohnii clinical isolates and 2 reference strains. Sequencing of a novel resistance determinant, fusF, and its flanking regions was performed by long and accurate PCR and inverse PCR. To evaluate the function of fusF, the MIC of fusidic acid was determined for recombinant Staphylococcus aureus carrying a plasmid expressing fusF. A total of 25 S. cohnii subsp. urealyticus (24 clinical isolates and 1 reference strain) and 2 S. cohnii subsp. cohnii displayed low-level resistance to fusidic acid (MICs 2-16 mg/L). Sequencing of a 4259 bp fragment from S. cohnii subsp. urealyticus ATCC 49330 revealed a novel resistance gene, designated fusF, which displayed 70.5% nucleotide and 67.3% amino acid identity to fusD. Expression of fusF in S. aureus confers resistance to fusidic acid. A novel FusB-family gene, fusF, was identified as a major resistance determinant in S. cohnii clinical isolates resistant to fusidic acid. © The Author 2014. Published by Oxford University Press on behalf of the British Society for Antimicrobial Chemotherapy. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

  16. The Comparative Accuracy of the 4 {pi} Liquid Scintillation Counting Method of Radioisotope Standardization; L'exactitude comparee de la methode de comptage 4 {pi} a scintillateurs liquides pour l'etalonnage des radioisotopes; Sravnitel'naya tochnost' 4 {pi} zhidkogo stsintillatsionnogo metoda podscheta standartiziruemykh radioizotopov; Exactitud del metodo de recuento con centelleador liquido 4 {pi} para normalizar radioisotopos, comparada con la de otros metodos

    Energy Technology Data Exchange (ETDEWEB)

    Steyn, J [National Physical Research Laboratory, Pretoria (South Africa)

    1960-06-15

    The accuracy of the 4 {pi} liquid scintillation counting method of standardizing {beta} emitters was compared to 4 l{pi} {beta}-{gamma} coincidence counting for the nuclides Co{sup 60}, I{sup 131} and Au{sup 198}. For P{sup 32} the liquid counting results were compared to 4 {pi} proportional counting. The efficiency of the liquid scintillation counting method was found to be energy dependent, dropping to about 97.5% for Co{sup 60} which was the lowest energy {beta} emitter investigated. (author) [French] La precision de la methode de comptage 4 {pi} a scintillateurs liquides pour l'etalonnage des emetteurs {beta} a ete comparee au comptage par coincidences 4 {pi} {beta}-{gamma} pour le So{sup 60}, le I{sup 131} et le Au{sup 198}. Dans le cas du P{sup 32}, les resultats du comptage au liquide ont ete compares a ceux du comptage 4 {pi} proportionnel. On a constate que le rendement de la methode de comptage a scintillateurs liquides variait en fonction de l'energie emise et qu'il descendait a environ 97.5% pour le Co{sup 60} qui, de tous les emetteurs {beta} etudies, emet l'energie la plus faible. (author) [Spanish] El autor compara la precision del metodo de recuento con centelleador iquido 4 {pi} para normalizar emisores {beta} con la del metodo de coincidencias {beta}-{gamma} 4 {pi}, para los siguientes nuclidos: So{sup 60}, I{sup 131} y Au{sup 198}. En el caso del P{sup 32}, confronta los resultados del primer metodo con los obtenidos mediante el recuento proporcional 4 {pi}. Comprueba que la eficacia del metodo de recuento con centelleador liquido depende de la energia y desciende al 97.5%, aproximadamente, para el Co{sup 60}, que fue el emisor {beta} mas debil que se investigo. (author) [Russian] Tochnost' 4 {pi} zhidkogo stsintillyatsionnog o metoda podscheta standartiziruemogo {beta}-izluchatelya sravnivalas' s 4 {pi} {beta}-{gamma} metodom podscheta na sovpadeniyakh dlya izotopov So{sup 60}, I{sup 131} i Au{sup 198}. Dlya R{sup 32} rezultaty zhidkogo

  17. Determination of free acid in plutonium (IV) solutions - thermometrically, potentiometrically

    International Nuclear Information System (INIS)

    Williams, T.L.; Tucker, G.M.; Huff, G.A.; Jordan, L.G.

    1981-09-01

    The thermometric titration technique was found to offer certain advantages over potentiometry in the determination of free acid in Pu(IV) solutions. The thermometric technique was applied to the determination of free acid in plutonium nitrate solutions using potassium fluoride to suppress the hydrolytic interference of plutonium(IV). The results indicate that 0.2 to 2.0 milliequivalents of free acid can be determined with acceptable bias and precision in solutions containing up to 30 milligrams of plutonium. In contrast, neither the thermometric nor the potentiometric technique was suitable for samples containing more than eight milligrams of plutonium complexed with potassium oxalate

  18. Radioimmunoassay compared to an enzymatic method for serum bile acid determination

    International Nuclear Information System (INIS)

    Samuelson, K.

    1980-01-01

    Radioimmunoassay (RIA) of cholic and chenodeoxycholic acid was compared to a total bile acid determination with 3α-hydroxysteroid dehydrogenase (3α HSD) and a gas liquid chromatographic (GLC) determination of individual bile acids. When sera from patients with increased bile acid concentration were analysed the results indicated a good correlation between GLC and the other methods. Analysis of sera from healthy subjects indicated a good correlation between GLC and RIA. No correlation existed between RIA and 3α-HSD when serum bile acids were analysed in healthy subjects partly due to the presence of varying amounts of secondary bile acids. (author)

  19. Use of hexadeuterated valproic acid and gas chromatography-mass spectrometry to determine the pharmacokinetics of valproic acid

    International Nuclear Information System (INIS)

    Acheampong, A.A.; Abbott, F.S.; Orr, J.M.; Ferguson, S.M.; Burton, R.W.

    1984-01-01

    Di-[( 3,3,3- 2 H3]propyl)acetic acid, a hexadeuterated analogue of valproic acid, was synthesized and its pharmacokinetic properties compared with valproic acid. Concentrations of valproic acid and [ 2 H]valproic acid in serum and saliva were determined by GC-MS using selected-ion monitoring. Saliva drug levels were measured with good precision down to 0.1 microgram/mL. Kinetic equivalence of valproic acid and [ 2 H]valproic acid was demonstrated in a single-dose study in a human volunteer. An isotope effect was observed for omega-oxidation, but the difference in metabolism was not sufficient to make [ 2 H]valproic acid biologically nonequivalent. The application of [ 2 H]valproic acid to determine the kinetics of valproic acid under steady-state concentrations was evaluated in the same volunteer. The kinetic data obtained with [ 2 H]valproic acid was consistent with previously reported values for valproic acid including kinetic differences observed between single-dose and steady-state experiments. Saliva levels of valproic acid were found to give a good correlation with total serum valproic acid under multiple-dose conditions. A concentration dependence was found for the ratio of saliva valproic acid to free valproic acid in serum, low ratios being observed at high serum concentrations of valproic acid

  20. Quantitative determination of glycyrrhizinic acid by square-wave

    Directory of Open Access Journals (Sweden)

    Aneta Dimitrovska

    2003-06-01

    Full Text Available Novel adsorptive stripping square-wave voltammetric method as well as a new high-pressure liquid chromatographic method for direct determination of glycyrrhizinic acid in dosage pharmaceutical preparation, used against virus infections, have been developed. Glycyrrhizinic acid is an electrochemically active compound, which undergoes irreversible reduction on a mercury electrode surface in an aqueous medium. Its redox properties were studied thoroughly by means of square-wave voltammetry, as one of the most advanced electroanalytical technique. The voltammetric response depends mainly on the pH of the medium, composition of the supporting electrolyte, as well as the parameters of the excitement signal. It was also observed that the voltammetric properties strongly depend on the accumulation time and potential, revealing significant adsorption of glycyrrhizinic acid onto the mercury electrode surface. Upon this feature, an adsorptive stripping voltammetric method for quantitative determination of glycyrrhizinic acid was developed. A simple, sensitive and precise reversed phase HPLC method with photodiode array UV detection has also been developed, mainly for comparison and conformation of the results obtained with the voltammetric method.

  1. Analytic techniques to quantify Tetrachlorohydroquinone and Chloranil; Tecnicas analiticas para cuantificar Tetraclorohidroquinona y Cloranilo

    Energy Technology Data Exchange (ETDEWEB)

    Castillo Escobedo, Ma. Teresa; Gutierrez de Gonzalez, Luz Ma; Gojon Zorrilla, Gabriel [Universidad Autonoma de Nuevo Leon, Monterrey, Nuevo Leon (Mexico)

    1995-02-01

    Tetrachlorohydroquinone (TCHQ) was determined by two methods: iodometry and cerimetry. Tritation with aqueous ceric ammonium sulphate using potentiometric end-point detection proved to be the method of choice on account of its coefficient of variation (CV=0.475%) and its excellent accuracy. Chloranil (TCQ) was quantified by titration with aqueous ascorbic acid in acetone-water-hexamethylene tetramine (HMT), the golden-yellow color of the TCQ-HMT complex disappearing at the end point. This method is accurate and has CV=0.396%. [Spanish] Se cuantifico la tetraclorohidroquinona (TCHQ) mediante una tecnica yodometrica y un metodo potenciometrico, basado en el uso de sulfato cerico amoniacal. Se concluyo que el metodo potenciometrico es el mejor, ya que tiene un coeficiente de variacion (CV) de 0.475%, y una exactitud muy aceptable. Se desarrollo un tecnica para cuantificar el Cloranilo (TCQ) por titulacion con Acido Ascorbico en presencia de Hexametilentetramina (HMT) en medio acetona-agua; el punto final se determino por la separacion del color amarillo oro del complejo TCQ-HMT. Esta tecnica presenta un coeficiente de variacion (CV) de 0.396% y una exactitud aceptable. Se realizaron pruebas de hipotesis para verificar la exactitud de los metodos elegidos.

  2. A method for the determination of D(-)-lactic acid

    NARCIS (Netherlands)

    Hamer, C.J.A. van den; Elias, R.W.

    A method for the determination of D(—)-lactic acid is described. An acetone powder from Escherichia coli B in the presence of methylene blue oxidizes D(—)-lactic specifically. Oxygen consumption in a Warburg apparatus was used as a measure of the D(—)-lactic acid.

  3. Iodometric determination of the ascorbic acid (Vitamin c) content of ...

    African Journals Online (AJOL)

    The ascorbic acid content of seven different fruits –grapefruit, lime, orange, tangerine, banana, pawpaw and pineapple was determined by iodine titration, in order to know which fruit would best supply the ascorbic acid need for the body. Results showed that tangerine had the highest value of ascorbic acid, ...

  4. Development of special analytical system for determination of free acid

    International Nuclear Information System (INIS)

    Zhang Lihua; Wu Jizong; Liu Huanliang; Liu Quanwei; Fan Dejun; Su Tao

    2008-01-01

    The determination of free-acid plays an important role in spent fuel reprocessing analysis. Its work accounts for about 30% of all analytical work in reprocessing. It is necessary to study and develop a special fast analytical system for determination of free acid. The special analytical system is particularly applicable to determination of free acid in high-level radioactive environment, which is composed of an optical fiber spectrophotometer and an automatic sample-in device. Small sample-in volume needed, fast procedure, easy operation and physical protection are its advantages. All kinds of performance and parameters satisfy the requirements of spent fuel reprocessing control analysis. For long-distance determination, the optical fiber spectrophotometer is connected with an 4.5 meters long optical fiber. To resolve the change of 0.1 mol/L acidity, the measuring optical path is 2 cm. Mass of 10-20 μm in diameter optical fibers are assembled. The optical fiber probe is composed of a reflecting mirror and a concave mirror on the top of optical fibers. To eliminate the interference of external light, a stainless steel measuring chamber is used. The automatic sample-in device is composed of state valve, quantifying pump and pipe. The sample-in precision of 15 μl and 35 μl quantifying loops is better than 0.5%. The special analytical system takes less than 7 minutes to complete one measurement. The linear range is 0.5 mol/L-3.5 mol/L. The relative standard deviation is better than 2.0% when the concentration of the free acid is about 2.0 mol/L. For samples in different medium, the results are comparable with the method of pH titration of determining the free acid in reprocessing. (authors)

  5. Survey of Pulsed Neutron Source Methods for Multiplying Media; Methodes des Neutrons Pulses Pour l'Etude des Milieux Multiplicateurs; Obzor metodov s ispol'zovaniem istochnikov impul'snykh nejtronov dlya razmnozhayushchej sredy; Estudio Panoramico de los Metodos de Empleo de Fuentes de Neutrons Pulsados en Medios Multiplicadores

    Energy Technology Data Exchange (ETDEWEB)

    Garelis, E. [General Electric Company, Vallecitos Atomic Laboratory, Pleasanton, CA (United States)

    1965-10-15

    -Small-L ). Il discute en outre l'emploi des methodes qui sont fondees sur la reponse a des impulsions pseudoaleatoires et utilisent une correlation entre l'entree et la sortie, pour la determination de la fonction de Green d'un milieu multiplicateur. H montre que les renseignements obtenus par ces methodes sont identiques a ceux fournis par les methodes de la source puisee a repetition, ce qui permet d'appliquer aux premieres les procedes qui ont ete mis au point pour les secondes. (author) [Spanish] En los ultimos afios ha habido dos tendencias principales acerca de la manera mas eficaz de medir la reactividad de parada, empleando fuentes de neutrones pulsados: la primera preconizaba el empleo de metodos tradicionales de medicion con fuentes neutronicas reiteradamente pulsadas, y la segunda propugnaba la aplicacion de metodos basados en una tecnica seudoaleatoria de respuesta a los impulsos, utilizando una correlacion entre los datos de entrada y los de salida. La informacion obtenida con una y otra tecnica es la misma; en teoria, ambos metodos sirven para determinar la funcion de respuesta. Se resefia el desarrollo de las tecnicas de empleo de fuentes de neutrones pulsados aplicadas a sistemas termicos con miras a medir la reactividad, desde los primeros intentos de Sjoestrand hasta el reciente metodo (k{beta}/ Script-Small-L ). Con el metodo usual de empleo de estas fuentes, la propiedad que se procuia determinar es la funcion de Green del conjunto subercritico empleado, es decir, la respuesta del reactor a una fuente de neutrones de funcion delta. El decrecimiento exponencial (e{sup {alpha}t}) de la funcion de Green proporciona una constante de decrecimiento de los neutrones instantaneos que es independiente del espacio. El autor examina los metodos para obtener el valor de la reactividad partiendo de la medida de a, como por ejemplo el metodo de la medicion de la criticidad por neutrones retardados a y el reciente metodo (k{beta}/ Script-Small-L ). Seguidamente examina el

  6. New method for the determination of bile acid turnover using /sup 75/Se-homocholic acid taurine

    Energy Technology Data Exchange (ETDEWEB)

    Delhez, H.; Meerwaldt, J.H.; van den Berg, J.W.O.; van Blankenstein, M.

    1982-06-01

    The introduction of /sup 75/Se-homocholic acid taurine (/sup 75/SeHCAT) greatly facilitates the investigation of diarrhoea of unknown origin. By using gamma-labelled bile acids, daily faecal bile acid loss can be measured in total collected stools, thus circumventing laborious mixing and sampling. The /sup 75/SeHCAT method proved to be reliable for the determination of bile acid turnover, giving results identical to the established turnover method using /sup 14/C-taurocholic acid. The new method however, is simpler and faster.

  7. A method for optimization of patient dose estimation in conventional radiology; Un metodo per l'ottimizzazione della stima della dose al paziente nella radiologia tradizionale

    Energy Technology Data Exchange (ETDEWEB)

    Tofani, A.; Del Corona, A. [Azienda Unita' Sanitaria Locale 6, Livorno (Italy). Unita' Ospedaliera di Fisica Sanitaria; Niespolo, A. [Azienda Ospedaliera Pisana, Pisa (Italy). Unita' Ospedaliera di Fisica Sanitaria

    2000-05-01

    found to depend on the average body surface, a parameter which takes into account both patient height and mass. Thus, determining the normalization factor for each projection and each view allows to estimate the absorbed dose under different geometrical conditions. The method has been verified by considering four of the most common X-ray procedures (chest AP, cervical spine LAT, lumbar spine AP and head LAT). The average error on dose estimation is about 13 %. In the very next future the method will be extended to all the projections and views of ICRP Report no. 34, and we plant to integrate the described algorithm in a computer program devoted to the automatic computation of patient dose. [Italian] Il metodo raccomandato dalla International Commission on Radiological Protection (ICRP) nel suo Report n. 34(1982) per il calcolo della dose al paziente negli esami di radiodiagnostica e' basato su dati dosimetrici tabulati ottenuti mediante simulazioni Monte Carlo su fantocci antropomorfi descritti da semplici funzioni matematiche. Nel caso del calcolo della dose per un paziente adulto, le limitazioni principali di questo metodo sono due: in primo luogo i parametri geometrici dell'esame - e in particolare la distanza fuoco-pellicola e il formato della pellicola- sono fissi, e questo rende problematico l'utilizzo dei dati dosimetrici nelle condizioni effettive in cui si e' svolto l'esame, che in genere non coincideranno con quelle standard ICRP. Inoltre quando le dimensioni e la massa del paziente differiscono sensibilmente da quelle del fantoccio utilizzato nelle simulazioni (il cosidetto uomo di riferimento, di altezza pari a 174 cm e massa di 70,9 Kg) il metodo ICRP puo' portare a errori considerevoli nella stima della dose. Lo scopo del presente lavoro e' quello di indicare una possibile via di uscita per superare queste limitazioni. L'algoritmo proposto in questo lavoro si basa sull'applicazione del metodo suggerito da Huda e

  8. Polarographic determination of stability constants of Eu(III) complexes with acrylic acid and crotonic acid

    Energy Technology Data Exchange (ETDEWEB)

    Rao, A L.J.; Makhan, S [Punjabi Univ., Patiala (India). Dept. of Chemistry

    1979-07-01

    Compositions and formation constants of Eu(III) complexes with acrylic acid and crotonic acid have been studied polarographically. The reductions are reversible and diffusion-controlled. The plot of Esub(1/2) versus -log Csub(x) is linear in the case of Eu(III)-acrylic acid system. The change in number of ligands bound to europium during reduction was found to be approximately equal to 1 and ratio of dissociation constants of Eu(III) and Eu(II) was found to be 40.76 x 10sup(-2). In the case of Eu(III)-crotonic acid system, composition and formation constants have been calculated by the method of Deford and Hume. Crotonic acid forms two complex species with europium (..beta../sub 1/, 60; ..beta../sub 2/, 4.2x10sup(+2)). The percentage distribution of various complex species as a function of ligand concentration has been calculated in the case of Eu(III)-crotonic acid system. A polarographic method for the determination of micro amounts of Eu(III) in the presence of diverse ions has been developed. Under optimum conditions Eu(III) in the concentration range 4x10sup(-4)-2x10sup(-3)M can be successfully determined in various mixtures.

  9. The application of hydrogen-palladium electrode for potentiometric acid-base determinations in tetrahydrofuran

    Directory of Open Access Journals (Sweden)

    Jokić Anja B.

    2013-01-01

    Full Text Available The application of the hydrogen-palladium electrode (H2/Pd as the indicator electrode for the determination of relative acidity scale (Es, mV of tetrahydrofuran (THF and the potentiometric titrations of acids in this solvent was investigated. The relative acidity scale tetrahydrofuran was determined from the difference half-neutralization potentials of perchloric acid and tetrabutylammonium hydroxide (TBAH, which were measured by using both H2/Pd-SCE and glass-SCE electrode pairs. The experimentally obtained value of Es scale THF with a H2/Pd-SCE electrode pair was 1155 mV, and those obtained with glass-SCE electrode pair 880 mV. By using a H2/Pd indicator electrode, the individual acids (benzoic acid, palmitic acid, maleic acid, acetyl acetone, α-naphthol and two component acid mixtures (benzoic acid + α-naphthol, palmitic acid + α-naphthol, maleic acid + α-naphthol and maleic acid + ftalic acid were titrated with a standard solution of TBAH. In addition, sodium methylate and potassium hydroxide proved to be very suitable titrating agents for titrating of the individual acids and the acids in mixtures, respectively. The relative error of the determination of acids in mixture was less than 3%. The results are in agreement with those obtained by a conventional glass electrode. The advantages of H2/Pd electrode over a glass electrode in potentiometric acid-base determinations in tetrahydrofuran lie in the following: this electrode gives wider relative acidity scale THF, higher the potential jumps at the titration end-point and relatively fast response time; furthermore, it is very durable, simple to prepare and can be used in the titrations of small volumes. [Projekat Ministarstva nauke Republike Srbije, br.172051

  10. Occurrence and Determination of Haloacetic Acids in Metro Manila Drinking Water

    Directory of Open Access Journals (Sweden)

    Irene B. Rodriguez

    2009-12-01

    Full Text Available Haloacetic acids are found in chlorinated water with high organic matter content. An analytical method based on a US EPA method for measuring these compounds in water is described. The optimized method used diethyl ether as extraction solvent with sulphuric acid-methanol as esterification agent and subsequent detection by gas chromatography-electron capture detection. Evaluation of this method showed that it was linear in the concentration range of 10 to 150 µg L-1 and the method detection limits were from 17 to 57 µg L-1. Although the method demonstrated low recoveries (16 to 43%, it is useful in the quantitative determination of monochloroacetic acid as well as the qualitative determination of other haloacetic acids in water. Drinking water samples taken from different areas in Metro Manila serviced by the local treatment plants were analysed using the method. Monochloroacetic acid, monobromoacetic acid, and bromochloroacetic acid were detected in these samples. Monochloroacetic acid was quantified and found in concentrations ranging from 19 to 157 µg L-1. In most of the water samples, the concentration of monochloroacetic acid exceeded the US EPA maximum allowable total concentration of 60 µg L-1 for the five haloacetic acids (monochloro-, dichloro-, trichloro-, monobromo-, and dibromoacetic acids in drinking water. This initial study established the occurrence of potentially harmful haloacetic acids in the local drinking water supplies.

  11. Atlas de aves: Un metodo para documentar distribucion y seguir poblaciones

    Science.gov (United States)

    Robbins, C.S.; Dowell, B.A.; Dawson, D.K.; Alvarez-Lopez, Humberto; Kattan, Gustavo; Murcia, Carolina

    1988-01-01

    Los Atlas de Aves son proyectos nacionales o regionalies para trazar en mapas la distribucion en reproduccion de cada especie de ave. Ese procedimiento se esta usando en Europa, Australia, Nueva Zelanda, Norteamerica, y partes de Africa. El tama?o de los cuadrados varia de medio grado de latitud y Iongitud hasta 5 x 5 km. El trabajo de campo de cada proyecto exige aproxlmadamente cinco a?os, pero los aficionados pueden llevar a cabo la mayor parte del trabajo. Es posible almacenar los resultados en un computador personal. Hay muchos beneficios: (I) se presenta la distribucion corriente de las aves de la nacion, del estado, o de la Iocalidad; (2) se desarrolla nueva informacion especialmente sobre especies raras o en peligro; (3) se descubren areas que tienen una avlfauna sobresaliente o habitats raros y ayuda a su proteccion, (4) se documentan cambios de dlstribucion; (5) se pueden usar para documentar cambios de poblacion, especialmente en los tropicos donde otros metodos son mas dificiles de usar porque hay muchas especies y no hay muchos observadores calificados en la identificacion de sonidos de las aves; (6) son proyectos buenos de investigacion para estudiantes graduados; (7) los turistas y los jefes de excursiones de historia natural pueden contribuir con muchas informaciones

  12. Determination of peracetic acid and hydrogen peroxide in the mixture

    OpenAIRE

    Bodiroga Milanka; Ognjanović Jasminka

    2002-01-01

    Iodometric and permanganometric titrations were used for determination of peracetic acid and hydrogen peroxide (H2O2) in the mixture. Two procedures were described and compared. Titrations could be done in only one vessel, in the same reaction mixture, when iodometric titration of peracetic acid was continued after the permanganometric titration of H2O2, (procedure A). Peracetic acid and H2O2, as oxidizing agents, reacted with potassium iodide in an acid medium, evolving iodine. This reaction...

  13. Determinants of folic acid knowledge and use among antenatal women.

    LENUS (Irish Health Repository)

    McDonnell, R

    1999-06-01

    Although recommendations on folic acid use were issued by health authorities in a number of countries in the early 1990s, uptake of peri-conceptional folic acid is still disappointingly low. Regardless of food fortification policies, folic acid promotion will probably be required in most countries to optimize folate levels among women of child-bearing age. The aim of this study was to examine folic acid knowledge and use, and their determinants among antenatal women in the east of Ireland in 1997.

  14. Determination of the protonation enthalpy of humic acid by calorimetric titration technique

    International Nuclear Information System (INIS)

    Kimuro, Shingo; Kirishima, Akira; Sato, Nobuaki

    2015-01-01

    Graphical abstract: The thermodynamic quantities of protonation of humic acid were determined by the combination of potentiometric titration and calorimetric titration. It was observed that the protonation enthalpy and Gibbs free energy had been affected by pH of solution. As a result, the thermodynamics of the protonation reaction of humic acid is influenced by the polyelectrolyte effect and the heterogeneity. - Highlights: • We applied calorimetric titration technique to the protonation of humic acid. • The thermodynamic quantities of protonation of humic acid were determined. • The protonation enthalpy of humic acid is affected by the heterogeneity. • Gibbs free energy of the protonation is affected by the polyelectrolyte effect. - Abstract: In this study, the calorimetric titration technique was used to determine the protonation enthalpy of two reference humic acids and polyacrylic acid. First, we obtained the apparent protonation constant of two kinds of humic acid purchased from IHSS (International Humic Substances Society) and polyacrylic acid by potentiometric titration. Second, we obtained the protonation enthalpy of them by calorimetric titration. The protonation enthalpy of humic acid was affected by pH and the ionic strength of bulk solution. From the comparison of ΔH between humic acid and polyacrylic acid, it was concluded that the pH dependence of ΔH is attributed to the heterogeneity of humic acid. And ΔH of phenolic hydroxyl group in humic acid is strongly influenced by the electric double layer of humic acid’s surface. This is considered to be a reason of the ionic strength dependence of ΔH. On the other hand, Gibbs free energy of the protonation of humic acid is affected by the electrostatic attraction with the progress of dissociation of functional groups such as carboxyl group and phenolic hydroxyl group. Consequently, the thermodynamics of the protonation of humic acid is affected by the polyelectrolyte effect and the

  15. Determination of amino acids in industrial effluents contaminated soil

    International Nuclear Information System (INIS)

    Mahar, M.T.; Khuhawar, M.Y.

    2014-01-01

    38 samples of soil for 19 locations partially irrigated on the effluents of sugar mill and oil andghee mill, bottom sediments of evaporation ponds of sugar and fertilizer industries were collected and analyzed for amino acids after acid digestion by gas chromatography using pre column derivatization with trifluroacetyleacetone and ethyl chloroformate. The results obtained were compared with the soil samples irrigated with fresh water. The soil samples were also analyzed for pH, total nitrogen contents and organic carbon. Nine essential (leucine (Leu), threonine (Thr), lysine (Lys), L-phenylalanine (Phe), tryptophan (Trp), histadine (His), L-valine (Val), methionine (Met) and isoleucine Ile) and ten non-essential ( alanine (Ala), cysteine (Cys), asparagine (Asn), glutamic acid (Glu), serine (Ser), glycine (Gly), proline (Pro), Glutamine (Gln), aspartic acid (Asp), tyrosine (Tyr)) amino acids were analyzed 13-15 amino acids were identified and determined quantitatively from soil samples. Amino acids Met, Asn, Gln and Trp were observed absent from all the samples. The variation in the amino acids contents in soil with the industrial effluents added and total nitrogen and organic carbon is discussed. (author)

  16. Selenium Derivatization of Nucleic Acids for Phase and Structure Determination in Nucleic Acid X-ray Crystallography

    Directory of Open Access Journals (Sweden)

    Zhen Huang

    2008-03-01

    Full Text Available Selenium derivatization (via selenomethionine of proteins for crystal structure determination via MAD phasing has revolutionized protein X-ray crystallography. It is estimated that over two thirds of all new crystal structures of proteins have been determined via Se-Met derivatization. Similarly, selenium functionalities have also been successfully incorporated into nucleic acids to facilitate their structure studies and it has been proved that this Se-derivatization has advantages over halogen strategy, which was usually used as a traditional method in this field. This review reports the development of site-specific selenium derivatization of nucleic acids for phase determination since the year of 2001 (mainly focus on the 2’-position of the ribose. All the synthesis of 2’-SeMe modified phosphoramidite building blocks (U, C, T, A, G and the according oligonucleotides are included. In addition, several structures of selenium contained nucleic acid are also described in this paper.

  17. Simultaneous Determination of Salicylic Acid, Jasmonic Acid, Methyl Salicylate, and Methyl Jasmonate from Ulmus pumila Leaves by GC-MS

    Directory of Open Access Journals (Sweden)

    Zhi-hong Huang

    2015-01-01

    Full Text Available Salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate are important phytohormones and defensive signaling compounds, so it is of great importance to determine their levels rapidly and accurately. The study uses Ulmus pumila leaves infected by Tetraneura akinire Sasaki at different stages as materials; after extraction with 80% methanol and ethyl acetate and purification with primary secondary amine (PSA and graphitized carbon blacks (GCB, the contents of signal compounds salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate were determined by GC-MS. The results showed that the level of salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate increased remarkably in U. pumila once infected by T. akinire Sasaki, but the maximums of these four compounds occurred at different times. Salicylic acid level reached the highest at the early stage, and jasmonic acid level went to the maximum in the middle stage; by contrast, change of content of methyl salicylate and methyl jasmonate was the quite opposite.

  18. Simultaneous Determination of Salicylic Acid, Jasmonic Acid, Methyl Salicylate, and Methyl Jasmonate from Ulmus pumila Leaves by GC-MS.

    Science.gov (United States)

    Huang, Zhi-Hong; Wang, Zhi-Li; Shi, Bao-Lin; Wei, Dong; Chen, Jian-Xin; Wang, Su-Li; Gao, Bao-Jia

    2015-01-01

    Salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate are important phytohormones and defensive signaling compounds, so it is of great importance to determine their levels rapidly and accurately. The study uses Ulmus pumila leaves infected by Tetraneura akinire Sasaki at different stages as materials; after extraction with 80% methanol and ethyl acetate and purification with primary secondary amine (PSA) and graphitized carbon blacks (GCB), the contents of signal compounds salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate were determined by GC-MS. The results showed that the level of salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate increased remarkably in U. pumila once infected by T. akinire Sasaki, but the maximums of these four compounds occurred at different times. Salicylic acid level reached the highest at the early stage, and jasmonic acid level went to the maximum in the middle stage; by contrast, change of content of methyl salicylate and methyl jasmonate was the quite opposite.

  19. Methods of Uranium Determination in solutions of Tributyl Phosphate and Kerosene; Metodos de determinacion de uranio en soluciones de fosfato de tributilo y queroseno

    Energy Technology Data Exchange (ETDEWEB)

    Petrement Eguiluz, J; Palomares Delgado, F

    1962-07-01

    A new analytical method for the determination of uranium in organic solutions of tributyl phosphate and kerosene is proposed. In this method the uranium is reectracted from the aqueous phase by reduction with cadmium in acid solution. The uranium can be determined in this solution by the usual methods. In case of very diluted solutions, a direct spectrophtometrical determination of uranium in the organic phase with dibenzoylmethane is proposed. (Author) 21 refs.

  20. Validation of lignocellulosic biomass carbohydrates determination via acid hydrolysis.

    Science.gov (United States)

    Zhou, Shengfei; Runge, Troy M

    2014-11-04

    This work studied the two-step acid hydrolysis for determining carbohydrates in lignocellulosic biomass. Estimation of sugar loss based on acid hydrolyzed sugar standards or analysis of sugar derivatives was investigated. Four model substrates (starch, holocellulose, filter paper and cotton) and three levels of acid/material ratios (7.8, 10.3 and 15.4, v/w) were studied to demonstrate the range of test artifacts. The method for carbohydrates estimation based on acid hydrolyzed sugar standards having the most satisfactory carbohydrate recovery and relative standard deviation. Raw material and the acid/material ratio both had significant effect on carbohydrate hydrolysis, suggesting the acid to have impacts beyond a catalyst in the hydrolysis. Following optimal procedures, we were able to reach a carbohydrate recovery of 96% with a relative standard deviation less than 3%. The carbohydrates recovery lower than 100% was likely due to the incomplete hydrolysis of substrates, which was supported by scanning electron microscope (SEM) images. Copyright © 2014 Elsevier Ltd. All rights reserved.

  1. Determination of free nitric acid in uranyl nitrate solution

    International Nuclear Information System (INIS)

    Mayankutty, P.C.; Ravi, S.; Nadkarni, M.N.

    1981-01-01

    Potentiometric titration of uranyl nitrate solution with sodium hydroxide exhibits two peaks. The first peak characterises the following reaction, UO 2 (C 2 O 4 )+NaOH Na[UO 2 (C 2 O 4 )(OH)]. This reaction, indicating the partial hydrolysis of uranyl oxalate complex, appears to be complete at pH9. If the titration is carried out to this end-point pH, the total alkali consumed can be equated to the sum of uranium content and the free acidity present in the sample volume. Based on this, a method was standardised to determine the free acidity in uranyl nitrate solution. The sample, taken in a solution of potassium oxalate previously adjusted to pH9, is titrated to this pH with standard sodium hydroxide. The free acidity in the sample can be computed by subtracting the alkali reacted with uranium from the total alkali consumed. Analyses of several synthetic samples containing uranium and nitric acid in a wide range of combinations indicate that the free acidity can be accurately determined by this method, if uranium concentration in the sample is known. The results are compared to those obtained by two other widely used methods, viz., (i) titration of pH7 in the presence of neutral potassium oxalate to suppress hydrolysis and (ii) separation of hydrolyzable ions on a cationic resin and alkali titration of the free acid released. The advantages of and the precision obtained with the present method over the above two methods are discussed. (author)

  2. Response of Substituted Indoleacetic Acids in the Indolo-alpha-pyrone Fluorescence Determination

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Böttger, M.; Kaiser, P.

    1978-01-01

    .-pyrones. Other halogenated indoleacetic acids show between zero and 60% of the fluorescence of IAA. Apparently the concentration of IAA cannot be determined in crude extracts in the presence of 4-chloro- or 5-hydroxy-indoleacetic acid, because separate determinations of each of these compounds are not possible...

  3. Spectrophotometric determination of copper with ascorbic acid

    International Nuclear Information System (INIS)

    Majeed, A.; Mustafa, M.M.; Asma, R.N.; Sareecha, N.

    1996-01-01

    Copper has been determined spectrophotometrically by using ascorbic acid as a chromagenic reagent. The complex formed in basic medium is measured for its absorbance at 340 n.m. Interference for 23 cations and 9 anions has also been checked. Effect of pH, time, temperature, ammonia, reagent concentration and interferents has been report. (author)

  4. Spectrophotometric determination of copper with ascorbic acid

    Energy Technology Data Exchange (ETDEWEB)

    Majeed, A; Mustafa, M M; Asma, R N; Sareecha, N [Islamia Univ., Bahawalpur (Pakistan). Chemistry Dept.

    1996-06-01

    Copper has been determined spectrophotometrically by using ascorbic acid as a chromagenic reagent. The complex formed in basic medium is measured for its absorbance at 340 n.m. Interference for 23 cations and 9 anions has also been checked. Effect of pH, time, temperature, ammonia, reagent concentration and interferents has been report. (author).

  5. Determination of Selected Amino Acids in Serum of Patients with Liver Disease.

    Science.gov (United States)

    Kanďár, Roman; Drábková, Petra; Toiflová, Tereza; Čegan, Alexander

    2016-01-01

    The determination of amino acids can be a reliable approach for extended diagnosis of liver diseases. This is because liver disease can be a cause of impaired amino acid metabolism. Therefore, a method for the determination of serum amino acids, applicable for clinical purposes, is necessary. The aim of this study was to find differences in the levels of selected amino acids between patients with liver disease and a control group. Samples of peripheral venous blood were obtained from a group of patients with liver disease (n = 131, 59 women at an average age of 60 years and 72 men at an average age of 52 years) and a control group (n = 105, 47 women at an average age of 62 years and 58 men at an average age of 58 years). Before the separation, the amino acids were derivatized with naphthalene-2,3-dicarboxaldehyde. For the separation, reverse phase column was used. The effluent was monitored with a fluorescence detector. There were significant differences in the concentrations of some amino acids between the patients and the control group, but also between women and men. Correlations between some amino acids and markers of liver blood tests and lipid metabolism were observed. A simple, relatively rapid and selective HPLC method with fluorescence detection for the determination of selected amino acids in serum has been developed.

  6. Determination of specific activity of phosphorus-32 labelled o-phosphoric acid

    International Nuclear Information System (INIS)

    Sane, S.U.

    2015-01-01

    Phosphorus-32 is one of the important radioisotopes used in therapeutic nuclear medicine. This work was aimed at developing a fast and sensitive procedure to determine trace amounts of 32 P which is present in various acidic chemical form thereby enabling to determine its specific activity. The method utilizes ammonium molybdate and metol for complexing with phosphorus in presence of sulphuric acid which was measured using UV-VIS spectrophotometer. The phosphate and molybdate ions form a stable complex which turns blue (molybdenum blue) by reduction with sulphuric acid. The absorbance of the complex thus formed was measured at 700 nm. Five batches of 32 P produced were analyzed using the procedure and specific activity was determined. It was found that radioactivity of 32 P did not interfere in absorbance measurements and the method could be successfully adopted for the determination of specific activity of 32 P. A scope of the method is to find the chemical purity of radioactive phosphorus ( 32 P) in quality control analysis. (author)

  7. A reverse method to estimate initial temperatures in geothermal reservoirs; Un metodo inverso para estimacion de la temperatura inicial de yacimientos geotermicos

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Gutierrez, Alfonso [Instituto de Investigaciones Electricas, Gerencia de Geotermia, Cuernavaca, Morelos (Mexico)]. E-mail: aggarcia@iie.org.mx; Ramos Alcantara, Jose R. [Centro Nacional de Investigacion y Desarrollo Tecnologico, Departamento de Ingenieria Mecanica, Cuernavaca, Morelos (Mexico); Arellano Gomez, Victor M. [Instituto de Investigaciones Electricas, Gerencia de Geotermia, Cuernavaca, Morelos (Mexico)

    2010-01-15

    A method is presented for estimating the initial temperature in geothermal-reservoir formations. The method is based on control theory where the measured temperatures or temperature logs are compared with corresponding simulated temperatures for different times with the well closed. The comparison is made using a control algorithm that makes changes to the originally assumed reservoir temperatures and performs iterations until the best fit between the temperature logs and the simulated temperatures is obtained. The simulation of fluid transport and heat in the well includes the processes of circulation and stop in the presence of circulation losses, modeled on macroscopic balances of momentum and energy. The transport processes in the formation regard the reservoir as an isotropic porous medium and fluid flow is described by Darcy's law. This model generates the fields of temperatures, pressures and speeds as a function of time and space. The method was tested with data from well LV-3 in Las Tres Virgenes geothermal field, Baja California Sur, Mexico. The estimated temperatures of the undisturbed formation-or initial temperatures-are compared within {+-}15 degrees Celsius with the measured temperatures, which is an acceptable outcome from an engineering point of view. [Spanish] Se presenta un metodo para la estimacion de la temperatura inicial en las formaciones de yacimientos geotermicos. El metodo se basa en la teoria de control donde las temperaturas medidas o registros de temperatura se comparan con las correspondientes temperaturas simuladas a diferentes tiempos con el pozo cerrado. La comparacion se hace usando un algoritmo de control el cual hace cambios a las temperaturas de yacimiento originalmente supuestas y realiza iteraciones hasta que se obtiene el mejor ajuste entre los registros de temperatura y las temperaturas simuladas. La simulacion del transporte de fluidos y calor en el pozo incluye los procesos de circulacion y paro en presencia de

  8. Determination of the acid value of instant noodles: interlaboratory study.

    Science.gov (United States)

    Hakoda, Akiko; Sakaida, Kenichi; Suzuki, Tadanao; Yasui, Akemi

    2006-01-01

    An interlaboratory study was performed to evaluate the method for determining the acid value of instant noodles, based on the Japanese Agricultural Standard (JAS), with extraction of lipid using petroleum ether at a volume of 100 mL to the test portion of 25 g. Thirteen laboratories participated and analyzed 5 test samples as blind duplicates. Statistical treatment revealed that the repeatability (RSDr) of acid value was noodles per unit weight, using the equation [acid value = percent free fatty acids (as oleic) x 1.99] and the extracted lipid contents. This method was shown to have acceptable precision by the present study.

  9. High Performance Liquid Chromatography Determination of Urinary Hippuric Acid and Benzoic Acid as Indices for Glue Sniffer Urine

    OpenAIRE

    Abdul Rahim Yacob; Mohamad Raizul Zinalibdin

    2010-01-01

    A simple method for the simultaneous determination of hippuric acid and benzoic acid in urine using reversed-phase high performance liquid chromatography was described. Chromatography was performed on a Nova-Pak C18 (3.9 x 150 mm) column with a mobile phase of mixed solution methanol: water: acetic acid (20:80:0.2) and UV detection at 254 nm. The calibration curve was linear within concentration range at 0.125 to 6.0 mg/ml of hippuric acid and benzoic acid. The recovery, ...

  10. Validation of Hiriart equation to compute steam production by the lip pressure method; Validacion de la ecuacion de Hiriart para calculo de gasto de vapor por el metodo de presion de labio

    Energy Technology Data Exchange (ETDEWEB)

    Flores Armenta, Magaly [Gerencia de Proyectos Geotermoelectricos de la Comision Federal de Electricidad, Morelia (Mexico)

    1996-09-01

    Mainly in new geothermal wells, it is necessary to evaluate the production in a very fast, simple and not expensive way, to know the convenience to install surface equipment, such as silencers and separators, to drive the steam to the commercial gathering system. In practice, one of the most known methods is the lip pressure one, which requires a simple set of installations. The objective of this paper is to validate the steam flow rate calculated by the lip pressure method, with respect to the ASME method. The ASME method is known for its accuracy, and is done by measuring the steam and liquid after a high pressure separator, by an orifice plate of known diameter and a triangular weir. Results of the validation show up the feasibility of application of the lip pressure method by using a simple adjustment equation. Percentage of mistake results less than 1%, without any notable influence of the production enthalpy. That equation to be applied in a general case, is as follows: Q{nu} =(20642)(F*P*D{sup 2}/{radical}h-2000). For the particular case of the Los Azufres geothermal field, the equation is: Q{nu}= 810*P*D{sup 2} [Espanol] En los pozos geotermicos, principalmente en los nuevos, es necesario evaluar su produccion de manera rapida, sencilla y economica, para determinar la conveniencia de instalar equipo superficial, como separadores, silenciadores, etc., que permita la integracion del vapor al sistema comercial de generacion electrica. Para fines practicos uno de los metodos mas conocidos es el de presion de labio, que solo requiere un arreglo sencillo de instalaciones superficiales. En este documento se validan y ajustan los calculos de produccion de vapor por ese metodo de presion de labio, con respecto a las mediciones exactas efectuadas con el metodo ASME. Este ultimo es reconocido internacionalmente por su precision, y se lleva a cabo separando la mezcla obtenida en superficie en un recipiente a presion para medir el vapor a traves de una placa de orificio

  11. The development of quantitative determination method of organic acids in complex poly herbal extraction

    Directory of Open Access Journals (Sweden)

    I. L. Dyachok

    2016-08-01

    Full Text Available Aim. The development of sensible, economical and expressive method of quantitative determination of organic acids in complex poly herbal extraction counted on izovaleric acid with the use of digital technologies. Materials and methods. Model complex poly herbal extraction of sedative action was chosen as a research object. Extraction is composed of these medical plants: Valeriana officinalis L., Crataégus, Melissa officinalis L., Hypericum, Mentha piperita L., Húmulus lúpulus, Viburnum. Based on chemical composition of plant components, we consider that main pharmacologically active compounds, which can be found in complex poly herbal extraction are: polyphenolic substances (flavonoids, which are contained in Crataégus, Viburnum, Hypericum, Mentha piperita L., Húmulus lúpulus; also organic acids, including izovaleric acid, which are contained in Valeriana officinalis L., Mentha piperita L., Melissa officinalis L., Viburnum; the aminoacid are contained in Valeriana officinalis L. For the determination of organic acids content in low concentration we applied instrumental method of analysis, namely conductometry titration which consisted in the dependences of water solution conductivity of complex poly herbal extraction on composition of organic acids. Result. The got analytical dependences, which describes tangent lines to the conductometry curve before and after the point of equivalence, allow to determine the volume of solution expended on titration and carry out procedure of quantitative determination of organic acids in the digital mode. Conclusion. The proposed method enables to determine the point of equivalence and carry out quantitative determination of organic acids counted on izovaleric acid with the use of digital technologies, that allows to computerize the method on the whole.

  12. Determination of silica in silicates by differential spectrophotometry as α-molybdosilicic acid

    International Nuclear Information System (INIS)

    Ohlweiler, O.A.; Meditsch, J.O.; Silva, S.

    1980-01-01

    A method for determining silica in silicates by differential spectrophotometry, using β-molybdosilic acid, is described. The sample is attacked by a mixture of boron trioxide and lithium carbonate (10:1). α-molydbosilicic acid is developed in a buffered solution (pH approximatelly 3.9) containing acetic acid and sodium acetate. The analytical procedure involves a series of preliminary steps which were previously elaborated for the gravimetric determination of silica as oxine molybdosilicate and which account for the removal of phosphorus, titanium and zirconium through ion exchange resins. (C.L.B.) [pt

  13. Fast mass spectrometry-based enantiomeric excess determination of proteinogenic amino acids.

    Science.gov (United States)

    Fleischer, Heidi; Thurow, Kerstin

    2013-03-01

    A rapid determination of the enantiomeric excess of proteinogenic amino acids is of great importance in various fields of chemical and biologic research and industries. Owing to their different biologic effects, enantiomers are interesting research subjects in drug development for the design of new and more efficient pharmaceuticals. Usually, the enantiomeric composition of amino acids is determined by conventional analytical methods such as liquid or gas chromatography or capillary electrophoresis. These analytical techniques do not fulfill the requirements of high-throughput screening due to their relative long analysis times. The method presented allows a fast analysis of chiral amino acids without previous time consuming chromatographic separation. The analytical measurements base on parallel kinetic resolution with pseudoenantiomeric mass tagged auxiliaries and were carried out by mass spectrometry with electrospray ionization. All 19 chiral proteinogenic amino acids were tested and Pro, Ser, Trp, His, and Glu were selected as model substrates for verification measurements. The enantiomeric excesses of amino acids with non-polar and aliphatic side chains as well as Trp and Phe (aromatic side chains) were determined with maximum deviations of the expected value less than or equal to 10ee%. Ser, Cys, His, Glu, and Asp were determined with deviations lower or equal to 14ee% and the enantiomeric excess of Tyr were calculated with 17ee% deviation. The total screening process is fully automated from the sample pretreatment to the data processing. The method presented enables fast measurement times about 1.38 min per sample and is applicable in the scope of high-throughput screenings.

  14. Determination of free acid by standard addition method in potassium thiocyanate

    International Nuclear Information System (INIS)

    1981-01-01

    An analytical method for determination of free acidity in all SRP process solutions has been developed. Free acidity was successfully determined in solutions of nitric acid and the nitrates of aluminum, chromium(III), iron(III), mercury(II), nickel(II), thorium, and uranium(VI), at metal-to-acid ratios <2.5. Sample requirements, instrumentation, and mode of operation are similar to those currently used in the Laboratories Department free acid procedures. The simple procedure would be suitable for automation and microprocessor control. The method consists of two additions of known increments of acid into a solution containing the sample aliquot (10 μmoles free acid) and 10 mL 1M potassium thiocyanate. The potential is determined in the initial solution and after each addition with a glass electrode and pH meter. The sample concentration is calculated by solution of three simultaneous Nernst equations. Two programs for this iterative computation are available: one written for the PDP-15 computer and another for a Hewlett-Packard 67 (or 97) programmable calculator. The accuracy of the result is verified by a slope that approximates the theoretical Nernst value. The relative standard deviation is <2.5%. This memorandum includes a survey of experiments with thermometric, pH, and Gran plot titrations in a variety of complexants, from which this particular system and technique logically evolved. The appendix includes a literature survey of sixty references, a discussion of the basic measurements, and a complete analytical procedure. The final step for completion of this RTA is training and consultation at the convenience of the Laboratories Department for demonstration of the method with process samples

  15. Determination of molybdenum with gallic acid and hydroxylamine

    International Nuclear Information System (INIS)

    Bermejo-Barrera, Ma.P.; Vazquez-Gonzalez, J.F.; Pazos-Naveira, Ma.C.; Bermejo-Martinez, F.

    1987-01-01

    A method for the spectrophotometric determination of molybdenum with gallic acid and hydroxylamine is proposed. The spectrum of the complex formed has a stable absorption maximum at 420 nm in acidic media and the molar absorptivity is 4.84 x 10 3 l mol -1 cm -1 in the range in which the complex obeys Beer's law (3.02-25.12 μg ml -1 of Mo). The effects of the concentration of reagent, pH, time and temperature were investigated, together with the stoicheiometry of the complex, the reproducibility and precision of the method and its susceptibility to interferences. (author)

  16. Separation and determination of some carboxylic acids by capillary electrophoresis

    International Nuclear Information System (INIS)

    Sladkov, V.; Fourest, B.

    2006-01-01

    Separation and determination of some organic acids, mono-carboxylic (formic and acetic), dicarboxylic (oxalic and tartaric), tricarboxylic (citric) acids and aromatic acids (phtalic, benzoic, mellitic and trimellitic), by capillary electrophoresis are reviewed. The method development parameters, such as separation and injection mode, are discussed. Special attention is paid to the comparison of different detection types (spectroscopic and electrochemical). The optimisation of the carrier electrolyte composition (choice of carrier electrolyte, effect of pH, ionic strength, electro-osmotic flow modifier) is treated. Different additives (alkali-earth and transition metal ions, cyclodextrins and alcohol), which are often used for improving organic acid separation, are also considered. (authors)

  17. Separation and determination of some carboxylic acids by capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Sladkov, V.; Fourest, B

    2006-07-01

    Separation and determination of some organic acids, mono-carboxylic (formic and acetic), dicarboxylic (oxalic and tartaric), tricarboxylic (citric) acids and aromatic acids (phtalic, benzoic, mellitic and trimellitic), by capillary electrophoresis are reviewed. The method development parameters, such as separation and injection mode, are discussed. Special attention is paid to the comparison of different detection types (spectroscopic and electrochemical). The optimisation of the carrier electrolyte composition (choice of carrier electrolyte, effect of pH, ionic strength, electro-osmotic flow modifier) is treated. Different additives (alkali-earth and transition metal ions, cyclodextrins and alcohol), which are often used for improving organic acid separation, are also considered. (authors)

  18. The separation and determination of fatty acids by isotopic dilution and radiogas-liquid chromatography

    International Nuclear Information System (INIS)

    Beardsley, D.A.

    1981-01-01

    A number of static phases have been evaluated for the GLC separation of fatty acids. Of those investigated, only AT 1200 was capable of resolving the isomeric forms of the acids. A radiogas-liquid chromatographic method incorporating isotopic dilution analysis has been developed for the determination of n-butyric acid. The proposed method has been applied to the determination of the acid in hydrolysed butter fat and milk chocolate extracts. (author)

  19. Fast high-throughput method for the determination of acidity constants by capillary electrophoresis: I. Monoprotic weak acids and bases.

    Science.gov (United States)

    Fuguet, Elisabet; Ràfols, Clara; Bosch, Elisabeth; Rosés, Martí

    2009-04-24

    A new and fast method to determine acidity constants of monoprotic weak acids and bases by capillary zone electrophoresis based on the use of an internal standard (compound of similar nature and acidity constant as the analyte) has been developed. This method requires only two electrophoretic runs for the determination of an acidity constant: a first one at a pH where both analyte and internal standard are totally ionized, and a second one at another pH where both are partially ionized. Furthermore, the method is not pH dependent, so an accurate measure of the pH of the buffer solutions is not needed. The acidity constants of several phenols and amines have been measured using internal standards of known pK(a), obtaining a mean deviation of 0.05 pH units compared to the literature values.

  20. Vanadium and titanium determination by resorcinalhydrazide of salicylic acid

    Energy Technology Data Exchange (ETDEWEB)

    Karpova, O I; Pilipenko, A T; Lukachina, V V [AN Ukrainskoj SSR, Kiev. Inst. Kolloidnoj Khimii i Khimii Vody

    1979-02-01

    The complexing of titanium and vanadium with resorcinalhydrazyl of salicylic acid (RHSA) in water-organic media is studied. Titanium (4) forms a complex at pH 0.8-1.8, vanadium - at pH 2.5-5.6, and at pH 7.6-9.8. The complexes are well extracted by polar and nonpolar solvents from acid solutions. The techniques are developed for the determination of titanium and vanadium by the RHSA agent in nickel alloys.

  1. Estimation of solubility of organo-phosphorus extractants by P determination using molybdovanadophosphoric acid method

    International Nuclear Information System (INIS)

    Gill, J.S.; Kotekar, M.K.; Singh, H.

    2005-01-01

    Solvent extraction processes have been found to be suitable for uranium recovery from phosphoric acid. Various extractants like di-2-ethyl hexylphosphoric acid (D2EHPA), di-nonylphenyl phosphoric acid (DNPPA) and synergistic agents like tri-butyl phosphate (TBP), tri-octyl phosphine oxide (TOPO) have been used in liquid-liquid extraction of uranium from phosphoric acid. Contents of these organo-phosphorus compounds in aqueous raffinates need estimation for process requirements. Solubility of Tri-butyl phosphate (TBP) and Di-2-ethylhexyl phosphoric acid (D2EHPA) extractants have been determined in different media of water, oxalic acid (0.6M) and sulphuric acid (3.75M) solutions. These compounds were estimated by determining their phosphorus (P) contents employing molybdovanadophosphoric acid method, after digesting and solubalizing them in nitric and perchloric acid. (author)

  2. Electrocatalytic and simultaneous determination of isoproterenol, uric acid and folic acid at molybdenum (VI) complex-carbon nanotube paste electrode

    International Nuclear Information System (INIS)

    Beitollahi, Hadi; Sheikhshoaie, Iran

    2011-01-01

    Highlights: → A molybdenum (VI) complex-carbon nanotube paste electrode have been fabricated. → This electrode reduced the oxidation potential of isoproterenol by about 175 mV. → It resolved the voltammetric waves of isoproterenol, uric acid and folic acid. - Abstract: This paper describes the development, electrochemical characterization and utilization of a novel modified molybdenum (VI) complex-carbon nanotube paste electrode for the electrocatalytic determination of isoproterenol (IP). The electrochemical profile of the proposed modified electrode was analyzed by cyclic voltammetry (CV) that showed a shift of the oxidation peak potential of IP at 175 mV to less positive value, compared with an unmodified carbon paste electrode. Differential pulse voltammetry (DPV) in 0.1 M phosphate buffer solution (PBS) at pH 7.0 was performed to determine IP in the range from 0.7 to 600.0 μM, with a detection limit of 35.0 nM. Then the modified electrode was used to determine IP in an excess of uric acid (UA) and folic acid (FA) by DPV. Finally, this method was used for the determination of IP in some real samples.

  3. Stereoselective determination of amino acids in beta-amyloid peptides and senile plaques.

    Science.gov (United States)

    Thorsén, G; Bergquist, J; Westlind-Danielsson, A; Josefsson, B

    2001-06-01

    A novel method for the determination of the enantiomeric composition of peptides is presented. In this paper, the focus has been on beta-amyloid peptides from deceased Alzheimer's disease patients. The peptides are hydrolyzed using mineral acid. The free amino acids are derivatized with the chiral reagent (+)- or (-)-1-(9-anthryl)-2-propyl chloroformate and subsequently separated using micellar electrokinetic chromatography (MEKC) and detected using laser-induced fluorescence (LIF) detection. The high separation efficiency of the MEKC-LIF system, yielding approximately 1 million theoretical plates/m for most amino acids, facilitates the simultaneous chiral determination of nine amino acids. The samples that have been analyzed were standard 1-40 beta-amyloid peptides, in vitro precipitated beta-amyloid fibrils, and human senile plaque samples.

  4. Non-Destructive Methods for Determining Burn-Up in Nuclear Fuel; Methodes Non Destructives d'Evaluation du Taux de Combustion dans le Combustible Nucleaire; Metody opredeleniya vygoraniya v yadernom toplive bez razrusheniya obraztsa; Metodos No Destructivos para Determinai el Grado de Combustion de los Elementos Combustibles Nucleares

    Energy Technology Data Exchange (ETDEWEB)

    McGonnagle, W. J. [Illinois Institute of Technology, Chicago, IL (United States)

    1966-02-15

    Non-destructive methods for quantitative measurement of burn-up in nuclear reactor fuel elements are useful and desirable. The ideal method for fuel assay would be one that requires no special information about the neutron spectra, radiation history, or cooling time. The irradiated fuel element contains a record of the fuel burn-up. This record is in the form of radioactive and stable isotopes resulting from the fission process. Unfortunately, in the non-destructive as well as the destructive fuel assay methods, the neutron spectrum, irradiation history, and cooling period influence this record. Likewise, the lack of precise nuclear data, such as values of nuclear cross-sections, affects any calculations that can be made. Another difficulty in the non-destructive assay is the presence of high radiation fields which contribute to the ''noise'' background of the measurements. The development of useful and realistic standards is difficult. The non-destructive burn-up methods do serve a useful purpose especially when an approximate value of burn-up is required quickly and economically even though in the present state of the art they lack the desired precision and accuracy. Several non-destructive methods for determining burn-up have been used, are being evaluated, or have been proposed. Various types of spectrometers including the bent crystal, magnetic Compton, Compton coincidence, and scintillation have been used to analyse the gamma radiation from the radioactive material formed during the fission process. Other non-destructive methods include foil activation, neutron transmission, activation analysis, measurement of capture gamma rays, and the measurement of prompt and delayed neutrons. The basic principles of each of the above instruments and methods, their sensitivities and their limitations will be reviewed. Non-destructive methods using stable isotopes produced during the fission process are proposed. In the use of stable isotopes, detailed irradiation history

  5. Application of the identification methods from Hilbert and Prony to the study of oscillatory phenomena in electrical power systems; Aplicacion de los metodos de identificacion de Hilbert y Prony al estudio de fenomenos oscilatorios en sistemas electricos de potencia

    Energy Technology Data Exchange (ETDEWEB)

    Andrade Soto, Manuel Antonio

    2002-10-15

    In the present thesis work the application of identification techniques is investigated based on methods of spectral analysis to the study of the instantaneous characteristics of signals obtained by means of digital simulation of the dynamic behavior of the power system. The study focuses on the perspectives developed from two different approaches of analysis: the use of lineal methods of spectral analysis and the use of methods of non-lineal analysis, based on the concept of an analytical signal. The developed tools are applied to the study of two phenomena of electromechanical origin of different characteristics in complex power systems. A comparison between the results obtained is performed for these techniques and the possibility of its application is discussed for the problem of on-line identification in power systems. [Spanish] En el presente trabajo de tesis se investiga la aplicacion de tecnicas de identificacion basadas en metodos de analisis espectral al estudio de las caracteristicas instantaneas de senales obtenidas mediante simulacion digital del comportamiento dinamico del sistema de potencia. El estudio se centra en las aproximaciones desarrolladas desde dos enfoques distintos de analisis: la utilizacion de metodos lineales de analisis espectral y la utilizacion de metodos de analisis no lineal, basados en el concepto de una senal analitica. Las herramientas desarrolladas se aplican al estudio de dos fenomenos de origen electromecanico de caracteristicas distintas en sistemas complejos de potencia. Se hace una comparacion entre los resultados obtenidos por estas tecnicas y se discute la posibilidad de su aplicacion al problema de identificacion en linea en sistemas de potencia.

  6. General analytical procedure for determination of acidity parameters of weak acids and bases.

    Science.gov (United States)

    Pilarski, Bogusław; Kaliszan, Roman; Wyrzykowski, Dariusz; Młodzianowski, Janusz; Balińska, Agata

    2015-01-01

    The paper presents a new convenient, inexpensive, and reagent-saving general methodology for the determination of pK a values for components of the mixture of diverse chemical classes weak organic acids and bases in water solution, without the need to separate individual analytes. The data obtained from simple pH-metric microtitrations are numerically processed into reliable pK a values for each component of the mixture. Excellent agreement has been obtained between the determined pK a values and the reference literature data for compounds studied.

  7. Determination of conjugated linoleic acid (CLA) concentrations in milk chocolate.

    Science.gov (United States)

    Hurst, W J; Tarka, S M; Dobson, G; Reid, C M

    2001-03-01

    The fatty acids from a series of milk-chocolate-based confectionery samples were analyzed as methyl esters by GC to determine the presence and amount of conjugated linoleic acid (CLA). A single peak corresponding to the 9-cis,11-trans isomer and ranging from less than 0.1% to nearly 0.2% of the total fatty acids, corresponding to up to 0.3 mg per g of chocolate, was observed. One of the chocolate extracts and a milk extract were subjected to silver ion HPLC and GC-MS in order to confirm the identity of the major isomer and tentatively identity minor isomers.

  8. The comparison of techniques and methods for L-ascorbic acid determination in the fruits

    Directory of Open Access Journals (Sweden)

    Cvetković Biljana R.

    2012-01-01

    Full Text Available Vitamin C is an essential vitamin for human nutrition; with the L-ascorbic acid (AA being the active form of vitamin C. Hence, determination of the L-ascorbic acid in the natural and processed foods is very important. In the past, plenty of methods based on the reversible redox reaction of AA oxidation/DHA reduction were developed. Because of L-ascorbic acid instability in aqueous solutions, it is useful to analyze various types of extraction. The aim of this study is to compare three different methods and three different extractants for the L-ascorbic acid determination. Fruits (kiwi, lemon, orange, and grapefruit were purchased from a local market. The L-ascorbic acid in these four samples was determined by the three different methods: the AOAC, the HPLC method with three different types of extractions, and the colorimetric method using ascorbate-oxidase. For the HPLC measurements, one part of the fruits was extracted with distilled water, the second with potassium hydrogen phosphate, and the third with 3% meta-phosphoric acid (MPA in 8% acetic acid. The HPLC measurements of each sample were repeated three times, the AOAC titration was repeated five times, and in the calorimetric method three measurements were performed. The results were statistically evaluated related to sample basis. Statistical analysis shows that there is a significant difference between the results for all three methods of extraction for all samples, except for the grapefruit sample where no significant difference was observed between the results obtained after the buffer extraction (E2 and the metaphosphoric acid in acetic acid extraction (E3. Discriminative analysis for the HPLC determinations proves that there is a clear difference and defined border between the samples in relation to the methods of extraction during the HPLC determination.

  9. Spectrophotometric determination of uranium and plutonium in nitric acid solutions at their co-presence

    International Nuclear Information System (INIS)

    Levakov, B.I.; Mishenev, V.B.; Nezgovorov, N.Yu.; Ryazanova, G.K.; Timofeev, G.A.

    1986-01-01

    The method of spectrophotometric determination of uranium (6) and plutonium (4) in nitric acid solutions is described. Uranium is determined by light absorption of the complex with arsenazo 3 in 0.05 mol/l nitric acid at λ=654 nm, plutonium - by light absorption of the complex with xylenol orange in 0.1 mol/l nitric acid at λ=540 nm. To disguise plutonium, tetravalent and certain trivalent elements DTPA is introduced into photometered solution for uranium determination. The relative root-mean square deviation of determination results does not exceed 0.03 in uranium concenration ranges 0.5-5 μg/ml, of plutonium -1-3 μg/ml

  10. Determination of hydrocyanic acid in Nipah fruit (Nypa fruticans)

    International Nuclear Information System (INIS)

    Mohd Zaidi Mat Satar; Mohd wahid samsudin; Mohamed Rozali Othman

    2011-01-01

    A study on hydrocyanic acid (anti nutrition) content in nipah (Nypa fruticans) plant components have been carried out. Analysis involve a sample of husk, seed and sap of Nypa fruticans collected from three different sampling location located at Seberang Perak (Perak), Merchang (Terengganu) and Kuala Sanglang (Perlis). A quantitative alkaline titration method was used to determine the content of hydrocyanic acid in all samples. Study carried out has proved that husk of Nypa fruticans fruit has higher content of hydrocyanic acid at all sampling location followed by seed and sap. Hydrocyanic content at all sampling location ranged from 0.03-0.06, 0.03-0.05 and 0.02-0.03 mg/ 100 g for husk, seed and sap of Nypa fruticans respectively. Statistical test carried out using one way ANOVA (at 95 % confidential level) signify that the different of sampling location and hydrocyanic acid content is significant (p<0.05) for husk of Nypa fruticans only. (author)

  11. Norepinephrine-modified glassy carbon electrode for the simultaneous determination of ascorbic acid and uric acid

    International Nuclear Information System (INIS)

    Zare, H.R.; Memarzadeh, F.; Ardakani, M. Mazloum; Namazian, M.; Golabi, S.M.

    2005-01-01

    The oxidation of norepinephrine (NE) on a preactivated glassy carbon electrode leads to the formation of a deposited layer of about 4.2 x 10 -10 mol cm -2 at the surface of the electrode. The electron transfer rate constant, k s , and charge transfer coefficient, α, for electron transfer between the electrode and immobilized NE film were calculated as 44 s -1 and 0.46, respectively. The NE-modified glassy carbon electrode exhibited good electrocatalytic properties towards ascorbic acid (AA) oxidation in phosphate buffer (pH 7.0) with an overpotential of about 475 mV lower than that of the bare electrode. The electrocatalytic response was evaluated by cyclic voltammetry, chronoamperometry, amperometry and rotating disk voltammetry. The overall number of electrons involved in the catalytic oxidation of AA and the number of electrons involved in the rate-determining step are 2 and 1, respectively. The rate constant for the catalytic oxidation of AA was evaluated by RDE voltammetry and an average value of k h was found to be 8.42 x 10 3 M -1 s -1 . Amperometric determination of AA in stirred solution exhibits a linear range of 2.0-1300.0 μM (correlation coefficient 0.9999) and a detection limit of 0.076 μM. The precision of amperometry was found to be 1.9% for replicate determination of a 49.0 μM solution of AA (n = 6). In differential pulse voltammetric measurements, the NE-modified glassy carbon electrode can separate the AA and uric acid (UA) signals. Ascorbic acid oxidizes at more negative potential than UA. Also, the simultaneous determination of UA and AA is achieved at the NE-modified electrode

  12. Simultaneous determination of shikimic acid, salicylic acid and jasmonic acid in wild and transgenic Nicotiana langsdorffii plants exposed to abiotic stresses.

    Science.gov (United States)

    Scalabrin, Elisa; Radaelli, Marta; Capodaglio, Gabriele

    2016-06-01

    The presence and relative concentration of phytohormones may be regarded as a good indicator of an organism's physiological state. The integration of the rolC gene from Agrobacterium rhizogenes and of the rat glucocorticoid receptor (gr) in Nicotiana langsdorffii Weinmann plants has shown to determine various physiological and metabolic effects. The analysis of wild and transgenic N. langsdorffii plants, exposed to different abiotic stresses (high temperature, water deficit, and high chromium concentrations) was conducted, in order to investigate the metabolic effects of the inserted genes in response to the applied stresses. The development of a new analytical procedure was necessary, in order to assure the simultaneous determination of analytes and to obtain an adequately low limit of quantification. For the first time, a sensitive HPLC-HRMS quantitative method for the simultaneous determination of salicylic acid, jasmonic acid and shikimic acid was developed and validated. The method was applied to 80 plant samples, permitting the evaluation of plant stress responses and highlighting some metabolic mechanisms. Salicylic, jasmonic and shikimic acids proved to be suitable for the comprehension of plant stress responses. Chemical and heat stresses showed to induce the highest changes in plant hormonal status, differently affecting plant response. The potential of each genetic modification toward the applied stresses was marked and particularly the resistance of the gr modified plants was evidenced. This work provides new information in the study of N. langsdorffii and transgenic organisms, which could be useful for the further application of these transgenes. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  13. Determination of free acid by standard addition method in potassium thiocyanate

    International Nuclear Information System (INIS)

    Baumann, E.W.

    1982-06-01

    The free acid content of solutions containing hydrolyzable ions has been determined potentiometrically by a standard addition method. Two increments of acid are added to the sample in 1M potassium thiocyanate solution. The sample concentration is calculated by solution of three simultaneous Nernst equations. The method has been demonstrated for solutions containing Al 3+ , Cr 3+ , Fe 3+ , Hg 2+ , Ni 2+ , Th 4+ , or UO 2 2+ with a metal-to-acid ratio of < 2.5. The method is suitable for determination of 10 μmoles acid in 10 mL total volume. The accuracy can be judged from the agreement of the Nernst slopes found in the presence and absence of hydrolyzable ions. The relative standard deviation is < 2.5%. The report includes a survey of experiments with thermometric, pH, and Gran plot titrations in a variety of complexants, from which the method was evolved. Also included is a literature survey of sixty references, a discussion of the basic measurements, and a complete analytical procedure

  14. Simultaneous determination of oleanolic acid, ursolic acid, quercetin and apigenin in Swertia mussotii Franch by capillary zone electrophoresis with running buffer modifier.

    Science.gov (United States)

    Gao, Ruibin; Wang, Litao; Yang, Yan; Ni, Jingman; Zhao, Liang; Dong, Shuqing; Guo, Mei

    2015-03-01

    The method of capillary zone electrophoresis (CZE) with direct UV detection was developed for the determination of oleanolic acid, ursolic acid, quercetin and apigenin. and then for the first time successfully applied to the analysis of four analytes in Swertia mussotii Franch and its preparations. Various factors affecting the CZE procedure were investigated and optimized, and the optimal conditions were: 50 × 10(-3) mol/L borate-phosphate buffer (pH 9.5) with 5.0 × 10(-3) mol/L β-cyclodextrin, 15 kV separation voltage, 20 °C column temperature, 250 nm detection wavelength and 5 s electrokinetic injection time (voltage 20 psi). Under the conditions, oleanolic acid, ursolic acid, quercetin and apigenin could be determined within the test ranges with a good correlation coefficient (r(2) > 0.9991). The limits of detection for conditions, oleanolic acid, ursolic acid, quercetin and apigenin were 0.3415, 0.2003, 0.0062 and 0.2538 µg/mL, respectively, and the intra- and inter-day relative standard deviations were no more than 4.72%. This procedure provided a convenient, sensitive and accurate method for simultaneous determination of oleanolic acid, ursolic acid, quercetin and apigenin in S. mussotii Franch. Copyright © 2014 John Wiley & Sons, Ltd.

  15. Simultaneous determination of acidic 3,4-dihydroxyphenylalanine metabolites and 5-hydroxyindole-3-acetic acid in urine by high-performance liquid chromatography

    NARCIS (Netherlands)

    Stroomer, A. E.; Overmars, H.; Abeling, N. G.; van Gennip, A. H.

    1990-01-01

    We describe a simple and rapid quantitative method for the simultaneous determination of 3,4-dihydroxyphenylalanine acid metabolites and 5-hydroxyindole-3-acetic acid. After solvent extraction from acidified urine, the acids are analyzed by reversed-phase high-performance liquid chromatography. For

  16. Determination of uric acid in the presence of ascorbic acid with hexacyanoferrate lanthanum film modified electrode

    International Nuclear Information System (INIS)

    Wang Guangfeng; Meng Jian; Liu Hongying; Jiao Shoufeng; Zhang Wei; Chen Daolei; Fang Bin

    2008-01-01

    A glassy carbon electrode modified with LaHCF was constructed and was characterized by cyclic voltammetry (CV) and electrochemical impedance spectrum (EIS). The resulting LaHCF modified glassy carbon electrode had a good catalytic character on uric acid (UA) and was used to detect uric acid and ascorbic acid (AA) simultaneously. This modified electrode exhibits potent and persistent electron-mediating behavior followed by well-separated oxidation peaks towards UA and AA with activation overpotential. For UA and AA in mixture, one can well separate from the other with a potential large enough to allow the determination of one in presence of the other. The DPV peak currents obtained increased linearly on the UA in the range of 2.0 x 10 -7 to 1.0 x 10 -4 mol/L with the detection limit (signal-to-noise ratio was 3) for UA 1.0 x 10 -7 mol/L. The proposed method showed excellent selectivity and stability, and the determination of UA and AA simultaneously in urine was satisfactory

  17. Gut luminal endogenous protein: implications for the determination of ileal amino acid digestibility in humans.

    Science.gov (United States)

    Moughan, Paul J; Rutherfurd, Shane M

    2012-08-01

    The true ileal digestibility assay provides the most informative measure of digestibility to assess bioavailability of amino acids in foods for humans. To determine 'true' estimates of ileal amino acid digestibility, requires that endogenous amino acids present in digesta at the terminal ileum be quantified. The amounts of endogenous amino acids in ileal digesta can be determined after feeding an animal or human a protein-free diet (traditional approach) or by various methods after giving a protein-containing diet. When the protein-free method has been applied with adult human subjects an overall mean value (three separate studies) for endogenous ileal nitrogen flow of 800 mg N/d has been reported. This value is considerably lower than a comparable value obtained after feeding protein of 1852 mg N/d (mean of four separate studies), and thus endogenous ileal N and amino acids should be measured under conditions of protein alimentation. There is some confusion concerning the terminology used to define digestibility, with the term "true" digestibility having different adopted meanings. Here, true amino acid digestibility is defined as apparent amino acid digestibility corrected for the basal amino acid losses determined after giving either a protein-free or a protein-containing diet. Basal losses should be determined at a defined dry-matter and protein intake. The protein-free diet approach to determining endogenous amino acids is considered unphysiological and basal losses refer to ileal endogenous amino acid flows associated with digesta dry-matter flow, and not including "specific" effects of dietary factors such as non starch polysaccharides and anti nutritional factors. Arguments are advanced that the enzyme hydrolysed protein/ultra filtration method may be suitable for routine application with a cannulated pig model, to obtain physiologically-valid basal estimates of ileal endogenous amino acids to allow calculation of true ileal amino acid digestibility in the

  18. Studies on the interference of hydrofluoric acid and phosphoric acid in the determination of uranium using Ti(III) reduction method-biamperometry end point

    International Nuclear Information System (INIS)

    Shiny, T.S.; Rajalakshmi, A.; Phal, D.G.; Charyulu, M.M.; Ramakumar, K.L.

    2007-01-01

    Accurate and precise determination of uranium in nuclear materials is necessary for chemical quality control as well as for nuclear material accounting purposes. Different types of uranium samples are received for the measurements. Depending upon the nature of the sample dissolution procedure is selected. Mixed oxide samples of uranium and plutonium, for example, are dissolved in nitric acid containing hydrofluoric acid under IR lamp. The fluoride ions are removed by repeated evaporation of the solution. However, some fluoride ions are left in the solutions depending on the conditions of evaporation. Uranium samples and alloy samples are dissolved in dilute hydrochloric acid. The rate of dissolution depends on concentration of acid. Sometimes a mixture of hydrochloric acid and hydrofluoric acid is used for the dissolution metal alloy samples, which may contain silica. Another method of dissolution of these samples is using a mixture of phosphoric acid and 1% hydrofluoric acid. It is necessary to study the interference of hydrofluoric acid and phosphoric acid on the determination of uranium

  19. [Determination of aristolochic acid A in Guanxinsuhe preparations by RP-HPLC].

    Science.gov (United States)

    Li, Lin; Gao, Hui-Min; Wang, Zhi-Min; Wang, Wei-Hao

    2006-01-01

    To establish a determination method of aristolochic acid A in Guanxisuhe preparations by RP-HPLC. The instrument used was Hewlett-Packard 1100 HPLC with a Alltech C18 column (4.6 mm x 250 mm, 5 microm). The mobile phase was methanol-water-acetic acid (68: 32:1) and the flow rate was 1.0 mL x min(-1). The UV detection wavelength was 390 nm and the column temperature was at 35 degrees C. The extracted solvent for the preparations was methanol solution contained 10% formic acid. The calibration curve was linear (r = 0.999 9) within the range of 0.119-1.89 microg for aristolochic acid A. The average recovery 99.0%, RSD 0.63%. The method with good linear relationship was convenient, quick, accurate, and suitable for the quality control of the aristolochic acid A in Guanxinsuhe and other traditional Chinese medicines containing aristolochic acid A.

  20. Determination of medronic acid by reversed-phase high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Zhao Xiuyan; Wang Xiaojing; Fu Bo; Ye Zhaoyun; Liu Yinli

    2012-01-01

    An isocratic liquid chromatographic method with evaporative light scattering detection (ELSD) was developed for the determination of medronic acid and its related sub- stances. Volatile pentylamine was used as the ion-pairing agent. Separations were performed on a Symmetry C8 column with an mobile phase of 98 : 2 (V : V) 30 mmol/L pentylamine (pH 5.0, adjusted with acetic acid)-methanol. The mobile phase was delivered at a flow-rate 1.0 mL/min. The method is applicable to the routine analysis and the quality con- trol of medronic acid. (authors)

  1. Determination of acid–base properties of HCl acid activated palygorskite by Potentiometrie titration

    OpenAIRE

    N. FriniSrasra; E.Srasra

    2008-01-01

    The surface acidity of raw and acid activated palygorskite clay were studied by acid-base potentiometric titration. The Gran plot method was applied for the hydroxide titration and the total surface site (Hs) and the average number of protons reacted per surface site (Z) of palygorskite samples at a given ionic strength were calculated. Acid treatment increases the clay acidity and modifies its surface charge. The point of zero charge value, determined by the common crossing point of Z vs pH ...

  2. Genetic determinism of oil acidity among some DELI oil palm ...

    African Journals Online (AJOL)

    Genetic determinism of oil acidity among some DELI oil palm (Elaeis guineensis Jacq.) progenies. Benoit Constant Likeng-Li-Ngue, Joseph Martin Bell, Georges Franck Ngando-Ebongue, Godswill Ntsefong Ntsomboh, Hermine Bille Ngalle ...

  3. Simultaneous determination of gallic acid and gentisic acid in organic anion transporter expressing cells by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wang, Li; Halquist, Matthew S; Sweet, Douglas H

    2013-10-15

    In order to elucidate the role of organic anion transporters (OATs) in the renal elimination of gallic acid and gentisic acid, a new, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous determination of gallic acid and gentisic acid in cell lysate, using Danshensu as the internal standard (IS). After a simple liquid-liquid extraction, the analytes were detected in negative ESI mode using selected reaction monitoring. The precursor-to-product ion transitions (m/z) were 169.0→125.0, 153.1→108.0, and 196.8→135.2 for gallic acid, gentisic acid, and the IS, respectively. Chromatographic separation was achieved on a C18 column using mobile phases consisting of water with 0.1% acetic acid (A) and acetonitrile with 0.05% formic acid. (B) The total run time was 3min and calibration curves were linear over the concentrations of 0.33-2400ng/mL for both compounds (r(2)>0.995). Good precision (between 3.11% and 14.1% RSD) and accuracy (between -12.7% and 11% bias) was observed for quality controls at concentrations of 0.33 (lower limit of quantification), 1, 50, and 2000ng/mL. The mean extraction recovery of gallic acid and gentisic acid was 80.7% and 83.5%, respectively. Results from post-column infusion and post-extraction methods indicated that the analytical method exhibited negligible matrix effects. Finally, this validated assay was successfully applied in a cellular uptake study to determine the intracellular concentrations of gallic acid and gentisic acid in OAT expressing cells. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. [Determination of glycyrrhizinic acid in biotransformation system by reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Li, Hui; Lu, Dingqiang; Liu, Weimin

    2004-05-01

    A method for determining glycyrrhizinic acid in the biotransformation system by reversed-phase high performance liquid chromatography (RP-HPLC) was developed. The HPLC conditions were as follows: Hypersil C18 column (4.6 mm i.d. x 250 mm, 5 microm) with a mixture of methanol-water-acetic acid (70:30:1, v/v) as the mobile phase; flow rate at 1.0 mL/min; and UV detection at 254 nm. The linear range of glycyrrhizinic acid was 0.2-20 microg. The recoveries were 98%-103% with relative standard deviations between 0.16% and 1.58% (n = 3). The method is simple, rapid and accurate for determining glycyrrhizinic acid.

  5. [A thin-layer chromatography method for determining the styrene metabolites mandelic and phenylglyoxylic acid in urine].

    Science.gov (United States)

    Gartzke, J; Burck, D

    1989-06-01

    A thin-layer chromatographic method is described for the determination of mandelic and phenyglyoxillic acid on silicagel (Silufol UV 254) after extraction from urine of styrene exposed workers. The quantitative determination was performed after eluting the spots. Phenylglyoxilic acid was measured at 255 nm and mandelic acid by derivative spectroscopically estimation of the .CH(OH).COOH -chromophore at 217 nm or by a three-wavelength mode, respectively. The recovery in urine was 80-104% for phenylglyoxilic acid and 99-105% for mandelic acid.

  6. Methods for extraction and determination of phenolic acids in medicinal plants: a review.

    Science.gov (United States)

    Arceusz, Agnieszka; Wesolowski, Marek; Konieczynski, Pawel

    2013-12-01

    Phenolic acids constitute a group of potentially immunostimulating compounds. They occur in all medicinal plants and are widely used in phytotherapy and foods of plant origin. In recent years, phenolic acids have attracted much interest owing to their biological functions. This paper reviews the extraction and determination methods of phenolic acids in medicinal plants over the last 10 years. Although Soxhlet extraction and ultrasonic assisted extraction (UAE) are commonly used for the extraction of phenolic acids from plant materials, alternative techniques such as supercritical fluid extraction (SFE), and accelerated solvent extraction (ASE) can also be used. After extraction, phenolic acids are determined usually by liquid chromatography (LC) owing to the recent developments in this technique, especially when it is coupled with mass spectrometry (MS). Also detection systems are discussed, including UV-Vis, diode array, electrochemical and fluorimetric. Other popular techniques for the analysis of this group of secondary metabolites are gas chromatography coupled with mass spectrometry (GC-MS) and capillary electrophoresis (CE).

  7. Determination of phosphorus in ortho-phorsphoric acid with high specific radioactivity

    International Nuclear Information System (INIS)

    Zhuravlev, A.A.; Bigeliene, T.A.

    1983-01-01

    An advanced photocolorimetric method of phosphorus determination (g/ml) in the preparation of orthophosphoric acid labelled by carrier-free phosphorus-32 based on the qualitative reaction, is suggested. In the reaction, ammonium molybdate produces stable dying with phosphates in the presence of bensidine, i.e. oxidation-reduction process between phosphorus-molybdenum acid and benzidine, in the result of which products of molybdenum reduction and benzidine oxidation appear

  8. Controlled-potential coulometric determination of plutonium with a hydrochloric acid-sulfamic acid electrolyte and phosphate complexing

    International Nuclear Information System (INIS)

    Jackson, D.D.; Hollen, R.M.; Roensch, F.R.; Rein, J.E.

    1981-01-01

    Total plutonium is selectively determined by a controlled-potential coulometric method in which plutonium is reduced to Pu(III) at 0.25 V (vs. SCE) in a 5.5 M hydrochloric acid-0.015 M sulfamic acid electrolyte, diverse ions are oxidized at 0.57 V, phosphate is added to reduce the Pu(III)-Pu(IV) potential, and Pu(III) is oxidized to Pu(IV) at 0.68 V. None of more than 50 metal ions present in nuclear fuel-cycle material interferes. Many anions are without effect and most interfering ones are removed by preliminary fuming with perchloric acid. The apparatus described consists mainly of commercial components. The relative standard deviation is < 0.1% at the 5-mg plutonium level

  9. Algerian mint species:high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Institute of Scientific and Technical Information of China (English)

    Brahmi Fatiha; Madani Khodir; Stvigny Caroline; Chibane Mohamed; Duez Pierre

    2014-01-01

    Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints,Mentha spicata L. (M. spicata), Mentha pulegium L. and Mentha rotundifolia (L.) Huds by high performance thin layer chromatography (HPTLC)-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation.Methods:The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform:acetone: formic acid (75:16.5:8.5, v/v) as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method.Results:Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively). The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox®equivalents) as a natural source for inhibitors of lipid peroxidation.Conclusions:Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  10. Algerian mint species: high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Directory of Open Access Journals (Sweden)

    Brahmi Fatiha

    2014-12-01

    Full Text Available Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints, Mentha spicata L. (M. spicata, Mentha pulegium L. and Mentha rotundifolia (L. Huds by high performance thin layer chromatography (HPTLC-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation. Methods: The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform: acetone: formic acid (75:16.5:8.5, v/v as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method. Results: Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1 000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively. The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox® equivalents as a natural source for inhibitors of lipid peroxidation. Conclusions: Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  11. Potentiometric Determination of Phytic Acid and Investigations of Phytate Interactions with Some Metal Ions.

    Science.gov (United States)

    Marolt, Gregor; Pihlar, Boris

    2015-01-01

    Determination of correct amount (concentration) of phytic acid is of vital importance when dealing with protonation and/or metal complexation equilibria. A novel approach for precise and reliable assay of phytic acid, based on the difference between end points by potentiometric titration, has been presented. Twelve phytic acid protons are classified into three groups of acidity, which enables detection of 2 to 3 distinct equivalent points (EPs) depending on experimental conditions, e.g. counter-ion concentration. Using the differences between individual EPs enables correct phytate determination as well as identification of potential contamination and/or determination of initial protonation degree. Impact of uncertainty of phytate amount on the calculation of protonation constants has been evaluated using computer simulation program (Hyperquad2013). With the analysis of titration curves different binding sites on phytate ligand have been proposed for complexation of Ca2+ and Fe3+ ions.

  12. Determination of Titratable Acidity in Wine Using Potentiometric, Conductometric, and Photometric Methods

    Science.gov (United States)

    Volmer, Dietrich A.; Curbani, Luana; Parker, Timothy A.; Garcia, Jennifer; Schultz, Linda D.; Borges, Endler Marcel

    2017-01-01

    This experiment describes a simple protocol for teaching acid-base titrations using potentiometry, conductivity, and/or photometry to determine end points without an added indicator. The chosen example examines the titratable acidity of a red wine with NaOH. Wines contain anthocyanins, the colors of which change with pH. Importantly, at the…

  13. L’utilizzo della ricostruzione nella comunicazione del patrimonio archeologico. L’approccio, il metodo, le finalità e alcuni spunti di discussione.

    Directory of Open Access Journals (Sweden)

    Elena Bacci

    2010-05-01

    In questo contributo si focalizza l’attenzione sulla ricostruzione grafica e virtuale del patrimonio e sulle sensazioni che la ricostruzione evoca nel fruitore del messaggio culturale. La ricostruzione si attua mediante la collaborazione tra archeologo e illustratore e costituisce un momento di verifica visiva dell’interpretazione archeologica e uno strumento di comunicazione del dato archeologico fruibile a più livelli. Ciò avviene grazie allo scambio costante di informazioni (dati scientifici e proposte di ricostruzione e il confronto che ne deriva determina i metodi e le fasi di avanzamento del progetto. Il metodo si basa sull’integrazione delle immagini 3D con il disegno tradizionale ed è finalizzato alla trasposizione del dato archeologico, in modo tale da garantire alla ricostruzione il duplice requisito di soddisfazione estetica e credibilità scientifica.

  14. Coulometric-potentiometric determination of autoprotolysis constant and relative acidity scale of water

    Directory of Open Access Journals (Sweden)

    Džudović Radmila M.

    2010-01-01

    Full Text Available The autoprotolysis constant and relative acidity scale of water were determined by applying the coulometric-potentiometric method and a hydrogen/palladium (H2/Pd generator anode. In the described procedure for the evaluation of autoprotolysis constant, a strong base generated coulometrically at the platinum cathode in situ in the electrolytic cell, in presence of sodium perchlorate as the supporting electrolyte, is titrated with hydrogen ions obtained by the anodic oxidation of hydrogen dissolved in palladium electrode. The titration was carried out with a glass-SCE electrode pair at 25.0±0.1°C. The value obtained pKw = 13.91 ± 0.06 is in agreement with literature data. The range of acidity scale of water is determined from the difference between the halfneutralization potentials of electrogenerated perchloric acid and that of sodium hydroxide in a sodium perchlorate medium. The halfneutralization potentials were measured using both a glass-SCE and a (H2/Pdind-SCE electrode pairs. A wider range of relative acidity scale of water was obtained with the glass-SCE electrode pair.

  15. Evaluation of Simple and Inexpensive High-Throughput Methods for Phytic Acid Determination

    DEFF Research Database (Denmark)

    Raboy, Victor; Johnson, Amy; Bilyeu, Kristin

    2017-01-01

    High-throughput/low-cost/low-tech methods for phytic acid determination that are sufficiently accurate and reproducible would be of value in plant genetics, crop breeding and in the food and feed industries. Variants of two candidate methods, those described by Vaintraub and Lapteva (Anal Biochem...... and legume flours regardless of endogenous phytic acid levels or matrix constituents....

  16. Simultaneous determination of equivalence volumes and acid dissociation constants from potentiometric titration data.

    Science.gov (United States)

    Papanastasiou, G; Ziogas, I

    1995-06-01

    New iterative methods for analysis of potentiometric titration data of (a) mixtures of weak monoprotic acids with their conjugate bases, (b) solutions of polyprotic (di- and triprotic) acids, and (c) mixtures of two diprotic acids are presented. These methods, using data exclusively resulting from the acidic region of the titration curve permits the accurate determination of the analytical concentration of one or more acids even if the titration is stopped well before the end point of the titration. For the titration of a solution containing a conjugate acid/base pair, the proposed procedure enables the extraction of the initial composition of the mixture, as well as the dissociation constant of the concerned acid. Thus, it is possible by this type of analysis to distinguish whether a weak acid has been contaminated by a strong base and define the extent of the contamination. On the other hand, for the titration of polyprotic acids, the proposed approach enables the extraction of the accurate values of the equivalence volume and the dissociation constants K(i) even when the ionization stages overlap. Finally, for the titration of a mixture of two diprotic acids the proposed procedure enables the determination of the composition of the mixture even if the sum of the concentrations of the acids is not known. This method can be used in the analysis of solutions containing two diastereoisomeric forms of a weak diprotic acid. The test of the proposed procedures by means of ideal and Monte Carlo simulated data revealed that these methods are fairly applicable even when the titration data are considerably obscured by 'noise' or contain an important systematic error. The proposed procedures were also successfully applied to experimental titration data.

  17. Weak Acid Ionization Constants and the Determination of Weak Acid-Weak Base Reaction Equilibrium Constants in the General Chemistry Laboratory

    Science.gov (United States)

    Nyasulu, Frazier; McMills, Lauren; Barlag, Rebecca

    2013-01-01

    A laboratory to determine the equilibrium constants of weak acid negative weak base reactions is described. The equilibrium constants of component reactions when multiplied together equal the numerical value of the equilibrium constant of the summative reaction. The component reactions are weak acid ionization reactions, weak base hydrolysis…

  18. Emissions monitoring in conveyed gas flow: (a) sulfur oxides and nitrogen oxides expressed respectively as SO{sub 2} and NO{sub 2}, (b) inorganic chlorine and fluorine compounds as gases and vapours expressed as HCl and HF; Rilevamento delle emissioni in flussi gassosi convogliati: (a) ossidid di zolfo e ossidi di azoto espressi rispettivamente come SO{sub 2} e NO{sub 2}, (b) composti inorganici del cloro e del fluoro sotto forma di gas e vapore espressi rispettivamente come HCl e HF

    Energy Technology Data Exchange (ETDEWEB)

    Ziemacki, G.; Viviano, G. [ed.] [Isituto Superiore di Sanita`, Rome (Italy). Gruppo di lavoro `Modifiche per il rilevamento delle emissioni in atmosfera da impianti industriali`

    1998-03-01

    The method (a) enables the determination of sulfur oxides (SO{sub 2}) and nitrogen oxides (NO{sub 2}) in conveyed atmospheric emissions. A stream of flue gas is a sampled by a heated with a filter housing and absorbed by an alkaline solution of potassium permanganate. The absorption solution is analyzed by ion-exchange chromatography for the determination of sulfate ion and nitrate ion as SO{sub 2} and NO{sub 2}. The method (b) enables the determination of hydrochloric acid (HCl) and hydrofluoric acid (HF) in conveyed atmospheric emissions. A stream of flue gas is sampled by a heated probe with a filter housing and absorbed by an alkaline solution (NaOH). The absorption solution is analyzed by ion-exchange chromatography for the determination of chloride ion and fluoride ion as HCl and HF. [Italiano] Il metodo a) consente la determinazione, in emissioni atmosferiche convogliate, degli ossidi di zolfo (SO{sub 2}) e degli ossidi di azoto (NO{sub 2}). Il campionamento viene effettuato mediante sonda riscaldata, munita di sistema filtrante, e sistema di assorbimento in soluzione alcalina di permanganato di potassio. La soluzione di assorbimento viene analizzata mediante cromatografia a scambio ionico, determinando le concentrazioni di ioni solfato e nitrato come SO{sub 2} ed NO{sub 2}. Il metodo b) consente la determinazione, in emissioni atmosferiche convogliate, dell`acido cloridrico (HCl) e dell`acido fluoridrico (HF). Il campionamento viene effettuato mediante sonda riscaldata, munita di sistema filtrante, e sistema di assorbimento in soluzione alcalina (NaOH). La soluzione alcalina viene quindi analizzata mediante cromatografia a scambio ionico, deter,mminando le concentrazioni di ioni cloro e fluoro come HCl e HF.

  19. SHORT COMMUNICATION DETERMINATION OF AMINO ACIDS ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    The purpose of this study was to assess the levels of free and total amino acid ... Gas chromatographic method with flame ionization detector (GC-FID) was ... Total amino acid analysis was done on acid hydrolysates of RJ samples by the ion-exchange ... The data of amino acids and protein content for all analyzed fresh and.

  20. Determination of fatty acid composition of {gamma}-irradiated hazelnuts, walnuts, almonds, and pistachios

    Energy Technology Data Exchange (ETDEWEB)

    Gecgel, Umit [Namik Kemal University, Agricultural Faculty, Department of Food Engineering, 59030 Tekirdag (Turkey); Gumus, Tuncay; Tasan, Murat; Daglioglu, Orhan; Arici, Muhammet [Namik Kemal University, Agricultural Faculty, Department of Food Engineering, 59030 Tekirdag (Turkey)

    2011-04-15

    Hazelnut, walnut, almonds, and pistachio nuts were treated with 1, 3, 5, and 7 kGy of gamma irradiation, respectively. Oil content, free fatty acid, peroxide value, and fatty acid composition of the nuts were investigated immediately after irradiation. The data obtained from the experiments indicated that gamma irradiation did not cause any significant change in the oil content of nuts. In contrast, free fatty acid and peroxide value of the nuts increased proportionally to the dose (p<0.05). Among the fatty acids determined, the concentration of total saturated fatty acids increased while total monounsaturated and total polyunsaturated fatty acids decreased with the irradiation dose (p<0.05 and <0.01).

  1. Determination of fatty acid composition of γ-irradiated hazelnuts, walnuts, almonds, and pistachios

    International Nuclear Information System (INIS)

    Gecgel, Umit; Gumus, Tuncay; Tasan, Murat; Daglioglu, Orhan; Arici, Muhammet

    2011-01-01

    Hazelnut, walnut, almonds, and pistachio nuts were treated with 1, 3, 5, and 7 kGy of gamma irradiation, respectively. Oil content, free fatty acid, peroxide value, and fatty acid composition of the nuts were investigated immediately after irradiation. The data obtained from the experiments indicated that gamma irradiation did not cause any significant change in the oil content of nuts. In contrast, free fatty acid and peroxide value of the nuts increased proportionally to the dose (p<0.05). Among the fatty acids determined, the concentration of total saturated fatty acids increased while total monounsaturated and total polyunsaturated fatty acids decreased with the irradiation dose (p<0.05 and <0.01).

  2. Determination of fatty acid composition of γ-irradiated hazelnuts, walnuts, almonds, and pistachios

    Science.gov (United States)

    Gecgel, Umit; Gumus, Tuncay; Tasan, Murat; Daglioglu, Orhan; Arici, Muhammet

    2011-04-01

    Hazelnut, walnut, almonds, and pistachio nuts were treated with 1, 3, 5, and 7 kGy of gamma irradiation, respectively. Oil content, free fatty acid, peroxide value, and fatty acid composition of the nuts were investigated immediately after irradiation. The data obtained from the experiments indicated that gamma irradiation did not cause any significant change in the oil content of nuts. In contrast, free fatty acid and peroxide value of the nuts increased proportionally to the dose (p<0.05). Among the fatty acids determined, the concentration of total saturated fatty acids increased while total monounsaturated and total polyunsaturated fatty acids decreased with the irradiation dose (p<0.05 and <0.01).

  3. Determination of gallic acid with rhodanine by reverse flow injection analysis using simplex optimization.

    Science.gov (United States)

    Phakthong, Wilaiwan; Liawruangrath, Boonsom; Liawruangrath, Saisunee

    2014-12-01

    A reversed flow injection (rFI) system was designed and constructed for gallic acid determination. Gallic acid was determined based on the formation of chromogen between gallic acid and rhodanine, resulting in a colored product with a λmax at 520 nm. The optimum conditions for determining gallic acid were also investigated. Optimizations of the experimental conditions were carried out based on the so-call univariate method. The conditions obtained were 0.6% (w/v) rhodanine, 70% (v/v) ethanol, 0.9 mol L(-1) NaOH, 2.0 mL min(-1) flow rate, 75 μL injection loop and 600 cm mixing tubing length, respectively. Comparative optimizations of the experimental conditions were also carried out by multivariate or simplex optimization method. The conditions obtained were 1.2% (w/v) rhodanine, 70% (v/v) ethanol, 1.2 mol L(-1) NaOH, flow rate 2.5 mL min(-1), 75 μL injection loop and 600 cm mixing tubing length, respectively. It was found that the optimum conditions obtained by the former optimization method were mostly similar to those obtained by the latter method. The linear relationship between peak height and the concentration of gallic acid was obtained over the range of 0.1-35.0 mg L(-1) with the detection limit 0.081 mg L(-1). The relative standard deviations were found to be in the ranges 0.46-1.96% for 1, 10, 30 mg L(-1) of gallic acid (n=11). The method has the advantages of simplicity extremely high selectivity and high precision. The proposed method was successfully applied to the determination of gallic acid in longan samples without interferent effects from other common phenolic compounds that might be present in the longan samples collected in northern Thailand. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Simultaneous determination of ascorbic acid, dopamine and uric acid based on tryptophan functionalized graphene

    International Nuclear Information System (INIS)

    Lian, Qianwen; He, Zhifang; He, Qian; Luo, Ai; Yan, Kaiwang; Zhang, Dongxia; Lu, Xiaoquan; Zhou, Xibin

    2014-01-01

    Highlights: • Trp-GR was synthesized by utilizing a facile ultrasonic method. • The material as prepared had well dispersivity in water and better conductivity than pure GR. • Trp-GR/GCE showed excellent potential for the determination of AA, DA and UA. • The proposed method was applied for the analysis of AA, DA and UA in real samples. - Abstract: A new type of tryptophan-functionalized graphene nanocomposite (Trp-GR) was synthesized by utilizing a facile ultrasonic method via π–π conjugate action between graphene (GR) and tryptophan (Trp) molecule. The material as prepared had well dispersivity in water and better conductivity than pure GR. The surface morphology of Trp-GR was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The electrochemical behaviors of ascorbic acid (AA), dopamine (DA), and uric acid (UA) were investigated by cyclic voltammetry (CV) on the surface of Trp-GR. The separation of the oxidation peak potentials for AA–DA, DA–UA and UA–AA was about 182 mV, 125 mV and 307 mV, which allowed simultaneously determining AA, DA, and UA. Differential pulse voltammetery (DPV) was used for the determination of AA, DA, and UA in their mixture. Under optimum conditions, the linear response ranges for the determination of AA, DA, and UA were 0.2–12.9 mM, 0.5–110 μM, and 10–1000 μM, with the detection limits (S/N = 3) of 10.09 μM, 0.29 μM and 1.24 μM, respectively. Furthermore, the modified electrode was investigated for real sample analysis

  5. Simultaneous determination of ascorbic acid, dopamine and uric acid based on tryptophan functionalized graphene

    Energy Technology Data Exchange (ETDEWEB)

    Lian, Qianwen; He, Zhifang; He, Qian; Luo, Ai; Yan, Kaiwang; Zhang, Dongxia [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Geography and Environment Science, Northwest Normal University, Lanzhou, 730070 (China); Lu, Xiaoquan, E-mail: Luxq@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou, 730070 (China); Zhou, Xibin, E-mail: zhouxb@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry and Environmental Analysis of Gansu Province, College of Geography and Environment Science, Northwest Normal University, Lanzhou, 730070 (China)

    2014-05-01

    Highlights: • Trp-GR was synthesized by utilizing a facile ultrasonic method. • The material as prepared had well dispersivity in water and better conductivity than pure GR. • Trp-GR/GCE showed excellent potential for the determination of AA, DA and UA. • The proposed method was applied for the analysis of AA, DA and UA in real samples. - Abstract: A new type of tryptophan-functionalized graphene nanocomposite (Trp-GR) was synthesized by utilizing a facile ultrasonic method via π–π conjugate action between graphene (GR) and tryptophan (Trp) molecule. The material as prepared had well dispersivity in water and better conductivity than pure GR. The surface morphology of Trp-GR was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. The electrochemical behaviors of ascorbic acid (AA), dopamine (DA), and uric acid (UA) were investigated by cyclic voltammetry (CV) on the surface of Trp-GR. The separation of the oxidation peak potentials for AA–DA, DA–UA and UA–AA was about 182 mV, 125 mV and 307 mV, which allowed simultaneously determining AA, DA, and UA. Differential pulse voltammetery (DPV) was used for the determination of AA, DA, and UA in their mixture. Under optimum conditions, the linear response ranges for the determination of AA, DA, and UA were 0.2–12.9 mM, 0.5–110 μM, and 10–1000 μM, with the detection limits (S/N = 3) of 10.09 μM, 0.29 μM and 1.24 μM, respectively. Furthermore, the modified electrode was investigated for real sample analysis.

  6. Preparation of 2H- and 3H-labeled phaseic acid and dihydrophaseic acid as standards for determination of abscisic acid metabolites in tomato fruit

    International Nuclear Information System (INIS)

    Kubik, M.; Buta, J.G.

    1990-01-01

    There have been reports that the level of abscisic acid (ABA) increases during the cold storage of tomatoes. However, the important ABA metabolites, phaseic acid (PA) and dihydrophaseic acid (DPA) were never quantitatively determined in such a system. In order to obtain the labeled standards for quantitative determination of those compounds by GC-MS-SIM, we fed bean plants with 6,6,6-[ 2 H 3 ]-ABA (mean isotopic enrichment 60%) with addition of about 10 5 Bq per mg of [ 3 H]-ABA. After 100 hours the plants were harvested and extracted with acetone. The extract were purified by solvent partitioning and, Prep-Sep amino column and on an HPLC C 18 reverse phase column. Two major radioactive metabolites of ABA were obtained and identified by GC-MS as PA and DPA. Some results on the quantitation of ABA, PA and DPA in tomato fruit after cold storage will be presented

  7. A review of calculation methods for fast and intermediate reactors; Expose des methodes pour le calcul de reacteurs a neutrons rapides et intermediaires; Obzor metodov rascheta reaktorov na promezhutochnykh i bystrykh nejtronakh; Estudio panoramico de los metodos de calculo de los reactores rapidos e intermedios

    Energy Technology Data Exchange (ETDEWEB)

    Marchuk, G I [Akademiya Nauk, Moskva, Union of Soviet Socialist Republics (Russian Federation)

    1962-03-15

    This paper discusses the development of methods for calculating intermediate and fast reactors. It deals with various approaches to the problems of physical calculation. The calculation of resonance effects is discussed. Consideration is given to multi-group systems of fundamental and conjugate equations, various applications of perturbation theory to the problems of physical reactor calculation, and numerical methods of solving fundamental and conjugate reactor equations, which approximate the method of spherical harmonics. The paper describes an application of the response method to the solution of critical-mass problems, and methods of calculating reactors with hydrogeneous moderators. The fundamental features of an effective one-group reactor model are described. (author) [French] L'auteur examine la mise au point de methodes pour le calcul de reacteurs a neutrons rapides et intermediaires . Il decrit diverses manieres d'aborder les problemes des calculs sur la physique des reacteurs, notamment le calcul des effets de resonance. Il s'attache particulierement aux points suivants: systemes d'equations fondamentales et conjuguees a plusieurs groupes; diverses applications de la theorie des perturbations aux problemes de calculs sur la physique des reacteurs; methodes numeriques pour resoudre les equations fondamentales et conjuguees, voisines de la methode des harmoniques spheriques. L'auteur decrit ensuite une maniere d'appliquer la methode de la reponse aux problemes de la masse critique ainsi que des methodes pour le calcul de reacteurs ralentis a l'hydrogene. Il decrit les caracteristique s fondamentale s d'un modele de reacteur a un groupe effectif. (author) [Spanish] El autor analiza el desarrollo de los metodos de calculo de los reactores nucleares que trabajan con neutrones rapidos y con neutrones intermedios. Examina diversos planteos de los problemas del calculo fisico. Indica la forma de tomar en cuenta los efectos de resonancia y menciona los sistemas

  8. Simultaneous determination of ascorbic acid, dopamine and uric acid using high-performance screen-printed graphene electrode.

    Science.gov (United States)

    Ping, Jianfeng; Wu, Jian; Wang, Yixian; Ying, Yibin

    2012-04-15

    A disposable and sensitive screen-printed electrode using an ink containing graphene was developed. This electrode combined the advantages of graphene and the disposable characteristic of electrode, which possessed wide potential window, low background current and fast electron transfer kinetics. Compared with the electrodes made from other inks, screen-printed graphene electrode (SPGNE) showed excellent electrocatalytic activity for the oxidation of ascorbic acid (AA), dopamine (DA), and uric acid (UA). Three well-defined sharp and fully resolved anodic peaks were found at the developed electrode. Differential pulse voltammetry was used to simultaneous determination of AA, DA, and UA in their ternary mixture. In the co-existence system of these three species, the linear response ranges for the determination of AA, DA, and UA were 4.0-4500 μM, 0.5-2000 μM, and 0.8-2500 μM, respectively. The detection limits (S/N=3) were found to be 0.95 μM, 0.12 μM, and 0.20 μM for the determination of AA, DA, and UA, respectively. Furthermore, the SPGNE displayed high reproducibility and stability for these species determination. The feasibility of the developed electrode for real sample analysis was investigated. Results showed that the SPGNE could be used as a sensitive and selective sensor for simultaneous determination of AA, DA, and UA in biological samples, which may provide a promising alternative in routine sensing applications. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2015-08-15

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

  10. Determination of scandium with salicylaldehyde and 2-aminobenzenearsonic acid

    International Nuclear Information System (INIS)

    Farias, P.A.M.; Hainberger, L.; Andrade, H.A.S.

    1984-01-01

    A new method for the spectrophotometric determination of scandium by means of a coloured complex formed with salicylaldehyde and 2-aminobenzenearsonic acid is described. Lambert-Beer's law is followed in the range of 0.2 - 2.0 μg/ml of the final solution. The maximum amounts of 39 ions that may be present without interfering in the method are listed. (Author) [pt

  11. [Determination of aristolochic acid A in Radix Aristolociae and Herba Asari by RP-HPLC].

    Science.gov (United States)

    Jiang, Xu; Wang, Zhi-min; You, Li-shuan; Dai, Li-ping; Ding, Guang-zhi

    2004-05-01

    To develop a HPLC method to determine the contents of aristolochic A in aristolochia debilis and Asarun spp.. Methanol-water-formic acid extracts were separated on an Alltech C18 column with methanol-water-acetic acid (68:32:1) as mobile phase. The flow rate was 1.0 mL x min(-1). UV detection wavelength was 390 nm. Column temperature was 35 degrees C. Aristolochic acid A was separated well. The relationship of injection amounts and peak areas was linear (r = 0.9999) the range of 0.12-1.89 microg x g(-1) and the recovery rate was 101.8% (n = 5). 11 samples of aristolochia debilis which bought from different areas in China were determined, and the contents of aristolochic acid A varied from 0.9 to 2 mg x g(-1). The difference of the contents in Asarum spp. was obvious. The highest is 0.35, and aristolochic acid A couldn't be detected in one sample.

  12. Photometric method for determination of acidity constants through integral spectra analysis

    Science.gov (United States)

    Zevatskiy, Yuriy Eduardovich; Ruzanov, Daniil Olegovich; Samoylov, Denis Vladimirovich

    2015-04-01

    An express method for determination of acidity constants of organic acids, based on the analysis of the integral transmittance vs. pH dependence is developed. The integral value is registered as a photocurrent of photometric device simultaneously with potentiometric titration. The proposed method allows to obtain pKa using only simple and low-cost instrumentation. The optical part of the experimental setup has been optimized through the exclusion of the monochromator device. Thus it only takes 10-15 min to obtain one pKa value with the absolute error of less than 0.15 pH units. Application limitations and reliability of the method have been tested for a series of organic acids of various nature.

  13. Folic acid supplementation is not the sole factor in determining ...

    African Journals Online (AJOL)

    Folic acid supplementation is not the sole factor in determining neural tube defects: The possible role of autoantibodies. Keat Wei Loo, Siew Hua Gan. Abstract. Neural tube defects (NTDs) are severe but common congenital malformations. Neonates who suffer from NTDs may experience long-term complications throughout ...

  14. Optimized Analytical Method to Determine Gallic and Picric Acids in Pyrotechnic Samples by Using HPLC/UV (Reverse Phase); Optimizacion del Metodo Analitico mediante HPLC/UV Operando en Fase Inversa para la Determinacion de Acido Galico y Acido Picrico en Muestras de Origen Pirotecnico

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.

    2013-10-01

    A study on the optimization and development of a chromatographic method for the determination of gallic and picric acids in pyrotechnic samples is presented. In order to achieve this, both analytical conditions by HPLC with diode detection and extraction step of a selected sample were studied. (Author)

  15. Nucleic acid helix structure determination from NMR proton chemical shifts

    Energy Technology Data Exchange (ETDEWEB)

    Werf, Ramon M. van der; Tessari, Marco; Wijmenga, Sybren S., E-mail: S.Wijmenga@science.ru.nl [Radboud University Nijmegen, Department of Biophysical Chemistry, Institute of Molecules and Materials (Netherlands)

    2013-06-15

    We present a method for de novo derivation of the three-dimensional helix structure of nucleic acids using non-exchangeable proton chemical shifts as sole source of experimental restraints. The method is called chemical shift de novo structure derivation protocol employing singular value decomposition (CHEOPS) and uses iterative singular value decomposition to optimize the structure in helix parameter space. The correct performance of CHEOPS and its range of application are established via an extensive set of structure derivations using either simulated or experimental chemical shifts as input. The simulated input data are used to assess in a defined manner the effect of errors or limitations in the input data on the derived structures. We find that the RNA helix parameters can be determined with high accuracy. We finally demonstrate via three deposited RNA structures that experimental proton chemical shifts suffice to derive RNA helix structures with high precision and accuracy. CHEOPS provides, subject to further development, new directions for high-resolution NMR structure determination of nucleic acids.

  16. Determination of Conditional Stability Constants for Metal Ions with Humic Acid using Chemically Immobilised Humic Acid on Silica Gel

    Energy Technology Data Exchange (ETDEWEB)

    Szabo, G.; Guszi, J. [Frederic Joliot-Curie' National Research Inst. for Rad iobiology and Radiohygiene, Budapest, H-1775 (Hungary)]. e-mail: szabogy@hp.osski.hu; Miyajima, T. [Dept. of Chemistry, Faculty of Science and Engineering, Saga Univ ., 1-Honjo, Saga (Japan); Geckeis, H. [Forschungszentrum Karlsruhe, Inst. fuer Nuk leare Entsorgung, 76021 Karlsruhe (Germany); Reiller, P. [Commissariat a l' Energie A tomique, CE Saclay, Laboratoire de Speciation des Radionucleides et des Molecule s, F-91191 Gif-sur-Yvette (France); Bulman, R.A. [Radiation Protection Div., Health Protection Agency, Chilton, Didcot (United Kingdom)

    2007-06-15

    Limitations on aqueous solution chemistries of humic acid, and also hydrolysis of some cationic species, restrict measurement of conditional stability constants of 4f- and 5f-series elements as humate complexes. Reported log {beta} values are determined by using non-linear regression binding isotherms, of Am(III) and Th(IV), and also Ag(I) and Sr(II), bound by a humic acid composite.

  17. An automatic system for acidity determination based on sequential injection titration and the monosegmented flow approach.

    Science.gov (United States)

    Kozak, Joanna; Wójtowicz, Marzena; Gawenda, Nadzieja; Kościelniak, Paweł

    2011-06-15

    An automatic sequential injection system, combining monosegmented flow analysis, sequential injection analysis and sequential injection titration is proposed for acidity determination. The system enables controllable sample dilution and generation of standards of required concentration in a monosegmented sequential injection manner, sequential injection titration of the prepared solutions, data collecting, and handling. It has been tested on spectrophotometric determination of acetic, citric and phosphoric acids with sodium hydroxide used as a titrant and phenolphthalein or thymolphthalein (in the case of phosphoric acid determination) as indicators. Accuracy better than |4.4|% (RE) and repeatability better than 2.9% (RSD) have been obtained. It has been applied to the determination of total acidity in vinegars and various soft drinks. The system provides low sample (less than 0.3 mL) consumption. On average, analysis of a sample takes several minutes. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Adsorption properties and porous structure of sulfuric acid treated bentonites determined - SHORT COMMUNICATION

    Directory of Open Access Journals (Sweden)

    SNEZANA BREZOVSKA

    2005-02-01

    Full Text Available In a previous paper adsorption isotherms of benzene vapor on natural bentonite from Ginovci, Macedonia, and forms acid activated with 10 % and 15 % solutions of hydrochloric were interpreted by means of the Dubinin–Radushkevich–Stoeckli and Dubinin–Astakhov equations; the investigation has been continued with bentonites acid activated with 10 % and 15 % solutions of sulfuric acid where X-ray analysis indicates smaller structural changes. Using the above equations, the heterogeneity of the micropores and the energetic heterogeneity of the bentonites were determined from the differential distribution of the micropore volume with respect to the structural parameter of the equations characterizing the microporous structure and to the molar free energy of adsorption. Activated bentonites obtain bigger pores but also a certain quantity of new small pores appear during acid activation with the higher concentration of acid. The micropore volumes, determined from the adsorption of benzene vapor, of bentonites activated with 10 % and 15 % solution of hydrochloric acid (144.60 cm3 kg-1 and 110.06 cm3 kg-1, respectively, decrease in comparison with that of natural bentonite (162.55 cm3 kgv.1 In contrast, the values of the micropore volume for bentonities treated with 10 % and 15 % solutions of sulfuric acids increase (169.19 cm3 kg-1 and 227.74 cm3 kg-1. That is due to the difference in the structural changes occurring during activation with hydrochloric and sulfuric acids. The values of the free energy of adsorption of benzene vapor for natural bentonite are higher than those of the acid acitivated bentonities, what is in accordance with the structural and porosity changes.

  19. Determination of ascorbic acid content of some tropical fruits by ...

    African Journals Online (AJOL)

    The ascorbic acid content of three common juicy tropical fruits, orange, water melon and cashew, were determined using iodometric titration method under three temperature regimes (refrigerated, room temperature, and heated to about 80 oC), representing the range of temperatures the fruits may be exposed to during ...

  20. Amino Acid Profile as a Feasible Tool for Determination of the Authenticity of Fruit Juices

    OpenAIRE

    Mostafa Asadpoor; Masoud Ansarin; Mahboob Nemati

    2014-01-01

    Purpose: Fruit juice is a nutrient rich food product with a direct connection to public health. The purpose of this research was to determine the amino acid profile of juices and provide a quick and accurate indicator for determining their authenticity. Methods: The method of analysis was HPLC with fluorescence detector and pre-column derivatization by orthophtaldialdehyde (OPA). Sixty-six samples of fruit juices were analyzed, and fourteen amino acids were identified and determined in the...

  1. Amino acids analysis by total neutron cross-sections determinations: part V

    International Nuclear Information System (INIS)

    Voi, Dante L.; Ferreira, Francisco de O.; Rocha, Helio F. da

    2013-01-01

    Total neutron cross-sections of twenty essential and non-essential amino acids to human were determined using crystal spectrometer installed on the Argonauta reactor of IEN (Instituto de Engenharia Nuclear (CNEN-RJ) and compared with data generated by parceling and grouping methodologies developed at this institution. For each amino acid was calculated the respective neutron cross-section by molecular structure, conformation and chemistry analysis. The results obtained for eighteen of twenty amino acids confirm the specifications and product formulations indicated by manufactures. These initial results allow to build a neutron cross-sections database as part of quality control of the amino supplied to hospitals for production of nutriments for parenteral or enteral formulations used in critical patients dependent on artificial feed, and for application in future studies of structure and dynamics for more complex molecules, including proteins, enzymes, fatty acids, membranes, organelles and other cell components. (author)

  2. Factors application of MW-mile method and participation in the allocation of charges by the drills use in electricity markets; Aplicacion de los factores de participacion y del metodo de MW-milla en la asignacion de cargos por uso de redes de transmision en mercados de electricidad

    Energy Technology Data Exchange (ETDEWEB)

    Alba-Gomez, L; Tovar-Hernandez, J. H; Gutierrez-Alcaraz, G [Instituto Tecnologico de Morelia, Michoacan (Mexico)]. E-mail: horaciotovar@mexico.com; ggutier@itmorelia.edu.mx

    2007-04-15

    Use of network allocation costs by shift factors and MW-Mile method is reported in this paper. Conventional shift factors are computed based on DC power flow. DC power flow requires to selecting a slack bus in order to avoid matrix singularity. Therefore, shift factors are slack bus dependent. In order to evade slack bus dependency, two approaches are considered. [Spanish] Este trabajo presenta la asignacion de costos por uso de red mediante la aplicacion de Factores de Participacion (FP) y el metodo de MW-Milla. Los FP clasicos son calculados a partir del modelo lineal de flujos de potencia para lo que se requiere de establecer un nodo de referencia a fin de eliminar la singularidad de la matriz de coeficientes. Por lo tanto, los FP son dependientes de la asignacion del nodo de referencia. Dos metodos alternativos para evitar la dependencia del nodo compensador en la obtencion de los factores de participacion son presentados.

  3. Determination and modeling of binary and ternary solid-liquid phase equilibrium for the systems formed by 3,5-dinitrobenzoic acid, m-nitrobenzoic acid and acetone

    International Nuclear Information System (INIS)

    Li, Xinbao; Du, Cunbin; Zhao, Hongkun

    2017-01-01

    Highlights: • The solubility of 3,5-dinitrobenzoic acid in acetone was determined. • Solubility of m-nitrobenzoic acid + 3,5-dinitrobenzoic acid + acetone was determined. • Three ternary phase diagrams were constructed for the ternary system. • The ternary phase diagrams were calculated by Wilson model and NRTL model. - Abstract: The solubility of 3,5-dinitrobenzoic acid in acetone at the temperatures ranging from (283.15 to 318.15) K and the mutual solubility of the ternary m-nitrobenzoic acid + 3,5-dinitrobenzoic acid + acetone system at (283.15, 298.15 and 313.15) K were determined experimentally by using the isothermal saturation method under atmosphere pressure (101.2 kPa). Three isothermal ternary phase diagrams were constructed according to the measured mutual solubility data. In each ternary phase diagram, there was one co-saturated point, two boundary curves, and three crystalline regions. The modified Apelblat equation, λh equation, NRTL model and Wilson model were used to correlate the solubility of 3,5-dinitrobenzoic acid in acetone; and the NRTL and Wilson models, the mutual solubility for the ternary m-nitrobenzoic acid + 3,5-dinitrobenzoic acid + acetone system. The value of root-mean-square deviation (RMSD) was 8.53 × 10 −4 for the binary system of 3,5-dinitrobenzoic acid + acetone; and the largest value of RMSD was 81.08 × 10 −4 for the ternary system.

  4. A highly sensitive kinetic spectrophotometric method for the determination of ascorbic Acid in pharmaceutical samples.

    Science.gov (United States)

    Shishehbore, Masoud Reza; Aghamiri, Zahra

    2014-01-01

    In this study, a new reaction system for quantitative determination of ascorbic acid was introduced. The developed method is based on inhibitory effect of ascorbic acid on the Orange G-bromate system. The change in absorbance was followed spectrophotometrically at 478 nm. The dependence of sensitivity on the reaction variables including reagents concentration, temperature and time was investigated. Under optimum experimental conditions, calibration curve was linear over the range 0.7 - 33.5 μg mL(-1) of ascorbic acid including two linear segments and the relative standard deviations (n = 6) for 5.0 and 20.0 μg mL(-1) of ascorbic acid were 1.08 and 1.02%, respectively. The limit of detection was 0.21 μg mL(-) (1) of ascorbic acid. The effect of diverse species was also investigated. The developed method was successfully applied for the determination of ascorbic acid in pharmaceutical samples. The results were in a good agreement with those of reference method.

  5. The determination of acid-base properties of polymer surfaces by XPS: Present status and future prospects

    International Nuclear Information System (INIS)

    Chehimi, M.M.; Delamar, M.; Shahidzadeh-Ahmadi, N.; Arefi-Khonsari, F.; Amouroux, J.; Watts, J.F.

    1996-01-01

    The use of the molecular probe technique in conjunction with X-ray photoelectron spectroscopy (XPS) for the assessment of acid-base properties of polymer surfaces is reviewed. The method is based on the determination of the concentration and chemical shifts of Lewis acids (bases) sorbed in polymers of basic (acidic) character. In the case of chloroform (Lewis acid) sorbed in polymers of Lewis basic character, C12p binding energy is linearly correlated with ΔH AB , the heat of acid-base complex formation chloroform-polymer. This relationship has been used to determine the acid-base properties of poly(phenylene oxide), a homopolymer, and ammonia plasma-treated polypropylene. This work shows that XPS can now indeed be used to quantitatively assess the acid-base properties of modified polymer surfaces and perhaps be extended to map acid-base properties of polymer surfaces at the micron or submicron scale. copyright 1996 American Institute of Physics

  6. Simultaneous Determination of Salicylic Acid, Jasmonic Acid, Methyl Salicylate, and Methyl Jasmonate from Ulmus pumila Leaves by GC-MS

    OpenAIRE

    Huang, Zhi-hong; Wang, Zhi-li; Shi, Bao-lin; Wei, Dong; Chen, Jian-xin; Wang, Su-li; Gao, Bao-jia

    2015-01-01

    Salicylic acid, jasmonic acid, methyl salicylate, and methyl jasmonate are important phytohormones and defensive signaling compounds, so it is of great importance to determine their levels rapidly and accurately. The study uses Ulmus pumila leaves infected by Tetraneura akinire Sasaki at different stages as materials; after extraction with 80% methanol and ethyl acetate and purification with primary secondary amine (PSA) and graphitized carbon blacks (GCB), the contents of signal compounds sa...

  7. Determination of vanadium in Syrian commercial and raffinate phosphoric acid

    International Nuclear Information System (INIS)

    Al-Merey, R.

    2002-04-01

    This study presents two methods for vanadium determination in Syrian commercial phosphoric acid. The vanadium (V) in the oxidized commercial phosphoric acid by ammonium persulfate solution is extracted from 5-M hydrochloride acid medium using N-benzoyl-N-phenyl hydroxyl amine (BPHA) in chloroform as an extracting solution. The first method, the extract vanadium as VOL 2 Cl is changed to V 2 O 3 L 4 complex by the addition of benzimidazole in 1-butanol to the violet organic layer. The absorbance is then measured at 440 nm (the molar absorptivity was found to be 3865 M -1 cm -1 ), where Beer law is applicable up to 36-μg ml -1 . the accuracy, precision and detection limit were found to be 3.7%, 77 ppb and 37 ppb, respectively. the second method, the organic layer is heated to evaporate chloroform, the residue is digested using 20% ammonium persulfate and 2-M sulfuric acid solutions. The vanadium concentration is measured spectrophotometrically by oxidizing gallic acid with persulfate (S 2 O 8 2- ) anion in phosphoric acid medium, where the vanadium (V) acts as a catalyst in the oxidation reaction. This method has a high sensitivity (∼10 -12 ) with accuracy and precision 5% and 0.621 ppb, respectively. Also Beer law at λ m ax=415 nm (ε=∼2 x 10 6 M -1 ) is applicable in the range 2.58-33.3 ppb. (author)

  8. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-12-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  9. Determination of Monochloroacetic Acid in Swimming Pool Water by Ion Chromatography-Conductivity Detection

    Directory of Open Access Journals (Sweden)

    Maria Pythias B. Espino

    2013-02-01

    Full Text Available In this study, an analytical method involving ion chromatography with conductivity detection was developed and optimized for the determination of monochloroacetic acid in swimming pool water. The ion chromatographic method has a detection limit of 0.02 mg L-1 and linear range of 0.05 to 1.0 mg L-1 with correlation coeff icient of 0.9992. The method is reproducible with percent RSD of 0.052% (n=10. The recovery of monochloroacetic acid spiked in different water types (bottled, tap and swimming pool water ranged from 28 to 122%. In dilute solutions, chloride and bromide were simultaneously analyzed along with monochloroacetic acid using the optimized method. Chloride and bromide have detection limits of 0.01 to 0.05 mg L-1, respectively. The usefulness of the ion chromatographic method was demonstrated in the analysis of monochloroacetic acid in swimming pool water samples. In such highly-chlorinated samples, an Ag/H cartridge was used prior to the ion chromatographic determination so as to minimize the signal due to chloride ion. Monochloroacetic acid was detected in concentrations between 0.020 and 0.093 mg L-1 in three of the six swimming pool water samples studied. The presence of monochloroacetic acid in the swimming pool water samples suggests the possible occurrence of other disinfection by-products in these waters.

  10. Photometric method for determination of acidity constants through integral spectra analysis.

    Science.gov (United States)

    Zevatskiy, Yuriy Eduardovich; Ruzanov, Daniil Olegovich; Samoylov, Denis Vladimirovich

    2015-04-15

    An express method for determination of acidity constants of organic acids, based on the analysis of the integral transmittance vs. pH dependence is developed. The integral value is registered as a photocurrent of photometric device simultaneously with potentiometric titration. The proposed method allows to obtain pKa using only simple and low-cost instrumentation. The optical part of the experimental setup has been optimized through the exclusion of the monochromator device. Thus it only takes 10-15 min to obtain one pKa value with the absolute error of less than 0.15 pH units. Application limitations and reliability of the method have been tested for a series of organic acids of various nature. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Determining Total Phenolics, Anthocyanin Content and Ascorbic Acid Content in Some Plum Genotypes Grown in Ardahan Ecological Conditions

    Directory of Open Access Journals (Sweden)

    Z. T. ABACI

    2014-06-01

    Full Text Available In this study, total phenol content, total anthocyanin content, brix, pH, titrable acidity and total ascorbic acid content in the five plum genotypes cultivated in Ardahan City are determined and sustenance of the plums are revealed. Total phenol content was determined with folin-ciocalteu’s method, total anthocyanin content was determined with pH differential method and total ascorbic acid was determined with 2,6-dichlorophenolindophenol method.It is detected that the genotype with the highest brix content (%13.9 and lowest acidity (%0.98 is cancur, the genotype with the lowest brix content (%11 and highest acidity (%2.06 is wild plum, the genotype with the highest content of total anthocyanin, total phenolic substance and ascorbic acid is the wild plum and the genotype with the least content of these is the water plum. As a result of the study, it is revealed that the plum fruit has high levels of phenolic substance, anthocyanin and ascorbic acid content, so it has a high sustenance.

  12. The use of ion chromatography for the determination of impurities in crude phosphoric acid

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Atalla, L.T.; Abrao, A.

    1988-07-01

    The determination of fluoride, nitrate, sulphate and phosphate ions in crude phosphoric acid by means of ion chromatography is described. A previous separation of interferent cations was made by using a cationic resin or EDTA complexation. The last alternative allowed more reproductible results. The technique described is very quick and is being applied for the simultaneous determination of impurities in phosphoric acid and its own phosphospate concentration. The method is quick and has good reprodutibility. (author) [pt

  13. A new optical sensor for spectrophotometric determination of uranium (VI) and thorium (IV) in acidic medium

    Energy Technology Data Exchange (ETDEWEB)

    Elhefnawy, O.A. [Nuclear and Radiological Regulatory Authority (NRRA), Cairo (Egypt). Nuclear Safeguards and Physical Protection Dept.

    2017-07-01

    A spectrophotometric method was developed for U(VI) and Th(IV) determination in acidic medium by using proposed optical sensor. This sensor is base on the complexation reaction of the ionophore midodrine hydrochloride (L) with U(VI)/Th(IV) in plasticized (o-NPOE) high molecular weight (PVC). Several parameters such as effect of acidic medium, response time and sensor compositions were studied. The determination of the complexes stoichiometry was also studied using Job's method. The complexes stoichiometry were measured at the absorbance spectra 302 nm and the results were found to be 1:1 for both complexes U(VI)-L and Th(IV)-L. The complexation reaction was extremely rapid at room temperature; it takes 5, 10 min to complete the complexation reaction in U(VI) and Th(IV), respectively. Under the optimum conditions the calibration curves of U(VI)/Th(IV) determination, have good linearity at different acidic medium nitric, sulfuric, and phosphoric acids with low detection and quantification limits. The accuracy and precision studies proved that the proposed optical sensor is valid and qualified for U(VI)/Th(IV) spectrophotometric determination in different acidic medium. The selectivity of the proposed optical sensor was studied. The proposed optical sensor was applied successfully for U(VI)/Th(IV) determination in research and development (R and D) nuclear waste samples with satisfactory results. A comparative study of the proposed optical sensor with other previous spectrophotometric sensors for U(VI)/Th(IV) determination, proved the high efficiency of the proposed optical sensor, that it presents wide linear range and low detection limit. The proposed optical sensor could be applied for a quantitative determination of U(VI)/Th(IV) in acidic waste samples.

  14. A new optical sensor for spectrophotometric determination of uranium (VI) and thorium (IV) in acidic medium

    International Nuclear Information System (INIS)

    Elhefnawy, O.A.

    2017-01-01

    A spectrophotometric method was developed for U(VI) and Th(IV) determination in acidic medium by using proposed optical sensor. This sensor is base on the complexation reaction of the ionophore midodrine hydrochloride (L) with U(VI)/Th(IV) in plasticized (o-NPOE) high molecular weight (PVC). Several parameters such as effect of acidic medium, response time and sensor compositions were studied. The determination of the complexes stoichiometry was also studied using Job's method. The complexes stoichiometry were measured at the absorbance spectra 302 nm and the results were found to be 1:1 for both complexes U(VI)-L and Th(IV)-L. The complexation reaction was extremely rapid at room temperature; it takes 5, 10 min to complete the complexation reaction in U(VI) and Th(IV), respectively. Under the optimum conditions the calibration curves of U(VI)/Th(IV) determination, have good linearity at different acidic medium nitric, sulfuric, and phosphoric acids with low detection and quantification limits. The accuracy and precision studies proved that the proposed optical sensor is valid and qualified for U(VI)/Th(IV) spectrophotometric determination in different acidic medium. The selectivity of the proposed optical sensor was studied. The proposed optical sensor was applied successfully for U(VI)/Th(IV) determination in research and development (R and D) nuclear waste samples with satisfactory results. A comparative study of the proposed optical sensor with other previous spectrophotometric sensors for U(VI)/Th(IV) determination, proved the high efficiency of the proposed optical sensor, that it presents wide linear range and low detection limit. The proposed optical sensor could be applied for a quantitative determination of U(VI)/Th(IV) in acidic waste samples.

  15. Some Non-Destructive Testing Methods Applicable to Sintered Materials; Quelques Methodes d'Essais Non Destructifs Applicables aux Materiaux Frittes; Nekotorye metody nedestruktivnykh ispytanii, primenimye k spechennym materialam; Algunos Metodos de Ensayo No Destructivo Aplicables a los Materiales Sinterizados

    Energy Technology Data Exchange (ETDEWEB)

    Labusca, Elena; Mirion, I.; Andreescu, N.; Alecu, M.; Biscoveanu, I. [Institut de Physique Atomique, Bucarest (Romania)

    1965-10-15

    solides frittes, a l'aide de la metallographie et de la microscopie electronique. Ces methodes mettent en evidence l'homogeneite de la structure, les dimensions et l'orientation des grains, la presence de defauts divers (inclusions, pores) et revolution meme du processus de frittage, y compris la formation des cristaux, la croissance granulaire, etc. Dans quelques cas, on peut combiner l'examen microscopique a des essais de microdurete. Cet examen de la structure microcristalline represente l'une des methodes principales de controle qualitatif des materiaux frittes, et ne peut etre remplace par aucun autre moyen d'investigation. 2. Controle du degre de consolidation, qui determine essentiellement la qualite des materiaux frittes. Ce controle est effectue par la mesure de quelques proprietes, telles que la conductibilite electrique et thermique, en correlation avec la densite, etant donne que la conductibilite des materiaux frittes est directement porportionnelle au degre de frittage. On a essaye aussi une methode adequate de controle de la porosite; on a obtenu des donnees experimentales interessantes, surtout au point de vue de la porosite libre, laquelle est susceptible aux inclusions gazeuses. Le memoire contient des donnees experimentales concernant l'application de ces methodes de controle a quelques materiaux frittes interessants pour la technologie nucleaire. (author) [Spanish] Teniendo en cuenta la estructura granular especifica de los materiales sinterizados, elaborados a partir de polvos, cuyo proceso de consolidacion se desarrolla en funcion del tratamiento de sinterizacion, los autores han estudiado algunos metodos para verificar el grado de sinterizacion y controlar ciertas propiedades. Entre los metodos no destructivos utilizados, se mencionan en la presente memoria: 1. Examen de la estructura cristalina de los solidos sinterizados por metalografia y microscopfa electronica. Estos metodos ponen de manifiesto el giado de homogeneidad estructural, la dimension

  16. Benzohydroxamic acid as a reductometric titrant:determination of manganese, chromium and vanadium in steels

    International Nuclear Information System (INIS)

    Ahmed, M.K.; Subbarao, C.

    1981-01-01

    A method has been developed for the rapid determination of manganese and chromium by direct stepwise reductometric titration with benzohydroxamic acid, and of vanadium by titration with ascorbic acid (with benzohydroxamic acid as indicator) in the same aliquot. The method is free from the interference of common alloying elements present in steels. Some BCS steel samples have been analysed with good precision and accuracy. (author)

  17. Seed prepare for oil content determination by NMR method in six cotton varieties; Preparo de sementes para determinacao do teor de oleo pelo metodo de RMN em seis variedades de algodoeiro

    Energy Technology Data Exchange (ETDEWEB)

    Gondim-Tomaz, Rose Marry Araujo; Erismann, Norma de Magalhaes; Sabino, Nelson Paulieri; Kondo, Julio Isao; Cia, Edivaldo; Azzini, Anisio [Instituto Agronomico de Campinas, SP (Brazil). Centro de Algodao e Fibrosas Diversas]. E-mail: gondim@cec.iac.br; Soave, Daise [Instituto Agronomico de Campinas, SP (Brazil). Centro de Genetica, Biologia Molecular e Fitoquimica

    1998-07-01

    Three comparative methods (chemical seed-delinting with sulphuric acid solution, flaming and seed with linter) to prepare cotton seeds for oil determination by the Nuclear Magnetic Resonance (NMR) technique were considered. The chemical treatment with sulphuric acid was the best as long the linter interference was eliminated. The seed oil contents were determined by the NMR method in six cotton varieties from the national variety test. The IAPAR (Instituto Agronomico do Parana) 71 PR3 and IAC (Instituto Agronomico de Campinas) 20 varieties presented the highest oil content followed by the CNPA 7H, CS 50, IAC 22 and CNPA Precoce 2. (author)

  18. Chemiluminescence of graphene quantum dots and its application to the determination of uric acid

    International Nuclear Information System (INIS)

    Amjadi, Mohammad; Manzoori, Jamshid L.; Hallaj, Tooba

    2014-01-01

    We report on the chemiluminescence (CL) of graphene quantum dots (GQDs) induced by direct chemical oxidation. GQDs were prepared by a simple carbonization method and characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and Raman spectroscopy. It was found that Ce(IV) could oxidize GQDs to produce a relatively intense CL emission. The mechanism of CL generation was investigated based on the fluorescence and CL emission spectra. It was attributed to the radiative recombination of oxidant-injected holes and thermally excited electrons in the GQDs. In order to show the analytical application potential of GQDs-Ce(IV) CL system, it was applied to the determination of uric acid. Under the optimized conditions, the proposed CL system exhibited excellent analytical performance for determination of uric acid in the range of 1.0×10 −6 M–5.0×10 −4 M with a limit of detection of 5.0×10 −7 M. The method was applied to the determination of uric acid in human plasma and urine samples, with satisfactory results. - Highlights: • Chemiluminescence of graphene quantum dots by direct oxidation was studied. • Intense CL is produced by reaction of graphene quantum dots with Ce(IV). • The new CL system was applied to determination of uric acid in plasma and urine

  19. Chemiluminescence of graphene quantum dots and its application to the determination of uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Amjadi, Mohammad, E-mail: amjadi@tabrizu.ac.ir; Manzoori, Jamshid L.; Hallaj, Tooba

    2014-09-15

    We report on the chemiluminescence (CL) of graphene quantum dots (GQDs) induced by direct chemical oxidation. GQDs were prepared by a simple carbonization method and characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and Raman spectroscopy. It was found that Ce(IV) could oxidize GQDs to produce a relatively intense CL emission. The mechanism of CL generation was investigated based on the fluorescence and CL emission spectra. It was attributed to the radiative recombination of oxidant-injected holes and thermally excited electrons in the GQDs. In order to show the analytical application potential of GQDs-Ce(IV) CL system, it was applied to the determination of uric acid. Under the optimized conditions, the proposed CL system exhibited excellent analytical performance for determination of uric acid in the range of 1.0×10{sup −6} M–5.0×10{sup −4} M with a limit of detection of 5.0×10{sup −7} M. The method was applied to the determination of uric acid in human plasma and urine samples, with satisfactory results. - Highlights: • Chemiluminescence of graphene quantum dots by direct oxidation was studied. • Intense CL is produced by reaction of graphene quantum dots with Ce(IV). • The new CL system was applied to determination of uric acid in plasma and urine.

  20. Developing a rapid method for the determination of uranium in pure phosphoric acid and D2 EHPA

    International Nuclear Information System (INIS)

    Koudsi, Y.; Stas, J.; Al-Merey, R.; shaddoud, G.

    1996-02-01

    Arsenazo (III) used in titrate uranium spectrophotometrically in phosphoric acid after its extraction into organic phase. In this work we used arsenazo(III) to complex uranyl ion in pure phosphoric acid and in the aqueous phase. The spectrum of the complex shows that λ max is at 650 nm. The linearity of the method is corelated with acid molarity, it is (1 -4, 10 - 30, 10 - 40) ppm uranium for (0.2, 1, 2) M of phosphoric acid respectively. Uranium in D 2 EHPA stripped by phosphoric acid and then determined by this method. Also it has been applied to determine uranium in pure perchloric acid. The method is direct, rapid, very cheap and relatively accurate. (author)

  1. Determination of free acid in highly concentrated organic and aqueous solutions of plutonium (IV) and uranium (VI) nitrate

    International Nuclear Information System (INIS)

    Wagner, J.F.; Lacour, J.L.

    1989-01-01

    Free acidity is an important parameter in the nuclear reprocessing control. The accuracy on the determination of free acidity is not really required in the nuclear reprocessing control itself but is necessary for certain types of analysis such as spectrophotometry (Pu (VI), Am (III),...), density determinations. A new titripotentiometric method for free acidity determination in concentrated U(VI) and Pu(IV) solutions is presented. This method is based on the complexing properties of dipicolinic acid (pyridine 2.6 dicarboxylic acid) and medium effect with H 2 O/DMSO mixture. This method can be used either in organic or aqueous phases with ratio /H + I/ metal ≥ 5.10 -2 and a relative standard deviation of 1%

  2. Determination of total triterpenoid acids in different part and extract of Ganoderma lucidum

    Directory of Open Access Journals (Sweden)

    FENG Huiqin

    2013-04-01

    Full Text Available Aim To develop a method for determination of total triterpenoid acids in different part and extracts of Ganoderma lucidum. Method The samples of Ganoderma lucidum were extracted with ethanol and successively extracted with CHCl3 and 5% NaHCO3,the NaHCO3 layer was acidified to pH 3 with 2 mol/L HCl,the resulting precipitates were dissolved in CHCl3 and evaporated in vacuo then weighed. The total triterpenoid acids were obtained. Result The total triterpenoid acids of Ganoderma lucidum fruitbody,spore and mycelium were (8.58±0.25 mg/g,(3.48±0.03 mg/g and (1.75 ±0.09 mg/g respectively. The total triterpenoid acids of pileus and stipe were (12.62±0.22 mg/g and (7.66±0.08 mg/g. The range of total triterpenoid acid content among 10 batches of Ganoderma lucidum fruitbody purchased from the market was between 4.34 to 16.39 mg/g. The highest content fro/8/8/88/ m Ganoderma lucidum fruiting body with alcohol - water extracting was (208.70±5.54 mg/g and the lowest content with alkaline solution extracting was (123.07±4.99 mg/g. The composition of total triterpenoid acid from fruitbody,spores and extract of fruitbody analyzed by HPLC were almost the same. This method is reliable for determination of total triterpenoid acid in the fruiting body and its extracts,spore and mycelium from Ganoderma lucidum,which provides an indicator for the quality of Ganoderma lucidum product.

  3. Determination of organophosphorus acids by thermo-spray liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Wils, E.R.J.; Hulst, A.G.

    1988-01-01

    The determination of thirteen organophosphorus acids, hydrolysis products of nerve agents and pesticides, by a combination of ion-pair liquid chromatography on a reversed-phase C18 column and thermospray mass spectrometry was investigated. Ammonium acetate and three tetraalkylammonium salts with

  4. Determination of chlorogenic acids and caffeine in homemade brewed coffee prepared under various conditions.

    Science.gov (United States)

    Jeon, Jong-Sup; Kim, Han-Taek; Jeong, Il-Hyung; Hong, Se-Ra; Oh, Moon-Seog; Park, Kwang-Hee; Shim, Jae-Han; Abd El-Aty, A M

    2017-10-01

    Coffee, a complex mixture of more than 800 volatile compounds, is one of the most valuable commodity in the world, whereas caffeine and chlorogenic acids (CGAs) are the most common compounds. CGAs are mainly composed of caffeoylquinic acids (CQAs), dicaffeoylquinic acids (diCQAs), and feruloylquinic acids (FQAs). The major CGAs in coffee are neochlorogenic acid (3-CQA), cryptochlorogenic acid (4-CQA), and chlorogenic acid (5-CQA). Many studies have shown that it is possible to separate the isomers of FQAs by high-performance liquid chromatography (HPLC). However, some authors have shown that it is not possible to separate 4-feruloylquinic acid (4-FQA) and 5-feruloylquinic acid (5-FQA) by HPLC. Therefore, the present study was designated to investigate the chromatographic problems in the determination of CGAs (seven isomers) and caffeine using HPLC-DAD. The values of determination coefficient (R 2 ) calculated from external-standard calibration curves were >0.998. The recovery rates conducted at 3 spiking levels ranged from 99.4% to 106.5% for the CGAs and from 98.8% to 107.1% for the caffeine. The precision values (expressed as relative standard deviations (RSDs)) were coffee bean, coffee-ground size, and numbers of boiling-water pours, on the concentration of CGAs and caffeine in homemade brewed coffee, using nine green coffee bean samples of different origins. It was reported that medium-roasted, fine-ground coffees brewed using three pours of boiling water were the healthiest coffee with fluent CGAs. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Process monitored spectrophotometric titration coupled with chemometrics for simultaneous determination of mixtures of weak acids.

    Science.gov (United States)

    Liao, Lifu; Yang, Jing; Yuan, Jintao

    2007-05-15

    A new spectrophotometric titration method coupled with chemometrics for the simultaneous determination of mixtures of weak acids has been developed. In this method, the titrant is a mixture of sodium hydroxide and an acid-base indicator, and the indicator is used to monitor the titration process. In a process of titration, both the added volume of titrant and the solution acidity at each titration point can be obtained simultaneously from an absorption spectrum by least square algorithm, and then the concentration of each component in the mixture can be obtained from the titration curves by principal component regression. The method only needs the information of absorbance spectra to obtain the analytical results, and is free of volumetric measurements. The analyses are independent of titration end point and do not need the accurate values of dissociation constants of the indicator and the acids. The method has been applied to the simultaneous determination of the mixtures of benzoic acid and salicylic acid, and the mixtures of phenol, o-chlorophenol and p-chlorophenol with satisfactory results.

  6. DETERMINATION OF Cu, Fe, Mn, Zn AND FREE FATTY ACIDS IN PEQUI OIL

    Directory of Open Access Journals (Sweden)

    Aparecida M. S. Mimura

    2016-06-01

    Full Text Available Pequi (Caryocar brasiliense Camb., a typical fruit of the Brazilian Cerrado, is an important source of micronutrients and fatty acids. In this work, a new approach for the acid digestion (using H2SO4, HNO3 and H2O2 of pequi oil samples and the determination of Cu, Fe, Zn and Mn by flame atomic absorption spectrometry (F AAS was employed. Capillary zone electrophoresis (CZE was used for free fatty acid (FFA determination after simple and fast extraction with heated ethanol. Good results regarding precision (RSD < 10%, in most cases, sensitivity and adequate LOD and LOQ values were obtained. The accuracy was evaluated using spike tests and the recoveries were from 97 to 107%. The analytes were investigated in four different pequi oil samples. Fe was the trace element with the highest concentration (from 1.99 to 10.3 mg/100 g, followed by Zn, Mn and Cu (1.15 to 3.19, 0.42 to 0.91 and 0.31 to 0.56 mg/100 g, respectively. The main FFA found were oleic acid and palmitic acid (1.61 to 10.7 and 0.82 to 2.69 g/100 g, respectively, while linoleic acid (0.50 g/100 g was detected in only one sample. The pequi oil chemical composition showed good characteristics to be used as a food additive, in cosmetic formulations and for traditional medicine.

  7. Sensitive determination of buformin using poly-aminobenzoic acid modified glassy carbon electrode

    Directory of Open Access Journals (Sweden)

    Gui-Ying Jin

    2012-12-01

    Full Text Available Glassy carbon electrode, which is used to electrochemically determine the content of buformin, is modified with an electropolymerized film of p-aminobenzoic acid in pH 7.0 acetate buffer solution (ABS. The polymer showed an excellent electrocatalytic activity for the reduction of buformin. In pH 7.0 ABS, the cathodic peak current increased linearly over three concentration intervals of buformin, and the detection limit (S/N=3 was 2.0×10−9 g/mL. The method was successfully applied to directly determine buformin in tablets with standard addition recoveries of 95.8–102.5%. The proposed method is simple, cheap and highly efficient. Keywords: Chemically modified electrode, Aminobenzoic acid, Buformin

  8. Towards combinatorial spectroscopy: the case of minor milk fatty acids determination.

    Science.gov (United States)

    Stefanov, I; Baeten, V; De Baets, B; Fievez, V

    2013-08-15

    Chemometrical models for determination of milk fatty acids (FA) are typically developed using spectral data from a single spectroscopy technique, e.g., mid-infrared spectroscopy in milk control. Such models perform poorly in determining minor components and are highly dependent on the spectral data source and on the type of matrix. In milk fat, the unsuccessful determination of minor (fatty acids lower than 1.0 g/100g in total fat) FA is often the result of: (1) the molecular structure similarity between the minor and the major FA within the milk fat matrix (thus the chemical signature specific to individual fatty acids has restricted specificity), and (2) the low signal intensity (detection limit) for specific vibrational modes. To overcome these limitations, data from different types of spectroscopy techniques, which brings additional chemical information in relation to the variation of the FA, could be included in the regression models to improve quantification. Here, Fourier transform (FT) Raman spectra were concatenated with attenuated total reflectance FT infrared (ATR/FTIR) spectra. The new combinatorial models showed up to 25% decrease in the root mean squared error of cross-validation (RMSECV) values, accompanied with a higher Rcv(2) for most individual FA or sums of FA groups, as compared to regression models based on Raman only or ATR/FTIR only spectra. In addition, improved models included less PLS components indicating an increased robustness. Interpretation of the most contributing regression coefficients indicated the value of newly combined spectral regions as carriers of specific chemical information. Although requiring additional spectroscopy instrumentation and prolonged acquisition time, this new combinatorial approach can be automated and is sufficient for semi-routine determination of the milk FA profile. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Quantitative determination of conjugated linoleic acid and polyunsaturated fatty acids in milk with C17:0 as internal marker – Evaluation of different methylation procedures

    Directory of Open Access Journals (Sweden)

    S. Lashkari

    2017-12-01

    Full Text Available Fatty acids are commonly analysed by gas chromatography as their corresponding fatty acid (FA methyl esters (FAME. For quantitative determination of individual FA an internal standard like C17:0 is necessary. Conjugated FA and polyunsaturated fatty acid (PUFA represents a challenge in the methylation steps, as they are sensitive to pH changes and oxidation. The present study was carried out to determine the efficiency of different methylation procedures on quantitative determination of conjugated linoleic acid (CLA, PUFA and response of internal standard. The highest response of internal standard was observed for boron trifluoride (BF3/methanol and methanolic HCl followed by NaOCH3, while cis-9, trans-11 CLA, total CLA and PUFA was higher with methanolic HCl followed by NaOCH3 compared with the BF3 method. These data can be useful for quantitating of milk FA. Keywords: Methylation procedures, Milk fatty acid, Conjugated linoleic acid

  10. Polarographic determination of stability constants of Eu(III) complexes with acrylic and crotonic acid

    Energy Technology Data Exchange (ETDEWEB)

    Rao, A L.J.; Singh, Makhan [Punjabi Univ., Patiala (India). Dept. of Chemistry

    1979-07-01

    Compositions and formation constants of Eu(III) complexes with acrylic acid and crotonic acid have been studied polarographically. The reductions are reversible and diffusion-controlled. The plot of Esub(1/2) versus--log Csub(x) is linear in the case of Eu(III)-acrylic acid system. The change in number of ligands bound to europium during reduction was found to be approximately 1 and ratio of dissociation constants of Eu(III) and Eu(II) was found to be 40.76X10sup(-2). In the case of Eu(III)-crotonic acid system, composition and formation constants have been calculated by the method of Deford and Hume. Crotonic acid forms two complex species with europium (..beta../sub 1/,60; ..beta../sub 2/, 4.2x10sup(+2)). The percentage distribution of various complex species as a function of ligand concentration has been calculated in the case of Eu(III)-crotonic acid system. A polarographic method for the determination of micro amounts of Eu(III) in the presence of diverse ions has been developed. Under optimum conditions Eu(III) in the concentration range 4x19sup(-4)-2x10sup(-2)M can be successfully determined in various mixtures.

  11. Investigation of the use of thermometric titrimetry for the determination of acidic substances in wine.

    Science.gov (United States)

    Godinho, O E; Coelho, J A; Chagas, A P; Aleixo, L M

    1984-03-01

    The use of thermometric titrimetry in the determination of acidic substances in red wine is described. The titration curve obtained in the thermometric titration of red wine with strong base presents two inflections. The stoichiometry corresponding to the first inflection presents good agreement with the so-called "total acidity" of wine, and is proposed for its determination. The second inflection is related to the content of phenolic substances in red wine.

  12. Determination of ascorbic acid in pharmaceutical preparation and fruit juice using modified carbon paste electrode

    Directory of Open Access Journals (Sweden)

    Simona Žabčíková

    2016-06-01

    Full Text Available Acrobic acid is key substance in the human metabolism and the rapid and accurate determination in food is of a great interest. Ascorbic acid is an electroactive compound, however poorly responded on the bare carbon paste electrodes. In this paper, brilliant cresyl blue and multi-walled carbon nanotubes were used for the modification of carbon paste electrode. Brilliant cresyl blue acts as a mediator improving the transition of electrons, whereas multiwalled carbon nanotubes increased the surface of the electrode. Both brilliant cresyl blue and multiwalled carbon nanotubes were added directly to the composite material. The electrochemical behavior of modified electode was determined in electrolyte at various pH, and the effect of the scan rate was also performed. It was shown that the electrochemical process on the surface of the modified carbon paste electrode was diffusion-controlled. The resulted modified carbon paste electrode showed a good electrocatalytic activity towards the oxidation of ascorbic acid at a reduced overpotential of +100 mV descreasing the risk of interferences. A linear response of the ascorbic acid oxidation current measured by the amperometry in the range of 0.1 - 350 µmol.L-1 was obtained applying the sensor for the standard solution. The limit of detection and limit of quantification was found to be 0.05 and 0.15 µmol.L-1, respectively. The novel method was applied for the determination of ascorbic acid in pharmaceutical vitamin preparation and fruit juice, and the results were in good agreement with the standard HPLC method. The presented modification of carbon paste electrode is suitable for the fast, sensitive and very accurate determination of ascorbic acid in fruit juices and pharmaceutical preparation.

  13. Determination of uranium by direct titration with dipicolinic acid

    International Nuclear Information System (INIS)

    Baumann, E.W.

    1984-01-01

    Direct titration of uranium with dipicolinic acid, in the presence of Arsenazo I, is a simple, precise, and accurate method for uranium determination. The method is particularly attractive because it can be totally automated. Detecting the end point (color change from blue to pink) depends on the concentration range. For the Micro Method (1 to 20 ppM U in the solution titrated), the gradual color change is monitored spectrophotometrically. For the Macro Method (20 to 300 ppM), the end point is determined either visually or spectrophotometrically. The spectrophotometric end point is computed by fitting the titration curve. The relative standard deviation is +-1 to 3% for the Micro Method and +-0.3% for the Macro Method

  14. Determination of acid dissociation constants of warfarin and hydroxywarfarins by capillary electrophoresis.

    Science.gov (United States)

    Nowak, Paweł; Olechowska, Paulina; Mitoraj, Mariusz; Woźniakiewicz, Michał; Kościelniak, Paweł

    2015-08-10

    In this work the acid dissociation constants--pKa of warfarin and its all important oxidative metabolites have been determined by capillary electrophoresis-based methods. It has resulted in a complete description of two acid-base dissociation equilibria, yet not investigated experimentally for phase I metabolites of warfarin. The capillary electrophoresis (CE) method based on the relation between effective electrophoretic mobilities and pH has proven to be a suitable tool for pKa determination, while the spectrophotometric (CE-DAD) and the internal standard methods (IS-CE), have appeared to be promising alternative approaches. The CE-DAD approach based on the change in absorbance spectra between the acidic and basic forms is a combination between capillary electrophoresis and spectrophotometric titration, and yields very consistent values of pKa1 with CE. The IS-CE, in turn, enables an estimation of pKa1 and pKa2 from only two analytical runs, however, less accurate than CE and CE-DAD. The Debye-Hückel model has been confirmed experimentally as a good predictor of pKa values at various ionic strengths. Therefore, it has been used in determination of thermodynamic pKa1 and pKa2, referring to the zero ionic strength. The results are important from the analytical, pharmacological, and theoretical points of view. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Determination of feedstuff amino acids composition by ion-exchange chromatography

    Directory of Open Access Journals (Sweden)

    A. A. Volnin

    2018-01-01

    Full Text Available Determination of animal feeds amino acids composition is the very important part of agricultural sciences and livestock management. This is necessary for normalization and balanced of farm animal’s diets parameters. Advances in husbandry techniques are making in response to the needs for rearing high genetic merit livestock. The nutrition of livestock has a critical role in these developments and is an element which needs to be continually updated as new scientific information becomes available. This article is devoted to the use of ion-exchange chromatography with post-colum derivatization by ninhydrin in the study of the amino acid composition and evaluation of the biological value of livestock feedstuff components. The amino acid composition (except tryptophan of the livestock feed-stuff component is presented for threonine – 3.26 g/100g of protein, leucine – 6.43, isoleucine – 3.24, valine – 4.77, methionine – 2.18, lysine – 2.90, phenylalanine – 3.16, histidine – 2.03, tyrosine – 2.33, sum of asparagine and aspartate – 6.76, serine – 3.97, sum of glutamine and glutamic acid – 12.04, glycine – 6.00, alanine – 6.71, arginine – 6.93, proline – 3.08, sum of cystine and cysteine – 1.38. Biological value of feedstuff component compared with the "ideal" protein (FAO WHO is estimated, limiting amino acids were found. The amino acid score was calculated: for threonine – 81.5%, leucine – 91.9%, isoleucine – 81%, valine – 95.4%, lysine – 52.7%, phenylalanine and tyrosine sum – 91.5%, methionine and cysteine sum – 101.7%. Feedstuff component had a low level of essential amino acids in compare with "ideal" protein (FAO WHO. Feedstuff component can be used for livestock nutrition as a component of essential amino-acid balanced diet.

  16. Determination of water-soluble forms of oxalic and formic acids in soils by ion chromatography

    Science.gov (United States)

    Karicheva, E.; Guseva, N.; Kambalina, M.

    2016-03-01

    Carboxylic acids (CA) play an important role in the chemical composition origin of soils and migration of elements. The content of these acids and their salts is one of the important characteristics for agrochemical, ecological, ameliorative and hygienic assessment of soils. The aim of the article is to determine water-soluble forms of same carboxylic acids — (oxalic and formic acids) in soils by ion chromatography with gradient elution. For the separation and determination of water-soluble carboxylic acids we used reagent-free gradient elution ion-exchange chromatography ICS-2000 (Dionex, USA), the model solutions of oxalate and formate ions, and leachates from soils of the Kola Peninsula. The optimal gradient program was established for separation and detection of oxalate and formate ions in water solutions by ion chromatography. A stability indicating method was developed for the simultaneous determination of water-soluble organic acids in soils. The method has shown high detection limits such as 0.03 mg/L for oxalate ion and 0.02 mg/L for formate ion. High signal reproducibility was achieved in wide range of intensities which correspond to the following ion concentrations: from 0.04 mg/g to 10 mg/L (formate), from 0.1 mg/g to 25 mg/L (oxalate). The concentration of formate and oxalate ions in soil samples is from 0.04 to 0.9 mg/L and 0.45 to 17 mg/L respectively.

  17. Contactless, probeless and non-titrimetric determination of acid-base reactions using broadband acoustic resonance dissolution spectroscopy (BARDS).

    Science.gov (United States)

    Ahmed, M Rizwan; McSweeney, Sean; Krüse, Jacob; Vos, Bastiaan; Fitzpatrick, Dara

    2018-02-12

    pH determination is a routine measurement in scientific laboratories worldwide. Most major advances in pH measurement were made in the 19th and early 20th century. pH measurements are critical for the determination of acid base reactions. This study demonstrates how an acid-base reaction can be monitored without the use of a pH probe, indicator and titres of reagent. The stoichiometric reaction between carbonate and HCl acid yields specific quantities of CO 2 , which causes reproducible changes to the compressibility of the solvent. This in turn slows down the speed of sound in solution which is induced by a magnetic follower gently tapping the inner wall of the vessel. As a consequence the frequencies of the acoustic resonances in the vessel are reduced. This approach is called Broadband Acoustic Resonance Dissolution Spectroscopy (BARDS) which harnesses this phenomenon for many applications. The acid-carbonate experiments have also been validated using H 2 SO 4 acid and using both potassium and sodium counterions for the carbonate. This method can be used to interrogate strong acid-base reactions in a rapid and non-invasive manner using carbonate as the base. The data demonstrate the first example of a reactant also acting as an indicator. The applicability of the method to weak acids has yet to be determined. A novel conclusion from the study is that a person with a well-trained ear is capable of determining the concentration and pH of a strong acid just by listening. This brings pH measurement into the realm of human perception.

  18. Separation and determination of the enantiomers of lactic acid and 2-hydroxyglutaric acid by chiral derivatization combined with GC-MS.

    Science.gov (United States)

    Ding, Xuemei; Lin, Shuhai; Weng, Hongbo; Liang, Jianying

    2018-03-30

    Lactic acid and 2-hydroxyglutaric acid are chiral metabolites that have two distinct d and l enantiomers with distinct biochemical properties. Perturbations of single enantiomeric form have been found to be closely related to certain diseases. The ability to differentiate the d and l enantiomers is therefore important for these disease studies. Herein, we describe a method for the separation and determination of lactic acid and 2-hydroxyglutaric acid enantiomers by chiral derivatization (with l-menthol and acetyl chloride) combined with gas chromatography and mass spectrometry. The two pairs of enantiomers mentioned above exhibited linear calibration curves with correlation coefficient (R 2 ) exceeding 0.99. The measured data were accurate in the acceptable recovery range of 88.17-102.30% with inter-day and intra-day precisions (relative standard deviations) in the 4.23-17.26% range. The limits of detection for d- lactic acid, l-lactic acid, d-2-hydroxyglutaric acid and l-2-hydroxyglutaric acid were 0.13, 0.11, 1.12 and 1.16 μM, respectively. This method was successfully applied to analyze mouse plasma. The d-lactic acid levels in type 2 diabetes mellitus mouse plasma were observed to be significantly higher (P lactic acid may serve as an indicator for type 2 diabetes mellitus. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  19. Determination of 5-caffeoylquinic acid (5-CQA as one of the major classes of chlorogenic acid in commercial tea and coffee samples

    Directory of Open Access Journals (Sweden)

    Grujić-Letić Nevena

    2015-01-01

    Full Text Available Background/Aim. Tea and coffee are one of the most widely consumed beverages in the world due to their beneficial health effects which are largely associated with their phenolic compounds composition, including chlorogenic acid. The main aim of this study was to determine 5-caffeoylquinic acid (5-CQA, as one of the major classes of chlorogenic acid, in various commercial tea and coffee samples present at the Serbian market. Methods. A high-performance liquid chromatography (HPLC method for determination of 5-CQA in plant extracts was applied to determine the content of this active compound in commercial tea and coffee samples. Mobile phase was aqueous 1.5% acetic acid - methanol (80:20, v/v with the flow rate of 0.8 mL/min. Run time was 15 min and column temperature 25°C. The detection was performed at 240 nm. Results. The HPLC method was modified and revalidated. The 5-CQA content varied depending on the type of tea (white, green, black tea and mate and the processing technology. Green tea had the highest 5-CQA content (16 mg/100 mL among the analyzed tea samples. The content of 5-CQA in coffee samples ranged 0-36.20 mg/g of coffee and 0-46.98 mg/100 mL of beverage, showing that the content varied depending on the type of coffee, coffee processing technology and the formulation. Conclusion. The modified and revalidated HPLC method showed a good accuracy, repeatability, selectivity and robustness. The highest amount of 5-CQA was determined in green tea in comparison to white, black and mate tea because the increased oxidation level decreases the amount of 5-CQA. The obtained results for commercial coffee samples indicated that the formulation was the most important factor determining the amount of 5-CQA. It can be concluded that plant material selection, processing conditions and formulation have great influence on the amount of chlorogenic acid (5-CQA in the final tea and coffee products. [Projekat Ministarstva nauke Republike Srbije, br. OI

  20. Determination of 5-caffeoylquinic acid (5-CQA) as one of the major classes of chlorogenic acid in commercial tea and coffee samples.

    Science.gov (United States)

    Nevena, Grujić-Letić; Branislava, Rakić; Emilia, Sefer; Dusica, Rakić; Ivan, Nedeljković; Nebojsa, Kladar; Biljana, Božin

    2015-11-01

    Tea and coffee are one of the most widely consumed beverages in the world due to their beneficial health effects which are largely associated with their phenolic compounds composition, including chlorogenic acid. The main aim of this study was to determine 5-caffeoylquinic acid (5-CQA), as one of the major classes of chlorogenic acid, in various commercial tea and coffee samples present at the Serbian market. A high-performance liquid chromatography (HPLC) method for determination of 5-CQA in plant extracts was applied to determine the content of this active compound in commercial tea and coffee samples. Mobile phase was aqueous 1.5% acetic acid-methanol (80:20, v/v) with the flow rate of 0.8 mL/min. Run time was 15 min and column temperature 25°C. The detection was performed at 240 nm. The HPLC method was modified and revalidated. The 5-CQA content varied depending on the type of tea (white, green, black tea and mate) and the processing technology. Green tea had the highest 5-CQA content (16 mg/100 mL) among the analyzed tea samples. The content of 5-CQA in coffee samples ranged 0-36.20 mg/g of coffee and 0-46.98 mg/100 mL of beverage, showing that the content varied depending on the type of coffee, coffee processing technology and the formulation. The modified and revalidated HPLC method showed a good accuracy, repeatability, selectivity and robustness. The highest amount of 5-CQA was determined in green tea in comparison to white, black and mate tea because the increased oxidation level decreases the amount of 5-CQA. The obtained results for commercial coffee samples indicated that the formulation was the most important factor determining the amount of 5-CQA. It can be concluded that plant material selection, processing conditions and formulation have great influence on the amount of chlorogenic acid (5-CQA) in the final tea and coffee products.

  1. Portable electrochemical sensor based on 4-aminobenzoic acid-functionalized herringbone carbon nanotubes for the determination of ascorbic acid and uric acid in human fluids.

    Science.gov (United States)

    Abellán-Llobregat, A; González-Gaitán, C; Vidal, L; Canals, A; Morallón, E

    2018-06-30

    A new portable electrochemical sensor based on 4-aminobenzoic acid-modified herringbone carbon nanotubes (hCNTs-4ABA/Au-IDA) has been developed for the simultaneous determination of ascorbic acid (AA) and uric acid (UA) in physiological fluids. AA and UA were quantified by chronoamperometry at 0.1 and 0.32 V, respectively, in phosphate buffer solution (PBS 0.25 M, pH 7.0). Significant results were obtained for the separate quantification of AA and UA, with a limit of detection (LOD) of 0.65 μM for both analytes, and sensitivities of (9.0 ± 0.4) A g -1 mM -1 and (8.8 ± 0.3) A g -1 mM -1 for AA and UA, respectively. Repeatability was studied at 50 μM for AA and UA, providing relative standard deviations (RSD) lower than 9%. Additions of glucose, dopamine and epinephrine did not interfere with the AA and UA determination. Furthermore, UA did not interfere with AA determination at 0.1 V, although AA additions increased the current recorded at 0.32 V. The method has been successfully applied to human urine, perspiration and serum samples, without significant matrix effects, which allows for the use of an external calibration and the analysis of all the matrices investigated. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. Comparison of commercially available radioimmunoassays for the determination of bile acids in serum

    Energy Technology Data Exchange (ETDEWEB)

    Wildgrube, H.J.; Schiller, W.; Winkler, M.; Weber, J.; Campana, H.; Mauritz, G.

    1982-05-01

    Three commercially available radioimmunoassays for the determination of bile acids in serum were evaluated with respect to specificity and precision. The SLCG-radioimmunoassay (Abbott) measures only sulphated glycolithocholic acid, the CG-radioimmunoassay (Abbott) measures chiefly cholic acid conjugates, and the CBA-radioimmunoassay (Becton-Dickinson) measures all conjugated bile acids, with an over-response to taurine metabolites. With respect to cross reactions, the performances of the CG-and the CBA-radioimmunoassays differed significantly from those stated by the manufacturers, the former showing a 32% response to taurocholic acid, the latter responding only 118% to taurochenodeoxycholic acid. At physiological concentrations of albumin + globulin, the recovery of defined cholanic acids was 85-101%. Good reproducibility was shown by the CG-radioimmunoassay in the range 0.5-10.9 ..mu..mol/l, by the CBA-radioimmunoassay in the range 1.0-25.0 ..mu..mol/l, and by the SLCG-radioimmunoassay in the range 0.5-3.0 ..mu..mol/l. There were no important differences in the inter- and intra-assay precision of the three methods.

  3. Sensitive spectrophotometric determination of ascorbic acid in drugs and foods using surface plasmon resonance band of silver nanoparticles

    Directory of Open Access Journals (Sweden)

    Kobra Zarei

    2015-12-01

    Full Text Available A simple and sensitive procedure was proposed for spectrophotometric determination of ascorbic acid. It was found that the reduction of Ag+ to silver nanoparticles (Ag-NPs by ascorbic acid in the presence of polyvinylpyrrolidone (PVP as a stabilizing agent produce very intense surface plasmon resonance peak of Ag-NPs. The plasmon absorbance of the Ag-NPs at λ = 440 nm allows the quantitative spectrophotometric detection of the ascorbic acid. The calibration curve was linear with concentration of ascorbic acid in the range of 0.5–60 μM. The detection limit was obtained as 0.08 μM. The influence of potential interfering substances on the determination of ascorbic acid was studied. The proposed method was successfully applied for the determination of ascorbic acid in some powdered drink mixtures, commercial orange juice, natural orange juice, vitamin C injection, effervescent tablet, and multivitamin tablet.

  4. Determination of aminoglycoside antibiotics using complex compounds of chromotropic acid bisazoderivatives with rare earth ions

    International Nuclear Information System (INIS)

    Alykov, N.M.

    1981-01-01

    Studies of complex formation of bisazo derivatives of chromotropic acid with rare earth ions and aminoglycoside antibiotics have made it possible to choose carboxyarsenazo, orthanyl R and carboxynitrazo as highly sensitive reagents for determining aminoglycoside antibiotics. Conditions have been found for the formation of precipitates of different-ligand complexes containing rare earth ions, bisazo derivatives of chromotropic acid and aminogylcoside antibiotics. A procedure has been worked out of determining the antibiotics in biological samples with carboxyarsenazo [ru

  5. Search for a developed method for the determination of Fe2 and Fe3 in Syrian Phosphoric acid

    International Nuclear Information System (INIS)

    Elian, Nuzhat; Kalak, Issam

    1988-08-01

    Phosphoric acid is the most important precursor for uranium production in Syria. Uranium extraction from phosphoric acid depends on the chemical composition of the acid, and most important is the relation between the proportions of iron I I/iron I II, and uranium I V/uranium V I, this proportion plays a very important role in different steps of the extraction. For this purposes two methods for determination of Iron I I and Iron I II in Syrian wet phosphoric acid spectrophotometrically were studied. The first one used 1.10 phenanthroline as complex agent. Iron I I formed red complex with 1.10 phenonstholine in the range of pH between 4 and 6, for determination of total iron. Iron I II was reduced to Iron I I with hydroxylamine hydrochloride. The second method used sulfosalycilic acid, Iron I II formed a yellow complex with sulfosalycilic acid. Total iron was determined in ammonium medium, but Iron I II was determined in pH=1.5. The sensibility of the tow methods and stability of their complex have been studied in normal laboratory conditions. 45 refs., 4 figs. (author)

  6. Determination of dissociation constants or propionic acid and lactic acid (2-hydroxypropionic acid) by potentiometry and conductometry

    International Nuclear Information System (INIS)

    Saeeduddin; Khanzada, A.W.K.

    2004-01-01

    Dissociation constants of propionic acid and 2-hydroxypropionic acid (lactic acid) have been studied at different temperatures between 25 to 50 deg. C interval. Propionic acid is analyzed by conductometry while 2-hydroxypropionic acid is analyzed by potentiometry. Both investigated compounds are symmetrical carboxylic acids having same length of carbon chain but are markedly different in ionic behavior. We were interested to see how the hydroxyl group (-OH) induction in propionic acid affects on pKa values of 2-hydroxypropionic acid. We observed that as temperature increases pKa values increase. The increase is observed for both the investigated compounds. PKa values of 2-hydroxypropionic acid are lower as compared to propionic acid because of electron withdrawing (-OH). (author)

  7. [Determination of geniposidic acid and chlorogenic acid in male flowers and related products of Eucommia ulmoides by reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Dong, Juane; Ma, Xihan

    2007-03-01

    A simple and rapid high performance liquid chromatographic method has been developed for the determination of geniposidic acid and chlorogenic acid in the male flowers and related products of Eucommia ulmoides. Two components were separated by a Shim-pack VP-ODS column (150 mm x4.6 mm, 5 [microm) with a mobile phase of methanol-water-acetic acid (24 :75: 1, v/v) at a flow rate of 1 mL/min, column temperature of 30 93 and detection wavelength of 240 nm. Under the chromatographic conditions mentioned above, the method performance, such as the number of theoretical plate, resolution, trailing etc have all reached required level. The linear ranges were 0. 025 - 0. 400 g/L for geniposidic acid and 0. 075 - 1. 200 g/L for chlorogenic acid, with the correlation coefficients of 0. 999 7 and 0. 999 9, respectively. The average recoveries were 100. 2% and 100. 5%, and the relative standard deviations (RSDs) were 1. 47% and 1. 49% respectively. The minimum detection limits were 0. 02 microg/L for geniposidic acid, and 0. 06 microg/L for chlorogenic acid. The method developed has demonstrated the characteristics of simple mobile phase composition, short retention, good resolution, high repeatability and precision. It is suitable for the determination of the two compounds in the male flowers of E. ulmoides and related products.

  8. Using Conductivity Measurements to Determine the Identities and Concentrations of Unknown Acids: An Inquiry Laboratory Experiment

    Science.gov (United States)

    Smith, K. Christopher; Garza, Ariana

    2015-01-01

    This paper describes a student designed experiment using titrations involving conductivity measurements to identify unknown acids as being either HCl or H[subscript 2]SO[subscript 4], and to determine the concentrations of the acids, thereby improving the utility of standard acid-base titrations. Using an inquiry context, students gain experience…

  9. Raman spectrometric determination of Pu(VI) and Pu(V) in nitric acid solutions

    International Nuclear Information System (INIS)

    Gantner, E.; Freudenberger, M.; Steinert, D.; Ache, H.J.

    1987-03-01

    The determination of Pu(VI) in nitric acid solutions by spontaneous Laser Raman Spectrometry (LRS) was investigated and a calibration curve was established using U(VI) as internal standard. In addition, the concentrations of Pu(VI) and Pu(V) as a function of time were measured by this method in Pu(VI) solutions of different acidity containing H 2 O 2 as the reducing agent. In solutions which are intensely coloured by the presence of Ru(NO) complexes Pu(VI) can also be determined by LRS using a Kr + laser as excitation source. In future experiments, the study of the Pu(IV)-interaction with Ru using LRS and spectrophotometry as analytical techniques is therefore intended. (orig.) [de

  10. Spectrophotometric determination of mefenamic acid excreted as free drug in urine of human beings

    International Nuclear Information System (INIS)

    Naseer, M.M.; Nawaz, R.; Shafique, M.; Rehman, R.

    2007-01-01

    Urinary excretion of free mefenamic acid was investigated in 16 healthy human volunteers, eight males and eight females, following the oral administration of 500 mg tablet of mefenamic acid. Urine samples were collected at pre-determined schedule and drug concentration was determined by spectrophotometric method. The total recovery of free mefenamic acid was 1.526 +- 0.128 and 1.193 +- 0.112% in male and female volunteers respectively. The average +- S.E values for diuresis, pH and rate of excretion of mefenamic acid was 0.0160 +- 0.004 mL/min./kg of body weight, 6.22 +- 0.167, 0.077 +- 0.016 micro g min/sup -1/kg/sup -1/in male while 0.0084 +- 0.0023mL min/sup -1/kg-1 of body weight, 6.35 +- 0.164, 0.054 +- 0.008 micro g min/sup -1/kg/sup -1/respectively in female volunteers. The results obtained are different from the earlier studies due to variability in dose, gender variation, fluctuation in urine pH, environmental conditions and nutritional ingredients. (author)

  11. Determination of caffeic acid in root and rhizome of Black cohosh (Cimicifuga racemosa (L. Nutt.

    Directory of Open Access Journals (Sweden)

    Zapala Karolina

    2014-06-01

    Full Text Available Cimicifuga racemosa, is a plant with a diverse and long history of medicinal use. Caffeic acid, bioactive compound, which often occurs with other polyphenols can influence the biological activity of this plant. The aim of our work was quantitative analysis of caffeic acid in roots and rhizomes of two varieties of C. racemosa. Analysis was performed by HPLC method. The extracts were separated on C18 reversed-phase column using mixture of methanol, water and formic acid (25:75:0.5 v/v/v as a mobile phase. The flow rate of eluent was 1.0 ml·min-1. The obtained validation parameters such as linearity, linear regression equation and precision expressed as a relative standard deviation were adequate for quantitative determination. Caffeic acid was found in all tested extracts. The highest total amount of caffeic acid was determined in C. racemosa var. racemosa (255.3 μg·g-1 while its concentration in C. racemosa var. cordifolia was significantly lower (213.0 μg·g-1.

  12. Determination of ethanol in acetic acid-containing samples by a biosensor based on immobilized Gluconobacter cells

    Directory of Open Access Journals (Sweden)

    VALENTINA A. KRATASYUK

    2012-11-01

    Full Text Available Reshetilov AN, Kitova AE, Arkhipova AV, Kratasyuk VA, Rai MK. 2012. Determination of ethanol in acetic acid containing samples by a biosensor based on immobilized Gluconobacter cells. Nusantara Bioscience 4: 97-100. A biosensor based on Gluconobacter oxydans VKM B-1280 bacteria was used for detection of ethanol in the presence of acetic acid. It was assumed that this assay could be useful for controlling acetic acid production from ethanol and determining the final stage of the fermentation process. Measurements were made using a Clark electrode-based amperometric biosensor. The effect of pH of the medium on the sensor signal and the analytical parameters of the sensor (detection range, sensitivity were investigated. The residual content of ethanol in acetic acid samples was analyzed. The results of the study are important for monitoring the acetic acid production process, as they represent a method of tracking its stages

  13. Determination of humic acid in alkali leaching solution of uranium by spectophotrometry-COD method

    International Nuclear Information System (INIS)

    Feng Yu; An Wei; Chen Shusen

    2014-01-01

    It is one of the main causes of extraction emulsification or resin toxicosis during alkali leaching process in uranium metallurgy which organic matters including humic acid exist in lixiviums. In order to study the effect of humic acid in uranium metallurgy, a method for determination of content of humic acid in aqueous solution need to be established. Spectrophotometry is a simple and convenient method in humic acid analysis. However, accuracy of spectrophotometry can be reduced greatly because of interference of uranium and other elements in the humic acid solutions. Although chemical oxygen demand (COD) method is a common analysis way of organic matters in aqueous solutions, the concentration of humic acid cannot be directly measured. In this paper, COD method is related with spectrophotometry to avoid the interference of uranium and ensure the accurate analysis of humic acid. The results showed that the detection limit of the method was 1.78 mg/L and the recovery rate was 101.2%. (authors)

  14. Combining bar adsorptive microextraction with capillary electrophoresis--application for the determination of phenolic acids in food matrices.

    Science.gov (United States)

    da Rosa Neng, Nuno; Sequeiros, Rute C P; Florêncio Nogueira, José Manuel

    2014-09-01

    In this contribution, bar adsorptive microextraction coated with a mixed-mode anion exchange/RP followed by liquid desorption was combined for the first time with a capillary electrophoresis-diode array detection system (BAμE(MAX)-LD/CE-DAD), for the determination of phenolic acids in food matrices, using chlorogenic, ferulic, cumaric, and caffeic acids as model compounds. Assays performed in aqueous media spiked at the 0.8 mg/L level yielded average recoveries up to 40% for all four phenolic acids, under optimized experimental conditions. The analytical performance showed also good precision (RSD 0.9900). By using the standard addition method, the application to food matrices such as green tea, red fruit juice, and honey allowed very good performances for the determination of minor amounts of phenolic acids. The proposed methodology proved to be a suitable alternative for the analysis of polar to ionic compounds, showing to be easy to implement, reliable, sensitive, and requiring a low sample volume to determine phenolic acids in food samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Site specific incorporation of heavy atom-containing unnatural amino acids into proteins for structure determination

    Science.gov (United States)

    Xie, Jianming [San Diego, CA; Wang, Lei [San Diego, CA; Wu, Ning [Boston, MA; Schultz, Peter G [La Jolla, CA

    2008-07-15

    Translation systems and other compositions including orthogonal aminoacyl tRNA-synthetases that preferentially charge an orthogonal tRNA with an iodinated or brominated amino acid are provided. Nucleic acids encoding such synthetases are also described, as are methods and kits for producing proteins including heavy atom-containing amino acids, e.g., brominated or iodinated amino acids. Methods of determining the structure of a protein, e.g., a protein into which a heavy atom has been site-specifically incorporated through use of an orthogonal tRNA/aminoacyl tRNA-synthetase pair, are also described.

  16. Simultaneous determination of low-molecular-weight organic acids and chlorinated acid herbicides in environmental water by a portable CE system with contactless conductivity detection.

    Science.gov (United States)

    Xu, Yan; Wang, Weilong; Li, Sam Fong Yau

    2007-05-01

    This report describes a method to simultaneously determine 11 low-molecular-weight (LMW) organic acids and 16 chlorinated acid herbicides within a single run by a portable CE system with contactless conductivity detection (CCD) in a poly(vinyl alcohol) (PVA)-coated capillary. Under the optimized condition, the LODs of CE-CCD ranged from 0.056 to 0.270 ppm, which were better than for indirect UV (IUV) detection of the 11 LMW organic acids or UV detection of the 16 chlorinated acid herbicides. Combined with an on-line field-amplified sample stacking (FASS) procedure, sensitivity enhancement of 632- to 1078-fold was achieved, with satisfactory reproducibility (RSDs of migration times less than 2.2%, and RSDs of peak areas less than 5.1%). The FASS-CE-CCD method was successfully applied to determine the two groups of acidic pollutants in two kinds of environmental water samples. The portable CE-CCD system shows advantages such as simplicity, cost effectiveness, and miniaturization. Therefore, the method presented in this report has great potential for onsite analysis of various pollutants at the trace level.

  17. Determination of free fatty acids in beer.

    Science.gov (United States)

    Bravi, Elisabetta; Marconi, Ombretta; Sileoni, Valeria; Perretti, Giuseppe

    2017-01-15

    Free fatty acids (FFA) content of beer affects the ability to form a stable head of foam and plays an important role in beer staling. Moreover, the presence of saturated FAs is related sometimes to gushing problems in beer. The aim of this research was to validate an analytical method for the determination of FFAs in beer. The extraction of FFAs in beer was achieved via Liquid-Liquid Cartridge Extraction (LLCE), the FFAs extract was purified by Solid Phase Extraction (SPE), methylated by boron trifluoride in methanol, and injected into GC-FID system. The performance criteria demonstrate that this method is suitable for the analysis of medium and long chain FFAs in beer. The proposed method was tested on four experimental beers. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Development of a method for determination of fatty acid using FT-IR spectroscopy

    Directory of Open Access Journals (Sweden)

    Dimas Augusto Morozin Zaia

    2011-05-01

    Full Text Available In the present paper a new methodology has been developed for determination of fatty acids in biological systems using FT-IR spectroscopy. For this method is not necessary chromophore reagent or pre sample preparation. Palmitic acid was chosen as standard, because it is found in several biological systems. The FT-IR spectrum of palmitic acid showed two absorption bands in the region of 2852 and 2920 cm-1 attributed to CH stretching. The results for these bands showed that the Beer-Lambert Law was followed in wide range of concentration of palmitic acid (14 to 257 mmol L-1. Potassium ferricyanide (K3[Fe(CN6] was used as internal standard. Several interferents were tested and only cholesterol, ferric chloride (higher concentration, mixture of amino acids for the band at 2919 cm-1 (higher concentration and triglyceride could be interferent if they appear in high concentration. Thus, this new methodology has advantage to be not expensive and simple.

  19. Determination of Free Fatty Acids and Triglycerides by Gas Chromatography Using Selective Esterification Reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kail, Brian W; Link, Dirk D; Morreale, Bryan D

    2012-11-01

    A method for selectively determining both free fatty acids (FFA) and triacylglycerides (TAGs) in biological oils was investigated and optimized using gas chromatography after esterification of the target species to their corresponding fatty acid methyl esters (FAMEs). The method used acid catalyzed esterification in methanolic solutions under conditions of varying severity to achieve complete conversion of more reactive FFAs while preserving the concentration of TAGs. Complete conversion of both free acids and glycerides to corresponding FAMEs was found to require more rigorous reaction conditions involving heating to 120°C for up to 2 h. Method validation was provided using gas chromatography–flame ionization detection, gas chromatography–mass spectrometry, and liquid chromatography–mass spectrometry. The method improves on existing methods because it allows the total esterified lipid to be broken down by FAMEs contributed by FFA compared to FAMEs from both FFA and TAGs. Single and mixed-component solutions of pure fatty acids and triglycerides, as well as a sesame oil sample to simulate a complex biological oil, were used to optimize the methodologies. Key parameters that were investigated included: HCl-to-oil ratio, temperature and reaction time. Pure free fatty acids were found to esterify under reasonably mild conditions (10 min at 50°C with a 2.1:1 HCl to fatty acid ratio) with 97.6 ± 2.3% recovery as FAMEs, while triglycerides were largely unaffected under these reaction conditions. The optimized protocol demonstrated that it is possible to use esterification reactions to selectively determine the free acid content, total lipid content, and hence, glyceride content in biological oils. This protocol also allows gas chromatography analysis of FAMEs as a more ideal analyte than glyceride species in their native state.

  20. Amino Acid Profile as a Feasible Tool for Determination of the Authenticity of Fruit Juices

    Directory of Open Access Journals (Sweden)

    Mostafa Asadpoor

    2014-12-01

    Full Text Available Purpose: Fruit juice is a nutrient rich food product with a direct connection to public health. The purpose of this research was to determine the amino acid profile of juices and provide a quick and accurate indicator for determining their authenticity. Methods: The method of analysis was HPLC with fluorescence detector and pre-column derivatization by orthophtaldialdehyde (OPA. Sixty-six samples of fruit juices were analyzed, and fourteen amino acids were identified and determined in the sampled fruit juices. The fruit samples used for this analysis were apples, oranges, cherry, pineapple, mango, apricot, pomegranate, peach and grapes. Results: The results showed that 32% of samples tested in this study had a lower concentrate percentage as compared to that of their labels and/or other possible authenticity problems in the manufacturing process. The following samples showed probable adulteration: four cherry juice samples, two pomegranate juice samples, one mango, three grape, four peach, seven orange, two apple and one apricot juice samples. Conclusion: In general, determining the amount of amino acids and comparing sample amino acids profiles standard values seems to be an indicator for quality control. This method can the regulatory agencies with a tool, to help produce a healthier The aim of this study is the analytical control of the fruit juice composition is becoming an important issue, and HPLC can provide an important and essential tool for more accurate research as well as for routine analysis.

  1. Amino Acid profile as a feasible tool for determination of the authenticity of fruit juices.

    Science.gov (United States)

    Asadpoor, Mostafa; Ansarin, Masoud; Nemati, Mahboob

    2014-12-01

    Fruit juice is a nutrient rich food product with a direct connection to public health. The purpose of this research was to determine the amino acid profile of juices and provide a quick and accurate indicator for determining their authenticity. The method of analysis was HPLC with fluorescence detector and pre-column derivatization by orthophtaldialdehyde (OPA). Sixty-six samples of fruit juices were analyzed, and fourteen amino acids were identified and determined in the sampled fruit juices. The fruit samples used for this analysis were apples, oranges, cherry, pineapple, mango, apricot, pomegranate, peach and grapes. The results showed that 32% of samples tested in this study had a lower concentrate percentage as compared to that of their labels and/or other possible authenticity problems in the manufacturing process. The following samples showed probable adulteration: four cherry juice samples, two pomegranate juice samples, one mango, three grape, four peach, seven orange, two apple and one apricot juice samples. In general, determining the amount of amino acids and comparing sample amino acids profiles with the standard values seems to be an indicator for quality control. This method can provide the regulatory agencies with a tool, to help produce a healthier juice. The aim of this study is the analytical control of the fruit juice composition is becoming an important issue, and HPLC can provide an important and essential tool for more accurate research as well as for routine analysis.

  2. Simultaneous determination of free amino acids in Pu-erh tea and their changes during fermentation.

    Science.gov (United States)

    Zhu, Yuchen; Luo, Yinghua; Wang, Pengpu; Zhao, Mengyao; Li, Lei; Hu, Xiaosong; Chen, Fang

    2016-03-01

    Pu-erh ripened tea is produced through a unique microbial fermentation process from the sun-dried leaves of large-leaf tea species (Camellia sinensis (Linn.) var. assamica (Masters) Kitamura) in Yunnan province of China. In this study, the changes of amino acid profiles during fermentation of Pu-erh tea were investigated, based on the improved HPLC-UV method with PITC pre-column derivatization for the simultaneous determination of twenty free amino acids. Results showed that aspartic acid, glutamic acid, arginine, alanine, theanine and tyrosine were the major amino acids in tea samples. Fermentation significantly influenced on the amino acid profiles. The total free amino acid contents significantly decreased during fermentation (pfermentation and then decreased gradually. The results provided the useful information for the manipulation of fermentation process according to the changes of amino acids and acrylamide contents in Pu-erh ripened tea. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Hydrothermal synthesis of Fe2O3/graphene nanocomposite for selective determination of ascorbic acid in the presence of uric acid

    International Nuclear Information System (INIS)

    Yu, Zhiyuan; Li, Hejun; Lu, Jinhua; Zhang, Xinmeng; Liu, Ningkun; Zhang, Xu

    2015-01-01

    In this study, we had demonstrated a hydrothermal method to prepare Fe 2 O 3 /graphene (RG) nanocomposite for the determination of ascorbic acid (AA) in the presence of uric acid (UA). The synthesized materials were characterized by scanning electron microscopy (SEM), X-ray diffraction measurements (XRD), transmission electron microscopy (TEM) and inductively coupled plasma atomic emission spectrometry (ICP-AES). As a sensor, the Fe 2 O 3 /RG nanocomposite modified electrode exhibited synergistic effects which not only improved the electrochemical catalytic oxidation of AA, but also resolved the overlapping anodic peaks of AA and UA. And the results showed that Fe 2 O 3 /RG could be used for the determination of AA in the presence of low concentration of UA. Using the modified electrode with different concentrations of AA, the linear response range for the determination of AA in the presence UA was 0.57–3.97 mM (R = 0.9994). The detection limit (S/N = 3) was found to be 0.543 μM for the determination of AA. The results suggested that the Fe 2 O 3 /RG nanocomposite had the advantages of simplicity, high sensitivity and good selectivity for determination of AA

  4. Determination of contaminants in boric acid used as neutron moderator by means of ion chromatography and selective electrodes

    International Nuclear Information System (INIS)

    Pires, M.A.F.; Abrao, A.

    1988-07-01

    The boric acid used as neutron moderator in reactors must observe restrictions about the concentration of some impurities. According to Westinghouse (1) specification, the highest limits for sodium, sulphate, phosphate, fluoride, and chlorine are: Na + - 0,003%; SO 4 -2 - 0,0006%; PO 4 -3 - 0,003%; F - - 0,00002%; Cl - - 0,00004%. This paper describes the determination of ions above mentioned directly in the boric acid solution. The sample is dissolved in water or in an appropriate eluent and is injected in the ion chromatograph. Na + and F - are determined by means of selective electrodes. The determination limits found for F - (0,0002%) and Cl - (0,0002%) are not sufficiently low to attent the specifications. The determination limits found for SO 4 -2 (0,0005%), PO 4 -3 (0,0003%) and Na + (0,0005%) are good enough for nuclear pure boric acid analysis. In some samples nitrate (detection limit 0,0015%) was found as well. Boric acid from different suppliers were analysed. (author) [pt

  5. Development of a highly sensitive MIP based-QCM nanosensor for selective determination of cholic acid level in body fluids

    International Nuclear Information System (INIS)

    Gültekin, Aytaç; Karanfil, Gamze; Sönmezoğlu, Savaş; Say, Rıdvan

    2014-01-01

    Determination of cholic acid is very important and necessary in body fluids due to its both pharmaceutical and clinical significance. In this study, a quartz crystal microbalance (QCM) nanosensor, which is imprinted cholic acid, has been developed for the assignation of cholic acid. The cholic acid selective memories have been generated on QCM electrode surface by using molecularly imprinted polymer (MIP) based on methacryloylamidohistidine-copper (II) (MAH-Cu(II)) pre-organized monomer. The cholic acid imprinted nanosensor was characterized by atomic force microscopy (AFM) and then analytical performance of the cholic acid imprinted QCM nanosensor was studied. The detection limit was found to be 0.0065 μM with linear range of 0.01–1000 μM. Moreover, the high value of Langmuir constant (b) (7.3 * 10 5 ) obtained by Langmuir graph showed that the cholic acid imprinted nanosensor had quite strong binding sites affinity. At the last step of this procedure, cholic acid levels in body fluids were determined by the prepared imprinted QCM nanosensor. - Graphical abstract: QCM responses of the cholic acid imprinted and non-imprinted nanosensors (C CA = 0.1 μM). - Highlights: • The purpose is to synthesize a new cholic acid imprinted QCM nanosensor by MIP. • Analytical applications of QCM nanosensor were investigated. • The cholic acid levels in body fluids were determined by prepared QCM nanosensor

  6. Quantitative determination of carboxylic acids, amino acids, carbohydrates, ethanol and hydroxymethylfurfural in honey by (1)H NMR.

    Science.gov (United States)

    del Campo, Gloria; Zuriarrain, Juan; Zuriarrain, Andoni; Berregi, Iñaki

    2016-04-01

    A method using (1)H NMR spectroscopy has been developed to quantify simultaneously thirteen analytes in honeys without previous separation or pre-concentration steps. The method has been successfully applied to determine carboxylic acids (acetic, formic, lactic, malic and succinic acids), amino acids (alanine, phenylalanine, proline and tyrosine), carbohydrates (α- and β-glucose and fructose), ethanol and hydroxymethylfurfural in eucalyptus, heather, lavender, orange blossom, thyme and rosemary honeys. Quantification was performed by using the area of the signal of each analyte in the honey spectra, together with external standards. The regression analysis of the signal area against concentration plots, used for the calibration of each analyte, indicates a good linearity over the concentration ranges found in honeys, with correlation coefficients higher than 0.985 for the thirteen quantified analytes. The recovery studies give values over the 93.7-105.4% range with relative standard deviations lower than 7.4%. Good precision, with relative standard deviations over the range of 0.78-5.21% is obtained. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. Compositional characteristics of commercial yoghurt based on quantitative determination of viable lactic acid bacteria

    Directory of Open Access Journals (Sweden)

    Niketić Gordana B.

    2009-01-01

    Full Text Available Yoghurt quality is particularly difficult to standardize because of the many forms, varieties, manufacturing methods, ingredients and consumer preferences that exist. Since these factors will always play an important role, it is unlikely that a uniform yoghurt quality concept will ever emerge, such as has been developed for other dairy products. There are a number of common denominators, however that have bearing on yoghurt quality. Since a number of producers are recognized within the broad category entitled yoghurt. This situation makes yoghurt an interesting, challenging, but also a confusing area to work in. The present investigation was undertaken to isolate from commercial yoghurt the strains involved in its manufacture and determine the characteristics of Streptococcus thermophilus and Lactobacillus delbrueckii subsp.bulgaricus. This study is concerned with the lactic acid bacteria (L.delbrueckii subsp. bulgaricus and S. thermophilus growth in yoghurt from involving different procedures and with the determination of the number of lactic acid bacteria in dependence of the temperature and acidity in the period of storage. Predominant samples of yoghurt were with 11-107/ml lactic acid lactococci (44.28%.

  8. Simultaneous Determination of Caffeine and Chlorogenic Acids in Green Coffee by UV/Vis Spectroscopy

    Directory of Open Access Journals (Sweden)

    G. Navarra

    2017-01-01

    Full Text Available A simple method for the simultaneous determination of caffeine and chlorogenic acids content in green coffee was reported. The method was based on the use of UV/Vis absorption. It is relevant that the quantification of both caffeine and chlorogenic acids was performed without their preliminary chemical separation despite their spectral overlap in the range 250–350 nm. Green coffee was extracted with 70% ethanol aqueous solution; then the solution was analyzed by spectroscopy. Quantitative determination was obtained analytically through deconvolution of the absorption spectrum and by applying the Lambert-Beer law. The bands used for the deconvolution were the absorption bands of both caffeine and chlorogenic acids standards. The molar extinction coefficients for caffeine and chlorogenic acid in ethanol solution at 70% were calculated by using the chemical standards; the estimated values were ε(272 nm=12159±97 M−1 cm−1 for caffeine and ε(330 nm=27025±190 M−1 cm−1 for chlorogenic acids molecules, respectively. The estimate of concentration values was in agreement with the one obtained by High Performance Liquid Chromatography quantification. The method is fast and simple and allows us to realize routine controls during the coffee production. In addition, it could be applied on roasted coffee and espresso coffee.

  9. Perturbations in amino acids and metabolic pathways in osteoarthritis patients determined by targeted metabolomics analysis.

    Science.gov (United States)

    Chen, Rui; Han, Su; Liu, Xuefeng; Wang, Kunpeng; Zhou, Yong; Yang, Chundong; Zhang, Xi

    2018-05-15

    Osteoarthritis (OA) is a degenerative synovial joint disease affecting people worldwide. However, the exact pathogenesis of OA remains unclear. Metabolomics analysis was performed to obtain insight into possible pathogenic mechanisms and diagnostic biomarkers of OA. Ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-TQ-MS), followed by multivariate statistical analysis, was used to determine the serum amino acid profiles of 32 OA patients and 35 healthy controls. Variable importance for project values and Student's t-test were used to determine the metabolic abnormalities in OA. Another 30 OA patients were used as independent samples to validate the alterations in amino acids. MetaboAnalyst was used to identify the key amino acid pathways and construct metabolic networks describing their relationships. A total of 25 amino acids and four biogenic amines were detected by UPLC-TQ-MS. Differences in amino acid profiles were found between the healthy controls and OA patients. Alanine, γ-aminobutyric acid and 4-hydroxy-l-proline were important biomarkers distinguishing OA patients from healthy controls. The metabolic pathways with the most significant effects were involved in metabolism of alanine, aspartate, glutamate, arginine and proline. The results of this study improve understanding of the amino acid metabolic abnormalities and pathogenic mechanisms of OA at the molecular level. The metabolic perturbations may be important for the diagnosis and prevention of OA. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Determination of uranium content in phosphoric and sulfuric acids used by the phosphatized fertilizers industry

    International Nuclear Information System (INIS)

    Ramos, M.M.O.

    1984-05-01

    Uranium content in phosphoric and sulfuric acids is determined. The uranium was measured through the fission track registration technique, using Makrofol KG, 10 μg thick, as detector. The so-called 'wet' method was adopted and the acid samples were used directly as irradiation medium. This proceeding showed the advantages of simple sample preparation and avoided the need of changing the acid samples media to nitric medium, as commonly used. The analysis of the sulfuric acid samples showed uranium contents under the detection limit of the technique (4 ppb). The results found for phosphoric acid samples ranged from 31 to 845 ppm, with experimental errors between 7.9 and 9.7%. (Author) [pt

  11. A method for the determination of ascorbic acid using the iron(II)-pyridine-dimethylglyoxime complex

    International Nuclear Information System (INIS)

    Arya, S. P.; Mahajan, M.

    1998-01-01

    A simple and rapid spectrophotometric method for the determination of ascorbic acid is proposed. Ascorbic acid reduces iron (III) to iron (II) which forms a red colored complex with dimethylglyoxime in the presence of pyridine. The absorbance of the resulting solution is measured at 514 nm and a linear relationship between absorbance and concentration of ascorbic acid is observed up to 14 μg ml -1 . Studies on the interference of substances usually associated with ascorbic acid have been carried out and the applicability of the method has been tested by analysing pharmaceutical preparations of vitamin C [it

  12. Determination of formal potential of Amsup((4))/Amsup((3)) pair in phosphoric-acid solutions

    International Nuclear Information System (INIS)

    Mikhajlov, V.M.; Myasoedov, B.F.

    1977-01-01

    Values of formal potentials of the system Amsup((4))/Amsup((3)) in 12 and 15 M phosphoric acid at 20+-2 deg C are determined by potentiometric method. The effect is studied of metallic platinum on the process of self-reduction of tetravalent americium, and the optimum conditions are found for potentiostatic oxidation of Amsup((3)) to Amsup((4)) in 12 M phosphoric acid

  13. Determination of the activity concentration of 230Th in phosphoric acids produced in Brazil

    International Nuclear Information System (INIS)

    Taddei, M.H.T.; Ferreira, M.T.; Fukuma, H.T.; Xavier, T.T.; Sousa, F.V.T.S.

    2017-01-01

    The high uranium phosphate rock from Itataia, Brazil, was processed using the wet route in the dihydrate system to manufacture phosphoric acid. The uranium contained in phosphoric acid was recovered by the solvent extraction technique. The distribution of the long half-life radionuclides from the decay series of 238 U and 232 Th were evaluated in these processes. The 26 Ra, 228 Ra and 210 Pb radionuclides were found predominantly in phosphogypsum, while the isotopes of 228 Th, 230 Th and 232 Th predominated in phosphoric acid after extracting uranium. The main concern in the commercialization of phosphoric acid that will be produced in the Itataia plant is in relation to the content of 230 Th. This work determined the content of these radionuclides in phosphoric acid from different locations in the country in order to compare

  14. Rapid determination of amino acids in biological samples using a monolithic silica column.

    Science.gov (United States)

    Song, Yanting; Funatsu, Takashi; Tsunoda, Makoto

    2012-05-01

    A high-performance liquid chromatography method in which fluorescence detection is used for the simultaneous determination of 21 amino acids is proposed. Amino acids were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) and then separated on a monolithic silica column (MonoClad C18-HS, 150 mm×3 mm i.d.). A mixture of 25 mM citrate buffer containing 25 mM sodium perchlorate (pH 5.5) and acetonitrile was used as the mobile phase. We found that the most significant factor in the separation was temperature, and a linear temperature gradient from 30 to 49°C was used to control the column temperature. The limits of detection and quantification for all amino acids ranged from 3.2 to 57.2 fmol and 10.8 to 191 fmol, respectively. The calibration curves for the NBD-amino acid had good linearity within the range of 40 fmol to 40 pmol when 6-aminocaproic acid was used as an internal standard. Using only conventional instruments, the 21 amino acids could be analyzed within 10 min. This method was found to be suitable for the quantification of the contents of amino acids in mouse plasma and adrenal gland samples.

  15. Determination of submicromolar amounts of uranium(VI) by compleximetric titration with pyridine-2,6-dicarboxylic acid

    International Nuclear Information System (INIS)

    Marsh, S.F.; Betts, M.R.; Rein, J.E.

    1980-01-01

    Uranium(VI) is selectively determined by a compleximetric titration with pyridine-2,6-dicarboxylic acid, using arsenazo-I indicator and hexamethylenetetramine buffer at pH 4.9. Cyclohexanediaminetetraacetic acid and diethylenetriaminepentaacetic acid provide masking of interfering metal ions. A probe colorimeter apparatus is recommended for end-point detection. The relative standard deviation is 0.6% for 0.17-0.76 μmol of uranium. (Auth.)

  16. Determination of submicromolar amounts of uranium(VI) by compleximetric titration with pyridine-2,6-dicarboxylic acid

    Energy Technology Data Exchange (ETDEWEB)

    Marsh, S F; Betts, M R; Rein, J E [Los Alamos Scientific Lab., NM (USA)

    1980-10-01

    Uranium(VI) is selectively determined by a compleximetric titration with pyridine-2,6-dicarboxylic acid, using arsenazo-I indicator and hexamethylenetetramine buffer at pH 4.9. Cyclohexanediaminetetraacetic acid and diethylenetriaminepentaacetic acid provide masking of interfering metal ions. A probe colorimeter apparatus is recommended for end-point detection. The relative standard deviation is 0.6% for 0.17-0.76 ..mu..mol of uranium.

  17. [Determination a variety of acidic gas in air of workplace by Ion Chromatography].

    Science.gov (United States)

    Li, Shiyong

    2014-10-01

    To establish a method for determination of a variety of acid gas in the workplace air by Ion Chromatography. (hydrofluoric acid, hydrogen chloride or hydrochloric acid, sulfur anhydride or sulfuric acid, phosphoric acid, oxalic acid). The sample in workplace air was collected by the porous glass plate absorption tube containing 5 ml leacheate. (Sulfuric acid fog, phosphoric acid aerosol microporous membrane after collection, eluted with 5 ml of eluent.) To separated by AS14+AG14 chromatography column, by carbonate (2.0+1.0) mmol/L (Na(2)CO(3)-NaHCO(3)) as eluent, flow rate of 1 ml/min, then analyzed by electrical conductivity detector. The retain time was used for qualitative and the peak area was used for quantitation. The each ion of a variety of acid gas in the air of workplace were excellent in carbonate eluent separation. The linear range of working curve of 0∼20 mg/L. The correlation coefficient r>0.999; lower detection limit of 3.6∼115 µg/L; quantitative limit of 0.012∼0.53 mg/L; acquisition of 15L air were measured, the minimum detection concentration is 0.004 0∼0.13 mg/m(3). The recovery rate is 99.7%∼101.1%. In the sample without mutual interference ions. Samples stored at room temperature for 7 days. The same analysis method, the detection of various acidic gases in the air of workplace, simple operation, good separation effect, high sensitivity, high detection efficiency, easy popularization and application.

  18. Square-wave stripping voltammetric determination of caffeic acid on electrochemically reduced graphene oxide-Nafion composite film.

    Science.gov (United States)

    Filik, Hayati; Çetintaş, Gamze; Avan, Asiye Aslıhan; Aydar, Sevda; Koç, Serkan Naci; Boz, İsmail

    2013-11-15

    An electrochemical sensor composed of Nafion-graphene nanocomposite film for the voltammetric determination of caffeic acid (CA) was studied. A Nafion graphene oxide-modified glassy carbon electrode was fabricated by a simple drop-casting method and then graphene oxide was electrochemically reduced over the glassy carbon electrode. The electrochemical analysis method was based on the adsorption of caffeic acid on Nafion/ER-GO/GCE and then the oxidation of CA during the stripping step. The resulting electrode showed an excellent electrocatalytical response to the oxidation of caffeic acid (CA). The electrochemistry of caffeic acid on Nafion/ER-GO modified glassy carbon electrodes (GCEs) were studied by cyclic voltammetry and square-wave adsorption stripping voltammetry (SW-AdSV). At optimized test conditions, the calibration curve for CA showed two linear segments: the first linear segment increased from 0.1 to 1.5 and second linear segment increased up to 10 µM. The detection limit was determined as 9.1×10(-8) mol L(-1) using SW-AdSV. Finally, the proposed method was successfully used to determine CA in white wine samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Sensitive determination of D-lactic acid and L-lactic acid in urine by high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Henry, H; Marmy Conus, N; Steenhout, P; Béguin, A; Boulat, O

    2012-04-01

    D-lactic acid in urine originates mainly from bacterial production in the intestinal tract. Increased D-lactate excretion as observed in patients affected by short bowel syndrome or necrotizing enterocolitis reflects D-lactic overproduction. Therefore, there is a need for a reliable and sensitive method able to detect D-lactic acid even at subclinical elevation levels. A new and highly sensitive method for the simultaneous determination of L- and D-lactic acid by a two-step procedure has been developed. This method is based on the concentration of lactic acid enantiomers from urine by supported liquid extraction followed by high-performance liquid chromatography-tandem mass spectrometry. The separation was achieved by the use of an Astec Chirobiotic™ R chiral column under isocratic conditions. The calibration curves were linear over the ranges of 2-400 and 0.5-100 µmol/L respectively for L- and D-lactic acid. The limit of detection of D-lactic acid was 0.125 µmol/L and its limit of quantification was 0.5 µmol/L. The overall accuracy and precision were well within 10% of the nominal values. The developed method is suitable for production of reference values in children and could be applied for accurate routine analysis. Copyright © 2011 John Wiley & Sons, Ltd.

  20. Estimation of free acid content in lanthanide salt solution used for pH-potentiometric determination of their stability constants with organic ligands

    International Nuclear Information System (INIS)

    Zheltvaj, I.I.; Tishchenko, M.A.

    1985-01-01

    To improve the pH-potentiometric method for determining complex stability constants the possibility of alkalimetric titration of a free acid in the lanthanide perchlorate solution after binding metal ions by disodium salt of ethylene-diamine-tetraacetic acid is studied. The stability constants were determined from the difference between the total acid content after complexon addition and doubled metal cation content in the solution which has been preliminarily determined by the complexonometric method. It is shown that the alkaline (NaOH) equivalent quantities spent for free acid titration either in the absence or presence of the complexon is different. With increase of free acid content in the solution the difference in determinations with complexon and without it is somewhat reduced. Thus, the use of complexon contributes to a higher accuracy in determining the free acid, and in the first place in case of minor contents

  1. 230Th, 232Th and 238U determinations in phosphoric acid fertilizer and process products by ICP-MS

    International Nuclear Information System (INIS)

    Nascimento, Marcos R.L. do; Guerreiro, Luisa M.R.; Bonifacio, Rodrigo L.; Taddei, Maria H.T.

    2015-01-01

    Through processing of Santa Quiteria-CE mine phosphate rock, Brazil has established a project for production of phosphoric acid fertilizer and uranium as a by-product. Under leaching conditions of phosphate rock with sulfuric acid, which is the common route for preparing phosphoric acid fertilizer, a large part of uranium, thorium and their decay products naturally present in the rock are solubilized. In order to assess the contamination potential in phosphoric acid and others process products, this paper describes a previous precipitation and direct methods for routine analysis of thorium and uranium isotopes by ICP-MS. In all samples, 230 Th, 232 Th and 238 U were directly determined after dilution, except 230 Th in phosphoric acid loaded with uranium sample, which to overcome equipment contamination effect, was determined after its separation by oxalate precipitation using lanthanum as a carrier. The results obtained by the proposed method by ICP-MS, were in good agreement when compared to alpha spectrometry for 230 Th, and ICP-OES and spectrophotometry with arsenazo III for elementary uranium and thorium determinations. (author)

  2. Determination of free acidity in nuclear fuel reprocessing streams by fiber optic aided spectrophotometric technique

    International Nuclear Information System (INIS)

    Ganesh, S.; Velavendan, P.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

    2014-01-01

    A fiber optic aided spectrophotometric technique has been developed for the determination of free acidity in nuclear fuel reprocessing streams. The developed method is simple, accurate and applicable to all ranges of nitric acid and heavy metal concentrations relevant to the purex process. The method is based on the formation of yellow colour with an acid-sensitive indicator such as chrome azurol s, the intensity of yellow colour is proportional to the acid concentration. The system obeys Lambert-Beer's law at 455 nm in the range of acidity 1-10 M of nitric acid. The results obtained are reproducible with standard deviation 2% and relative error is less than 3%. The results obtained by the developed technique are in good agreement with those obtained by the standard procedure. This method is adaptable for remote operation and on-line monitoring. (author)

  3. Determination of the Acid Dissociation Constant of a Phenolic Acid by High Performance Liquid Chromatography: An Experiment for the Upper Level Analytical Chemistry Laboratory

    Science.gov (United States)

    Raboh, Ghada

    2018-01-01

    A high performance liquid chromatography (HPLC) experiment for the upper level analytical chemistry laboratory is described. The students consider the effect of mobile-phase composition and pH on the retention times of ionizable compounds in order to determine the acid dissociation constant, K[subscript a], of a phenolic acid. Results are analyzed…

  4. A Precise Method for Processing Data to Determine the Dissociation Constants of Polyhydroxy Carboxylic Acids via Potentiometric Titration.

    Science.gov (United States)

    Huang, Kaixuan; Xu, Yong; Lu, Wen; Yu, Shiyuan

    2017-12-01

    The thermodynamic dissociation constants of xylonic acid and gluconic acid were studied via potentiometric methods, and the results were verified using lactic acid, which has a known pKa value, as a model compound. Solutions of xylonic acid and gluconic acid were titrated with a standard solution of sodium hydroxide. The determined pKa data were processed via the method of derivative plots using computer software, and the accuracy was validated using the Gran method. The dissociation constants associated with the carboxylic acid group of xylonic and gluconic acids were determined to be pKa 1  = 3.56 ± 0.07 and pKa 1  = 3.74 ± 0.06, respectively. Further, the experimental data showed that the second deprotonation constants associated with a hydroxyl group of each of the two acids were pKa 2  = 8.58 ± 0.12 and pKa 2  = 7.06 ± 0.08, respectively. The deprotonation behavior of polyhydroxy carboxylic acids was altered using various ratios with Cu(II) to form complexes in solution, and this led to proposing a hypothesis for further study.

  5. Determination of major elements in annual tree rings by acid extraction

    International Nuclear Information System (INIS)

    Belacy, N.; Abou EL-Nour, F.; Simpson, H.J.

    1991-01-01

    A method utilizing acid extraction of Na, K, Ca and Mg from the wood of annual growth rings of egyptian trees was executed. The method was applied on a Morus Alba tree located at Nile delta, northern of egypt. The acid extraction method includes the use of dilute nitric acid to extract the elements of the wood. The wood was soaked for one hour with continuous stirring at room temperature. Element contents of both leachant and ash of the extracted wood dissolved in 2N HNO 3 , were then estimated using an atomic absorption spectrophotometer. The method was optimized and led to an accurate determination of the elements in the wood of the examined tree rings. The results showed a difference in the level of these elements along the annual rings of the examined tree. The data obtained in this work can help in understanding the correlation between the concentration of these elements in the annual growth rings of the egyptian trees and the expected changes in the salinity of water of irrigation before and after the high dam project

  6. Capillary electrophoresis tandem mass spectrometry determination of glutamic acid and homocysteine's metabolites: Potential biomarkers of amyotrophic lateral sclerosis.

    Science.gov (United States)

    Cieslarova, Zuzana; Lopes, Fernando Silva; do Lago, Claudimir Lucio; França, Marcondes Cavalcante; Colnaghi Simionato, Ana Valéria

    2017-08-01

    Amyotrophic lateral sclerosis (ALS) is a neurodegenerative disease that affects both lower and upper motor neurons, leading to muscle atrophy, paralysis, and death caused by respiratory failure or infectious complications. Altered levels of homocysteine, cysteine, methionine, and glutamic acid have been observed in plasma of ALS patients. In this context, a method for determination of these potential biomarkers in plasma by capillary electrophoresis tandem mass spectrometry (CE-MS/MS) is proposed herein. Sample preparation was carefully investigated, since sulfur-containing amino acids may interact with plasma proteins. Owing to the non-thiol sulfur atom in methionine, it was necessary to split sample preparation into two methods: i) determination of homocysteine and cysteine as S-acetyl amino acids; ii) determination of glutamic acid and methionine. All amino acids were separated within 25min by CE-MS/MS using 5molL -1 acetic acid as background electrolyte and 5mmolL -1 acetic acid in 50% methanol/H 2 O (v/v) as sheath liquid. The proposed CE-MS/MS method was validated, presenting RSD values below 6% and 11% for intra- and inter-day precision, respectively, for the middle concentration level within the linear range. The limits of detection ranged from 35 (homocysteine) to 268nmolL -1 (glutamic acid). The validated method was applied to the analysis of plasma samples from a group of healthy individuals and patients with ALS, showing the potential of glutamic acid and homocysteine metabolites as biomarkers of ALS. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Acidity Constants Determination of Triazine Dye Derivative in the presence of some Surfactants by Multiwavelength Spectrophotometric and Spectrofluorimetric

    Directory of Open Access Journals (Sweden)

    Ali Yeganeh Faal

    2014-03-01

    Full Text Available In this work, acidity constants protonated form of 4.4'-bis astilbene-2,2'-disulfonic-disodium salts (TRIAZ have been determined spectrophotometrically and spectrofluorimetrically at 25◦C and ionic strength of 0.1M KNO3. A program based on MCR-ALS applied for determination of acidity constants. The results show that the peak values of dye are influenced by the presence of anionic, cationic, and nonionic surfactants. The effects of sodium dodecyl sulfate (SDS, Triton X-100 (TX-100 and cetyl trimethyl ammonium bromide (CTAB as a surface-active agent on the acidic and basic forms, and the spectral properties of dye were studied. Also, we determined the critical micelle concentration (CMC for these surfactants by spectrophotometric and spectrofluorimetric triazine dye probes. In addition, by using of evolving factor analysis (EFA and multivariate curve resolution alternative least squares (MCR-ALS methods, acidity constants were acquired.

  8. Determination of free radical reaction products and metabolites of salicylic acid using capillary electrophoresis and micellar electrokinetic chromatography

    NARCIS (Netherlands)

    Coolen, S.A.J.; Huf, F.A.; Reijenga, J.C.

    1998-01-01

    Hydroxylated radical products of salicylic acid are often used as a relative measurement in free radical research. Several analytical methods exist to determine the amount of 2,3-dihydroxybenzoic acid and 2,5-dihydroxybenzoic acid. In this study we use capillary zone electrophoresis (CZE) and

  9. Electrocatalytic oxidation and voltammetric determination of ciprofloxacin employing poly(alizarin red)/graphene composite film in the presence of ascorbic acid, uric acid and dopamine

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xin; Wei, Youli; Ding, Yaping, E-mail: wdingyp@sina.com

    2014-07-04

    Graphical abstract: An electrochemical sensor based on PAR/EGR/GCE via a cooperation of the potentiostatic technique and cyclic voltammetry was first fabricated for the determination of CPFX with satisfied detecting result of real samples. - Highlights: • PAR/EGR composite film was prepared for the first time. • The sensor can be applied to determinate CPFX in the presence of AA, UA and DA. • The sensor indicated the feasibility in drug samples and biological media. - Abstract: A glassy carbon electrode modified with poly(alizarin red)/electrodeposited graphene (PAR/EGR) composite film was prepared and applied to detect ciprofloxacin (CPFX) in the presence of ascorbic, uric acid and dopamine. The morphology and interface property of PAR/EGR films were examined by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electrocatalytic oxidation of CPFX on AR/EGR was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The linearity ranged from 4 × 10{sup −8} to 1.2 × 10{sup −4} M with a detection limit (S/N = 3) of 0.01 μM. The modified electrode could be applied to the individual determination of CPFX as well as the simultaneous determination of CPFX, ascorbic acid, uric acid and dopamine. This method proved to be a simple, selective and rapid way to determine CPFX in pharmaceutical preparation and biological media.

  10. Electrocatalytic oxidation and voltammetric determination of ciprofloxacin employing poly(alizarin red)/graphene composite film in the presence of ascorbic acid, uric acid and dopamine

    International Nuclear Information System (INIS)

    Zhang, Xin; Wei, Youli; Ding, Yaping

    2014-01-01

    Graphical abstract: An electrochemical sensor based on PAR/EGR/GCE via a cooperation of the potentiostatic technique and cyclic voltammetry was first fabricated for the determination of CPFX with satisfied detecting result of real samples. - Highlights: • PAR/EGR composite film was prepared for the first time. • The sensor can be applied to determinate CPFX in the presence of AA, UA and DA. • The sensor indicated the feasibility in drug samples and biological media. - Abstract: A glassy carbon electrode modified with poly(alizarin red)/electrodeposited graphene (PAR/EGR) composite film was prepared and applied to detect ciprofloxacin (CPFX) in the presence of ascorbic, uric acid and dopamine. The morphology and interface property of PAR/EGR films were examined by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS). The electrocatalytic oxidation of CPFX on AR/EGR was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The linearity ranged from 4 × 10 −8 to 1.2 × 10 −4 M with a detection limit (S/N = 3) of 0.01 μM. The modified electrode could be applied to the individual determination of CPFX as well as the simultaneous determination of CPFX, ascorbic acid, uric acid and dopamine. This method proved to be a simple, selective and rapid way to determine CPFX in pharmaceutical preparation and biological media

  11. [Determination of acidity and vitamin C in apples using portable NIR analyzer].

    Science.gov (United States)

    Yang, Fan; Li, Ya-Ting; Gu, Xuan; Ma, Jiang; Fan, Xing; Wang, Xiao-Xuan; Zhang, Zhuo-Yong

    2011-09-01

    Near infrared (NIR) spectroscopy technology based on a portable NIR analyzer, combined with kernel Isomap algorithm and generalized regression neural network (GRNN) has been applied to establishing quantitative models for prediction of acidity and vitamin C in six kinds of apple samples. The obtained results demonstrated that the fitting and the predictive accuracy of the models with kernel Isomap algorithm were satisfactory. The correlation between actual and predicted values of calibration samples (R(c)) obtained by the acidity model was 0.999 4, and for prediction samples (R(p)) was 0.979 9. The root mean square error of prediction set (RMSEP) was 0.055 8. For the vitamin C model, R(c) was 0.989 1, R(p) was 0.927 2, and RMSEP was 4.043 1. Results proved that the portable NIR analyzer can be a feasible tool for the determination of acidity and vitamin C in apples.

  12. Impact of Sampling and Cellular Separation on Amino Acid Determinations in Drosophila Hemolymph.

    Science.gov (United States)

    Cabay, Marissa R; Harris, Jasmine C; Shippy, Scott A

    2018-04-03

    The fruit fly is a frequently used model system with a high degree of human disease-related genetic homology. The quantitative chemical analysis of fruit fly tissues and hemolymph uniquely brings chemical signaling and compositional information to fly experimentation. The work here explores the impact of measured chemical content of hemolymph with three aspects of sample collection and preparation. Cellular content of hemolymph was quantitated and removed to determine hemolymph composition changes for seven primary amine analytes. Hemolymph sampling methods were adapted to determine differences in primary amine composition of hemolymph collected from the head, antenna, and abdomen. Also, three types of anesthesia were employed with hemolymph collection to quantitate effects on measured amino acid content. Cell content was found to be 45.4 ± 22.1 cells/nL of hemolymph collected from both adult and larvae flies. Cell-concentrated fractions of adult, but not larvae, hemolymph were found to have higher and more variable amine content. There were amino acid content differences found between all three areas indicating a robust method to characterize chemical markers from specific regions of a fly, and these appear related to physiological activity. Methods of anesthesia have an impact on hemolymph amino acid composition related to overall physiological impact to fly including higher amino acid content variability and oxygen deprivation effects. Together, these analyses identify potential complications with Drosophila hemolymph analysis and opportunities for future studies to relate hemolymph content with model physiological activity.

  13. Preliminary study for the determination of heavy metal in ground samples by GF-ASS Zeeman; Studio preliminare per la determinazione di metalli pesanti in campioni di suolo mediante analisi GF-AAS Zeeman

    Energy Technology Data Exchange (ETDEWEB)

    Casabianca, T.; Bitonte, R.; Epifani, M.; Ubaldi, C. [ENEA, Divisione Tecnologie Ingegneria e Servizi Ambientali, Centro Ricerche Trisaia, MT (Italy)

    2001-07-01

    In the framework of SIMOA project have been investigated methods to evaluate the level of soil contamination due to heavy metals. In this wok, it is discussed a procedure to measure topsoil bioavailable fraction of seven heavy metals (Cd, Cu, Pb, Ni, Cr, Hg). The adopted procedure is based on acid digestion followed by instrumental detection by means of graphite furnace atomic-absorption spectrophotometry (GFAAS) using Zeeman effect to reduce background contribution. Details of samples preparation and analysis, experimental setup optimization and statistical data analysis are presented, together with a discussion on method accuracy and data interpretation. [Italian] Nell'ambito del progetto SIMOA (Sistema Integrato di Monitoraggio Ambientale) per il monitoraggio ambientale nel bacino del Basento (Regione Basilicata, Italia), vengono investigati i metodi per il controllo dei livelli di inquinamento del suolo da parte di metalli pesanti. Nel presente lavoro viene proposta una procedura per determinare il livello di concentrazione della frazione biodisponibile di sette metalli pesanti (Cadmio, Rame, Piombo, Nickel, Cromo, Mercurio) in campion di suolo superficiale. Il metodo e' basato su di un trattamento di digestione acida in forno a microonde cui segue la rivelazione strumentale mediante spettrofotometria di assorbimento atomico in fornetto di grafite (GFAAS) con effetto Zeeman per la correzione del fondo. Si descrivono in dettaglio le fasi di preparazione dei campioni, la metodologia di misura e l'analisi statistica dei dati, oltre ad una discussione sull'attendibilita' del metodo e sui futuri sviluppi.

  14. Analytical applications of condensed phosphoric acid-I Determination of ferrous and total iron in iron ores after decomposition with condensed phosphoric acid.

    Science.gov (United States)

    Mizoguchi, T; Ishii, H

    1978-06-01

    A simple method is described for the determination of ferrous and total iron in iron ores. Iron ores are dissolved by condensed phosphoric acid (CPA) very rapidly without any tedious and time-consuming manipulations such as elimination of silica and filtration. Under the proposed conditions (amount of sample 100 mg, amount of CPA added 10 g, heating temperature 290 degrees , heating time 30 min), magnetite, limonite and hematite are completely dissolved. The iron content can be determined in the presence of condensed phosphoric acid by titration with dichromate solution, if a slight modification is made. The total iron in iron ores, determined by the present method, is in agreement with that found by the JIS method. The ferrous iron in iron ores can be determined by dissolving the samples with CPA in a nitrogen atmosphere and titrating with dichromate solution. Chelatometric titration of iron after solvent extraction with MIBK from solutions prepared by use of CPA is found to be accurate for samples such as pyrite cinder. The ability of CPA to dissolve various materials has been investigated.

  15. Development and Validation of a Reversed-Phase Liquid Chromatography Method for the Simultaneous Determination of Indole-3-Acetic Acid, Indole-3-Pyruvic Acid, and Abscisic Acid in Barley (Hordeum vulgare L.).

    Science.gov (United States)

    Nakurte, Ilva; Keisa, Anete; Rostoks, Nils

    2012-01-01

    A simple, sensitive, precise, and specific reverse HPLC method was developed and validated for the determination of plant hormones in barley (Hordeum vulgare L.). The method includes extraction in aqueous organic solvent followed by solid-phase extraction, sample evaporation, and reversed-phase HPLC analysis in a general purpose UV-visible (abscisic acid (ABA)) and fluorescence detection (indole-3-acetic acid (IAA) and indole-3-pyruvic acid (IPA)), high-performance liquid chromatography system. The separation was carried out on Zorbax Eclipse XDB C8 column (150  ×  4.6  mm I.D) with a mobile phase composed of methanol and 1% acetic acid (60 : 40 v/v) in isocratic mode at a flow rate of 1 ml min(-1). The detection was monitored at 270 nm (ABA) and at 282 nm (Ex) and 360 nm (Em) (IAA, IPA). The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification, and robustness. The determined validation parameters are in the commonly acceptable ranges for that kind of analysis.

  16. Equilibrium dialysis-ligand exchange: adaptation of the method for determination of conditional stability constants of radionuclide-fulvic acid complexes

    International Nuclear Information System (INIS)

    Glaus, M.A.; Hummel, W.; Van Loon, L.R.

    1995-01-01

    The equilibrium dialysis-ligand exchange technique (EDLE) is used to determine conditional stability constants for the complexation of metal ions with humic acid, particularly in high pH solutions. Here, this technique has been adapted to measure conditional stability constants with fulvic acid. Fulvic acid permeates across all membranes during the experiment. The quantities involved therefore have to be determined analytically and taken into account when calculating the conditional stability constants. Co(II) and Laurentian Soil fulvic (LFA) acid were selected as a test system in order to investigate the time scale required to establish chemical and diffusion equilibria. After an incubation time of approximately two days, the conditional stability constants measured for the formation of Co-LFA-complexes are not time dependent, although across the whole time period investigated, LFA was still diffusing in increasing amounts across the dialysis membrane. This work demonstrates that the modified EDLE technique can be used in the determination of conditional metal stability constants of fulvic acid. (authors)

  17. Towards an efficient protocol for the determination of triterpenic acids in olive fruit: a comparative study of drying and extraction methods.

    Science.gov (United States)

    Goulas, Vlasios; Manganaris, George A

    2012-01-01

    Triterpenic acids, such as maslinic acid and oleanolic acid, are commonly found in olive fruits and have been associated with many health benefits. The drying and extraction methods, as well as the solvents used, are critical factors in the determination of their concentration in plant tissues. Thus, there is an emerging need for standardisation of an efficient extraction protocol that determines triterpenic acid content in olive fruits. To evaluate common extraction methods of triterpenic acids from olive fruits and to determine the effect of the drying method on their content in order to propose an optimum protocol for their quantification. The efficacy of different drying and extraction methods was evaluated through the quantification of maslinic acid and oleanolic acid contents using the reversed-phase HPLC technique. Data showed that ultrasonic assisted extraction with ethanol or a mixture of ethanol:methanol (1:1, v/v) resulted in the recovery of significantly higher amounts of triterpenic acids than other methods used. The drying method also affected the estimated triterpenic acid content; frozen or lyophilised olive fruit material gave higher yields of triterpenic acids compared with air-dried material at both 35°C and 105°C. This study provides a rapid and low-cost extraction method, i.e. ultrasonic assisted extraction with an eco-friendly solvent such as ethanol, from frozen or lyophilised olive fruit for the accurate determination of the triterpenic acid content in olive fruit. Copyright © 2011 John Wiley & Sons, Ltd.

  18. Determination of ascorbic acid, dopamine, and uric acid by a novel electrochemical sensor based on pristine graphene

    International Nuclear Information System (INIS)

    Qi, Shaopeng; Zhao, Bo; Tang, Heqing; Jiang, Xiaoqing

    2015-01-01

    In this article, a novel electrochemical sensor based on pristine graphene (PG) is successfully constructed to detect ascorbic acid (AA), dopamine (DA), and uric acid (UA). The PG is obtained by liquid-phase exfoliation of graphite and characterized by transmission electron microscopy and X-ray photoelectron spectroscopy. The sensor based on PG prepared by this method to realize simultaneous determination of AA, DA, and UA is firstly reported. The linear detection ranges for AA, DA, and UA are 9.00–2314 μM, 5.00–710 μM, and 6.00–1330 μM, respectively, with detection limits of 6.45, 2.00, and 4.82 μM. This PG based sensor exhibits excellent performance for detection of AA, DA, and UA, which is much better than those electrochemical sensors based on chemical converted graphene

  19. Determination of free acid in U(VI)-Al(III) solution by Gran plot titration

    International Nuclear Information System (INIS)

    Suh, Moo Yul; Lee, Chang Heon; Sohn, Se Chul; Kim, Jung Suk; Kim, Won Ho; Eom, Tae Yoon

    1999-01-01

    The determination method of free acid in spent U-Al nuclear fuel solutions by Gran plot titration was described. Effect of U(VI) and Al(III) on the alkalimetric titration of nitric acid was investigation in oxalate complexing media as well as in noncomplexing media. Positive biases were observed in both titration media when the end-point was estimated by the Gran plot method. It was found that the cause of the bias was U(VI) in the oxalate complexing media, but Al(III) in the noncomplexing media. The relative error was less than 1% in the titration of 0.1 M HNO 3 at a U(VI):Al(III):H + mole ratio of up to 2:12:1 as long as the pH of the oxalate titration media was sustained to be below 5.0 at the beginning of titration. The method was successfully applied to the determination of nitric acid in a solution of HANARO reactor fuel with U:Al mole ratio of 1:6

  20. Error causes in the determination of the acid-base reactivity of oxi-hydroxides

    International Nuclear Information System (INIS)

    Duc, M.; Lefevre, G.; Fedoroff, M.

    2004-01-01

    The long term safety of radioactive waste depositories is based on the sorption of radionuclides from underground water onto engineered and natural barriers. For a quantitative prediction of the migration in such barriers, we need accurate sorption data. Models should be in agreement with the sorption mechanism. Surface complexation is the most often used model for oxides and hydroxides. In fact, there are several types of surface complexation models such as 1-pK and 2-pK monosite, 1-pK and 2-pK multisite, pK-distribution models. Furthermore, there are several ways to describe the distribution of the electrostatic potential in the vicinity of the solid surface (CCM, DLM, BSM, TLM,..). However, all these models are based on the acid-base properties of superficial hydroxide or oxide groups of the solid. It is necessary to determine the surface charge versus pH (titration curves), the point of zero charge (pzc), the surface density of sites active towards protons and hydroxides in aqueous solutions, the acid-base constants of these sites. These parameters are then used for calculating the sorption constants of ions other than protons and hydroxide ions. It is therefore important to determine these parameters very accurately. A comparison of acid-base parameters published in the literature shows a large scatter for the ''same'' oxides [1,2]. Several causes could explain this scatter. One reason is the use of different models, each electrostatic models leading to different values of site density and constants. However, titration curves and pzc are independent of the model chosen. Another reason may be uncontrolled differences in the composition and purity of oxides. Finally, other causes could be found in the titration procedure, in the solubility and the stability of the solid. In order to understand more about the acid-base properties of oxides and about the origin of the discrepancies between measurements, we have performed a systematic experimental study of several

  1. Luminescent determination of trace amounts of terbium using diantipyrylmethane and salicylic acid

    Energy Technology Data Exchange (ETDEWEB)

    Tishchenko, M A; Gerasimenko, G I; Poluehktov, N S [AN Ukrainskoj SSR, Odessa. Inst. Obshchej i Neorganicheskoj Khimii

    1978-01-01

    To elucidate the possibility of using pyrazolone-5-diantipyril-methane (DAM) derivative for determination of terbium microimpurities, the conditions have been studied of luminescent determination of terbium in complex compounds containing an ion of rare-earth element, diantipyrilmethane, and salicylic acid (Sal.). The ratio between the components in the complex REE-DAM-Sal is 1:1:3. La, Y, Gd do not affect the luminescence intensity of terbium complex. A luminescent method of determining terbium traces in highly pure oxides of lanthanum, gadolinium, lutetium, and yttrium has been developed in which suspensions of complex precipitation are used. The amount of terbium determined in oxide of lanthanum, gadolinium, and lutetium is (1-5)x10/sup -6/% and (2-3)x10/sup -5/% in yttrium oxide.

  2. Determining surface areas of marine alga cells by acid-base titration method.

    Science.gov (United States)

    Wang, X; Ma, Y; Su, Y

    1997-09-01

    A new method for determining the surface area of living marine alga cells was described. The method uses acid-base titration to measure the surface acid/base amount on the surface of alga cells and uses the BET (Brunauer, Emmett, and Teller) equation to estimate the maximum surface acid/base amount, assuming that hydrous cell walls have carbohydrates or other structural compounds which can behave like surface Brönsted acid-base sites due to coordination of environmental H2O molecules. The method was applied to 18 diverse alga species (including 7 diatoms, 2 flagellates, 8 green algae and 1 red alga) maintained in seawater cultures. For the species examined, the surface areas of individual cells ranged from 2.8 x 10(-8) m2 for Nannochloropsis oculata to 690 x 10(-8) m2 for Dunaliella viridis, specific surface areas from 1,030 m2.g-1 for Dunaliella salina to 28,900 m2.g-1 for Pyramidomonas sp. Measurement accuracy was 15.2%. Preliminary studies show that the method may be more promising and accurate than light/electron microscopic measurements for coarse estimation of the surface area of living algae.

  3. Determination of acid ionization constants for weak acids by osmometry and the instrumental analysis self-evaluation feedback approach to student preparation of solutions

    Science.gov (United States)

    Kakolesha, Nyanguila

    One focus of this work was to develop of an alternative method to conductivity for determining the acid ionization constants. Computer-controlled osmometry is one of the emerging analytical tools in industrial research and clinical laboratories. It is slowly finding its way into chemistry laboratories. The instrument's microprocessor control ensures shortened data collection time, repeatability, accuracy, and automatic calibration. The equilibrium constants of acetic acid, chloroacetic acid, bromoacetic acid, cyanoacetic acid, and iodoacetic acid have been measured using osmometry and their values compared with the existing literature values obtained, usually, from conductometric measurements. Ionization constant determined by osmometry for the moderately strong weak acids were in reasonably good agreement with literature values. The results showed that two factors, the ionic strength and the osmotic coefficient, exert opposite effects in solutions of such weak acids. Another focus of the work was analytical chemistry students solution preparation skills. The prevailing teacher-structured experiments leave little room for students' ingenuity in quantitative volumetric analysis. The purpose of this part of the study was to improve students' skills in making solutions using instrument feedback in a constructivist-learning model. After making some solutions by weighing and dissolving solutes or by serial dilution, students used the spectrophotometer and the osmometer to compare their solutions with standard solutions. Students perceived the instrument feedback as a nonthreatening approach to monitoring the development of their skill levels and liked to clarify their understanding through interacting with an instructor-observer. An assessment of the instrument feedback and the constructivist model indicated that students would assume responsibility for their own learning if given the opportunity. This study involved 167 students enrolled in Quantitative Chemical

  4. Comparison of acid ethanol extraction and acid gel filtration prior to IGF-I and IGF-II radioimmunoassays; Improvement of determinations in acid ethanol extracts by the use of truncated IGF-I as radioligand

    Energy Technology Data Exchange (ETDEWEB)

    Bang, P; Eriksson, U; Wivall, I -L; Hall, K [Department of Endocrinology, Karolinska Institute, Stockholm (Sweden); Sara, V [Department of Pathology, Karolinska Institute, Stockholm (Sweden)

    1991-01-01

    Insulin-like growth factor binding proteins interfere in the IGF-I and -II radioimmunoassays. In an attempt to overcome this problem, we have compared the use of truncated IGF-I, with reduced IGFBP affinity, and IGF-I as radioligands for IGF-I RIA measurements in serum separated by acid gel filtration or acid ethanol extraction followed by cryo-precipitation. With truncated IGF-I as radioligand the IGF-I measurements in acid gel filtrates and acid ethanol extracts were significantly correlated in healthy subjects (N=42, r=0.91, p<0.001) and in patients with acromegaly (N=10, r=0.85, p<0.01), GH deficiency (N=10, r=0.88, p<0.001) or Type I diabetes mellitus (N=10, r=0.90, p<0.001). In contrast, the IGF-I concentrations in acid ethanol extracts determined with IGF-I as radioligand did not correlate with those in acid gel filtrates using truncated IGF-I radioligand in patients with acromegaly (r=0.61, NS) or GH deficiency (r=0.46, NS). In the latter group the mean IGF-I concentrations measured in acid ethanol extracts were erroneously elevated by 112%. Low-affinity antibodies used for IGF-II RIA determinations failed to give reliable results in acid ethanol extracts from patients with Type I diabetes mellitus or GH deficiency. In conclusion, erroneously high IGF-I concentrations owing to binding of the radioligand to IGFBPs not completely removed by acid ethanol extraction can be avoided by the use of truncated IGF-I as radioligand. (author).

  5. Monolayer covalent modification of 5-hydroxytryptophan on glassy carbon electrodes for simultaneous determination of uric acid and ascorbic acid

    International Nuclear Information System (INIS)

    Lin Xiangqin; Li Yongxin

    2006-01-01

    5-Hydroxytryptophan (5-HTP) was covalently grafted on the surface of glassy carbon electrodes (GCEs) using cyclic voltammetric method in a phosphate buffer solution. The prepared electrode, denoded as 5-HTP/GCE, was characterized by X-ray photoelectron spectroscopy, cyclic voltammetry and differential pulse voltammetry (DPV). Tryptophan grafted GCE (TRP/GCE) and 5-hydroxytryptamine grafted GCE (5-HTP/GCE) were also prepared by the same method for comparison. It was found that the electrocatalytic activities toward the oxidation of uric acid (UA) and ascorbic acid (AA) was in the order of 5-HT/GCE > 5-HTP/GCE > TRP/GCE for UA oxidation and 5-HT/GCE 5-HTP/GCE > TRP/GCE for AA oxidation. However, the CV current sensitivity was estimated as 4:2:1 for 5-HTP/GCE:5-HT/GCE:TRP/GCE. The DPV peaks for UA and AA oxidation appeared at 0.07 V and 0.34 V versus SCE, respectively, allowing simultaneous determination in mixtures. A linearly response in the range of: 5.0 x 10 -7 to 1.1 x 10 -5 M with the detection limit (s/n = 3) of 2.8 x 10 -7 M for UA determination, and a linear response in the range of: 5.0 x 10 -6 to 1.0 x 10 -4 M with the detection limit of 4.2 x 10 -6 M for AA determination were obtained. This electrode was used for UA and AA determinations in human urine samples satisfactorily

  6. [Determination of aspirin and free salicylic acid in lysinipirine injection by high performance liquid chromatography].

    Science.gov (United States)

    Dong, Yu; Zhao, Yuan-zheng; Zhang, Yi-na

    2002-05-01

    The contents of aspirin and free salicylic acid in lysinipirine injection were determined by high performance liquid chromatography (HPLC). A Hypersil BDS C18 column was used with the mobile phase of methanol-water-acetic acid (35:65:3, volume ratio) and the detection wavelength of 280 nm. The average recoveries of aspirin and salicylic acid added were 99.27% (RSD = 0.8%) and 99.61%(RSD = 1.3%), respectively. The calibration curves had good linearity in the range of 0.028 g/L -0.141 mg/L and 0.77 mg/L -3.85 mg/L, and the correlation coefficients were 0.9999 and 0.9998 for aspirin and salicylic acid respectively.

  7. Analysis of Reaction between α-Lipoic Acid and 2-Chloro-1-methylquinolinium Tetrafluoroborate Used as a Precolumn Derivatization Technique in Chromatographic Determination of α-Lipoic Acid

    Directory of Open Access Journals (Sweden)

    Magdalena Godlewska

    2015-01-01

    Full Text Available The present study offers results of analysis concerning the course of reaction between reduced α-lipoic acid (LA and 2-chloro-1-methylquinolinium tetrafluoroborate (CMQT. In water environments, the reaction between CMQT and hydrophilic thiols proceeds very rapidly and the resultant products are stable. For the described analysis, optimum reaction conditions, such as concentration of the reducing agent, environment pH, and concentration of the reagent were carefully selected. The spectrophotometric assay was carried out measuring absorbance at λ=348 nm (i.e., the spectral band of the obtained reaction product. Furthermore, the calibration curve of lipoic acid was registered. It was concluded that the Lambert-Beer law was observed within the range 1–10 μmol L−1. Later, the reaction between LA and CMQT was used as precolumn derivatization in a chromatographic determination of the lipoic acid in the range 2.5–50 μmol L−1. Practical applicability of the designed methods was evaluated by determining lipoic acid in Revitanerv pharmaceutical preparation which contains 300 mg LA in a single capsule. The error of the determination did not exceed 0.5% in relation to the declared value.

  8. [Quantitative determination of the main metabolites of acetylsalicylic acid/2nd communication: the concentrations of salicylic acid and its metabolites in patients with renal insufficiency (author's transl)].

    Science.gov (United States)

    Daneels, R; Loew, D; Pütter, J

    1975-07-01

    Quantitative Determination of the Main Metabolites of Acetylsalicylic Acid / 2nd Communication: The concentrations of salicylic acid and its metabolies in patients with renal insufficiency 9 patients suffering from renal insufficiencies of varing degrees and treated regularly by hemodialysis were given 1.5 g Colfarit (microcapsulated acetyl salicylic acid) as a single dose. The concentrations of salicylic acid (SA), salicyluric acid (SU), further salicylic acid conjugates (SAC) and salicyluric acid conjugates (SUC) were determined in the blood plasma. Likewise urea and creatinine were determined. SA concentration decreased continually and, at the end of the trial (72 h after application), had vanished almost completely from the plasma of most patients. SU increased at first and decreased afterwards. With the exception of the dailysis time SAC and SUC increased during the trial. After 3 days the SUC level was more than 50% of total salicylate (SSS) in most patients. SSS (the sum of SA + SU + SAC + SUC) did not change very much before dialysis, but showed a rather high decrease during the first hours of dialysis. tafter dialysis the SSS levels rose again, apparently as a consequence of a redistribution and of the synthesis of conjugates with decreased tissue affinity. It could be shown that SSS in the blood plasma does not parallel SSS in the whole body. The interindividual variation of SA metabolism as well as the variation of the biological blank values was rather high. The results are discussed with regard to salicylate pharmacokinetics in renal insufficiency and to normal salicylate metabolism.

  9. Determination of Fatty Acid in Asparagus by Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Zehra HAJRULAI-MUSLIU

    2016-05-01

    Full Text Available Asparagus contain a lot of macronutrients and micronutrients including folate, dietary fibre (soluble and insoluble and phenolic compounds. Also asparagus is a good source of unsaturated linoleic and linolenic fatty acids which are precursors for Eicosapentanoic acid (EPA and Docosahexanoic acid (DHA. Unsaturated fatty acids have important biological effects and they have important role in human health. The objective of this study was to analyze fatty acid composition of asparagus as a potential source of linoleic and linolenic acid - a precursor for EPA and DHA. For this reason we analyzed fifty seven samples of asparagus collected from the local market. We used AOAC 996.06 method and analyses were performed with gas chromatograph with flame-ionization detector (GC-FID. The highest concentration of fatty acid in the asparagus was linoleic acid (C18:2n6 which content in asparagus is 25.620±1.0%. Also, asparagus is good source of -linolenic fatty acid (C18:3n3 and content of this fatty acid in asparagus is 8.840±0.3%. The omega-6 to omega-3 (n6/n3 ratio in asparagus was 3.19. Polyunsaturated fatty acids (PUFAs were higher than monounsaturated fatty acids (MUFAs, and from saturated fatty acids, palmitic acid was most frequent with 24.324±1.0%. From our study we can conclude that asparagus is very good source of unsaturated fatty acids, especially linoleic and linolenic fatty acids.

  10. Simultaneous determination of oxalic, citric, nitrilotriacetic and ethylenediamenetetraacetic acids by gas liquid chromatography of their methyl esters

    International Nuclear Information System (INIS)

    Eskell, C.J.; Pick, M.E.

    1980-04-01

    A procedure for simultaneous determination of ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), citric acid and oxalic acid by gas liquid chromatography is described. The involatile acids are first concerted to their volatile methyl ester derivatives by reaction with boron trifluoride in methanol. Transition metal ions (Fe 3+ , Cr 3+ and Ni 2+ ) which will be present in decontamination liquors from nuclear reactors, and form strong chelates with the acids, have been shown to cause no interference to the esterification reaction. The esters were separated by temperature programming on a 3.5 metre capillary column packed with 3% OV1 on Diatomite CQ and were detected by flame ionisation. (author)

  11. A pre-anodized inlaying ultrathin carbon paste electrode for simultaneous determination of uric acid and folic acid

    International Nuclear Information System (INIS)

    Huo, Jing’e; Shangguan, Enbo; Li, Quanmin

    2013-01-01

    Graphical abstract: In 0.10 mol/L PBS (pH 6.00), oxidation reaction occurred at the PAIUCPE owing to uric acid (UA) loss electrons, while oxygen dissolved in the feed was reduced at the platinum electrode. Furthermore, the effect of electrode reaction at the platinum electrode on that of working electrode is detailedly discussed. Highlights: ► The simultaneous determination of UA and FA is achieved at the PAIUCPE. ► The effect of reaction at the Pt electrode on that of working electrode is discussed. ► The effect of pH on peak currents is detailedly explained for the first time. -- Abstract: A pre-anodized inlaying ultrathin carbon paste electrode (PAIUCPE) was prepared by electrochemical pretreatment. The scanning electron microscope (SEM) was applied to characterize the surface morphology of PAIUCPE and the performance of the electrode was characterized by cyclic voltammetry (CV). The results indicated that PAIUCPE displayed excellent electrocatalysis for the oxidation of uric acid (UA) and folic acid (FA). The separated extent between the two oxidation peaks of UA and FA was 324 mV, which was enough for the simultaneous detection. In 0.10 mol/L PBS (pH 6.00), the linear scan voltammetry (LSV) response of UA and FA increased linearly with the concentration in the range of 4.0 × 10 −6 –3.5 × 10 −4 mol/L and 3.0 × 10 −6 –2.0 × 10 −4 mol/L with the detection limits of 1.1 × 10 −7 mol/L and 1.5 × 10 −7 mol/L, respectively. It was successfully used to determine UA and FA in human urine simultaneously

  12. Spectrophotometric determination of tungsten with salicylic acid

    International Nuclear Information System (INIS)

    Goncalves, Z.C.

    1976-10-01

    The method comprises the complexation of tungsten with salicylic acid in concentrated sulphuric acid yielding a reddish color. The maximum absorbance of the complex lies within 410-420 nm, 420 nm being the chosen wavelenght. The final concentration of salicylic acid is 0,080 g/ml. The sensitivity is 0,13 μg W(%T) -1 ml -1 . Titanium, vanadium, rhenium, niobium and molybdenum interferes and must be separated, titanium being the strongest interferent. The separation procedures, advantages of the process, stoichiometric relations and equilibrium constant are discussed. (Author) [pt

  13. Determination of fruit characteristics, fatty acid profile and total antioxidant capacity of Mespilus germanica L. fruit

    Directory of Open Access Journals (Sweden)

    Hale Seçilmiş Canbay

    2015-11-01

    Full Text Available Objective: To determine fruit characteristics, fatty acid profile and total antioxidant capacitiy of first cultured Mespilus germanica L. Methods: A total of 15 fruits were taken randomly from four directions of adult trees. Then the physical and chemical properties of first cultured medlar fruit (Istanbul/Turkey were measured by using refractometer, colorimeter, spectrophotometer and gas chromatograph mass spectrometer, respectivly. Results: In the fruit studied, the results showed that palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid, arachidic acid and behenic acid were the most abundant fatty acids (FAs, and the main FA was palmitic acid [(35.35 ± 1.20%]. The percentage of linoleic acid and stearic acid in this fruit oil were (29.10 ± 1.70% and (8.53 ± 0.25%, respectively. As a result of the analysis, the total antioxidant capacity of medlar fruit was (1.1 ± 0.2 mmol trolox equivalents/L. Conclusions: The present study has demonstrated the concentrations of FAs and the antioxidantive capacity of first cultured Istanbul medlar fruits by using many tested methods. It is proved that in our daily life, medlar fruit plays a significant role with its nutrition and health effect.

  14. Determination of the titratable acidity and the pH of wine based on potentiometric flow injection analysis.

    Science.gov (United States)

    Vahl, Katja; Kahlert, Heike; von Mühlen, Lisandro; Albrecht, Anja; Meyer, Gabriele; Behnert, Jürgen

    2013-07-15

    A FIA system using a pH-sensitive detector based on a graphite/quinhydrone/silicone composite electrode was applied to determine sequentially the titratable acidity and the pH of wine, as well as the sum of calcium and magnesium ions. For all measurements the same FIA configuration was used employing different carrier solutions. The results for the determination of acidity and pH are in good agreement with those obtained by classical potentiometric titrations and by pH measurements using a conventional glass electrode. The standard deviation was less than 1.5% for both kinds of measurements and the sample volume was 150 μL. The method allows about 40 determinations of titratable acidity per hour and 30 pH measurements per hour. The titration method can be adjusted to the legal requirements in USA and Europe. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Voltammetric determination of carbidopa and folic acid using a modified carbon nanotubes paste electrode

    Directory of Open Access Journals (Sweden)

    Keshtkar Nasrin

    2015-01-01

    Full Text Available A novel electrochemical sensor for the selective and sensitive detection of carbidopa in presence of large excess of folic acid at physiological pH was developed by the bulk modification of carbon paste electrode (CPE with carbon nanotubes (CNTs and vinylferrocene. Large peak separation, good sensitivity and stability allow this modified electrode to analyze carbidopa individually and simultaneously along with folic acid. Applying square wave voltammetry (SWV, a linear dynamic range of 1.0×10-6- 7.0×10-4 M with detection limit of 2.0×10-7 M was obtained for carbidopa. Finally, the proposed method was applied to the determination of carbidopa and folic acid in urine sample.

  16. An acridinium sulphonylamide as a new chemiluminescent label for the determination of carboxylic acids in liquid chromatography

    NARCIS (Netherlands)

    Steijger, O.M.; Kamminga, D.A.; Lingeman, H.; Brinkman, U.A.T.

    1998-01-01

    The synthesis of a new acridinium sulphonylamide label for the liquid chromatographic determination of carboxylic acids is described. The label 10-methyl-N-(p-tolyl)-N-(p-iodoacetamidobenzenesulphonyl)-9-acridinium carboxamide iodide is synthesized from 9-acridinecarboxylic acid by a seven-step

  17. Determination of true digestible amino acids of feedstuffs utilizing cecectomized roosters

    Directory of Open Access Journals (Sweden)

    Eliane Aparecida da Silva

    2012-09-01

    Full Text Available The objective of this study was to estimate the true digestibility coefficients of amino acids and digestible amino acid values of some poultry feedstuffs. The feedstuffs were: babassu meal, sunflower meal, corn gluten meal, babassu starchy meal, meat and bone meal, common beans, pearl millet and residues of cookies, pasta and bread. The precise feeding method of Sibbald was used with adult cecectomized Leghorn roosters distributed in a completely randomized design, consisting of ten treatments and six replications with a rooster in each. The treatments were represented by the feedstuffs evaluated. The roosters were kept in a period of fasting for 36 hours and then fed 30 grams of feed. Samples were collected during 56 hours. Simultaneously, six roosters were kept fasting to make corrections to the metabolic and endogenous losses of amino acids. At the end of collections, the excreta obtained were weighed, freeze-dried and subsequently processed, so laboratory analyses were carried out and the coefficients of true digestibility of amino acids were determined. The mean values of the coefficients of true digestibility of essential and non-essential amino acids in percentage were respectively: 0.702 and 0.652 for the babassu meal; 0.852 and 0.786 for the sunflower meal; 0.928 and 0.887 for the corn gluten meal; 0.797 and 0.720 for the meat and bone meal; 0.364 and 0.339 for ground raw beans; 0.924 and 0.837 for ground pearl millet; 0.839 and 0.810 for cookie residue; 0.929 and 0.914 for pasta residue; and 0.904 and 0.899 for bread residue.

  18. Direct determination of fatty acids in fish tissues: quantifying top predator trophic connections.

    Science.gov (United States)

    Parrish, Christopher C; Nichols, Peter D; Pethybridge, Heidi; Young, Jock W

    2015-01-01

    Fatty acids are a valuable tool in ecological studies because of the large number of unique structures synthesized. They provide versatile signatures that are being increasingly employed to delineate the transfer of dietary material through marine and terrestrial food webs. The standard procedure for determining fatty acids generally involves lipid extraction followed by methanolysis to produce methyl esters for analysis by gas chromatography. By directly transmethylating ~50 mg wet samples and adding an internal standard it was possible to greatly simplify the analytical methodology to enable rapid throughput of 20-40 fish tissue fatty acid analyses a day including instrumental analysis. This method was verified against the more traditional lipid methods using albacore tuna and great white shark muscle and liver samples, and it was shown to provide an estimate of sample dry mass, total lipid content, and a condition index. When large fatty acid data sets are generated in this way, multidimensional scaling, analysis of similarities, and similarity of percentages analysis can be used to define trophic connections among samples and to quantify them. These routines were used on albacore and skipjack tuna fatty acid data obtained by direct methylation coupled with literature values for krill. There were clear differences in fatty acid profiles among the species as well as spatial differences among albacore tuna sampled from different locations.

  19. Spectrophotometric determination of boron by solvent extraction with 2-hydroxy-2-methylbutyric acid and malachite green

    International Nuclear Information System (INIS)

    Sato, Shigeya; Uchikawa, Sumio

    1984-01-01

    A very simple and sensitive method for the spectrophotometric determination of boron was developed. Boron was found to react with 2-hydroxy-2-methylbutyric acid in weak acidic aqueous solution at room temperature to form a complex anion which can be extracted into chlorobenzene with malachite green in a single extraction; boron is determined indirectly by measuring the absorbance of malachite green in the extract at 629 nm. The calibration graph is linear over the range (7.50 x 10 -7 - 2.00 x 10 -5 ) mol dm -3 boron; the apparent molar absorptivity is 6.50 x 10 4 dm 3 mol -1 cm -1 . The method is applied to the determination of micro amounts of boron in natural waters with satisfactory results. (author)

  20. Determination of Some Physicochemical Properties, Fatty Acid Composition and Antioxidant Capacity, of Organic and Conventional Milk in Turkey Produced

    Directory of Open Access Journals (Sweden)

    Bayram Ürkek

    2018-04-01

    Full Text Available In this study, determination of effect of production systems (conventional and organic and time of milk collection on some physicochemical properties, fatty acids and antioxidant capacity of conventional and organic raw milk in produced Turkey were aimed. In this research, the milk samples was collected from nine conventional farms and nine organic farms at bimonthly years for one year. Fatty acid composition, antioxidant capacity, total phenolic matter, dry matter, fat, protein, ash, titratable acidity (lactic acid % and pH values of organic and conventional milk were investigated. According to results of this research, the mean values of conventional and organic milk samples respectively for dry matter, fat, protein, ash, specific gravity, acidity and pH was determined as 12.06-11.97%, 3.67-3.50%, 3.33-3.34%, 0.67-0.66%, 1.0381-1.0381 g mL-1, 0.18-0.16% and 6.67-6.73, respectively. Conjugated linoliec acid proportions changed between 1.39% and 2.87% in organic milk, between 1.67% and 2.96% in conventional milk. Consequently, the farm production type did not have effects on the milk compassion (dry matter, fat, protein and ash, fatty acid composition, EC50 and total phenolic compounds. On the other hand, the significant variations in the fat, protein, fatty acid proportions, EC50, inhibition and total phenolic compound values were determined as regarding time of milk collection.

  1. Electrochemical Preparation of a Molecularly Imprinted Polypyrrole-modified Pencil Graphite Electrode for Determination of Ascorbic Acid

    Directory of Open Access Journals (Sweden)

    Yücel Sahin

    2008-09-01

    Full Text Available A molecularly imprinted polymer (MIP polypyrrole (PPy-based film was fabricated for the determination of ascorbic acid. The film was prepared by incorporation of a template molecule (ascorbic acid during the electropolymerization of pyrrole onto a pencil graphite electrode (PGE in aqueous solution using a cyclic voltammetry method. The performance of the imprinted and non-imprinted (NIP films was evaluated by differential pulse voltammetry (DPV. The effect of pH, monomer and template concentrations, electropolymerization cycles and interferents on the performance of the MIP electrode was investigated and optimized. The molecularly imprinted film exhibited a high selectivity and sensitivity toward ascorbic acid. The DPV peak current showed a linear dependence on the ascorbic acid concentration and a linear calibration curve was obtained in the range of 0.25 to 7.0 mM of ascorbic acid with a correlation coefficient of 0.9946. The detection limit (3σ was determined as 7.4x10-5 M (S/N=3. The molecularly-imprinted polypyrrole-modified pencil graphite electrode showed a stable and reproducible response, without any influence of interferents commonly existing in pharmaceutical samples. The proposed method is simple and quick. The PPy electrodes have a low response time, good mechanical stability and are disposable simple to construct.

  2. Electrochemical Sensor for Determination of Ascorbic Acid Using a 2-Chlorobenzoyl Ferrocene/Carbon Nanotube Paste Electrode

    Directory of Open Access Journals (Sweden)

    Sayed Zia Mohammadi

    2016-12-01

    Full Text Available A chemically modified carbon paste electrode with 2-chlorobenzoyl ferrocene (2CBF and carbon nanotube (2CBFCNPE was employed to study the electrocatalytic oxidation of ascorbic acid in aqueous solution using cyclic voltammetry, square wave voltammetry and chronoamperometry. The diffusion coefficient (D = 1.42 × 10-6 cm2 s-1, and the kinetic parameter such as the catalytic rate constant (k = 3.7 × 10 3 M-1 s-1 of ascorbic acid oxidation at the surface of 2CBFCNPE were determined using electrochemical approaches. It has been found that under an optimum condition (pH 4.0, the oxidation of ascorbic acid at the surface of such an electrode occurs at a potential about 85 mV less positive than that of an unmodified carbon paste electrode. Applying square wave voltammetry, in phosphate buffer solution (PBS of pH 4.0, the oxidation current increases linearly with two concentration intervals of ascorbic acid, one is 1.0 × 10-7-2.5 × 10-6 M and the other is 2.5 × 10-6-7.0 × 10-5 M. Detection limit (3δ was obtained 64.0 nM. This method was also examined for determination of ascorbic acid in some real samples.

  3. Determination of Antioxidant, Anticholinesterase, Tyrosinase Inhibitory Activities and Fatty Acid Profiles of 10 Anatolian Klasea Cass. Species

    Directory of Open Access Journals (Sweden)

    Gülsen Tel

    2016-01-01

    Full Text Available In search of new natural fatty acid sources, extract of 10 different Turkish Klasea species were studies. Fatty acids of Klasea species were studied by GC and GC-MSD. Oleic acid (4.8-45.8%, palmitic acid (15.6-51.8%, linoleic acid (0.3-45.5%, palmitoleic acid (0.8-28.4% and linolenic acid (15.6-34.6% were the main fatty acids elucidated. All extracts were also subjected to acetylcholinesterase, butyrylcholinesterase, tyrosinase, β-carotene-linoleic acid, DPPH • scavenging, CUPRAC and ferrous ion-chelating ability activities. Total flavonoid and phenolic contents were determined as quercetin and pyrocatechol equivalents. All extracts showed significant antioxidant activity in all tests, except hexane extracts of K. serratuloides and K. cerinthifolia that showed weak inhibition against BChE and AChE. The hexane extract of K. coriaceae and methanol extract of K. serratuloides exhibited notable tyrosinase inhibitory activity.

  4. Thermal expansion coefficient determination of polylactic acid using digital image correlation

    Directory of Open Access Journals (Sweden)

    Botean Adrian - Ioan

    2018-01-01

    Full Text Available This paper aims determining the linear thermal expansion coefficient (CTE of polylactic acid (PLA using an optical method for measuring deformations called digital image correlation method (DIC. Because PLA is often used in making many pieces with 3D printing technology, it is opportune to know this coefficient to obtain a higher degree of precision in the construction of parts and to monitor deformations when these parts are subjected to a thermal gradient. Are used two PLA discs with 20 and 40% degree of filling. In parallel with this approach was determined the linear thermal expansion coefficient (CTE for the copper cylinder on the surface of which are placed the two discs of PLA.

  5. Thermal expansion coefficient determination of polylactic acid using digital image correlation

    Science.gov (United States)

    Botean, Adrian-Ioan

    2018-02-01

    This paper aims determining the linear thermal expansion coefficient (CTE) of polylactic acid (PLA) using an optical method for measuring deformations called digital image correlation method (DIC). Because PLA is often used in making many pieces with 3D printing technology, it is opportune to know this coefficient to obtain a higher degree of precision in the construction of parts and to monitor deformations when these parts are subjected to a thermal gradient. Are used two PLA discs with 20 and 40% degree of filling. In parallel with this approach was determined the linear thermal expansion coefficient (CTE) for the copper cylinder on the surface of which are placed the two discs of PLA.

  6. Determination of branched chain amino acids, methionine, phenylalanine, tyrosine and alpha-keto acids in plasma and dried blood samples using HPLC with fluorescence detection.

    Science.gov (United States)

    Kand'ár, Roman; Záková, Pavla; Jirosová, Jana; Sladká, Michaela

    2009-01-01

    The determination of branched chain amino acids [BCAA; valine (Val), leucine (Leu), isoleucine (Ile)], alpha-keto acids derived from BCAA [BCKA; alpha-ketoisovaleric acid (KIV), alpha-ketoisocaproic acid (KIC), alpha-ketomethylvaleric acid (KMV)], methionine (Met), phenylalanine (Phe) and tyrosine (Tyr) is currently the most reliable approach for the diagnosis of maple syrup urine disease (MSUD), hypermethioninemia, phenylketonuria (PKU) and tyrosinemia. The aim of this study was to develop rapid and simple HPLC methods for measurement of BCAA, Met, Phe, Tyr and BCKA in plasma and dried blood samples. Samples of peripheral venous blood with EDTA as anticoagulant were obtained from a group of healthy blood donors (n=70, 35 females, 27-41 years of age and 35 males, 28-43 years of age). Blood-spot samples from a group of newborns (n=80, 40 girls and 40 boys 3-5 days of age) were collected onto #903 Specimen Collection Paper and allowed to dry for at least 24 h before analysis. Prior to separation, the amino acids (AA) were derivatized with o-phthaldialdehyde (OPA) and BCKA with o-phenylenediamine (OPD). Reverse phase column chromatography (LiChroCart 125-4 Purospher RP-18e, 5 microm) was used for separation and fluorescence detection used to monitoring of effluent. For AA analysis, 25 mmol/L sodium hydrogenphosphate-methanol (90:10, v/v), pH 6.5+/-0.1 was used as mobile phase A and 100% methanol was used as mobile phase B. Measurement of BCKA used a mixture of methanol and deionized water (55:45, v/v) as mobile phase A and mobile phase B consisted of 100% methanol. Analytical performance of these methods was satisfactory for the determination of all AA and BCKA. The intra-assay and inter-assay coefficients of variation were below 10% and recovery ranged from 90%-110%. We have developed simple, rapid and selective HPLC methods with fluorescence detection for the determination of BCAA, Met, Phe, Tyr and BCKA in plasma and dried blood samples.

  7. Study of free acidity determinations in aqueous solution; Etude des dosages d'acidite libre en solution aqueuse

    Energy Technology Data Exchange (ETDEWEB)

    Kergreis, A [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1966-04-01

    The object of this work is the study of the principal methods which can be applied to the measurement of 'free' acidity. In the first part, we define the various types of acidity which can exist in aqueous solution; then, after having studied some hydrolysis reactions, we compare the value of the neutralisation pH of the hydrated cation and that of the precipitation of the hydroxide. In the second part we have started to study the determination of the acidity of an aqueous solution. After having rapidly considered the 'total' acidity determination, we deal with the problem of the 'free' acidity titration. We have considered in particular certain methods: extrapolation of the equivalent point, colorimetric titrations with or without a complexing agent, and finally the use of ion-exchange resins with mixed aqueous and solvent solutions. (author) [French] Le but de ce travail est l'etude des principales methodes de determination de l'acidite 'libre'. Dans une premiere partie nous avons defini les differentes sortes d'acidites pouvant exister en solution aqueuse, puis apres avoir etudie quelques reactions d'hydrolyse, nous avons compare la valeur de pH de neutralisation du cation hydrate et celle de precipitation de l'hydroxyde. Dans la seconde partie nous avons aborde l'etuce des dosages de l'acidite d'une solution aqueuse. Apres avoir envisage assez rapidement la determination de l'acidite 'totale', nous traitons du probleme du titrage de l'acidite 'libre'. Nous avons porte notre attention sur certaines methodes: extrapolation du point equivalent, titrimetrie colorimetrique avec ou sans complexant, et enfin utilisation des resines echangeuses d'ions en milieu aqueux et solvant mixte.

  8. Potentiometric determination of acid dissociation constants (pKa) for human and veterinary antibiotics.

    Science.gov (United States)

    Qiang, Zhimin; Adams, Craig

    2004-07-01

    This work determined the acid dissociation constants (pKa) of 26 common human and veterinary antibiotics by potentiometric titration. Selected antibiotics consisted of sulfonamides, macrolides, tetracyclines, fluoroquinolones, and other miscellaneous antibiotics. After validation of analysis methods using phosphoric acid as a model compound, a second-derivative (delta2pH/deltaV2) method was primarily applied to determining pKa's from titration curves for most antibiotics due to its convenience and accuracy. For tetracyclines, however, a least-square non-linear regression method was developed to determine their pKa's because the second-derivative method cannot well distinguish the pKa,2 and pKa,3 of tetracyclines. Results indicate that the pKa values are approximately 2 and 5-7.5 for sulfonamides; 7.5-9 for macrolides; 3-4, 7-8 and 9-10 for tetracyclines; 3-4, 6, 7.5-9 and 10-11 for fluoroquinolones; while compound-specific for other miscellaneous antibiotics. The moieties corresponding to specific pKa's were identified based on chemical structures of antibiotics. In addition, the pKa's available in literature determined by various techniques are compiled in comparison with the values of this work. These results are expected to essentially facilitate the research on occurrence, fate and effects, analysis methods development, and control of antibiotics in various treatment operations.

  9. Simple Method to Determine the Partition Coefficient of Naphthenic Acid in Oil/Water

    DEFF Research Database (Denmark)

    Bitsch-Larsen, Anders; Andersen, Simon Ivar

    2008-01-01

    The partition coefficient for technical grade naphthenic acid in water/n-decane at 295 K has been determined (K-wo = 2.1 center dot 10(-4)) using a simple experimental technique with large extraction volumes (0.09 m(3) of water). Furthermore, nonequilibrium values at different pH values...

  10. Potentiometric determination of free nitric-acid in trilaurylamine solutions containing plutonium nitrate

    International Nuclear Information System (INIS)

    Perez, J.J.; Saey, J.C.

    1965-01-01

    A potentiometric method of determination of the free nitric acid in trilaurylamine solutions containing plutonium or thorium nitrates is described. The potentiometric titration is carried out in a mixture of benzene and 1,2-dichloro ethane with a standard solution of trilaurylamine as the titrant. When thorium nitrate is present the metal complex is not dissociated then the titration has a single end-point. In the case of plutonium nitrate the partial dissociation of the plutonium complex corresponds to a second point. The experimental error in duplicate analyses of 50 samples is about 1 per cent for free acid concentrations in the range of 0,03 to 0,1 N and plutonium concentrations between 1 to 5 g/l. (authors) [fr

  11. Flameless atomic absorption determination of noble metals after extraction by mixture of di-2-ethylhexyldithiophosphoric acid and n-octylaniline

    International Nuclear Information System (INIS)

    Yukhin, Yu.M.; Udalova, T.A.; Tsimbalist, V.G.; AN SSSR, Novosibirsk. Inst. Geologii i Geofiziki)

    1985-01-01

    A possibility of using the mixture of di-2-ethylhexyl dithiophosphoric acid (D2EHDTPA) and p-octylaniline (OA) (extractants of acid and basic character) for extraction atomic absorption determination of noble metals is studied. The mixture of D2EHDTPA with OA is shown to extract noble metals from hydrochloric acid solutions with distribution factors > 10 3 . An extraction atomic absorption method for determination of noble metals in copperbearing materials is suggested. The minimum determined contents of noble metals at the initial sample equal to 100 for gold, silver, platinum, palladium, rhodium and ruthenium make up (g/t) 0.0005, 0.0001, 0.015, 0.005, 0.002 and 0.015 respectively. Relative standard deviation constitutes Ssub(r)<0.2

  12. Disposable biosensor based on cathodic electrochemiluminescence of tris(2,2-bipyridine)ruthenium(II) for uric acid determination

    International Nuclear Information System (INIS)

    Ballesta-Claver, J.; Rodríguez-Gómez, R.; Capitán-Vallvey, L.F.

    2013-01-01

    Highlights: ► Cathodic ECL offers conventional and non-aggressive analysis conditions. ► The ECL hydrogen peroxide/ruthenium complex system for uric acid determination is novel. ► The ruthenium complex is electrochemically immobilized on graphite screen-printed electrodes. ► The quantification of the uric acid is based on a Stern–Volmer type equation. ► The use of the cathodic ECL working methodology reduces interferences during analysis. -- Abstract: A new method for uric acid (UA) determination based on the quenching of the cathodic ECL of the tris(2,2-bipyridine)ruthenium(II)–uricase system is described. The biosensor is based on a double-layer design containing first tris(2,2-bipyridine)ruthenium(II) (Ru(bpy) 3 2+ ) electrochemically immobilized on graphite screen-printed cells and uricase in chitosan as a second layer. The uric acid biosensing is based on the ECL quenching produced by uric acid over the cathodic ECL caused by immobilized Ru(bpy) 3 2+ in the presence of uricase. The use of a −1.1 V pulse for 1 s with a dwelling time of 10 s makes it possible to estimate the initial enzymatic rate, which is used as the analytical signal. The Stern–Volmer type calibration function shows a dynamic range from 1.0 × 10 −5 to 1.0 × 10 −3 M with a limit of detection of 3.1 × 10 −6 M and an accuracy of 13.6% (1.0 × 10 −4 M, n = 5) as relative standard deviation. Satisfactory results were obtained for urine samples, creating an affordable alternative for uric acid determination

  13. Spectrophotometric determination of boron by solvent extraction with 2-hydroxy-2-methylbutyric acid and malachite green

    Energy Technology Data Exchange (ETDEWEB)

    Sato, Shigeya; Uchikawa, Sumio [Kumamoto Univ. (Japan). Faculty of Education

    1984-03-01

    A very simple and sensitive method for the spectrophotometric determination of boron was developed. Boron was found to react with 2-hydroxy-2-methylbutyric acid in weak acidic aqueous solution at room temperature to form a complex anion which can be extracted into chlorobenzene with malachite green in a single extraction; boron is determined indirectly by measuring the absorbance of malachite green in the extract at 629 nm. The calibration graph is linear over the range (7.50 x 10/sup -7/ - 2.00 x 10/sup -5/) mol dm/sup -3/ boron; the apparent molar absorptivity is 6.50 x 10/sup 4/ dm/sup 3/ mol/sup -1/ cm/sup -1/. The method is applied to the determination of micro amounts of boron in natural waters with satisfactory results.

  14. [Determination of triterpenoic acids in fruits of Ziziphus jujuba using HPLC-MS with polymeric ODS column].

    Science.gov (United States)

    Zhang, Yong; Zhou, An; Xie, Xiao-Mei

    2013-03-01

    A simple and sensitive method has been developed to simultaneously determine betunilic acid, oleanolic acid and ursolic acid in the fruits of Ziziphus jujuba from different regions by HPLC-MS. This HPLC assay was performed on PAH polymeric C18 bonded stationary phase column with mobile phase contained acetonitrile-water (90: 10) and with negative ESI detection mode. The developed approach was characterized by short time consumption for chromatographic separation, high sensitivity and good reliability so as to meet the requirements for rapid analysis of large-batch fruits of Z. jujuba from different habitats.

  15. [Determination of ferulic acid absorbed into human serum from oral decoction of rhizoma chuanxiong and pharmacokinetic study of ferulic acid].

    Science.gov (United States)

    Sun, S; Huang, X; Zhang, L; Ren, P; Chang, Z

    2001-10-01

    To improve the HPLC method for determining ferulic acid(FA) in the human serum and to research FA clinical pharmacokinetics. Serum concentrations of FA were determined by HPLC using methanol-water-acetic acid (40:59.7:0.3, v/v) as the mobile phase and the column packed with ODS (150 mm x 4.6 mm, 5 microns) as a fixed phase and the flow rate was 1.0 ml/min. FA was detected at 320 nm wave length. The internal standard was coumarin. The serum samples were treated by the water-boiling method. Peak of FA in serum was recognized by photodiode-array detection. FA and internal standard were separated completely under the condition described as above. FA was linear in the range of (40.16-8032 ng/ml) (r = 0.9975). The CV was less than 10%, the average recovery was 100.3%, and the limit concentration in serum was 25.1 ng/ml. PK was in accordance with open bicameral model. This method can be applied to clinical pharmacokinetic study of FA.

  16. Employing natural reagents from turmeric and lime for acetic acid determination in vinegar sample.

    Science.gov (United States)

    Supharoek, Sam-Ang; Ponhong, Kraingkrai; Siriangkhawut, Watsaka; Grudpan, Kate

    2018-04-01

    A simple, rapid and environmentally friendly sequential injection analysis system employing natural extract reagents was developed for the determination of acetic acid following an acid-base reaction in the presence of an indicator. Powdered lime and turmeric were utilized as the natural base and indicator, respectively. Mixing lime and turmeric produced an orange to reddish-brown color solution which absorbed the maximum wavelength at 455 nm, with absorbance decreasing with increasing acetic acid concentration. Influential parameters including lime and turmeric concentrations, reagent and sample aspirated volumes, mixing coil length and dispensing flow rate were investigated and optimized. A standard calibration graph was plotted for 0-5.0 mmol/L acetic acid with r 2  = 0.9925. Relative standard deviations (RSD) at 2.0 and 4.0 mmol/L acetic acid were less than 3% (n = 7), with limit of detection (LOD) and limit of quantification (LOQ) at 0.12 and 0.24 mmol/L, respectively. The method was successfully applied to assay acetic acid concentration in cooking vinegar samples. Results achieved were not significantly different from those obtained following a batchwise standard AOAC titration method. Copyright © 2017. Published by Elsevier B.V.

  17. Employing natural reagents from turmeric and lime for acetic acid determination in vinegar sample

    Directory of Open Access Journals (Sweden)

    Sam-ang Supharoek

    2018-04-01

    Full Text Available A simple, rapid and environmentally friendly sequential injection analysis system employing natural extract reagents was developed for the determination of acetic acid following an acid–base reaction in the presence of an indicator. Powdered lime and turmeric were utilized as the natural base and indicator, respectively. Mixing lime and turmeric produced an orange to reddish-brown color solution which absorbed the maximum wavelength at 455 nm, with absorbance decreasing with increasing acetic acid concentration. Influential parameters including lime and turmeric concentrations, reagent and sample aspirated volumes, mixing coil length and dispensing flow rate were investigated and optimized. A standard calibration graph was plotted for 0–5.0 mmol/L acetic acid with r2 = 0.9925. Relative standard deviations (RSD at 2.0 and 4.0 mmol/L acetic acid were less than 3% (n = 7, with limit of detection (LOD and limit of quantification (LOQ at 0.12 and 0.24 mmol/L, respectively. The method was successfully applied to assay acetic acid concentration in cooking vinegar samples. Results achieved were not significantly different from those obtained following a batchwise standard AOAC titration method. Keywords: Acetic acid assay, Natural reagent, Turmeric, Lime, Sequential injection analysis

  18. Determination of americium and curium using ion-exchange in the nitric-acid-methanol medium for environmental analysis

    International Nuclear Information System (INIS)

    Holm, E.; Fukai, R.

    1976-01-01

    While transplutonic elements are only slightly sorbed to anion exchangers from hydrochloric or nitric acid media, the presence of alcohol enhances the anionic exchange of these elements, especially in nitric and sulfuric solutions. In the present work a method has been developed for determining americium and curium in environmental samples, on the basis of the difference between the sorption characteristics to anion exchangers in the acid-methanol system of these transplutonic elements and those of plutonium, polonium and thorium. The method also permits us to perform sequential determination of plutonium, when necessary

  19. Gas Chromatographic Determination of Fatty Acids in Oils with Regard to the Assessment of Fire Hazard

    Science.gov (United States)

    Bartošová, Alica; Štefko, Tomáš

    2017-06-01

    The aim of the paper was to study and research the application of processing gas chromatographic method for the rapid and accurate determination of the composition of different types of oils, such as substances with the possibility of an adverse event spontaneous combustion or self-heating. Tendency to spontaneous combustion is chemically characterized mainly by the amount of unsaturated fatty acids, which have one or more double bonds in their molecule. Vegetable oils essentially consist of the following fatty acids: palmitic, stearic, oleic, linoleic, and linoleic. For the needs of assessment, the fire hazard must be known, in which the double bond is present, as well as their number in a molecule. As an analytical method, GCMS was used for determination of oils content. Three types of oil were used - rapeseed, sunflower, and coconut oil. Owing to the occurrence of linoleic acid C18:2 (49.8 wt.%) and oleic acid C18:1 (43.3 wt.%) with double bonds, sunflower oil is the most prone to self-heating. The coconut and rapeseed oils contain double bond FAME in lesser amount, and their propensity to self-heating is relatively low.

  20. Comparison of methods for the determination of reduced inorganic sulphur in acid sulphate soils

    International Nuclear Information System (INIS)

    Santomartino, S.L.

    1999-01-01

    Full text: The management of acid sulphate soils requires analytical methods that provide accurate data on the quantity of reduced inorganic sulphur within a soil, as it is this fraction that produces acid upon oxidation. This study uses sulphidic Coode Island Silt samples to compare common analytical methods including POCAS (Peroxide Oxidation-Combined Acidity and Sulphate) which consists of TSA (Total Sulphidic Acidity), S pos (Peroxide Oxidisable Sulphur), TOS (Total Oxidisable Sulphur) and chromium-reducible sulphur. The determination of total sulphur by Leco sulphur is strongly correlated with, but slightly less than, that analysed by XRF. Comparison of soil sulphide content by chromium-reducible sulphur, TSA and TOS methods indicates that TOS values are substantially higher than both other methods. The problem with the TOS method lies in the sulphate extraction procedure. Hot distilled water and HCI are commonly used as extractants, however hot distilled water fails to remove organic sulphur, thereby overestimating the sulphide content of the soil. Leco carbon analyses verify that a substantial proportion of organic matter exists within the samples. The HCI extraction process, which uses Ion Chromatography to analyse for sulphate, produces highly inaccurate results due to the interference of the sulphate peak by the chloride peak during analysis. An alternative method involving HCI extraction and XRF analysis of the soil residue is currently being undertaken. The use of KCI to extract sulphate generally produces values similar to the hot distilled water method. The sulphidic content measured by TSA is strongly correlated with, but slightly higher than that determined by the chromium-reducible sulphur method. This is attributed to the use of hydrogen peroxide in the TSA method, which oxidises organic matter to organic acids in addition to oxidising sulphides. These preliminary findings indicate that the chromium-reducible sulphur method is the most suitable

  1. Apparent formation constants of Pu(IV) and Th(IV) with humic acids determined by solvent extraction method

    Energy Technology Data Exchange (ETDEWEB)

    Sasaki, T.; Aoyama, S.; Yoshida, H.; Kobayashi, T.; Takagi, I. [Tokyo Univ. (Japan). Dept. of Nuclear Engineering; Kulyako, Y.; Samsonov, M.; Miyasoedov, B. [Russian Academy of Sciences, Moscow (Russian Federation). V. I. Vernadsky Institute of Geochemistry and Analytical Chemistry (GEOKHI); Moriyama, H. [Kyoto Univ. (Japan). Research Reactor Inst.

    2012-07-01

    Apparent formation constants of Pu(IV) and Th(IV) with two kinds of humic acids were determined in 0.1 M NaClO{sub 4} at 25 C using a solvent extraction method with thenoyltrifluoroacetone in xylene. The acid dissociation constants of humic acids were also measured by potentiometric titration and used as the degree of dissociation for calculating the formation constants. The effect of solution conditions, such as the pH, the initial metal and humic acid concentrations, and the ionic strength, on the formation constants was examined. The obtained data were compared with the ones in the literature. (orig.)

  2. Comparison of amino acid digestibility of feedstuffs determined with the precision-fed cecectomized rooster assay and the standardized ileal amino acid digestibility assay.

    Science.gov (United States)

    Kim, E J; Utterback, P L; Applegate, T J; Parsons, C M

    2011-11-01

    The objective of this study was to evaluate and compare amino acid digestibility of several feedstuffs using 2 commonly accepted methods: the precision-fed cecectomized rooster assay (PFR) and the standardized ileal amino acid assay (SIAAD). Six corn, 6 corn distillers dried grains with or without solubles (DDGS/DDG), one wet distillers grains, one condensed solubles, 2 meat and bone meal (MBM) and a poultry byproduct meal were evaluated. Due to insufficient amounts, the wet distillers grains and condensed solubles were only evaluated in roosters. Standardized amino acid digestibility varied among the feed ingredients and among samples of the same ingredient for both methods. For corn, there were generally no differences in amino acid digestibility between the 2 methods. When differences did occur, there was no consistent pattern among the individual amino acids and methods. Standardized amino acid digestibility was not different between the 2 methods for 4 of the DDG samples; however, the PFR yielded higher digestibility values for a high protein DDG and a conventionally processed DDGS. The PFR yielded higher amino acid digestibility values than the SIAAD for several amino acids in 1 MBM and the poultry byproduct meal, but it yielded lower digestibility values for the other MBM. Overall, there were no consistent differences between methods for amino acid digestibility values. In conclusion, the PFR and SIAAD methods are acceptable for determining amino acid digestibility. However, these procedures do not always yield similar results for all feedstuffs evaluated. Thus, further studies are needed to understand the underlying causes in this variability.

  3. Determination of 35S-aminoacyl-transfer ribonucleic acid specific radioactivity in small tissue samples

    International Nuclear Information System (INIS)

    Samarel, A.M.; Ogunro, E.A.; Ferguson, A.G.; Lesch, M.

    1981-01-01

    Rate determination of protein synthesis utilizing tracer amino acid incorporation requires accurate assessment of the specific radioactivity of the labeled precursor aminoacyl-tRNA pool. Previously published methods presumably useful for the measurement of any aminoacyl-tRNA were unsuccessful when applied to [ 35 S]methionine, due to the unique chemical properties of this amino acid. Herein we describe modifications of these methods necessary for the measurement of 35 S-aminoacyl-tRNA specific radioactivity from small tissue samples incubated in the presence of [ 35 S]methionine. The use of [ 35 S]methionine of high specific radioactivity enables analysis of the methionyl-tRNA from less than 100 mg of tissue. Conditions for optimal recovery of 35 S-labeled dansyl-amino acid derivatives are presented and possible applications of this method are discussed

  4. Simultaneous determination of ochratoxin A, mycophenolic acid and fumonisin B-2 in meat products

    DEFF Research Database (Denmark)

    Sørensen, Louise Marie; Mogensen, Jesper; Nielsen, Kristian Fog

    2010-01-01

    Here we present a method for simultaneous determination of the fungal metabolites mycophenolic acid, ochratoxin A (OTA) and fumonisin B-2 (FB2) in meat products. Extraction was performed with water-acetonitrile, followed by acetone-induced precipitation of salts and proteins. Purification...

  5. Silver nanoparticles plasmon resonance-based method for the determination of uric acid in human plasma and urine samples

    International Nuclear Information System (INIS)

    Amjadi, M.; Rahimpour, E.

    2012-01-01

    We have developed a simple and sensitive colorimetric procedure for the quantification of trace amounts of uric acid. It is based on the finding that uric acid in a medium containing ammonia and sodium hydroxide at 65 0 C can reduce silver ions to form yellow silver nanoparticles (Ag NPs). These are stabilized in solution by using poly(vinyl alcohol) as a capping agent. The yellow color of the solution that results from the localized surface plasmon resonance of Ag NPs can be observed by the bare eye. The absorbance at 415 nm is proportional to the concentration of uric acid which therefore can be determined quantitatively. The calibration curve is linear in the concentration range from 10 to 200 nM, with a limit of detection of 3.3 nM. The method was successfully applied to the determination of uric acid in human plasma and urine samples. (author)

  6. Determination of the total acidity in soft drinks using potentiometric sequential injection titration.

    Science.gov (United States)

    van Staden, J Koos F; Mashamba, M Mulalo G; Stefan, R Raluca I

    2002-12-06

    A potentiometric SI titration system for the determination of total acidity in soft drinks is proposed. The concept is based on the aspiration of the acid soft drink sample between two base zones into a holding coil with the volume of the first base zone twice to that of the second one and channelled by flow reversal through a reaction coil to a potentiometric sensor. A solution of 0.1 mol l(-1) sodium chloride is used as ionic strength adjustment buffer in the carrier stream. The system has been applied to the analysis of some South African soft drinks having a total acidity level of about 0.2-0.3% (w/v). The method has a sample frequency of 45 samples per h with a linear range of 0.1 and 0.6% (w/v). It is easy to use, fully computerised, and gives the results that are comparable to both automated batch titration and manual titration.

  7. An Exact Method to Determine the Conductivity of Aqueous Solutions in Acid-Base Titrations

    Directory of Open Access Journals (Sweden)

    Norma Rodríguez-Laguna

    2015-01-01

    Full Text Available Several works in the literature show that it is possible to establish the analytic equations to estimate the volume V of a strong base or a strong acid (Vb and Va, resp. being added to a solution of a substance or a mix of substances during an acid-base titration, as well as the equations to estimate the first derivative of the titration plot dpH/dV, and algebraic expressions to determine the buffer β capacity with dilution βdil. This treatment allows establishing the conditions of thermodynamic equilibria for all species within a system containing a mix of species from one or from various polyacid systems. The present work shows that it is possible to determine exactly the electric conductivity of aqueous solutions for these Brønsted acid-base titrations, because the functional relation between this property and the composition of the system in equilibrium is well known; this is achieved using the equivalent conductivity λi values of each of the ions present in a given system. The model employed for the present work confirms the experimental outcomes with the H2SO4, B(OH3, CH3COOH, and H3PO4 aqueous solutions’ titration.

  8. Disposable biosensor based on cathodic electrochemiluminescence of tris(2,2-bipyridine)ruthenium(II) for uric acid determination

    Energy Technology Data Exchange (ETDEWEB)

    Ballesta-Claver, J.; Rodríguez-Gómez, R. [ECsens, Department of Analytical Chemistry, Campus Fuentenueva, Faculty of Sciences, University of Granada, E-18071 Granada (Spain); Capitán-Vallvey, L.F., E-mail: lcapitan@ugr.es [ECsens, Department of Analytical Chemistry, Campus Fuentenueva, Faculty of Sciences, University of Granada, E-18071 Granada (Spain)

    2013-04-03

    Highlights: ► Cathodic ECL offers conventional and non-aggressive analysis conditions. ► The ECL hydrogen peroxide/ruthenium complex system for uric acid determination is novel. ► The ruthenium complex is electrochemically immobilized on graphite screen-printed electrodes. ► The quantification of the uric acid is based on a Stern–Volmer type equation. ► The use of the cathodic ECL working methodology reduces interferences during analysis. -- Abstract: A new method for uric acid (UA) determination based on the quenching of the cathodic ECL of the tris(2,2-bipyridine)ruthenium(II)–uricase system is described. The biosensor is based on a double-layer design containing first tris(2,2-bipyridine)ruthenium(II) (Ru(bpy){sub 3}{sup 2+}) electrochemically immobilized on graphite screen-printed cells and uricase in chitosan as a second layer. The uric acid biosensing is based on the ECL quenching produced by uric acid over the cathodic ECL caused by immobilized Ru(bpy){sub 3}{sup 2+} in the presence of uricase. The use of a −1.1 V pulse for 1 s with a dwelling time of 10 s makes it possible to estimate the initial enzymatic rate, which is used as the analytical signal. The Stern–Volmer type calibration function shows a dynamic range from 1.0 × 10{sup −5} to 1.0 × 10{sup −3} M with a limit of detection of 3.1 × 10{sup −6} M and an accuracy of 13.6% (1.0 × 10{sup −4} M, n = 5) as relative standard deviation. Satisfactory results were obtained for urine samples, creating an affordable alternative for uric acid determination.

  9. Application of UHPLC for the determination of free amino acids in different cheese varieties.

    Science.gov (United States)

    Mayer, Helmut K; Fiechter, Gregor

    2013-10-01

    A rapid ultra-high performance liquid chromatography (UHPLC) protocol for the determination of amino acids as their respective 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) derivatives was successfully applied for assessing free amino acid levels in commercial cheese samples representing typical product groups (ripening protocols) in cheesemaking. Based on the Waters AccQ.Tag™ method as a high performance liquid chromatography (HPLC) amino acid solution designed for hydrolyzate analyses, method adaptation onto UHPLC was performed, and detection of AQC derivatives was changed from former fluorescence (λ(Ex) 250 nm/λ(Em) 395 nm) to UV (254 nm). Compared to the original HPLC method, UHPLC proved to be superior by facilitating excellent separations of 18 amino acids within 12 min only, thus demonstrating significantly shortened runtimes (>35 min for HPLC) while retaining the original separation chemistry and amino acid elution pattern. Free amino acid levels of the analyzed cheese samples showed a high extent of variability depending on the cheese type, with highest total amounts found for original Italian extra-hard cheeses (up to 9,000 mg/100 g) and lowest for surface mold- or bacterial smear-ripened soft cheeses (200-600 mg/100 g). Despite the intrinsic variability in both total and specific concentrations, the established UHPLC method enabled reliable and interference-free amino acid profiling throughout all cheese types, thus demonstrating a valuable tool to generate high quality data for the characterization of cheese ripening.

  10. Determination of anions in pure and commercial phosphoric acid by ion chromatography and manual of 792 basic IC

    International Nuclear Information System (INIS)

    Al-Kabani, F.; Abdulbaki, M. K.

    2007-01-01

    A method for determination of anions in pure and concentrated phosphoric and samples (85%) and commercial phosphoric acid ion chromatography was developed, in order to control the specification of phosphoric acid produced in the pilot plant for phosphoric acid purification. The accuracy of the method was studied and the standard deviation was found to be between 0.09 and 0.10. Operation instructions of 792 Basic IC was described. (author)

  11. Determination of neurotransmitters and their metabolites using one- and two-dimensional liquid chromatography with acidic potassium permanganate chemiluminescence detection.

    Science.gov (United States)

    Holland, Brendan J; Conlan, Xavier A; Stevenson, Paul G; Tye, Susannah; Reker, Ashlie; Barnett, Neil W; Adcock, Jacqui L; Francis, Paul S

    2014-09-01

    High-performance liquid chromatography with chemiluminescence detection based on the reaction with acidic potassium permanganate and formaldehyde was explored for the determination of neurotransmitters and their metabolites. The neurotransmitters norepinephrine and dopamine were quantified in the left and right hemispheres of rat hippocampus, nucleus accumbens and prefrontal cortex, and the metabolites vanillylmandelic acid, 3,4-dihydrophenylacetic acid, 5-hydroxyindole-3-acetic acid and homovanillic acid were identified in human urine. Under optimised chemiluminescence reagent conditions, the limits of detection for these analytes ranged from 2.5 × 10(-8) to 2.5 × 10(-7) M. For the determination of neurotransmitter metabolites in urine, a two-dimensional high-performance liquid chromatography (2D-HPLC) separation operated in heart-cutting mode was developed to overcome the peak capacity limitations of the one-dimensional separation. This approach provided the greater separation power of 2D-HPLC with analysis times comparable to conventional one-dimensional separations.

  12. Modified method for zirconium or hafnium gravimetric determination with glycolic acid derivatives

    International Nuclear Information System (INIS)

    Barbieri, R.S.; Rocha, J.C.; Terra, V.R.; Marques Neto, A.

    1989-01-01

    The conditions for gravimetric determination of zirconium or hafnium by glicolic acid derivatives were studied by thermogravimetric analysis. The method utilized shown that after precipitation, washing and drying of precipitates at 150 0 C, the resulting solid was weighed in the form of [M{RCH(OH)COO} 4 ] (M = Zr,Hf;R = C 6 H 5 , β-C 10 H 7 ,p-BrC 6 H 4 ). (author) [pt

  13. First report on hemoglobin electrostatic immobilization on WO3 nanoparticles: application in the simultaneous determination of levodopa, uric acid, and folic acid.

    Science.gov (United States)

    Ghodsi, Javad; Rafati, Amir Abbas; Shoja, Yalda

    2016-05-01

    This work describes the first report about the simultaneous determination of levodopa (L-DOPA) with folic acid (FA) and uric acid (UA) based on electrocatalytic oxidation of L-DOPA with peroxidase properties of hemoglobin (Hb) in the presence of H2O2 as Hb activator. Bovine Hb was electrostatically immobilized on WO3 nanoparticles (WO3NPs) in pH between Hb and WO3NP isoelectric points, and subsequently, a carbon paste electrode (CPE) was modified with the obtained WO3NPs-Hb and multiwalled carbon nanotubes (MWCNTs). The resulting biosensor supplied a sensitive and suitably stable biosensor for the simultaneous determination of L-DOPA, UA, and FA. The obtained linear range and detection limit for L-DOPA, UA, and FA were completely acceptable, and the biosensor response time for these molecules was relatively short so that it reaches about 95 % of its maximum response in less than 10 s. The applicability of the current biosensor was confirmed with the determination of L-DOPA in the presence of fixed amounts of FA and UA in some real samples by the standard addition method.

  14. Determination of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid in cereals by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matos Reyes, M.N. [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain); Department of Chemistry, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900, Rio de Janeiro, RJ (Brazil); Cervera, M.L. [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain)], E-mail: m.luisa.cervera@uv.es; Campos, R.C. [Department of Chemistry, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900, Rio de Janeiro, RJ (Brazil); Guardia, M. de la [Department of Analytical Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia (Spain)

    2007-09-15

    A fast, sensitive and simple non-chromatographic analytical method was developed for the speciation analysis of toxic arsenic species in cereal samples, namely rice and wheat semolina. An ultrasound-assisted extraction of the toxic arsenic species was performed with 1 mol L{sup -1} H{sub 3}PO{sub 4} and 0.1% (m/v) Triton XT-114. After extraction, As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) concentrations were determined by hydride generation atomic fluorescence spectrometry using a series of proportional equations corresponding to four different experimental reduction conditions. The detection limits of the method were 1.3, 0.9, 1.5 and 0.6 ng g{sup -1} for As(III), As(V), DMA and MMA, respectively, expressed in terms of sample dry weight. Recoveries were always greater than 90%, and no species interconversion occurred. The speciation analysis of a rice flour reference material certified for total arsenic led to coherent results, which were also in agreement with other speciation studies made on the same certified reference material.

  15. Study on the stability of adrenaline and on the determination of its acidity constants

    Science.gov (United States)

    Corona-Avendaño, S.; Alarcón-Angeles, G.; Rojas-Hernández, A.; Romero-Romo, M. A.; Ramírez-Silva, M. T.

    2005-01-01

    In this work, the results are presented concerning the influence of time on the spectral behaviour of adrenaline (C 9H 13NO 3) (AD) and of the determination of its acidity constants by means of spectrophotometry titrations and point-by-point analysis, using for the latter freshly prepared samples for each analysis at every single pH. As the catecholamines are sensitive to light, all samples were protected against it during the course of the experiments. Each method rendered four acidity constants corresponding each to the four acid protons belonging to the functional groups present in the molecule; for the point-by-point analysis the values found were: log β 1=38.25±0.21 , log β 2=29.65±0.17 , log β 3=21.01±0.14 , log β 4=11.34±0.071 .

  16. Simultaneous determination of amoxicillin and clavulanic acid in the human plasma by high performance liquid chromatography: Mass spectrometry (UPLC/MS

    Directory of Open Access Journals (Sweden)

    Ćirić Biljana

    2010-01-01

    Full Text Available Background/Aim. Quantitative analysis of amoxicillin and clavulanic acid in biological matrices requires sensitive and specific methods which allow determination of therapeutic concentration in μg/mL range. Analytical methods for determination of their concentrations in body fluids described in literature include high performance liquid chromatography coupled to UV detector (HPLC-UV and liquid chromatography-mass spectrometry (LC-MS. The aim of this study was to develop sensitive and specific ultra performance liquid chromatography/ mass spectrometry (UPLC/MS method which could be used for the spectral identification and quantification of the low concentrations of amoxicillin and clavulanic acid in the human plasma. Method. A sensitive and specific UPLC/MS method for amoxicillin and clavulanic acid determination was developed in this study. The samples were taken from the adult healthy volunteers receiving per os one tablet of amoxicillin (875 mg in combination with clavulanic acid (125 mg. Results. Plasma samples were pretreated by direct deproteinization with perchloric acid. Quantification limit of 0.01 μg/ml for both amoxicillin and clavulanic acid was achieved. The method was reproducible day by day (RSD < 7 %. Analytical recoveries for amoxicillin ranged from 98.82% to 100.9% (for concentrations of 1, 5 and 20 μg/mL, and recoveries for clavulanic acid were 99,89% to 100.1% (for concentrations of 1, 2 and 5 μg/mL. This assay was successfully applied to a pilot pharmacokinetic study in healthy volunteers after a single-oral administration of amoxicillin/ clavulanic combination. The determined plasma concentrations of both amoxicillin and clavulanic acid were in the range of the expected values upon the literature data for HPLC-UV and LC-MS methods. Conclusion. The described method provided a few advantages comparing with LC/MS-MS method. The method is faster using running time of 5 minute, has lower limit of quantification (LOQ and it

  17. Sensitive determination of nucleic acids using organic nanoparticle fluorescence probes

    Science.gov (United States)

    Zhou, Yunyou; Bian, Guirong; Wang, Leyu; Dong, Ling; Wang, Lun; Kan, Jian

    2005-06-01

    This paper describes the preparation of organic nanoparticles by reprecipitation method under sonication and vigorous stirring. Transmission electron microscopy (TEM) was used to characterize the size and size distribution of the luminescent nanoparticles. Their average diameter was about 25 nm with a size variation of ±18%. The fluorescence decay lifetime of the nanoparticles also was determined on a self-equipped fluorospectrometer with laser light source. The lifetime (˜0.09 μs) of nanoparticles is about three times long as that of the monomer. The nanoparticles were in abundant of hydrophilic groups, which increased their miscibility in aqueous solution. These organic nanoparticles have high photochemical stability, excellent resistance to chemical degradation and photodegradation, and a good fluorescence quantum yield (25%). The fluorescence can be efficiently quenched by nucleic acids. Based on the fluorescence quenching of nanoparticles, a fluorescence quenching method was developed for determination of microamounts of nucleic acids by using the nanoparticles as a new fluorescent probe. Under optimal conditions, maximum fluorescence quenching is produced, with maximum excitation and emission wavelengths of 345 and 402 nm, respectively. Under optimal conditions, the calibration graphs are linear over the range 0.4-19.0 μg ml -1 for calf thymus DNA (ct-DNA) and 0.3-19.0 μg ml -1 for fish sperm DNA (fs-DNA). The corresponding detection limits are 0.25 μg ml -1 for ct-DNA and 0.17 μg ml -1 for fs-DNA. The relative standard deviation of six replicate measurements is 1.3-2.1%. The method is simple, rapid and sensitive with wide linear range. The recovery and relative standard deviation are very satisfactory.

  18. Determination of nitric acid in highly radioactive solutions by the method of coulometric titration

    International Nuclear Information System (INIS)

    Gromov, V.S.; Kuperman, A.Ya.; Smirnov, Yu.A.

    1988-01-01

    A procedure, a cell, and an electronic block have been developed for a long-distance determination of nitric acid in highly radioactive industrial solutions by coulometric titration under hot chamber conditions. A solution of a mixture of ammonium and potassium oxalates was used for the background and anoide electrolytes. This solution prevents the hydrolysis of the metal ions and appreciably decreases the rate of accumulation of the acid in the anode chamber of the cell. Titration with 0.1-0.5 A currents is carried out with internal generation of hydroxyl ions. The cell was prepared from a radiation-resistant and transparent material, poly(methyl methacrylate). The anode and cathode chambers were separated by a cellophane membrane, reinforced by a porous glass filter. By using the electronic coulometric block working together with a pH-meter (EV-74 or I-130) and with an automatic titration block (BAT-15), the titration can be carried out automatically, and the determination results can be obtained in a digital form

  19. A study on the alkalimetric titration with gran plot in noncomplexing media for the determination of free acid in spent fuel solutions

    International Nuclear Information System (INIS)

    Suh, Moo Yul; Lee, Chang Heon; Sohn, Se Chul; Kim, Jung Suk; Kim, Won Ho; Eom, Tae Yoon

    1999-01-01

    Based on the study of hydrolysis behaviour of U(VI) ion and major fission product metal ions such as Cs(I), Ce(III), Nd(III), Mo(VI), Ru(II), and Zr(VI) in the titration media, the performance of noncomplexing-alkalimetric titration method for the determination of free acid in the presence of these metal ions was investigated and its results were compared to those from the complexing methods. The free acidities could be determined as low as 0.05 meq in uranium solutions in which the molar ratio of U(VI)/H + was less than 5, when the end-point of titration was estimated by Gran plot. The biases in the determinations were less than ±1% and about +3% respectively for 0.4 meq and 0.05 meq of free acid at the U(VI)/H + molar ratio of up to 5. Applicability of this method to the determination of free acid in spent fuel solutions was confirmed by the analysis of nitric acid content in simulated spent fuel solutions and in a real spent fuel solution

  20. A new sensor based on glassy carbon electrode modified with nanocomposite for simultaneous determination of acetaminophen, ascorbic acid and uric acid

    Directory of Open Access Journals (Sweden)

    Mohammad Afrasiabi

    2016-09-01

    Full Text Available A chemically-modified electrode has been constructed based on a single walled carbon nanotube/chitosan/room temperature ionic liquid nanocomposite modified glassy carbon electrode (SWCNTs–CHIT–RTIL/GCE. It was demonstrated that this sensor could be used for simultaneous determination of acetaminophen (ACT, uric acid (URI and ascorbic acid (ASC. The measurements were carried out by application of differential pulse voltammetry (DPV, cyclic voltammetry (CV and chronoamperometry (CA methods. Electrochemical studies suggested that the RTIL and SWCNTs provided a synergistic augmentation that can increase current responses by improvement of electron transfers of these compounds on the electrode surface. The presence of the CHIT in the modified electrode can enhance the repeatability of the sensor by its antifouling effect. The modified electrode showed electrochemical responses with high sensitivity for ACT, URI and ASC determination, which makes it a suitable sensor for simultaneous sub-μmol L−1 detection of ACT, URI and ASC in aqueous solutions. The analytical performance of this sensor has been evaluated for detection of ACT, URI and ASC in human serum and urine with satisfactory results.

  1. Melamine and Cyanuric Acid do not interfere with Bradford and Ninhydrin assays for protein determination

    OpenAIRE

    Field, Anjalie; Field, Jeffrey

    2010-01-01

    In the fall of 2007 pet food contaminated with melamine and cyanuric acid caused kidney stones in thousands of animals. In the summer of 2008, a more serious outbreak of adulterated dairy food caused the deaths of six infants and sickened about 290,000 children in China. In all cases, melamine was likely added to inflate the apparent protein content of the foods. To determine if we could measure protein without interference from melamine and cyanuric acid we tested these compounds in the Brad...

  2. Voltammetric determination of polyphenolic content in pomegranate juice using a poly(gallic acid/multiwalled carbon nanotube modified electrode

    Directory of Open Access Journals (Sweden)

    Refat Abdel-Hamid

    2016-07-01

    Full Text Available A simple and sensitive poly(gallic acid/multiwalled carbon nanotube modified glassy carbon electrode (PGA/MWCNT/GCE electrochemical sensor was prepared for direct determination of the total phenolic content (TPC as gallic acid equivalent. The GCE working electrode was electrochemically modified and characterized using scanning electron microscope (SEM, cyclic voltammetry (CV, chronoamperometry and chronocoulometry. It was found that gallic acid (GA exhibits a superior electrochemical response on the PGA/MWCNT/GCE sensor in comparison with bare GCE. The results reveal that a PGA/MWCNT/GCE sensor can remarkably enhance the electro-oxidation signal of GA as well as shift the peak potentials towards less positive potential values. The dependence of peak current on accumulation potential, accumulation time and pH were investigated by square-wave voltammetry (SWV to optimize the experimental conditions for the determination of GA. Using the optimized conditions, the sensor responded linearly to a GA concentration throughout the range of 4.97 × 10−6 to 3.38 × 10−5 M with a detection limit of 3.22 × 10−6 M (S/N = 3. The fabricated sensor shows good selectivity, stability, repeatability and (101% recovery. The sensor was successfully utilized for the determination of total phenolic content in fresh pomegranate juice without interference of ascorbic acid, fructose, potassium nitrate and barbituric acid. The obtained data were compared with the standard Folin–Ciocalteu spectrophotometric results.

  3. The Determination of "Apparent" pKa's. Part II: An Experiment Using Very Weak Acids (pKa's > 11.4).

    Science.gov (United States)

    Cawley, John J.

    1995-01-01

    Presents an experiment designed to show students that the Henderson-Hasselbalch equation will fail when they use this particular one-half titration technique for acids with large pKa's. Involves determining the apparent pKa for such acids and using that to calculate the true pKa. (JRH)

  4. Determination of dopamine in presence of ascorbic acid and uric acid using poly (Spands Reagent) modified carbon paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Veera Manohara Reddy, Y.; Prabhakara Rao, V.; Vijaya Bhaskar Reddy, A.; Lavanya, M.; Venu, M.; Lavanya, M.; Madhavi, G., E-mail: gmchem01@gmail.com

    2015-12-01

    In this paper, we have fabricated a modified carbon paste electrode (CPE) by electropolymerisation of spands reagent (SR) onto surface of CPE using cyclic voltammetry (CV). The developed electrode was abbreviated as poly(SR)/CPE and the surface morphology of the modified electrode was studied by using scanning electron microscopy (SEM). The developed electrode showed higher electrocatalytic properties towards the detection of dopamine (DA) in 0.1 M phosphate buffer solution (PBS) at pH 7.0. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at poly(SR)/CPE. The poly(SR)/CPE was successfully used as a sensor for the selective determination of DA in presence of ascorbic acid (AA) and uric acid (UA) without any interference. The poly(SR)/CPE showed a good detection limit of 0.7 μM over the linear dynamic range of 1.6 μM to 16 μM, which is extremely lower than the reported methods. The prepared poly(SR)/CPE exhibited good stability, high sensitivity, better reproducibility, low detection limit towards the determination of DA. The developed method was also applied for the determination of DA in real samples. - Highlights: • Electropolymerization of spands reagent was fabricated by cyclic voltammetry • The Poly (spands reagent) electrode shows excellent electrocatalytic activity for the detection of dopamine. • The detection limit for dopamine was found to be 0.7 μM. • The proposed method can be applied for DA in injection and human blood serum samples.

  5. Very fast electrophoretic determination of creatinine and uric acid in human urine using a combination of two capillaries with different internal diameters.

    Science.gov (United States)

    Pavlíček, Václav; Tůma, Petr; Matějčková, Jana; Samcová, Eva

    2014-04-01

    A capillary system formed by combining 25 and 100 μm id capillaries was used in the short-end injection mode to determine creatinine and uric acid in human urine. The separation was performed at an electric field intensity of 2.3 kV/cm. Creatinine was determined in a BGE with a composition of 20 mM citric acid/NaOH (pH 3.0), and uric acid was determined in 20 mM MES/NaOH (pH 6.0). Under these conditions, migration times of 12.2 s for creatinine and 8.6 s for uric acid were achieved. The LOD value is 2.4 mg/L for creatinine and 0.9 mg/L for uric acid; the RSD for the migration time varies in the range 0.7-1.1% (intra day) to 1.0-7.5% (inter day); RSDs for the peak areas equalled 3.4-4.0% (intra day) and 4.3-4.7% (inter day). The determined creatinine values in seven urine samples vary in the range 221-1394 mg/L for creatinine and 87-615 mg/L for uric acid. t-Test did not reveal any statistically significant difference between the developed CE methodologies and reference methods - Jaffé reaction for creatinine and enzymatic uricase test for uric acid. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Determination of betulinic acid, oleanolic acid and ursolic acid from Achyranthes aspera L. using RP-UFLC-DAD analysis and evaluation of various parameters for their optimum yield.

    Science.gov (United States)

    Pai, Sandeep R; Upadhya, Vinayak; Hegde, Harsha V; Joshi, Rajesh K; Kholkute, Sanjiva D

    2016-03-01

    Achyranthes aspera L. is a well known herb commonly used in traditional system of Indian medicine to treat various disorders, such as cough, dysentery, gonorrhea, piles, kidney stone, pneumonia, renal dropsy, skin eruptions, snake bite, etc. Here, we used RP-UFLC-DAD method for determining triterpenoids betulinic acid (BA), oleanolic acid (OA) and ursolic acid (UA) from A. aspera. Optimum yield of these compounds were studied and evaluated using parameters viz., method of extraction, time of extraction, age of plant and plant parts (leaves, stem and roots). Linear relationships in RP-UFLC-DAD analysis were obtained in the range 0.05-100 µg/mL with 0.035, 0.042 and 0.033 µg/mL LOD for BA, OA and UA, respectively. Of the variables tested, extraction method and parts used significantly affected content yield. Continuous shaking extraction (CSE) at ambient temperature gave better extraction efficiency than exposure to ultra sonic extraction (USE) or microwave assisted extraction (MAE) methods. The highest content of BA, OA and UA were determined individually in leaf, stem and root extracts with CSE. Collective yield of these triterpenoids were higher in leaf part exposed to 15 min USE method. To best of our knowledge, the study newly reports UA from A. aspera and the same was confirmed using ATR-FT-IR studies. This study explains the distribution pattern of these major triterpenoids and optimum extraction parameters in detail.

  7. Determination of boron as boric acid by automatic potentiometric titration

    International Nuclear Information System (INIS)

    Midgley, D.

    1988-06-01

    Boron in PWR primary coolant and related waters may be determined as boric acid by titration with sodium hydroxide, using a glass electrode as a pH indicator. With a modern automatic titrator, the analysis is quick, convenient, accurate and precise. In the titration of 8 mg B (e.g. 4 ml of 2000 mg 1 -1 solution), no significant bias was observed and relative standard deviations were about 0.25%. With 0.8 g B, a bias of about 2% appears, although this could be reduced by restandardizing the titrant, but the relative standard deviation was still -1 B, depending on the stage of the fuel cycle. (author)

  8. Determination expediency of the omega-3 unsaturated acids in fatty oils by NMR 1"H spectroscopy

    International Nuclear Information System (INIS)

    Ananikyan, H.S.

    2016-01-01

    1"H NMR spectra of fatty oils obtained from seeds of 55 plants were investigated 8 groups of signals were identified in all NMR spectra. Omega-3 fatty acids CH_3 groups signals were noticed in some of the spectra as a triplet in the area of 0.85-1.05 p.p.m. (oil CH_3 groups signals area). Integral intensities of omega-3 fatty acids CH_3 groups signals were calculated by using integral intensities of oils all CH_3 groups signals. Percents of omega-3 unsaturated fatty acids in each of the investigated oils were then calculated. Theoretical percents of omega-3 fatty acids in oils were calculated. For that it was assumed that the signals of 2 CH_2 groups corresponds to 4"H signal and the signals of 3CH_3 group corresponds to 9"H signal. The experimental and theoretical percents of omega-3 fatty acids calculations were compared, and the accuracy of omega-3 fatty acids percent in oil was determined

  9. The issue of HPLC determination of endogenous lipoic acid in human plasma.

    Science.gov (United States)

    Sechovcová, Soňa; Královcová, Pavla; Kanďár, Roman; Ventura, Karel

    2018-05-01

    Lipoic acid (LA) is used extensively as a therapeutic agent for the treatment of various diseases. Many methods have been reported for the determination of LA plasma levels and its metabolites after its supplementation, but available information concerning endogenous plasma levels is still scarce. Studies which directly focused on determining the endogenous plasma levels provided highly controversial results, endogenous plasma levels of LA: 2.4 and 4.9 nmol/L respectively. However, the levels of free LA in the plasma of nonsupplemented voluntary blood donors were not detectable in all cases. The presented results of our study show that endogenous concentrations of LA are <1.85 nmol/L. Copyright © 2017 John Wiley & Sons, Ltd.

  10. Specificity determinants for the abscisic acid response element.

    Science.gov (United States)

    Sarkar, Aditya Kumar; Lahiri, Ansuman

    2013-01-01

    Abscisic acid (ABA) response elements (ABREs) are a group of cis-acting DNA elements that have been identified from promoter analysis of many ABA-regulated genes in plants. We are interested in understanding the mechanism of binding specificity between ABREs and a class of bZIP transcription factors known as ABRE binding factors (ABFs). In this work, we have modeled the homodimeric structure of the bZIP domain of ABRE binding factor 1 from Arabidopsis thaliana (AtABF1) and studied its interaction with ACGT core motif-containing ABRE sequences. We have also examined the variation in the stability of the protein-DNA complex upon mutating ABRE sequences using the protein design algorithm FoldX. The high throughput free energy calculations successfully predicted the ability of ABF1 to bind to alternative core motifs like GCGT or AAGT and also rationalized the role of the flanking sequences in determining the specificity of the protein-DNA interaction.

  11. Selective extraction and determination of chlorogenic acids as combined quality markers in herbal medicines using molecularly imprinted polymers based on a mimic template.

    Science.gov (United States)

    Ji, Wenhua; Zhang, Mingming; Yan, Huijiao; Zhao, Hengqiang; Mu, Yan; Guo, Lanping; Wang, Xiao

    2017-12-01

    We describe a solid-phase extraction adsorbent based on molecularly imprinted polymers (MIPs), prepared with use of a mimic template. The MIPs were used for the selective extraction and determination of three chlorogenic acids as combined quality markers for Lonicera japonica and Lianhua qingwen granules. The morphologies and surface groups of the MIPs were assessed by scanning electron microscopy, Brunauer-Emmett-Teller surface area analysis, and Fourier transform infrared spectroscopy. The adsorption isotherms, kinetics, and selectivity of the MIPs were systematically compared with those of non-molecularly imprinted polymers. The MIPs showed high selectivity toward three structurally similar chlorogenic acids (chlorogenic acid, cryptochlorogenic acid, and neochlorogenic acid). A procedure using molecularly imprinted solid-phase extraction coupled with high-performance liquid chromatography was established for the determination of three chlorogenic acids from Lonicera japonica and Lianhua qingwen granules. The recoveries of the chlorogenic acids ranged from 93.1% to 101.4%. The limits of detection and limits of quantification for the three chlorogenic acids were 0.003 mg g -1 and 0.01 mg g -1 , respectively. The newly developed method is thus a promising technique for the enrichment and determination of chlorogenic acids from herbal medicines. Graphical Abstract Mimic molecularly imprinted polymers for the selective extraction of chlorogenic acids.

  12. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Karina B. de [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Farmacia; Oliveira, Bras H. de, E-mail: bho@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica

    2013-01-15

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C{sub 18} column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min-1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 {+-} 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  13. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    International Nuclear Information System (INIS)

    Oliveira, Karina B. de; Oliveira, Bras H. de

    2013-01-01

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C 18 column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min−1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 ± 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  14. Simultaneous determination of phenolic acids and flavonoids in Chenopodium formosanum Koidz. (djulis) by HPLC-DAD-ESI-MS/MS.

    Science.gov (United States)

    Hsu, B Y; Lin, S W; Inbaraj, B Stephen; Chen, B H

    2017-01-05

    A high performance liquid chromatography-diode array detection-tandem mass spectrometry method (HPLC-DAD-MS/MS) was developed for simultaneous determination of phenolic acids and flavonoids in djulis (Chenopodium formosanum Koidz.), a traditional Chinese herb reported to possess vital biological activities. A high yield of phenolic acids and flavonoids was attained by employing 50% ethanol in water as the extraction solvent and shaking in a 60°C water bath for 3h. A total of 8 phenolic acids and 14 flavonoids were separated and identified within 55min by using a Poroshell 120 EC-C18 column with detection at 280nm, flow rate at 0.8mL/min, column temperature at 35°C, and a gradient solvent system of 0.1% formic acid in water and acetonitrile. Two internal standards caffeic acid and kaempferol-3-O-rutinoside were used for quantitation of phenolic acids and flavonoids in djulis respectively. The amounts of phenolic acids ranged from 11.5±0.8μg/g (caffeoyl-putrescine-derivative (2)) to 1855.3±16.9μg/g (hydroxylphenylacetic acid pentoside), while the flavonoids ranged from 19.93±2.29μg/g (quercetin-3-O-(coumaryl)-rutinoside-pentoside (1)) to 257.3±2.05μg/g (rutin-O-pentoside (2)). A high recovery (89.68-97.20%) and high reproducibility was obtained for both phenolic acids and flavonoids with the relative standard deviation (RSD) for the latter ranging from 0.09-8.22% (intra-day variability) and 0.80-8.48% (inter-day variability). This method may be applied to determination of both phenolic acids and flavonoids in food products and Chinese herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Development of an analytic outline for the aflatoxins analysis in grains and flours; Desarrollo de un esquema analitico para el analisis de aflatoxinas en granos y harinas

    Energy Technology Data Exchange (ETDEWEB)

    Sibaja Adams, Roxana

    2000-07-01

    The instrumental and analytic conditions were optimized for the aflatoxine determination B1, B2, 1 and G2 in corn and peanut byl iquid chromatography of high discharge following the analyzing method AOAC 994,08. Besides, it was defined a function for evaluating the dependence of the chromatographic discharge with the aflatoxine concentration. The analyzing method was validated, and four calibration curves were obtained for the aflatoxine B1, B2, G1 and G2, which turned to have a heterocedastico behavior. The applicability of this method was demonstrated, obtaining imagines of appropriate merit and comparable with those reported by the AOAC. Additionally, the applicability of the chromatographic method was demonstrated in fine layer for the presumptive analysis of aflatoxine, allowing both methods to propose an outline of reliable analysis of real samples. [Spanish] Se optimizaron las condiciones instrumentales y analiticas para la determinacion de aflatoxinas B1, B2, G1 y G2 en maiz y mani por Cromatografia liquida de alto desempeno siguiendo el metodo de analisis AOAC 994,08. Ademas, se definio una funcion para evaluar la dependencia del desempeno cromatografico con la concentracion de aflatoxinas.Se valido el metodo de analisis y se obtuvieron las cuatro curvas de calibracion para las aflatoxinas B1, B2, G1 y G2, las que resultaron tener un comportamiento heterocedastico. Se demostro la aplicabilidad del metodo, obteniendose figuras de merito adecuadas y comparables con las reportadas por el AOAC.Adicionalmente, se demostro la aplicabilidad del metodo de cromatografia en capa fina para el analisis presuntivo de aflatoxinas, permitiendo ambos metodos proponer un esquema de analisis confiable de muestras reales.

  16. Lower pH values of weakly acidic refluxes as determinants of heartburn perception in gastroesophageal reflux disease patients with normal esophageal acid exposure.

    Science.gov (United States)

    de Bortoli, N; Martinucci, I; Savarino, E; Franchi, R; Bertani, L; Russo, S; Ceccarelli, L; Costa, F; Bellini, M; Blandizzi, C; Savarino, V; Marchi, S

    2016-01-01

    Multichannel impedance pH monitoring has shown that weakly acidic refluxes are able to generate heartburn. However, data on the role of different pH values, ranging between 4 and 7, in the generation of them are lacking. The aim of this study was to evaluate whether different pH values of weakly acidic refluxes play a differential role in provoking reflux symptoms in endoscopy-negative patients with physiological esophageal acid exposure time and positive symptom index and symptom association probability for weakly acidic refluxes. One hundred and forty-three consecutive patients with gastroesophageal reflux disease, nonresponders to proton pump inhibitors (PPIs), were allowed a washout from PPIs before undergoing: upper endoscopy, esophageal manometry, and multichannel impedance pH monitoring. In patients with both symptom index and symptom association probability positive for weakly acidic reflux, each weakly acidic reflux was evaluated considering exact pH value, extension, physical characteristics, and correlation with heartburn. Forty-five patients with normal acid exposure time and positive symptom association probability for weakly acidic reflux were identified. The number of refluxes not heartburn related was higher than those heartburn related. In all distal and proximal liquid refluxes, as well as in distal mixed refluxes, the mean pH value of reflux events associated with heartburn was significantly lower than that not associated. This condition was not confirmed for proximal mixed refluxes. Overall, a low pH of weakly acidic reflux represents a determinant factor in provoking heartburn. This observation contributes to better understand the pathophysiology of symptoms generated by weakly acidic refluxes, paving the way toward the search for different therapeutic approaches to this peculiar condition of esophageal hypersensitivity. © 2014 International Society for Diseases of the Esophagus.

  17. Age determination of marine sediments in the western North Pacific by aspartic acid chronology

    International Nuclear Information System (INIS)

    Harada, Naomi; Kusakabe, Masashi; Handa, Nobuhiko; Oba, Tadamichi; Matsuoka, Hiromi; Kimoto, Katsunori.

    1997-01-01

    The ages of fossil planktonic foraminifera, Pulleniatina obliquiloculata, in sediments (core 3bPC) from the western North Pacific were determined by aspartic acid chronology, which uses the racemization reaction rate constant of aspartic acid (k Asp ). Aspartic acid racemization-based ages (Asp ages) ranged from 7,600 yrBP at the surface, to 307,000 yrBP at a depth of 352.9 cm in the sediments. This sediment core was also dated by the glacial-interglacial fluctuation of σ 18 O chronology, and the ages determined by both chronologies were compared. The ages derived from aspartic acid chronology and σ 18 O stratigraphy were more or less consistent, but there appeared to be some differences in age estimates between these two dating methods at some depths within the core. In the core top sediments, the likely cause for the age discrepancy could be the loss of the surface sediment during sampling of the core. At depths of 66.3 and 139 cm within the core, Asp ages indicated reduced sedimentation rates during ca. 60,000-80,000 yrBP and ca. 140,000-190,000 yrBP. The maximum age differences in both chronologies are 33,000 yr and 46,600 yr during each of these periods. These anomalous reductions in sedimentation rates occurring during these periods could possibly be related to some geological events, such as an increased dissolution effect of the calcium carbonate in the western North Pacific. Another possible reason for these age differences could be the unreliability in σ 18 O ages of core 3bPC as they were estimated by σ 18 O ages of another core, 3aPC. (author)

  18. Differential pulse polarography of cadmium-and lead-urate and adsorptive stripping voltammetric determination of uric acid.

    Science.gov (United States)

    Gandour, M A; Ensaf-Aboul-Kasim; Amrallah, A H; Farghaly, O A

    1994-03-01

    The complex formation between uric acid and zinc, cadmium and lead ions has been investigated using differential pulse polarography in 0.01M NaNO(3). It is found that the complexes formed by Cd(II) and Pb(II) ions with uric acid have the stoichiometry of 1:2 and the logarithmic values of the apparent stability constant are 9.47 and 11.7, respectively. On the other hand, zinc(II) ions do not give any indication of complexation with uric acid. A sensitive voltammetric method is developed for the quantitative determination of uric acid. This method is based on controlled adsorptive preconcentration of uric acid on the hanging mercury drop electrode (HMDE), followed by tracing the voltammogram in the cathodic going potential scan. The modes used are direct current stripping voltammetry (DCSV) and differential pulse stripping voltammetry (DPSV). The detection limits found were 8 x 10(-9)M (quiescent period 15 sec) by DPSV and 1.6 x 10(-8)M by DCSV.

  19. Determination of Free Fatty Acid by FT-NIR Spectroscopy in Esterification Reaction for Biodiesel Production

    Directory of Open Access Journals (Sweden)

    Djéssica Tatiana Raspe

    2013-01-01

    Full Text Available This work reports the use of FT-NIR spectroscopy coupled with multivariate calibration to determine the percentage of free fatty acids (FFA in samples obtained by the esterification of FFA in vegetable oils. The analytical method used as calibration matrix samples of the reaction medium of esterification of oleic acid in soybean oil in proportions of 0.3 to 40 wt% (by weight of oleic acid obtained under different experimental conditions and utilized the partial least squares (PLS regression. The efficiency of the method was tested to predict the content of FFA in reactions of esterification of oleic acid in soybean oil catalysed by KSF clay and Amberlyst 15 commercial resin, both in a batch mode. Good Correlations were observed between the FT-NIR/PLS method and the reference method (AOCS. The results confirm that FT-NIR spectroscopy, in combination with multivariate calibration, is a promising technique for monitoring esterification reaction for biodiesel production.

  20. Quantitative determination of pneumococcal capsular polysaccharide serotype 14 using a modification of phenol-sulfuric acid method.

    Science.gov (United States)

    Cuesta, Gabriela; Suarez, Norma; Bessio, Maria I; Ferreira, Fernando; Massaldi, Hugo

    2003-01-01

    The capsular polysaccharide of Streptococcus pneumoniae, serotype 14, is part of every pneumococcal vaccine presently in the market or under development. A strategy for the quantitative determination of this polysaccharide by the phenol-sulfuric acid method is described. The modality of acid addition is shown to be the critical step for obtaining reproducible test results between different technicians. Raising the incubation temperature above 80 degrees C increased the consistency of the method by more than 60% regardless of the acid addition modality, but at the expense of some loss of sensitivity. Incubation at 110 degrees C was found necessary to obtain reproducible results within 3% for this technique, which was used to follow the enrichment of the polysaccharide during the last steps of purification. A model mixture of the component polysaccharide sugars provided an adequate and economic standard to construct the calibration curve for this assay, with absorbance reading either in the reaction tubes or in a microplate. A similar procedure may be applied to the determination of other bacterial polysaccharides as well.

  1. Determination of trace elements by neutron activation analysis using dinonylnaphtalene sulfonic acid as a preconcentrating agent

    International Nuclear Information System (INIS)

    Yang, M.H.; Chen, P.Y.; Tseng, C.L.; Yeh, S.J.; Weng, P.S.

    1977-01-01

    Dinonylnaphthalene sulfonic acid (HD) has been used as a preconcentrating agent to enrich trace metal ions and to separate the interfering elements such as Na, K, Cl and Br, which normally exist in the natural aqueous systems. Experiments were performed by extracting the ions in the aqueous medium with HD in n-hexane and subsequently backextracted into a minimal volume of acid solution. Factors influencing the extraction efficiency of the ions of interest were investigated. The preconcentration technique has been successfully applied to the determination by neutron activation analysis of trace elements in natural water and biological materials. Both short-lived nuclides (Mg, Al, Ca, Mn) and long-lived nuclides (Sm, Eu, Zn, La, Cr, Sc, Fe, Co) in the ppb-level concentrations were determined. (T.G.)

  2. Construction of the Tangent to a Cycloid Proposed by Wallis and Fermat

    Directory of Open Access Journals (Sweden)

    Loredana Biacino

    2017-02-01

    Full Text Available In this paper some methods used in the XVII century for the construction of the tangents to a cycloid in a point are exposed: the kinematical method employed by Roberval, the classical geometrical  method used by Wallis and the Fermat’s construction as a consequence of his tangents method. Le Costruzioni della Tangente alla Cicloide Proposte da Wallis e da Fermat In questo lavoro sono esposti vari metodi in uso nel ‘600 per la costruzione della tangente ad una cicloide in un suo punto: il metodo cinematico impiegato da Roberval, il metodo geometrico classico usato dal Wallis e la costruzione di Fermat come conseguenza del suo metodo delle tangenti. Parole Chiave: Cicloide, Tangente ad una curva, Metodo cinematico delle tangenti, Metodo delle tangenti di Fermat.

  3. Determination of beryllium in water using silica gel chemically modified with aminophosphonic acid

    International Nuclear Information System (INIS)

    Zajtseva, G.N.; Strelko, V.V.

    2001-01-01

    Considered are methods of Be determination based on Be isolation from the solutions using aminophosphonic acid covalently bound on silica gel surface (APA-SiO 2 ) and subsequent photometric or atomic-absorption determination of Be in eluate ( the limit of Be determination is 0.00005 mg/l or 0.00008 mg/l, respectively). APA-SiO 2 high efficiency and a possibility of beryllium ions extraction from diluted solutions by means of sorbent small weighed portions is shown. High efficiency of the sorbent both for concentration and waters purification from beryllium is shown. Methods are tested in analysis of waste water. To assess the accuracy of the proposed methods, parallel determination of beryllium in tests by means of the additions method was carried out. The given data testify to a sufficient accuracy and reproducibility of the proposed methods [ru

  4. Validation of a method by gas chromatography for the determination of fatty acids that comprise the active ingredient D-004

    International Nuclear Information System (INIS)

    Rodriguez Leyes, Eduardo A; Marrero Delange, David; Gonzalez Canavaciolo, Victor L; Sierra Perez, Roxana; Adames Fajardo, Yuliamny

    2009-01-01

    D-004 is a new active ingredient obtained from the Cuban royal palm (Roystonea regia) fruits. This substance is mainly composed by a mixture of saturated and unsaturated free fatty acids, from 8 to 18 carbon atoms, and has shown to be effective in experimental model of prostate hyperplasia. A capillary gas chromatographic method for the determination of the fatty acids in D-004 was developed and validated. The acids were analyzed as methyl ester derivatives, which were obtained by reaction with 10 % acetyl chloride in methanol and separated in a BPX-5 wide-bore column using tridecanoic acid as internal standard. The specificity study showed no interferences regarding the determination of this mixture, once the samples were submitted to stress conditions. Determination of the total fatty acid content was linear (r > 0.999; CVs of the response factors and of the slopes lower than 5 and 2 %, respectively) and without bias in the studied concentration range, from 50 to 150 % of the nominal mass. In the accuracy study, over the range 80 to 120 % of the nominal fatty acid concentration, high recoveries (100.4 to 100.8 %) were reached. Good results were obtained in the repeatability and intermediate precision studies (CV < 2%), proving that the method is precise. These results support that this method is properly validated, being appropriate for the quality control and stability studies of this active ingredient

  5. Sequential injection titration method using second-order signals: determination of acidity in plant oils and biodiesel samples.

    Science.gov (United States)

    del Río, Vanessa; Larrechi, M Soledad; Callao, M Pilar

    2010-06-15

    A new concept of flow titration is proposed and demonstrated for the determination of total acidity in plant oils and biodiesel. We use sequential injection analysis (SIA) with a diode array spectrophotometric detector linked to chemometric tools such as multivariate curve resolution-alternating least squares (MCR-ALS). This system is based on the evolution of the basic specie of an acid-base indicator, alizarine, when it comes into contact with a sample that contains free fatty acids. The gradual pH change in the reactor coil due to diffusion and reaction phenomenona allows the sequential appearance of both species of the indicator in the detector coil, recording a data matrix for each sample. The SIA-MCR-ALS method helps to reduce the amounts of sample, the reagents and the time consumed. Each determination consumes 0.413ml of sample, 0.250ml of indicator and 3ml of carrier (ethanol) and generates 3.333ml of waste. The frequency of the analysis is high (12 samples h(-1) including all steps, i.e., cleaning, preparing and analysing). The utilized reagents are of common use in the laboratory and it is not necessary to use the reagents of perfect known concentration. The method was applied to determine acidity in plant oil and biodiesel samples. Results obtained by the proposed method compare well with those obtained by the official European Community method that is time consuming and uses large amounts of organic solvents.

  6. Determination of Radiotracer Stability of Tritium-Labelled Compounds in Biological Studies; Determination de la Stabilite des Composes Trities Employes comme Indicateurs en Biologie; 041e 043f 0440 0435 0434 0414 043b ; Determinacion de la Estabilidad de los Compuestos Tritiados en los Estudios Biologicos Mediante Indicadores

    Energy Technology Data Exchange (ETDEWEB)

    Okita, G. T.; Spratt, J. L. [Argonne Cancer Research Hospital and Department of Pharmacology, University of Chicago, Chicago, IL (United States)

    1962-02-15

    The recent extensive use of tritium-labelled compounds in biological studies makes it imperative that investigators verify the radiotracer stability of tritiated compounds. Even purification of labelled compounds to constant specific activity does not preclude the possibility of the tritium atom exchanging with hydrogen within a biological system. Radiotracer stability can be demonstrated by various methods once, meticulous radiochemical purification of the labelled material has been effected. In this report three different methods for establishing radiotracer stability of tritiated compounds are described. One approach is to compare the biological half-life of a H{sup 3}-compound to that of a similar compound labelled with C{sup 14}. This method is especially applicable to endogenous substances which undergo isotopic dilution when administered to animals. Stability of exogenous compounds can be verified by a second method. Here it is only necessary to demonstrate no diminution in specific activity when the labelled material is re-isolated from biological samples. A third method, less time-consuming than the first, and applicable to both endogenous and exogenous material is the determination of H{sup 3} to C{sup 14} isotope ratio in a mixture of the same compound labelled with both isotopes. Identical isotope ratios before administration of the double-labelled material and after re-isolation from organs or excreta demonstrate radiotracer stability. This method is particularly applicable where isolation of minute amounts of material necessitates the use of non-radioactive carrier. Data demonstrating the use of these methods for the verification of radiotracer stability will be presented with special reference to labelled cholesterol, morphine and digitoxin as examples for the three respective methods. (author) [French] L'emploi, repandu depuis peu, de composes trities dans les etudes biologiques, impose aux chercheurs la necessite de verifier la stabilite de ces

  7. Graphitic carbon nitride nanosheets doped graphene oxide for electrochemical simultaneous determination of ascorbic acid, dopamine and uric acid

    International Nuclear Information System (INIS)

    Zhang, Hanqiang; Huang, Qitong; Huang, Yihong; Li, Feiming; Zhang, Wuxiang; Wei, Chan; Chen, Jianhua; Dai, Pingwang; Huang, Lizhang; Huang, Zhouyi; Kang, Lianping; Hu, Shirong; Hao, Aiyou

    2014-01-01

    Graphical abstract: Schematic drawing of electrochemical oxidize AA, DA and UA on graphitic carbon nitride nanosheets-graphene oxide composite modified electrode. - Highlights: • Synthesize g-C 3 N 4 , GO and CNNS-GO composite. • CNNS-GO composite was the first time for simultaneous determination of AA, DA and UA. • CNNS-GO/GCE displays fantastic selectivity and sensitivity for AA, DA and UA. • CNNS-GO/GCE was applied to detect real sample with satisfactory results. - Abstract: Graphitic carbon nitride nanosheets with a graphite-like structure have strong covalent bonds between carbon and nitride atoms, and nitrogen atoms in the carbon architecture can accelerate the electron transfer and enhance electrical properties effectually. The graphitic carbon nitride nanosheets-graphene oxide composite was synthesized. And the electrochemical performance of the composite was investigated by cyclic voltammetry and differential pulse voltammetry ulteriorly. Due to the synergistic effects of layer-by-layer structures by π-π stacking or charge-transfer interactions, graphitic carbon nitride nanosheets-graphene oxide composite can improved conductivity, electro-catalytic and selective oxidation performance. The proposed graphitic carbon nitride nanosheets-graphene oxide composite modified electrode was employed for simultaneous determination of ascorbic acid, dopamine and uric acid in their mixture solution, it exhibited distinguished sensitivity, wide linear range and low detection limit. Moreover, the modified electrode was applied to detect urine and dopamine injection sample, and then the samples were spiked with certain concentration of three substances with satisfactory recovery results

  8. Direct electrodeposition of gold nanotube arrays of rough and porous wall by cyclic voltammetry and its applications of simultaneous determination of ascorbic acid and uric acid

    International Nuclear Information System (INIS)

    Yang Guangming; Li Ling; Jiang Jinhe; Yang Yunhui

    2012-01-01

    Gold nanotube arrays of rough and porous wall has been synthesized by direct electrodeposition with cyclic voltammetry utilizing anodic aluminum oxide template (AAO) and polycarbonate membrane (PC) during short time (only 3 min and 2 min, respectively). The mechanism of the direct electrodeposition of gold nanotube arrays by cyclic voltammetry (CV) has been discussed. The morphological characterizations of the gold nanotube arrays have been investigated by scanning electron microscopy (SEM). A simultaneous determination of ascorbic acid (AA) and uric acid (UA) by differential pulse voltammetry (DPV) was constructed by attaching gold nanotube arrays (using AAO) onto the surface of a glassy carbon electrode (GCE). The electrochemical behavior of AA and UA at this modified electrode has been studied by CV and differential pulse voltammetry (DPV). The sensor offers an excellent response for AA and UA and the linear response range for AA and UA were 1.02 × 10 −7 –5.23 × 10 −4 mol L −1 and 1.43 × 10 −7 –4.64 × 10 −4 mol L −1 , the detection limits were 1.12 × 10 −8 mol L −1 and 2.24 × 10 −8 mol L −1 , respectively. This sensor shows good regeneration, stability and selectivity and has been used for the determination of AA and UA in real human urine and serum samples with satisfied results. - Graphical abstract: The schematic diagram of formation of Au nanotube arrays (a) and the stepwise procedure of the sensor (b). Highlights: ► Gold nanotubes array has been synthesized by cyclic voltammetry. ► The mechanism of deposition of gold nanotube has been discussed. ► A determination of ascorbic acid and uric acid was constructed by gold array. ► A satisfied determination of samples can be obtained by this sensor.

  9. Quantitative determination of chlorogenic acid in γ-ray-irradiated potato tubers by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Nishizawa, Makoto; Chonan, Takao; Yamagishi, Takashi; Ando, Yoshiaki

    1984-01-01

    Chlorogenic acid (CGA) and caffeic acid (CA) in lyophilized potato tubers were quantitatively determined by high performance liquid chromatography (HPLC), and the changes in CGA contents of γ-ray-irradiated potato tubers (100 Gy) during storage at 25 0 C were studied. The CGA contents of the irradiated potato tubers slightly increased immediately after irradiation, but decreased gradually after 29th day and reached the same level as that in the beginning of storage on the 73rd day after irradiation. However, the CGA contents of the unirradiated potato tubers increased steadily with increasing days of storage period, and reached twice that in the beginning of storage on the 73rd day after irradiation. The CGA contents in potato tubers determined by Diazo and Folin-Denis methods were shown to be two - eight times higher than those by HPLC method, and there appeared to be no significant relation between the CGA contents determined by HPLC method and by colorimetrical methods. (author)

  10. Determination of Water Vapor Pressure Over Corrosive Chemicals Versus Temperature Using Raman Spectroscopy as Exemplified with 85.5% Phosphoric Acid

    DEFF Research Database (Denmark)

    Rodier, Marion; Li, Qingfeng; Berg, Rolf W.

    2016-01-01

    A method to determine the water vapor pressure over a corrosive substance was developed and tested with 85.5 ± 0.4% phosphoric acid. The water vapor pressure was obtained at a range of temperatures from ∼25 ℃ to ∼200 ℃ using Raman spectrometry. The acid was placed in an ampoule and sealed...... with a reference gas (either hydrogen or methane) at a known pressure (typically ∼0.5 bar). By comparing the Raman signals from the water vapor and the references, the water pressure was determined as a function of temperature. A considerable amount of data on the vapor pressure of phosphoric acid are available...... in the literature, to which our results could successfully be compared. A record value of the vapor pressure, 3.40 bar, was determined at 210 ℃. The method required a determination of the precise Raman scattering ratios between the substance, water, and the used reference gas, hydrogen or methane. In our case...

  11. MgO nanobelt-modified graphene-tantalum wire electrode for the simultaneous determination of ascorbic acid, dopamine and uric acid

    International Nuclear Information System (INIS)

    Zhao, Liwei; Li, Hongji; Gao, Sumei; Li, Mingji; Xu, Sheng; Li, Cuiping; Guo, Wenlong; Qu, Changqing; Yang, Baohe

    2015-01-01

    Graphical abstract: Display Omitted -- Highlights: •Graphene and MgO nanobelts are deposited on tantalum wires to form biosensors. •Ascorbic acid, dopamine and uric acid are determined with the biosensors. •The biosensors show high electrocatalytic activity for oxidation of these species. •The biosensors show high selectivity and good sensitivity. -- ABSTRACT: A promising electrochemical biosensor for simultaneous detection of ascorbic acid (AA), dopamine (DA) and uric acid (UA) was fabricated by electrochemical deposition of MgO nanobelts on a graphene-modified tantalum wire (denoted as MgO/Gr/Ta) electrode. The MgO nanobelts and graphene were verified by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Electrochemical performances of the electrodes were characterized by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The CV results show that AA, DA and UA could be detected simultaneously using MgO/Gr/Ta electrode with peak-to-peak separation of 300 mV, 147 mV and 447 mV for AA-DA, DA-UA and AA-UA, respectively. In the threefold co-existence system, the linear calibration plots for AA, DA and UA were obtained over the concentration range of 5.0–350 μM, 0.1–7 μM and 1–70 μM with detection limits of 0.03 μM, 0.15 μM and 0.12 μM, respectively. The modified electrode shows excellent selectivity, good sensitivity and good stability, making it attractive as a sensor for simultaneous detection of AA, DA and UA in biological fluids

  12. Determination of the seasonal changes on total fatty acid ...

    African Journals Online (AJOL)

    USER

    2010-07-26

    Jul 26, 2010 ... Docosahexaenoic acid (C22:6 ω3), linoleic acid (C18:2 ω6) and eicosapentaenoic acid. (C20:5 ω3) had the highest levels among the PUFAs. ... coronary artery disease, diabetes, hyper-tension and .... factors such as season, the type and amount of feed ..... composition of some Malaysian freswater fish.

  13. Determination of cholesterol oxides in anchovies (Engraulis encrasicolus treated with a commercial mixture of citric acid, trisodium acid and hydrogen peroxide

    Directory of Open Access Journals (Sweden)

    Aniello Anastasio

    2013-02-01

    Full Text Available A new additive formulation containing hydrogen peroxide, citric acid and trisodium acid is illegally used in fishery products due its whitening and antioxidant features. Aim of this study was to evaluate the possible presence of COPs and their role as markers of illegal treatment in anchovies (Engraulis encrasicolus stored at different temperatures. Sensory analysis was also performed by the specific QIM test. The quantitative determinations (% of cholesterol oxides (COPs showed changing amounts during storage. Not always The COPs measured in the treated samples were significantly higher than control samples. Considering the volatility of hydrogen peroxide and the poor repeatability of COPs analyses, as shown in the present study, it is crucial to intensify the control by the Authorities.

  14. Binary and ternary solid-liquid phase equilibrium for the systems formed by succinic acid, urea and diethylene glycol: Determination and modelling

    International Nuclear Information System (INIS)

    Li, Yanxun; Li, Congcong; Han, Shuo; Zhao, Hongkun

    2017-01-01

    Highlights: • Solubility of succinic acid in diethylene glycol was determined. • Solubility of succinic acid + urea + diethylene glycol was determined. • Three ternary phase diagrams were constructed for the ternary system. • The ternary phase diagrams were correlated using NRTL model. - Abstract: In this work, the solid-liquid phase equilibrium for binary system of succinic acid + diethylene glycol at the temperatures ranging from (298.15 to 333.15) K and ternary system of (succinic acid + urea + diethylene glycol) at 298.15 K, 313.15 K and 333.15 K was built by using the isothermal saturation method under atmospheric pressure (101.2 kPa), and the solubilities were determined by a high-performance liquid chromatography. The solid-phases formed in the ternary system of ((succinic acid + urea + diethylene glycol)) were confirmed by Schreinemaker’s method of wet residue, which corresponded to urea, succinic acid, and adduct 2:1 urea-succinic acid (mole ratio). Three isothermal phase diagrams for the ternary system were constructed based on the measured mutual solubility. Each isothermal phase diagram included six crystallization fields, three invariant curves, two invariant points and two co-saturated points. The crystalline region of adduct 2:1 urea-succinic acid is larger than those of the other two solids. The solubility of succinic acid in diethylene glycol was correlated with the modified Apelblat equation, λh equation and NRTL model; and the mutual solubility of the ternary ((succinic acid + urea + diethylene glycol)) system was correlated and calculated by the NRTL model. The interaction parameters’ values of succinic acid-urea were acquired. The value of RMSD was 7.11 × 10 −3 for the ternary system. The calculation results had good agreement with the experiment values. Furthermore, the densities of equilibrium liquid phase were acquired. The phase diagrams and the thermodynamic model of the ternary system could provide the basis for design of

  15. Determination of carnosic acid in Rosmarinus officinalis L. using square wave voltammetry and electrochemical behavior

    Directory of Open Access Journals (Sweden)

    Ümmihan Taşkoparan Yilmaz

    2018-01-01

    Full Text Available A new, fast, sensitive and simple voltammetric method is established for the direct determination of carnosic acid (CA. And the electroreduction of carnosic acid (CA was studied using electrochemical methods. The number of electrons transferred in electrode mechanisms were calculated for reversible and adsorption-controlled electrochemical reduction of CA at 17 mV versus Ag/AgCl at pH 7.0 in Britton–Robinson buffer (BR on a hanging mercury drop electrode. Square-wave voltammetry was developed and validated for direct determination of CA. Square-wave parameters were optimized as accumulation potential = 0.0 mV, accumulation time = 5 s, frequency = 50 Hz, pulse amplitude = 50 mV, and staircase step potential = 5 mV. The developed method displays three linear responses from 2 to 9 μM, 10 to 30 and 40 to 90 μM for carnosic acid with a correlation coefficient of 0.996, 0.999 and 0.999. The detection limits were found to be 1.5 μM, 4.0 μM and 40.1 μM, respectively. The interference effect of most common organic and inorganic species was investigated. Proposed method was successfully applied for determination of CA in natural extract of rosemary and the average content was determined as 11.9 ± 1.0 (μg CA/1 g rosemary. The results were in agreement with that obtained by HPLC-UV comparison method. The developed method can be widely used in routine quality control of herbal materials as well as other in foods, medicinal, pharmaceutical and environmental analysis.

  16. Determination of oil and fatty acids concentration in seeds of coastal halophytic Sueada aegyptica plant

    Directory of Open Access Journals (Sweden)

    Tahereh Assadi

    2013-04-01

    Full Text Available Background: Suaeda aegyptica (S. aegyptica species belong to the Chenepodiaceae family, the second largest family in the world of plants kingdom. It is indigenous to arid and semi-arid regions of the world and salty coastal zones Persian Gulf of Iran. It is an annual succulent halophyte plant which is characterized by producing oily seeds, high growth rate and large number of biomass. The aim of this study was analysis and determination of oil and fatty acids concentration in the S. aegyptica seed. Material and Methods: The seeds of S. aegyptica were collected form coastal zones of Persian Gulf in Bushehr province, washed and dried. The fatty acids content of the dried seeds were extracted in n-hexane solvent by soxhellet apparatus. The residue of n-hexane in oily phase was evaporated by rotary evaporator and remaining oil was collected for fatty acids analysis. In the presence of potassium hydroxide and BF3 by refluxing for 30 minutes, the methyl ester derivative of fatty acids were produced. Then the resulted derivatives were analyzed by gas chromatography (GC-FID. Results: The seeds of S. aegyptica contains eight fatty acids as: Pelargonic (C9, Capric (C10, Undecylic (C11, Tridecylic (C13, Myristic (C14, Palmitic (C16, Stearic (C18, Linoleic (18:2 and Linolenic (18:3. Average oil content in seeds 014/0 ± 87 / percent. Conclusion: The ratio of unsaturated fatty acids was higher than the saturated ones. Linoleic and Palmitic acids are major unsaturated and saturated fatty acids of S. aegyptica seed respectively.

  17. Determination of the biodiesel acidity index by potentiometric titration by using different methods; Determinacao do indice de acidez de biodiesel por titulacao potenciometrica utilizando-se diferentes metodos

    Energy Technology Data Exchange (ETDEWEB)

    Goncalves, Mary Ane; Sobral, Sidney Pereira; Borges, Paulo Paschoal [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (DIMCI/INMETRO), Duque de Caxias, RJ (Brazil). Diretoria de Metrologia Cientifica e Industrial], E-mail: magoncalves@inmetro.gov.br

    2009-07-01

    This work determined the index of the soybean/fat bio diesel through the potentiometric titration. Four different methods were used with variation of solvent and electrodes. The results were compared by F and t (Student) and it was verified that they were agreed in a 95% confidence interval.

  18. Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

    1980-01-01

    4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

  19. Morphology-dependent Electrochemical Enhancements of Porous Carbon as Sensitive Determination Platform for Ascorbic Acid, Dopamine and Uric Acid

    Science.gov (United States)

    Cheng, Qin; Ji, Liudi; Wu, Kangbing; Zhang, Weikang

    2016-02-01

    Using starch as the carbon precursor and different-sized ZnO naoparticles as the hard template, a series of porous carbon materials for electrochemical sensing were prepared. Experiments of scanning electron microscopy, transmission electron microscopy and Nitrogen adsorption-desorption isotherms reveal that the particle size of ZnO has big impacts on the porous morphology and surface area of the resulting carbon materials. Through ultrasonic dispersion of porous carbon and subsequent solvent evaporation, different sensing interfaces were constructed on the surface of glassy carbon electrode (GCE). The electrochemical behaviors of ascorbic acid (AA), dopamine (DA) and uric acid (UA) were studied. On the surface of porous carbon materials, the accumulation efficiency and electron transfer ability of AA, DA and UA are improved, and consequently their oxidation signals enhance greatly. Moreover, the interface enhancement effects of porous carbon are also controlled by the particle size of hard template. The constructed porous carbon interface displays strong signal amplification ability and holds great promise in constructing a sensitive platform for the simultaneous determination of AA, DA and UA.

  20. A new method for determining the acid number of biodiesel based on coulometric titration.

    Science.gov (United States)

    Barbieri Gonzaga, Fabiano; Pereira Sobral, Sidney

    2012-08-15

    A new method is proposed for determining the acid number (AN) of biodiesel using coulometric titration with potentiometric detection, basically employing a potentiostat/galvanostat and an electrochemical cell containing a platinum electrode, a silver electrode, and a combination pH electrode. The method involves a sequential application of a constant current between the platinum (cathode) and silver (anode) electrodes, followed by measuring the potential of the combination pH electrode, using an isopropanol/water mixture as solvent and LiCl as the supporting electrolyte. A preliminary evaluation of the new method, using acetic acid for doping a biodiesel sample, showed an average recovery of 100.1%. Compared to a volumetric titration-based method for determining the AN of several biodiesel samples (ranging from about 0.18 to 0.95 mg g(-1)), the new method produced statistically similar results with better repeatability. Compared to other works reported in the literature, the new method presented an average repeatability up to 3.2 times better and employed a sample size up to 20 times smaller. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Determination of acrolein, ethanol, volatile acidity, and copper in different samples of sugarcane spirits

    Directory of Open Access Journals (Sweden)

    José Masson

    2012-09-01

    Full Text Available Seventy-one samples of sugarcane spirits from small and average size stills produced in the northern and southern Minas Gerais (Brazil were analyzed for acrolein using HPLC (High Performance Liquid Chromatography. Ethanol and copper concentrations and volatile acidity were also determined according to methods established by the Ministry of Agriculture, Livestock and Supply (MAPA. A total of 9.85% of the samples tested showed levels of acrolein above the legal limits, while the copper concentrations of 21.00% of the samples and the volatile acidity of 8.85% of the samples were higher than the limits established by the Brazilian legislation. The concentration of acrolein varied from 0 to 21.97 mg.100 mL-1 of ethanol. However, no significant difference at 5% of significance was observed between the samples produced in the northern and southern Minas Gerais. The method used for determination of acrolein in sugarcane spirits involved the formation of a derivative with 2,4-dinitrophenylhydrazine (2,4-DNPH and subsequent analysis by HPLC.

  2. Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue

    Directory of Open Access Journals (Sweden)

    Elena Barbaro

    2016-01-01

    Full Text Available Domoic acid (DA, a neurotoxic amino acid produced by diatoms, is the main cause of amnesic shellfish poisoning (ASP. In this work, we propose a very simple and fast analytical method to determine DA in mussel tissue. The method consists of two consecutive extractions and requires no purification steps, due to a reduction of the extraction of the interfering species and the application of very sensitive and selective HILIC-MS/MS method. The procedural method was validated through the estimation of trueness, extract yield, precision, detection, and quantification limits of analytical method. The sample preparation was also evaluated through qualitative and quantitative evaluations of the matrix effect. These evaluations were conducted both on the DA-free matrix spiked with known DA concentration and on the reference certified material (RCM. We developed a very selective LC-MS/MS method with a very low value of method detection limit (9 ng g−1 without cleanup steps.

  3. Determination of small amounts of nitric acid in the presence of large amounts of uranium (VI) and extraction of nitric acid into TBP solutions highly loaded with uranyl nitrate

    International Nuclear Information System (INIS)

    Kolarik, Z.; Schuler, R.

    1982-10-01

    A new method for the determination of small amounts of nitric acid in the presence of large amounts of uranium(VI) was elaborated. The method is based on the precipitation of uranium(VI) as iodate and subsequent alkalimetric titration of the acid in the supernatant. The extraction of nitric acid and uranium(VI) with 30% TBP in dodecane was studied at high loading of the organic phase with uranyl nitrate and at 25, 40 and 60 0 C. The results are compared with available published data on the extraction of nitric acid under similar conditions. (orig.) [de

  4. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

    Energy Technology Data Exchange (ETDEWEB)

    Varanusupakul, Pakorn [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)], E-mail: pakorn.v@chula.ac.th; Vora-adisak, Narongchai; Pulpoka, Bancha [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)

    2007-08-15

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na{sub 2}SO{sub 4}. The linear calibration curves were observed for the concentrations ranging from 1 to 300 {mu}g L{sup -1} with the correlation coefficients (R{sup 2}) being greater than 0.99. The method detection limits of most analytes were below 1 {mu}g L{sup -1} except DCAA and MCAA that were 2 and 18 {mu}g L{sup -1}, respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

  5. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

    International Nuclear Information System (INIS)

    Varanusupakul, Pakorn; Vora-adisak, Narongchai; Pulpoka, Bancha

    2007-01-01

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na 2 SO 4 . The linear calibration curves were observed for the concentrations ranging from 1 to 300 μg L -1 with the correlation coefficients (R 2 ) being greater than 0.99. The method detection limits of most analytes were below 1 μg L -1 except DCAA and MCAA that were 2 and 18 μg L -1 , respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water

  6. Determination of amino acid neurotransmitters in rat hippocampi by HPLC-UV using NBD-F as a derivative.

    Science.gov (United States)

    Wu, Xiaomeng; Wang, Rui; Jiang, Qingqing; Wang, Shue; Yao, Yao; Shao, Lihua

    2014-04-01

    A simple, rapid and accurate high-performance liquid chromatography method with ultraviolet-visible detection was developed for the determination of five amino acid neurotransmitters - aspartate, glutamic acid, glycine, taurine and γ-aminobutyric acid - in rat hippocampi with pre-column derivatization with 4-fluoro-7-nitrobenzofurazan. Several conditions which influenced derivatization and separation, such as pH, temperature, acetonitrile percentage mobile phase and flow rate, were optimized to obtain a suitable protocol for amino acids quantification in samples. The separation of the five neurotransmitter derivatives was performed on a C18 column using a mobile phase consisting of phosphate buffer (0.02 mol/L, pH 6.0)-acetonitrile (84:16, v/v) at a flow rate of 1.0 mL/min with the column temperature at 30°C. The detection wavelength was 472 nm. Without gradient elution, the five neurotransmitter derivatives were completely separated within 15 min. The linear relation was good in the range from 0.50 to 500 µmol/L, and the correlation coefficients were ≥0.999. Intra-day precision was between 1.8 and 3.2%, and inter-day precision was between 2.4 and 4.7%. The limits of detection (signal-to-noise ratio 3) were from 0.02 to 0.15 µmol/L. The established method was used to determine amino acid neurotransmitters in rat hippocampi with satisfactory recoveries varying from 94.9 to 105.2%. Copyright © 2013 John Wiley & Sons, Ltd.

  7. In-vial liquid-liquid microextraction-capillary electrophoresis method for the determination of phenolic acids in vegetable oils.

    Science.gov (United States)

    Abu Bakar, Nur Bahiyah; Makahleh, Ahmad; Saad, Bahruddin

    2012-09-12

    An in-vial liquid-liquid microextraction method was developed for the selective extraction of the phenolic acids (caffeic, gallic, cinnamic, ferulic, chlorogenic, syringic, vanillic, benzoic, p-hydroxybenzoic, 2,4-dihydroxybenzoic, o-coumaric, m-coumaric and p-coumaric) in vegetable oil samples. The optimised extraction conditions for 20 g sample were: volume of diluent (n-hexane), 2 mL; extractant, methanol: 5 mM sodium hydroxide (60:40; v/v); volume of extractant, 300 μL (twice); vortex, 1 min; centrifugation, 5 min. Recoveries for the studied phenolic acids were 80.1-119.5%. The simultaneous determination of the phenolic acid extracts was investigated by capillary electrophoresis (CE). Separations were carried out on a bare fused-silica capillary (50 μm i.d.× 40 cm length) involving 25 mM sodium tetraborate (pH 9.15) and 5% methanol as CE background electrolyte in the normal polarity mode, voltage of 30 kV, temperature of 25°C, injection time of 4s (50 mbar) and electropherograms were recorded at 200 nm. The phenolic acids were successfully separated in less than 10 min. The validated in-vial LLME-CE method was applied to the determination of phenolic acids in vegetable oil samples (extra virgin olive oil, virgin olive oil, pure olive oil, walnut oil and grapeseed oil). The developed method shows significant advantages over the current methods as lengthy evaporation step is not required. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. RP-HPLC Determination of vitamins B1, B3, B6, folic acid and B12 in multivitamin tablets

    Directory of Open Access Journals (Sweden)

    SOTE VLADIMIROV

    2005-10-01

    Full Text Available Abstract:Asimple and sensitive reversed-phase, ion-pair HPLC method was developed and validated for the simultaneous determination of B-group vitamins, thiamine chloride hydrochloride (B1, nicotinamide (B3, pyridoxine hydrochloride (B6 and folic acid in Pentovit® coated tablets. The cyanocobalamine (B12 was determined separately, because of its low concentration in the investigated multivitamin preparation. RP-HPLC analysis was performed with a LKB 2150 HPLC system, equipped with a UV/VIS Waters M484 detector. The procedures for the determination of B1, B2, B6 and folic acid were carried out on a Supelcosil ABZ+ (15 cm 4.6 mm; 5 µm column with methanol-5mM heptanesulphonic acid sodium salt 0.1%triethylamine TEA(25:75 V/V; pH 2.8 as themobile phase. For the determination of B12 a Suplex pKb-100 (15 cm 4.6 mm; 5 µm column andmethanol–water (22:78 V/V as themobile phase were used. The column effluentsweremonitored at 290 nm for B 1, B3, B6 and folic acid, and at 550 nm for B12. The obtained results and statistical parameters for all the investigated vitamins of the B-group in Pentovit® coated tablets were satisfactory and ranged from 90.4 % to 108.5 % (RSD. from 0.5% to 4.1 %. The parameters for the validation of the methods are given.

  9. The role of membrane cholesterol in determining bile acid cytotoxicity and cytoprotection of ursodeoxycholic acid

    Science.gov (United States)

    Zhou, Yong; Doyen, Rand; Lichtenberger, Lenard M.

    2013-01-01

    In cholestatic liver diseases, the ability of hydrophobic bile acids to damage membranes of hepatocytes/ductal cells contributes to their cytotoxicity. However, ursodeoxycholic acid (UDC), a hydrophilic bile acid, is used to treat cholestasis because it protects membranes. It has been well established that bile acids associate with and solubilize free cholesterol (CHOL) contained within the lumen of the gallbladder because of their structural similarities. However, there is a lack of understanding of how membrane CHOL, which is a well-established membrane stabilizing agent, is involved in cytotoxicity of hydrophobic bile acids and the cytoprotective effect of UDC. We utilized phospholipid liposomes to examine the ability of membrane CHOL to influence toxicity of individual bile acids, such as UDC and the highly toxic sodium deoxycholate (SDC), as well as the cytoprotective mechanism of UDC against SDC-induced cytotoxicity by measuring membrane permeation and intramembrane dipole potential. The kinetics of bile acid solubilization of phosphatidylcholine liposomes containing various levels of CHOL was also characterized. It was found that the presence of CHOL in membranes significantly reduced the ability of bile acids to damage synthetic membranes. UDC effectively prevented damaging effects of SDC on synthetic membranes only in the presence of membrane CHOL, while UDC enhances the damaging effects of SDC in the absence of CHOL. This further demonstrates that the cytoprotective effects of UDC depend upon the level of CHOL in the lipid membrane. Thus, changes in cell membrane composition, such as CHOL content, potentially influence the efficacy of UDC as the primary drug used to treat cholestasis. PMID:19150330

  10. A method of sample preparation for N15 determination in amino acids separated by paper chromatography

    International Nuclear Information System (INIS)

    Secer, M.

    1988-01-01

    The amino acids separated with two dimensional paper chromatography were isolated in two ways which make their 15 N determination possible 1) After developing the spots of chromatograms with ninhydrin they were cut out and shaken 30' with 2 ml dist. H 2 O. To destroy the ninhydrin-NH 3 colour complex, the extraction solution was heated in boiling waterbath for 10' and then 0.5 ml 2 N HCl was added to the solution and continued to heat for further 10'. For the 15 N determination of amino acids by emissionspectrometer this colour complex must be destroyed completely. It was reached with adding 2 ml 30% H 2 O 2 to the solution and heating it 5' in 100 0 C waterbath. After the evaporation of colourless solution under IR-lamp at 70 0 C, the white powder was dissolved with 50 ul dist. H 2 O and centrifuged 10'. The clear supernatant was used to gain N 2 gas by the CuO/CaO combustion. N 2 gas is necessary for the 15 N/ 14 N ratio determination by emissionsspectrometer. 2) In the second way, the destroying of ninhydrin-NH 3 colour complex was easier and quicker this way the spots were eluted (extracted) with 50% alcohol and 30% H 2O2 with 1:1 ratio. After shaking the solution 30', it turns quite colourless. It means that the ninhydrin-NH 3 colour complex was completely destroyed. Further works have been done as described in the first way. We have found out that one amino acid should have 10-20 ug N in it to assess the 15 N enrichment. In order to attain this quantity of N for certain amino acids, the spots of three separately run chromatograms were combined

  11. Determination of /sup 35/S-aminoacyl-transfer ribonucleic acid specific radioactivity in small tissue samples

    Energy Technology Data Exchange (ETDEWEB)

    Samarel, A.M.; Ogunro, E.A.; Ferguson, A.G.; Lesch, M.

    1981-11-15

    Rate determination of protein synthesis utilizing tracer amino acid incorporation requires accurate assessment of the specific radioactivity of the labeled precursor aminoacyl-tRNA pool. Previously published methods presumably useful for the measurement of any aminoacyl-tRNA were unsuccessful when applied to (/sup 35/S)methionine, due to the unique chemical properties of this amino acid. Herein we describe modifications of these methods necessary for the measurement of /sup 35/S-aminoacyl-tRNA specific radioactivity from small tissue samples incubated in the presence of (/sup 35/S)methionine. The use of (/sup 35/S)methionine of high specific radioactivity enables analysis of the methionyl-tRNA from less than 100 mg of tissue. Conditions for optimal recovery of /sup 35/S-labeled dansyl-amino acid derivatives are presented and possible applications of this method are discussed.

  12. An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid.

    Science.gov (United States)

    van Staden, J F; Mashamba, Mulalo G; Stefan, Raluca I

    2002-09-01

    An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid is proposed. A solution of 0.1 mol L(-1) sodium chloride is used as carrier. Titration is achieved by aspirating acetic acid samples between two strong base-zone volumes into a holding coil and by channelling the stack of well-defined zones with flow reversal through a reaction coil to a potentiometric sensor where the peak widths were measured. A linear relationship between peak width and logarithm of the acid concentration was obtained in the range 1-9 g/100 mL. Vinegar samples were analysed without any sample pre-treatment. The method has a relative standard deviation of 0.4% with a sample frequency of 28 samples per hour. The results revealed good agreement between the proposed sequential injection and an automated batch titration method.

  13. Evaluation of methods for wax determination in crude oil; Avaliacao de metodos de determinacao de parafinas em petroleo

    Energy Technology Data Exchange (ETDEWEB)

    Dias, Julio Cesar M.; Silva, Maria do Socorro A.J. da; Vasconcellos, Rosa C.U. [PETROBRAS S.A., Rio de Janeiro, RJ (Brazil). Centro de Pesquisas; Tamanqueira, Juliana B. [Fundacao Gorceix, Ouro Preto, MG (Brazil)

    2008-07-01

    Determining the wax content of crude oil is of great importance for petroleum industry, especially for production, storage and transportation of crude oils. Many different methodologies of wax determining are available in the technical literature. However, the selection of the most suitable method must be in accordance with the aim of the analysis and observing the specificities of each technique. The purpose of this work was to determine the performance of different techniques of wax determining applied to characterization of precipitation properties of waxy compounds in crude oils. Twelve samples of crude oils proceeding from the main Brazilian oil producing sedimentary basins were selected for this study. These samples were analyzed by three important analytical techniques of wax determining: precipitation by cooled solvent; liquid chromatography with precipitation by cooled solvent; and liquid chromatography followed by gas chromatography. Differential scanning calorimetry data related to the wax crystallization in these oils were used as parameters of validation. The results obtained in this study indicate that the liquid chromatography followed by gas chromatography method has the best performance for wax determining in crude oils. (author)

  14. Determination of free acid in high level liquid wastes by means of fixed pH value

    International Nuclear Information System (INIS)

    Li Jifu; Duan Shirong; Wu Xi; Yu Xueren

    1991-01-01

    For the determination of free acid in high level liquid wastes, 8% potassium oxalate solution with pH 6.50 as a complex agent of hydrolizable ion is added to 1 AW and the solution is titrated with standard sodium hydroxide to reach the original pH value. The quantity of free acid is calculated by standard sodium hydroxide consumed. This method is simple, rapid and accurate. The relative error of analysis is less than ±4%. The average percentage of recovery is 99.6-101.0%

  15. Development of a chromatographic method for the study of the stability and compatibility of Mexican fuel oils; Desarrollo de un metodo cromatografico para el estudio de estabilidad y compatibilidad de combustoleos mexicanos

    Energy Technology Data Exchange (ETDEWEB)

    Blass Amador, Georgina; Panama Tirado, Luz Angelica [Instituto de Investigaciones Electricas, Cuernavaca (Mexico)

    1992-11-01

    In Mexico, the largest part of the generated electric energy comes from the use of residual heavy oils known as fuel oils which have suffered quality degradation due to a combination of factors, among which stands out the changes in the refining process. It is necessary to develop methods capable of indicating the instability (formation of sediment or viscosity increase during storage or heating) or incompatibility (formation of sediment in mixing two or more fuel oils) of the fuel oils employed in fossil fuel power plants. This work objective was to develop an alternative test for the study of the compatibility and/or stability of Mexican fuel oils using high resolution liquid chromatography (CLAR) and so to determine structural aspects of the fuel oil that determine its stability. Since the formation of sediments occurs when the dissolving ability of the fuel is inadequate to keep the asphaltenes in solution, it is important to know the solvent power degree or aromaticity of the diluent; so, in the first part of this work the attention was centered in the determination of the profile of aromatic compounds of the fuel oil diluents, the other part was dedicated to the determination of the distribution profile the molecular weights of the asphaltenes present in the fuel oils. The profiles of the aromatic fraction, as well as of the molecular weight distribution were determined using liquid chromatography, in which a variety of columns and solvents were used. A combination of routine tests was accomplished, such as asphaltenes content, toluene equivalence, viscosity, etc., in order to obtain correlation with the chromatographic method developed. In this article it is only discussed the section corresponding to the obtainment of the profile of aromatics content in the fuel oils. It has been found a correlation among the asphaltenes content, toluene equivalence, aromaticity profiles and stability. As a direct consequence, it is expected to be able to predict the

  16. Determination of efficacy of fingermark enhancement reagents; the use of propyl chloroformate for the derivatization of fingerprint amino acids extracted from paper.

    Science.gov (United States)

    Mink, Tineke; Voorhaar, Annelies; Stoel, Reinoud; de Puit, Marcel

    2013-09-01

    The analysis of the constituents of fingerprints has been described numerous times, mainly with the purpose of determining the aging effect on fingerprints or showing the differences between donors or groups of donors. In this paper we describe the use of derivatized amino acids to determine the efficacy of the visualization reagents 1,8-diazafluoren-9-one (DFO) and ninhydrin. At present certain conditions are used for the application of these reagents, as determined by trial-and-error investigations, to the effect on fingerprints. The recovery of amino acids from a porous surface can be used as a measure for the efficacy of a visualization agent. In this paper we describe a method for the determination of the amount of amino acid left after reaction with well known fingerprint visualization reagents. This will allow a more scientific approach to method development for fingermark enhancement techniques. Furthermore, investigations on the influence of the concentration of fingermark amino acids, the order of application of and exposure time to reagents and the influence of age of the amino acids were carried out. These studies have resulted in a broader understanding of the mechanism involved in visualization of fingermarks using DFO and ninhydrin. Copyright © 2013 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

  17. A glassy carbon electrode modified with a nickel(II) norcorrole complex and carbon nanotubes for simultaneous or individual determination of ascorbic acid, dopamine, and uric acid

    International Nuclear Information System (INIS)

    Deng, Keqin; Li, Xiaofang; Huang, Haowen

    2016-01-01

    The authors report on the synthesis of a hybrid material consisting of the porphyrinoid metal complex nickel(II) norcorrole that was noncovalently bound to carbon nanotubes (CNT-NiNC). The hybrid was characterized by UV–vis, FTIR spectroscopy, and thermogravimetric analysis. The CNT-NiNC hybrid possesses high catalytic activity and selectivity toward the oxidation of ascorbic acid, dopamine, and uric acid. It was used to modify a glassy carbon electrode which then is shown to enable simultaneous or individual determination of ascorbic acid (AA), dopamine (DA), and uric acid (UA) at pH 6.5 and typical working potentials of −70, 200 and 380 mV (vs. SCE). The detection limits (at an SNR of 3) are 2.0 μM for AA, 0.1 μM for DA, and 0.4 μM for UA. (author)

  18. Spectrophotometric Determination of Zinc Using 7-(4-Nitrophenylazo-8-Hydroxyquinoline-5-Sulfonic Acid

    Directory of Open Access Journals (Sweden)

    Korn Maria das Graças Andrade

    1999-01-01

    Full Text Available A sensitive and selective spectrophotometric method is proposed for the rapid determination of zinc(II using an 8-hydroxyquinoline derivative, 7-(4-nitrophenylazo-8-hydroxyquinoline-5-sulfonic acid (p-NIAZOXS, as a new spectrophotometric reagent. The reaction between the p-NIAZOXS and zinc(II is instantaneous at pH 9.2 (borax buffer and the absorbance remains stable for over 24 h. The method allows the determination of zinc over the range of 0.05-1.0 mug mL-1 with a molar absorptivity of 3.75x10(4 L mol-1 cm-1 and features a detection limit of 15 ng mL-1. The proposed method has been successfully applied to the determination of zinc in several pharmaceutical preparations and copper alloys. The precision (R.S.D. < 2% and the accuracy obtained were satisfactory.

  19. A Nanostructured Sensor Based on Gold Nanoparticles and Nafion for Determination of Uric Acid

    Directory of Open Access Journals (Sweden)

    Natalia Stozhko

    2018-03-01

    Full Text Available The paper discusses the mechanism of uric acid (UA electrooxidation occurring on the surface of gold nanoparticles. It has been shown that the electrode process is purely electrochemical, uncomplicated with catalytic stages. The nanoeffects observed as the reduction of overvoltage and increased current of UA oxidation have been described. These nanoeffects are determined by the size of particles and do not depend on the method of particle preparation (citrate and “green” synthesis. The findings of these studies have been used to select a modifier for carbon screen-printed electrode (CSPE. It has been stated that CSPE modified with gold nanoparticles (5 nm and 2.5% Nafion (Nf may serve as non-enzymatic sensor for UA determination. The combination of the properties of nanoparticles and Nafion as a molecular sieve at the selected pH 5 phosphate buffer solution has significantly improved the resolution of the sensor compared to unmodified CSPE. A nanostructured sensor has demonstrated good selectivity in determining UA in the presence of ascorbic acid. The detection limit of UA is 0.25 μM. A linear calibration curve has been obtained over a range of 0.5–600 μM. The 2.5%Nf/Au(5nm/CSPE has been successfully applied to determining UA in blood serum and milk samples. The accuracy and reliability of the obtained results have been confirmed by a good correlation with the enzymatic spectrophotometric analysis (R2 = 0.9938 and the “added−found” technique (recovery close to 100%.

  20. Determination of ursolic acid and ursolic acid lactone in the leaves of Eucalyptus tereticornis by HPLC

    International Nuclear Information System (INIS)

    Maurya, Anupam; Srivastava, Santosh Kumar

    2012-01-01

    A simple isocratic HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and ursolic acid lactone in E. tereticornis leaves. Samples were analyzed on RP-18 (4.6 x 250 mm, 5 m u m ) column with methanol and water acidified to pH 3.5 with TFA (88:12) at 210 nm. The method was validated and applied for the simultaneous quantification of the individual triterpenes in E. tereticornis extract. The calibration curves were linear over a concentration range of 0.05-0.3 mg mL -1 (r = 0.999 and 0.998, respectively). The limits of detection and quantification were 0.190 and 0.644 μg for ursolic acid, and 0.176 and 0.587 μg for ursolic acid lactone, while the percentage recoveries were 97.32 and 96.23% for ursolic acid and ursolic acid lactone, respectively. This is the first report on the HPLC method of ursolic acid lactone with high precision and accuracy. (author)

  1. Determination of ursolic acid and ursolic acid lactone in the leaves of Eucalyptus tereticornis by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Maurya, Anupam; Srivastava, Santosh Kumar [Analytical Chemistry Division, Central Institute of Medicinal and Aromatic Plants, Lucknow (India)

    2012-03-15

    A simple isocratic HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and ursolic acid lactone in E. tereticornis leaves. Samples were analyzed on RP-18 (4.6 x 250 mm, 5 {sup m}u{sup m}) column with methanol and water acidified to pH 3.5 with TFA (88:12) at 210 nm. The method was validated and applied for the simultaneous quantification of the individual triterpenes in E. tereticornis extract. The calibration curves were linear over a concentration range of 0.05-0.3 mg mL{sup -1} (r = 0.999 and 0.998, respectively). The limits of detection and quantification were 0.190 and 0.644 {mu}g for ursolic acid, and 0.176 and 0.587 {mu}g for ursolic acid lactone, while the percentage recoveries were 97.32 and 96.23% for ursolic acid and ursolic acid lactone, respectively. This is the first report on the HPLC method of ursolic acid lactone with high precision and accuracy. (author)

  2. Separation of zirconium through extraction in hydrochloric medium with tri-n-octilamine and its spectrophotometric determination with chloroanilic acid

    International Nuclear Information System (INIS)

    Floh, B.; Abrao, A.; Federgruen, L.

    1976-01-01

    A procedure is outlined for the spectrophotometric determination of zirconium using its complex with chloroanilic acid in HC10 4 2M. Interfering elements like Fe, Zn, U, Cy, Cd, Sb, Co, Pb, Hg, Tl, Pt, Au, Pd, Ga, In, Mo and W are previously extracted with tri-n-octylamine 7,5%-benzene from 4 M HCL. Then, the acid content of the solution is ascertained to 10 M HCL and zirconium is extracted with the amine. Nb is a strong interference, being extracted by the amine as well as zirconium and absorbing at the same region as zirconium chloroanilate. Zirconium is stripped from the organic phase with Na 2 CO 3 . The colour development is done with chloroanilic acid in 2 M HC10 4 and the measurements at 340 nm. The method allows the determination of 5 micrograms of Zr. The work curve covers the 0.2 - 2.0 μg Zr/mL range. The procedure is being applied to the determination of zirconium in several alloys and in samples containing zinc, magnesium, iron, aluminium, uranium and thorium [pt

  3. Application of titanium oxide nanotube films containing gold nanoparticles for the electroanalytical determination of ascorbic acid

    Energy Technology Data Exchange (ETDEWEB)

    Hosseini, Mir Ghasem, E-mail: mg-hosseini@tabrizu.ac.ir; Faraji, Masoud; Momeni, Mohamad Mohsen

    2011-03-31

    Au/TiO{sub 2}/Ti electrodes have been prepared by galvanic deposition of gold particles on TiO{sub 2} nanotube substrates. Titanium oxide nanotubes are fabricated by anodizing titanium foil in a Dimethyl Sulfoxide electrolyte containing fluoride. The scanning electron microscopy results indicated that gold particles are homogeneously deposited on the surface of TiO{sub 2} nanotubes. The TiO{sub 2} layers consist of individual tubes of about 40-80 nm diameters. The electro-catalytic behavior of Au/TiO{sub 2}/Ti and flat gold electrodes for the ascorbic acid electro-oxidation was studied by cyclic voltammetry. The results showed that the flat gold electrode is not suitable for the oxidation of ascorbic acid. However, the Au/TiO{sub 2}/Ti electrodes are shown to possess catalytic activity toward the oxidation reaction. Catalytic oxidation peak current showed a linear dependence on the ascorbic acid concentration and a linear calibration curve is obtained in the concentration range of 1-5 mM of ascorbic acid. Also, determination of ascorbic acid in real samples was evaluated. The obtained results were found to be satisfactory. Finally the effects of interference on the detection of ascorbic acid were investigated.

  4. Direct electrodeposition of gold nanotube arrays of rough and porous wall by cyclic voltammetry and its applications of simultaneous determination of ascorbic acid and uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Yang Guangming, E-mail: yangguangmingbs@126.com [Department of Resources and Environment, Baoshan University, Baoshan 678000 (China); Ling, Li [Department of Resources and Environment, Baoshan University, Baoshan 678000 (China); Jinhe, Jiang; Yunhui, Yang [College of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming 650092 (China)

    2012-08-01

    Gold nanotube arrays of rough and porous wall has been synthesized by direct electrodeposition with cyclic voltammetry utilizing anodic aluminum oxide template (AAO) and polycarbonate membrane (PC) during short time (only 3 min and 2 min, respectively). The mechanism of the direct electrodeposition of gold nanotube arrays by cyclic voltammetry (CV) has been discussed. The morphological characterizations of the gold nanotube arrays have been investigated by scanning electron microscopy (SEM). A simultaneous determination of ascorbic acid (AA) and uric acid (UA) by differential pulse voltammetry (DPV) was constructed by attaching gold nanotube arrays (using AAO) onto the surface of a glassy carbon electrode (GCE). The electrochemical behavior of AA and UA at this modified electrode has been studied by CV and differential pulse voltammetry (DPV). The sensor offers an excellent response for AA and UA and the linear response range for AA and UA were 1.02 Multiplication-Sign 10{sup -7}-5.23 Multiplication-Sign 10{sup -4} mol L{sup -1} and 1.43 Multiplication-Sign 10{sup -7}-4.64 Multiplication-Sign 10{sup -4} mol L{sup -1}, the detection limits were 1.12 Multiplication-Sign 10{sup -8} mol L{sup -1} and 2.24 Multiplication-Sign 10{sup -8} mol L{sup -1}, respectively. This sensor shows good regeneration, stability and selectivity and has been used for the determination of AA and UA in real human urine and serum samples with satisfied results. - Graphical abstract: The schematic diagram of formation of Au nanotube arrays (a) and the stepwise procedure of the sensor (b). Highlights: Black-Right-Pointing-Pointer Gold nanotubes array has been synthesized by cyclic voltammetry. Black-Right-Pointing-Pointer The mechanism of deposition of gold nanotube has been discussed. Black-Right-Pointing-Pointer A determination of ascorbic acid and uric acid was constructed by gold array. Black-Right-Pointing-Pointer A satisfied determination of samples can be obtained by this sensor.

  5. Single-column ion chromatography with determination of hydrazoic acid produced in spent nuclear fuel reprocessing

    International Nuclear Information System (INIS)

    Ma Guilan; Tan Shuping

    2006-01-01

    The reaction of hydrazine and its derivative with ammonium metavanadate may produce hydrazoic acid (HN 3 ). A single-column ion chromatography is used for the determination of HN 3 after neutralizing the rest acid in the sample with sodium hydroxide. Chromatography separation of HN 3 is carried out on a 25 cm x 0.46 cm (inside diameter) stainless steel column packed with Vydac IC302 ion Chromatography packing. The eluent is 1 mmol/L o-phthalic acid, and the ion is detected by conductivity detector. The detection limit in the presence chromatography is 5 μg/mL, the linear range is from 5 to 201 μg/mL, the linear correlation coefficient is 0.9994, respectively. The analysis accuracy is 2% for standard sample, and the detection limit is 51 μg/mL for HN 3 in the real sample. (authors)

  6. Uses and updating of the Benders method in the integer-mixed programming in the planning of the electric power systems expansion; Usos y actualizacion del metodo de Benders en la programacion entera-mixta y en la planeacion de la expansion de los sistemas electricos de potencia

    Energy Technology Data Exchange (ETDEWEB)

    De la Torre Vega, Eli

    1997-04-01

    of some potential improvements that the proposed method has. [Espanol] En el primer capitulo se presenta la deduccion de los cortes de Benders partiendo de las propiedades de la dualidad. Tambien se presentan las propiedades de los cortes de Benders asi como el algoritmo inicial de Benders para resolver cualquier problema de programacion lineal entera-mixta. En el segundo capitulo, se presenta el problema de la planeacion de la expansion de los medios de generacion y transmision en un sistema electrico de potencia, las distintas estructuras de la programacion matematica a que da lugar y como se puede adaptar el metodo de Benders a estas. En el tercer capitulo se presentan las aportaciones teoricas de este trabajo: a) Como inicializar el problema maestro para aprovechar la experiencia adquirida despues de haber resuelto un problema similar, de modo que se pueda resolver mas eficientemente, la sucesion de problemas de programacion lineal entero-mixtos que surgen al resolver el problema de la planeacion de la expansion de los medios de generacion y transmision en un sistema electrico de potencia. b) Como generar un problema maestro cuya solucion optima continua corresponda al optimo continuo del problema entero-mixto, de modo que la busqueda de soluciones enteras se realice en la vecindad del optimo continuo. c) Como generar una solucion entera, cercana al optimo continuo del problema entero-mixto, que tenga mucha probabilidad de ser factible, y que quizas sea la solucion optima entera, en un tiempo menor al que se requiere para resolverlo en forma exacta. Ademas, se presentan otras ideas que se le pueden incorporar al metodo de Benders. A fin de mostrar la efectividad de las ideas propuestas, en el capitulo 4 se presentan los resultados obtenidos al resolver varios problemas usando: 1. El metodo de Benders in actualizacion, 2. El metodo de Ramificacion y Acotamiento, 3. La actualizacion de Benders al agregar restricciones y 4. La actualizacion de Benders al considerar

  7. [Simultaneous determination of eight kinds of conjunct bile acids in human bile by R-HPLC].

    Science.gov (United States)

    Dai, Z; Tan, G; Qian, K; Chen, X

    1997-01-01

    A method for the simultaneous determination of eight kinds of conjunct bile acids in human bile was developed by HPLC. They were separated on a YWG-C18 (3 microns) column at 30 degrees C, with methanol/water (65/35, V/V, pH3.0) as mobile phase, and detection wavelength at UV 210 nm. The linear ranges were 50-1,000 microns.ml-1, the recoveries were 91.2%-108.6%. The biles of 30 cases with cholelithiasis cholecystolithiasis and 20 cases without gallstone were detected by HPLC. The results showed that the constitution of bile acids was different between patients with cholelithiasis cholecystolithiasis and patients without gallstone.

  8. Determination of the Molar Volume of Hydrogen from the Metal-Acid Reaction: An Experimental Alternative.

    Science.gov (United States)

    de Berg, Kevin; Chapman, Ken

    1996-01-01

    Describes an alternative technique for determining the molar volume of hydrogen from the metal-acid reaction in which the metal sample is encased in a specially prepared cage and a pipette filler is used to fill an inverted burette with water. Eliminates some difficulties encountered with the conventional technique. (JRH)

  9. FT-midIR determination of fatty acid profiles, including trans fatty acids, in bakery products after focused microwave-assisted Soxhlet extraction.

    Science.gov (United States)

    Ruiz-Jiménez, J; Priego-Capote, F; Luque de Castro, M D

    2006-08-01

    A study of the feasibility of Fourier transform medium infrared spectroscopy (FT-midIR) for analytical determination of fatty acid profiles, including trans fatty acids, is presented. The training and validation sets-75% (102 samples) and 25% (36 samples) of the samples once the spectral outliers have been removed-to develop FT-midIR general equations, were built with samples from 140 commercial and home-made bakery products. The concentration of the analytes in the samples used for this study is within the typical range found in these kinds of products. Both sets were independent; thus, the validation set was only used for testing the equations. The criterion used for the selection of the validation set was samples with the highest number of neighbours and the most separation between them (H/=0.90, SEP=1-1.5 SEL and R (2)=0.70-0.89, SEP=2-3 SEL, respectively. The results obtained with the proposed method were compared with those provided by the conventional method based on GC-MS. At 95% significance level, the differences between the values obtained for the different fatty acids were within the experimental error.

  10. A high-throughput microtiter plate based method for the determination of peracetic acid and hydrogen peroxide.

    Science.gov (United States)

    Putt, Karson S; Pugh, Randall B

    2013-01-01

    Peracetic acid is gaining usage in numerous industries who have found a myriad of uses for its antimicrobial activity. However, rapid high throughput quantitation methods for peracetic acid and hydrogen peroxide are lacking. Herein, we describe the development of a high-throughput microtiter plate based assay based upon the well known and trusted titration chemical reactions. The adaptation of these titration chemistries to rapid plate based absorbance methods for the sequential determination of hydrogen peroxide specifically and the total amount of peroxides present in solution are described. The results of these methods were compared to those of a standard titration and found to be in good agreement. Additionally, the utility of the developed method is demonstrated through the generation of degradation curves of both peracetic acid and hydrogen peroxide in a mixed solution.

  11. Separation of uranium and other metals from commercial phosphoric acid by ion-exchange and voltammetric determination of uranium

    International Nuclear Information System (INIS)

    Ferreira, J.B.C.; Carvalho, F.M.S. de; Abrao, A.

    1985-11-01

    The separation of metals from crude commercial phosphoric acid is achieved by simple dilution and percolation through a strong cationic ion exchanger. Uranium, calcium, magnesium, manganese, iron and aluminum are quantitatively fixed by the exchanger and can be detected or analysed after their complete elution with 6 M HCI. Titanium and zirconium are only partially retained. Specially for its separation and determination uranium is retained selectively by the resin from the phosphoric acid-EDTA solution, the column is washed with water and then eluted with hydrochloric acid. Uranium is analyzed by voltametry with the hanging drop mercury electrode. (Author) [pt

  12. Determination of Acid Dissociation Constants (pKa) of Bicyclic Thiohydantoin-Pyrrolidine Compounds in 20% Ethanol-Water Hydroorganic Solvent

    Science.gov (United States)

    Nural, Yahya; Döndaş, H. Ali; Sarı, Hayati; Atabey, Hasan; Belveren, Samet; Gemili, Müge

    2014-01-01

    The acid dissociation constants of potential bioactive fused ring thiohydantoin-pyrrolidine compounds were determined by potentiometric titration in 20% (v/v) ethanol-water mixed at 25 ± 0.1°C, at an ionic background of 0.1 mol/L of NaCl using the HYPERQUAD computer program. Proton affinities of potential donor atoms of the ligands were calculated by AM1 and PM3 semiempiric methods. We found, potentiometrically, three different acid dissociation constants for 1a–f. We suggest that these acid dissociation constants are related to the carboxyl, enol, and amino groups. PMID:24799905

  13. Determination of volatile, phenolic, organic acid and sugar components in a Turkish cv. Dortyol (Citrus sinensis L. Osbeck) orange juice.

    Science.gov (United States)

    Kelebek, Hasim; Selli, Serkan

    2011-08-15

    Orange flavour is the results of a natural combination of volatile compounds in a well-balanced system including sugars, acids and phenolic compounds. This paper reports the results of the first determination of aroma, organic acids, sugars, and phenolic components in Dortyol yerli orange juices. A total of 58 volatile components, including esters (nine), terpenes (19), terpenols (13), aldehydes (two), ketones (three), alcohols (four) and acids (eight) were identified and quantified in Dortyol yerli orange juice by GC-FID and GC-MS. Organic acids, sugars and phenolic compositions were also determined by HPLC methods. The major organic acid and sugar found were citric acid and sucrose, respectively. With regard to phenolics, 14 compounds were identified and quantified in the orange juice. Terpenes and terpenols were found as the main types of volatile components in Dortyol yerli orange juice. In terms of aroma contribution to orange juice, 12 compounds were prominent based on the odour activity values (OAVs). The highest OAV values were recorded for ethyl butanoate, nootkatone, linalool and DL-limonene. When we compare the obtained results of cv. Dortyol orange juice with the other orange juice varieties, the composition of Dortyol orange juice was similar to Valencia and Navel orange juices. Copyright © 2011 Society of Chemical Industry.

  14. Combined enzymatic and colorimetric method for determining the uronic acid and methylester content of pectin: Application to tomato products.

    Science.gov (United States)

    Anthon, Gordon E; Barrett, Diane M

    2008-09-01

    A simple procedure for determining the galacturonic acid and methanol contents of soluble and insoluble pectins, relying on enzymatic pectin hydrolysis and colorimetric quantification, is described. Pectin samples are incubated with a commercial pectinase preparation, Viscozyme, then the galacturonic acid content of the hydrolyzed pectin is quantified colorimetrically using a modification of the Cu reduction procedure originally described by Avigad and Milner. This modification, substituting the commonly used Folin-Ciocalteau reagent for the arsenic containing Nelson reagent, gives a response that is linear, sensitive, and selective for uronic acids over neutral sugars. This method also avoids the use of concentrated acids needed for the commonly used m-phenylphenol method. Methanol, released by the action of the pectin methylesterase found in the Viscozyme, is quantified using alcohol oxidase and Purpald. This combined enzymatic and colorimetric procedure correctly determined the galacturonic acid and methanol content of purified, soluble citrus pectin. Application of the procedure to water insoluble pectins was evaluated with water insoluble material from apples and oranges. In both cases good agreement was obtained between this method and commonly used methods based on chemical pectin hydrolysis. Good agreement between these procedures was also found in the analysis of both soluble and insoluble pectins from several tomato products. Copyright © 2008 Elsevier Ltd. All rights reserved.

  15. Evaluation of scission and crosslinking yields in γ-irradiated poly(acrylic acid) and poly(methacrylic acid) from weight- and Ζ-average molecular weights determined by sedimentation equilibrium

    International Nuclear Information System (INIS)

    Hill, D.J.T.; O'Donnell, J.H.; Winzor, C.L.; Winzor, D.J.

    1990-01-01

    Weight- and Ζ-average molecular weights, M-bar W (D) and M-bar Ζ (D), of poly(methacrylic acid) (PMMA) and poly(acrylic acid) (PAA) have been determined by sedimentation equilibrium in the ultracentrifuge after various doses D of γ-radiation in vacuum. Relationships between [M i (0)/M i (D)-1]/D and D (i=w or Ζ), derived recently by O'Donnell and coworkers, have been used to determine radiation chemical yields for scission and crosslinking of G(S)=6.0, G(X)=0 for PMAA and G(S)=0, G(X)=0.44 for PAA. Allowance was necessary for the effects of COOH decomposition on the average values of the molecular weight and partial specific volume for irradiated PAA. (author)

  16. Effect of intraarticular osmic acid on synovial membrane volume and inflammation, determined by magnetic resonance imaging

    DEFF Research Database (Denmark)

    Østergaard, Mikkel; Stoltenberg, M; Gideon, P

    1995-01-01

    The changes in MR-determined synovial membrane volume, early synovial enhancement, and cartilage and bone erosions after osmic acid knee synovectomy were studied. Gadolinium-DTPA enhanced magnetic resonance imaging (MRI) of 18 knees with persistent arthritis was performed before and 1 month after...

  17. Resonance light scattering technique for the determination of proteins with polymethacrylic acid (PMAA)

    Science.gov (United States)

    Chen, Yanhua; Gao, Dejiang; Tian, Yuan; Ai, Peng; Zhang, Hanqi; Yu, Aimin

    2007-07-01

    As a resonance light scattering (RLS) probe, the polyelectrolyte polymethacrylic acid (PMAA) was applied in this assay. The bovine serum albumin (BSA) and human serum albumin (HSA) were determined by the electrostatic interaction of PMAA and proteins. At pH 3.8 Na 2HPO 4-citric acid buffer solution, the RLS intensities of PMAA-BSA (HSA) system were greatly enhanced. The characteristic peaks were appeared at the wavelength 320, 546 and 594 nm. The optimization conditions of the reaction were also examined and selected. Under the selected conditions, the RLS intensities were proportional to the protein concentrations in the range of (0.0200-2.00) × 10 -6 mol/L for BSA and (0.0200-2.40) × 10 -6 mol/L for HSA. The influences of some foreign substances were also examined. The synthetic samples containing proteins and some real samples were analyzed and the results obtained were satisfactory.

  18. SHORT COMMUNICATION DETERMINATION OF AMINO ACIDS ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    ABSTRACT. Royal jelly (RJ) is popular among consumers around the world due to its perceived health benefits. The purpose of this study was to assess the levels of free and total amino acid profile as well as protein content in order to characterize Bulgarian RJ samples. A total of 17 fresh and commercial RJ samples from.

  19. Demographic, reproductive, and dietary determinants of perfluorooctane sulfonic (PFOS) and perfluorooctanoic acid (PFOA) concentrations in human colostrum

    NARCIS (Netherlands)

    Jusko, T.A.; Oktapodas, M.; Palkovičová Murinová, L.; Babjaková, J.; Verner, M.A.; DeWitt, J.C.; Babinská, K.; Thevenet-Morrison, K.; Čonka, K.; Drobná, B.; Thurston, S.W.; Lawrence, B.P.; Dozier, A.M.; Jarvinen-Seppo, K.M.; Patayová, H.; Trnovec, T.; Legler, J.; Hertz-Picciotto, I.; Lamoree, M.H.

    2016-01-01

    To determine demographic, reproductive, and maternal dietary factors that predict perfluoroalkyl substance (PFAS) concentrations in breast milk, we measured perfluorooctane sulfonic (PFOS) and perfluorooctanoic acid (PFOA) concentrations, using liquid chromatography-mass spectrometry, in 184

  20. Study and Elimination of the Interference of Aluminium on the Voltammetric Determination of Uranium with Chloranilic Acid. Application to the Determination of Uranium in Waters and Geological Samples

    International Nuclear Information System (INIS)

    Fernandez, C.; Sanchez, M.; Ballesteros, O.; Fernandez, M.; Clavero, M. A.; Gonzalez, A. M.

    2000-01-01

    The interference of aluminium during the voltammetric determination of uranium with 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone (chloranilic acid) has been investigated. The presence of aluminium originates a voltammetric signal due to its chloranilic acid complex at the same potential range as the uranium analytical signal appears. The interference of aluminium can be overcome by addition of an appropriate amount of sodium fluoride as complexing reagent. The determination of uranium by adsorptive stripping voltammetry (AdSV) can be carried out at concentration levels as low as 1 μg/L in the presence of 100 μg/L aluminium after the addition of 100μL of 0.1 mol/L NaF. The method can be applied to the determination of uranium in aluminium-containing waters and geological samples containing high aluminium levels. (Author) 19 refs

  1. Direct determination of creatinine based on poly(ethyleneimine)/phosphotungstic acid multilayer modified electrode.

    Science.gov (United States)

    Han, Ping; Xu, Shimei; Feng, Shun; Hao, Yanjun; Wang, Jide

    2016-05-01

    In this work, the direct determination of creatinine was achieved using a poly(ethyleneimine)/phosphotungstic acid multilayer modified electrode with the assistance of Copper(II) ions by cyclic voltammetry. The quantity of creatinine were determined by measuring the redox peak current of Cu(II)-creatinine complex/Cu(I)-creatinine complex. Factors affecting the response current of creatinine at the modified electrode were optimized. A linear relationship between the response current and the concentration of creatinine ranging from 0.125 to 62.5μM was obtained with a detection limit of 0.06μM. The proposed method was applied to determine creatinine in human urine, and satisfied results were gotten which was validated in accordance with high performance liquid chromatography. The proposed electrode provided a promising alternative in routine sensing for creatinine without enzymatic assistance. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Multi-wavelength spectrophotometric determination of acidity constant of some newly synthesized Schiff bases and their QSPR study

    Science.gov (United States)

    Hemmateenejad, Bahram; Emami, Leila; Sharghi, Hashem

    2010-01-01

    The acidity constants of some newly synthesized Schiff base derivatives were determined by hard-model based multivariate data analysis of the spectrophotometric data in the course of pH-metric titration in 50% (v/v) methanol-water binary solvent. The employed data analysis method was also able to extract the pure spectra and pH-dependent concentration profiles of the acid-base species. The molecules that possess different substituents (both electron donating and withdrawing) on the ortho-, meta- and para-positions of one of the phenyl ring showed variable acidity constants ranging from 8.77 to 11.07 whereas the parent molecule had an acidity constant of 10.25. To investigate the quantitative effects of changing of substitution pattern on the acidity constant, a quantitative structure-property relation analysis was conducted using substituent constants and molecular descriptor. Some models with high statistical quality (measured by cross-validation Q2) were obtained. It was found that the acidity constant of the studied molecules in the methanol-water mixed solvent not only is affected by electronic features of the solutes but also by the lipophilic interaction between methanol part of solvent and the deprotonated solutes.

  3. Rapid Determination of Bile Acids in Bile from Various Mammals by Reversed-Phase Ultra-Fast Liquid Chromatography.

    Science.gov (United States)

    Si, Gu Leng Ri; Yao, Peng; Shi, Luwen

    2015-08-01

    A valid and efficient reversed-phase ultra-fast liquid chromatography method was developed for the simultaneous determination of 13 bile acids in the bile of three mammal species, including rat, pig and human gallstone patients. Chromatographic separation was performed with a Shim-pack XR-ODS column, and the mobile phase consisted of acetonitrile and potassium phosphate buffer (pH 2.6) at a flow rate of 0.5 mL min(-1). The linear detection range of most bile acids ranged from 2 to 600 ng µL(-1) with a good correlation coefficient (>0.9995). The precision of each bile acid was bile acids were separated in 15 min with satisfactory resolution, and the total analysis time was 18 min, including equilibration. The method was successfully applied in rapid screening of bile samples from the three mammals. Significant metabolic frameworks of bile acids among various species were observed, whereas considerable quantitative variations in both inter- and intraspecies were also observed, especially for gallstone patients. Our results suggest that detecting the change of bile acid profiles could be applied for the diagnosis of gallstone disease. © Crown copyright 2014.

  4. Investigation of the luminescent properties of terbium-anthranilate complexes and application to the determination of anthranilic acid derivatives in aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Arnaud, N.; Georges, J

    2003-01-10

    The luminescent properties of terbium complexes with furosemide (FR), flufenamic (FF) acid, tolfenamic (TF) acid and mefenamic (MF) acid have been investigated in aqueous solutions. For all four compounds, complexation occurs when the carboxylic acid of the aminobenzoic group is dissociated and is greatly favoured in the presence of trioctylphosphine oxide as co-ligand and Triton X-100 as surfactant. Under optimum conditions, luminescence of the lanthanide ion is efficiently sensitised and the lifetime of the {sup 5}D{sub 4} resonance level of terbium in the complex is ranging between 1 and 1.9 ms, against 0.4 ms for the aqua ion. The sensitivity of the method for the determination of anthranilic acid derivatives is improved by one to two orders of magnitude with respect to that achieved using native fluorescence or terbium-sensitised luminescence in methanol. The limits of detection are 2x10{sup -10}, 5x10{sup -10} and 2x10{sup -9} mol l{sup -1} for flufenamic acid, furosemide and tolfenamic acid, and mefenamic acid, respectively, with within-run RSD values of less than 1%. The method has been applied to the determination of flufenamic acid in spiked calf sera with and without sample pretreatment. Depending on the method and the analyte concentration, the recovery was ranging between 83 and 113% and the lowest concentration attainable in serum samples was close to 1x10{sup -7} mol l{sup -1}.

  5. Control Methods Used in the Department of Metallurgy for Structure and Fuel Elements; Methodes de Controle Utilisees au Departement de Metallurgie pour les Elements de Structure et les Elements Combustibles; Metody kontrolya struktury toplivnykh ehlementov v departamente metallurgii; Metodos de Control Utilizados en el Departamento de Metalurgia para los Elementos Estructurales y Combustibles

    Energy Technology Data Exchange (ETDEWEB)

    Destribats, Marie-Therese; Allain, C.; Prot, A.; Thome, P. [Centre d' Etudes Nucleaires de Saclay (France)

    1965-09-15

    Studies of various reactor types undertaken by the Commissariat a l'energie atomique have led to the use and-development of many non-destructive methods of testing the various materials employed in their construction, and especially methods involving the use of X- and {gamma}-rays, ultrasonic waves and eddy currents. A summary is given below of the tests carried out during the construction of EDF (graphite gas) and EL 4 (heavy water) reactor types and of co-laminated elements. Emphasis is laid on certain typical aspects of these various methods, some of which are well known. EDF type: ultrasonic measurement of the wall thicknesses of uranium or uranium alloy tubes; gamma- radiographic detection of voids in the tubes; ultrasonic inspection following heat treatment of the tubes ultrasonic flaw detection (inclusions, pipes) in billets and rough casts for MgZr cladding; leak-tightness testing of slugs by helium eliquation. EL4 type: ultrasonic and eddy-current measurements of the wall thicknesses of Zircaloy pressure and guide tubes; ultrasonic inspection of Zircaloy pressure tubes and stainless-steel cladding tubes; in vacuo radiography of Be claddings; leak-tightness testing of pencils by helium eliquation. Co-laminated elements; cladding thickness measurements by pulsed eddy currents; determination of core position in tubes and plates, using X-rays, gamma counting and pulsed eddy currents; checking of fuel homogeneity by gamma counting; ultrasonic and gamma-radiographic flaw detection in ZrU billets; detection of unbonded areas in plates, using ultrasonic waves, pulsed eddy currents and resistivity measurements. The methods have been developed for industrial use. Several of the inspections already constitute routine manufacturing procedures, others will be introduced shortly and a further number are likely to come into use at a later date. (author) [French] Les etudes de divers types de reacteurs entreprises par le CEA ont conduit a utiliser et a mettre au point de

  6. Determination of glutamine and glutamic acid in mammalian cell cultures using tetrathiafulvalene modified enzyme electrodes.

    Science.gov (United States)

    Mulchandani, A; Bassi, A S

    1996-01-01

    Tetrathiafulvalene (TTF) mediated amperometric enzyme electrodes have been developed for the monitoring of L-glutamine and L-glutamic acid in growing mammalian cell cultures. The detection of glutamine was accomplished by a coupled enzyme system comprised of glutaminase plus glutamate oxidase, while the detection of glutamic acid was carried out by a single enzyme, glutamate oxidase. The appropriate enzyme(s) were immoblized on the Triton-X treated surface of tetrathiafulvalene modified carbon paste electrodes by adsorption, in conjunction with entrapment by an electrochemically deposited copolymer film of 1,3-phenylenediamine and resorcinol. Operating conditions for the glutamine enzyme electrode were optimized with respect to the amount of enzymes immoblized, pH, temperature and mobile phase flow rate for operation in a flow injection (FIA) system. When applied to glutamine and glutamic acid measurements in mammalian cell culture in FIA, the results obtained with enzyme electrodes were in excellent agreement with those determined by enzymatic analysis.

  7. Determination of long-chain fatty acids in serum by gas chromatography coupled to mass spectrometry

    International Nuclear Information System (INIS)

    Nuevas Paz, Lauro; Camayd Viera, Ivette

    2014-01-01

    The quantification of long-chain fatty acids is fundamental for the diagnosis of several peroxisome disorders, particularly those in which the β-oxidation peroxisome of fatty acids is affected. In this work the implementation of an analytical method for the determination of these markers in serum by gas chromatography coupled to mass spectrometry is described. Besides, samples from patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome were analyzed. The necessary experimental conditions were achieved for the separation and quantification of C22:0, C24:0 and C26:0 fatty acids in serum, which are biochemical markers of various peroxisome diseases. The application of this method allowed confirming the diagnosis of three patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome. The application of the method in daily practice will allow the Cuban medical system to count on a new laboratory parameter for the diagnosis of peroxisome disorders

  8. Determination of alcohols, ethers and organic acids in irradiated sweet potato wine by capillary gas chromatography

    International Nuclear Information System (INIS)

    Zhou Yingcai; Yuan Bihuai; Xu Peishu; Wang Xiuying

    1986-01-01

    Alcohols, ethers and organic acids in irradiated sweet potato wine have been determined with capillary GC. The results show that the contents of some components have changed after irradiation, but no new species are formed. The G values of the changed components have been calculated

  9. Hexuronic Acid Stereochemistry Determination in Chondroitin Sulfate Glycosaminoglycan Oligosaccharides by Electron Detachment Dissociation

    Science.gov (United States)

    Leach, Franklin E.; Ly, Mellisa; Laremore, Tatiana N.; Wolff, Jeremy J.; Perlow, Jacob; Linhardt, Robert J.; Amster, I. Jonathan

    2012-09-01

    Electron detachment dissociation (EDD) has previously provided stereo-specific product ions that allow for the assignment of the acidic C-5stereochemistry in heparan sulfate glycosaminoglycans (GAGs), but application of the same methodology to an epimer pair in the chondroitin sulfate glycoform class does not provide the same result. A series of experiments have been conducted in which glycosaminoglycan precursor ions are independently activated by electron detachment dissociation (EDD), electron induced dissociation (EID), and negative electron transfer dissociation (NETD) to assign the stereochemistry in chondroitin sulfate (CS) epimers and investigate the mechanisms for product ion formation during EDD in CS glycoforms. This approach allows for the assignment of electronic excitation products formed by EID and detachment products to radical pathways in NETD, both of which occur simultaneously during EDD. The uronic acid stereochemistry in electron detachment spectra produces intensity differences when assigned glycosidic and cross-ring cleavages are compared. The variations in the intensities of the doubly deprotonated 0,2X3 and Y3 ions have been shown to be indicative of CS-A/DS composition during the CID of binary mixtures. These ions can provide insight into the uronic acid composition of binary mixtures in EDD, but the relative abundances, although reproducible, are low compared with those in a CID spectrum acquired on an ion trap. The application of principal component analysis (PCA) presents a multivariate approach to determining the uronic acid stereochemistry spectra of these GAGs by taking advantage of the reproducible peak distributions produced by electron detachment.

  10. Sensitive determination of phenolic acids in extra-virgin olive oil by capillary zone electrophoresis.

    Science.gov (United States)

    Carrasco Pancorbo, Alegría; Cruces-Blanco, Carmen; Segura Carretero, Antonio; Fernández Gutiérrez, Alberto

    2004-11-03

    A sensitive, rapid, efficient, and reliable method for the separation and determination of phenolic acids by capillary zone electrophoresis has been carried out. A detailed method optimization was carried out to separate 14 different compounds by studying parameters such as pH, type and concentration of buffer, applied voltage, and injection time. The separation was performed within 16 min, using a 25 mM sodium borate buffer (pH 9.6) at 25 kV with 8 s of hydrodynamic injection. With this method and using a liquid-liquid extraction system, with recovery values around 95%, it has been possible to detect small quantities of phenolic acids in olive oil samples. This is apparently the first paper showing the quantification of this specific family of phenolic compounds in virgin olive oil samples.

  11. Determination of lactic acid level in systemic liquids in children with progressive encephalopathies.

    Science.gov (United States)

    Marszał, Elzbieta; Wojaczyńska-Stanek, Katarzyna; Pietruszewski, Jerzy; Emich-Widera, Ewa; Bielińska-Bujniewicz, Eugenia

    2002-03-01

    This article reports the results of research into the activities of lactic acid concentrations in the body fluids of children with progressive encephalopathies (PE) in comparison to patients with non-progressive encephalopathies (NPE) and those with non-progressive encephalopathies with concomitant epilepsy (NPEE). The study was designed to determine whether there is difference between the serum and CSF lactic acid concentrations in children with progressive encephalopathies (PE), static (non-progressive) encephalopathies (NPE) and non progressive encephalopathies with concomitant epilepsy (NPEE), and whether the clinical status correlates with the concentration of these biochemical markers in children with PE. The assessment involved 138 children of both sexes, whose age ranged between 8 months and 15 years, diagnosed and treated in the Neurology Department at the Pediatric Clinic of the Silesian Medical Academy in Katowice between 1995 and 1997. Lactate concentrations were determined in serum and cerebro-spinal fluid and analyzed statistically. The findings showed higher serum and CSF concentrations in children with PE than in patients who manifested non-progressive forms of encephalopathy. The degree of clinical symptom aggravation in PE children was likewise analyzed and compared to the values of lactate concentrations in body fluids; however, no correlation was found between these parameters. Children with progressive encephalopathies present higher lactate concentrations in serum and cerebrospinal fluid than patients with static (non-progressive) encephalopathy.

  12. Quantitative determination of deoxyribonucleic acid in rat brain

    Science.gov (United States)

    Penn, N. W.; Suwalski, R.

    1969-01-01

    1. A procedure is given for spectrophotometric analysis of rat brain DNA after its resolution into component bases. Amounts of tissue in the range 50–100mg. can be used. 2. The amount of DNA obtained by the present method is 80% greater than that reported for rat brain by a previous procedure specific for DNA thymine. Identity of the material is established by the base ratios of purines and pyrimidines. The features responsible for the higher yield are the presence of dioxan during alkaline hydrolysis of tissue, the determination of the optimum concentration of potassium hydroxide in this step and omission of organic washes of the initial acid-precipitated residues. 3. The requirement for dioxan during alkaline hydrolysis suggests a possible association of brain DNA with lipid. The concentration of potassium hydroxide that gives maximum yield is 0·1m, indicating that there may be internucleotide linkages in this DNA that are more sensitive to alkali than those of liver or thymus DNA. 4. This procedure gives low yields of DNA from liver. It is not suitable for analysis of the DNA from this tissue. PMID:5353529

  13. Poly(amidosulfonic acid) modified glassy carbon electrode for determination of isoniazid in pharmaceuticals.

    Science.gov (United States)

    Yang, Gongjun; Wang, Cunxiao; Zhang, Rui; Wang, Chenying; Qu, Qishu; Hu, Xiaoya

    2008-06-01

    Amidosulfonic acid was electropolymerized by cyclic voltammetry onto the surface of glassy carbon electrode (GCE) to fabricate the chemically modified electrode, which showed high stability, good selectivity and reproducibility for determination of isoniazid. The modified electrode showed an excellent electrocatalytical effect on the oxidation of isoniazid. Under the optimum conditions, there was a good linear relationship between anodic peak current and isoniazid concentration in the range of 5.0 x 10(-8)- 1.0 x 10(-5) M, and a detection limit of 1.0 x 10(-8) M (S/N = 3) was obtained after 120 s at the accumulation potential of - 0.2 V (vs. SCE). This developed method had been applied to the direct determination of isoniazid in injection and tablet samples with satisfactory results.

  14. Determination of critical pH and Al concentration of acidic Ultisols for wheat and canola crops

    Science.gov (United States)

    Abdulaha-Al Baquy, M.; Li, Jiu-Yu; Xu, Chen-Yang; Mehmood, Khalid; Xu, Ren-Kou

    2017-02-01

    Soil acidity has become a principal constraint in dry land crop production systems of acidic Ultisols in tropical and subtropical regions of southern China, where winter wheat and canola are cultivated as important rotational crops. There is little information on the determination of critical soil pH as well as aluminium (Al) concentration for wheat and canola crops. The objective of this study is to determine the critical soil pH and exchangeable aluminium concentration (AlKCl) for wheat and canola production. Two pot cultures with two Ultisols from Hunan and Anhui (SE China) were conducted for wheat and canola crops in a controlled growth chamber. Aluminium sulfate (Al2(SO4)3) and hydrated lime (Ca(OH)2) were used to obtain the target soil pH levels from 3.7 (Hunan) and 3.97 (Anhui) to 6.5. Plant height, shoot dry weight, root dry weight, and chlorophyll content (SPAD value) of wheat and canola were adversely affected by soil acidity in both locations. The critical soil pH and AlKCl of the Ultisol from Hunan for wheat were 5.29 and 0.56 cmol kg-1, respectively. At Anhui, the threshold soil pH and AlKCl for wheat were 4.66 and 1.72 cmol kg-1, respectively. On the other hand, the critical soil pH for canola was 5.65 and 4.87 for the Ultisols from Hunan and Anhui, respectively. The critical soil exchangeable Al for canola cannot be determined from the experiment of this study. The results suggested that the critical soil pH and AlKCl varied between different locations for the same variety of crop, due to the different soil types and their other soil chemical properties. The critical soil pH for canola was higher than that for wheat for both Ultisols, and thus canola was more sensitive to soil acidity. Therefore, we recommend that liming should be undertaken to increase soil pH if it falls below these critical soil pH levels for wheat and canola production.

  15. Gallic Acid: Review of the Methods of Determination and Quantification.

    Science.gov (United States)

    Fernandes, Felipe Hugo Alencar; Salgado, Hérida Regina Nunes

    2016-05-03

    Gallic acid (3,4,5 trihydroxybenzoic acid) is a secondary metabolite present in most plants. This metabolite is known to exhibit a range of bioactivities including antioxidant, antimicrobial, anti-inflammatory, and anticancer. There are various methods to analyze gallic acid including spectrometry, chromatography, and capillary electrophoresis, among others. They have been developed to identify and quantify this active ingredient in most biological matrices. The aim of this article is to review the available information on analytical methods for gallic acid, as well as presenting the advantages and limitations of each technique.

  16. Rich biotin content in lignocellulose biomass plays the key role in determining cellulosic glutamic acid accumulation by Corynebacterium glutamicum.

    Science.gov (United States)

    Wen, Jingbai; Xiao, Yanqiu; Liu, Ting; Gao, Qiuqiang; Bao, Jie

    2018-01-01

    Lignocellulose is one of the most promising alternative feedstocks for glutamic acid production as commodity building block chemical, but the efforts by the dominant industrial fermentation strain Corynebacterium glutamicum failed for accumulating glutamic acid using lignocellulose feedstock. We identified the existence of surprisingly high biotin concentration in corn stover hydrolysate as the determining factor for the failure of glutamic acid accumulation by Corynebacterium glutamicum . Under excessive biotin content, induction by penicillin resulted in 41.7 ± 0.1 g/L of glutamic acid with the yield of 0.50 g glutamic acid/g glucose. Our further investigation revealed that corn stover contained 353 ± 16 μg of biotin per kg dry solids, approximately one order of magnitude greater than the biotin in corn grain. Most of the biotin remained stable during the biorefining chain and the rich biotin content in corn stover hydrolysate almost completely blocked the glutamic acid accumulation. This rich biotin existence was found to be a common phenomenon in the wide range of lignocellulose biomass and this may be the key reason why the previous studies failed in cellulosic glutamic acid fermentation from lignocellulose biomass. The extended recording of the complete members of all eight vitamin B compounds in lignocellulose biomass further reveals that the major vitamin B members were also under the high concentration levels even after harsh pretreatment. The high content of biotin in wide range of lignocellulose biomass feedstocks and the corresponding hydrolysates was discovered and it was found to be the key factor in determining the cellulosic glutamic acid accumulation. The highly reserved biotin and the high content of their other vitamin B compounds in biorefining process might act as the potential nutrients to biorefining fermentations. This study creates a new insight that lignocellulose biorefining not only generates inhibitors, but also keeps nutrients

  17. A high-throughput microtiter plate based method for the determination of peracetic acid and hydrogen peroxide.

    Directory of Open Access Journals (Sweden)

    Karson S Putt

    Full Text Available Peracetic acid is gaining usage in numerous industries who have found a myriad of uses for its antimicrobial activity. However, rapid high throughput quantitation methods for peracetic acid and hydrogen peroxide are lacking. Herein, we describe the development of a high-throughput microtiter plate based assay based upon the well known and trusted titration chemical reactions. The adaptation of these titration chemistries to rapid plate based absorbance methods for the sequential determination of hydrogen peroxide specifically and the total amount of peroxides present in solution are described. The results of these methods were compared to those of a standard titration and found to be in good agreement. Additionally, the utility of the developed method is demonstrated through the generation of degradation curves of both peracetic acid and hydrogen peroxide in a mixed solution.

  18. Simultaneous determination of amino acids and carbohydrates in culture media of Clostridium thermocellum by valve-switching ion chromatography.

    Science.gov (United States)

    Fa, Yun; Yang, Haiyan; Ji, Chengshuai; Cui, He; Zhu, Xinshu; Du, Juan; Gao, Jun

    2013-10-10

    An improved method for the simultaneous determination of 20 amino acids and 7 carbohydrates using one-valve switching after injection, ion chromatography, and integrated pulsed amperometric detection is proposed. The resolution of the amino acids and carbohydrates in the cation trap column was investigated. In addition, parameters including flow liquid type, flow rate, concentration, and valve-switch timing were optimized. The method is time-saving, effective, and accurate for the simultaneous separation of amino acids and carbohydrates, with a mean correlation coefficient of >0.99 and repeatability of 0.5-4.6% for eight replicates. The method was successfully applied in the analysis of amino acids and carbohydrates in aseptic media and in extracellular culture media of three phenotypes of Clostridium thermocellum. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Ibotenic acid and thioibotenic acid

    DEFF Research Database (Denmark)

    Hermit, Mette B; Greenwood, Jeremy R; Nielsen, Birgitte

    2004-01-01

    In this study, we have determined and compared the pharmacological profiles of ibotenic acid and its isothiazole analogue thioibotenic acid at native rat ionotropic glutamate (iGlu) receptors and at recombinant rat metabotropic glutamate (mGlu) receptors expressed in mammalian cell lines....... Thioibotenic acid has a distinct pharmacological profile at group III mGlu receptors compared with the closely structurally related ibotenic acid; the former is a potent (low microm) agonist, whereas the latter is inactive. By comparing the conformational energy profiles of ibotenic and thioibotenic acid...... with the conformations preferred by the ligands upon docking to mGlu1 and models of the other mGlu subtypes, we propose that unlike other subtypes, group III mGlu receptor binding sites require a ligand conformation at an energy level which is prohibitively expensive for ibotenic acid, but not for thioibotenic acid...

  20. Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

    Science.gov (United States)

    Rezende, Helen Cristine; Coelho, Nivia Maria Melo

    2014-01-01

    An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

  1. Simplified method for gravimetric determination of zirconium or hafnium with α-hydroxy carboxylic acids

    International Nuclear Information System (INIS)

    Barbieri, R.S.; Rocha, J.C.; Terra, V.R.; Marques Netto, A.

    1989-01-01

    The conditions for gravimetric determination of zirconium or hafnium by glicoloc acids derivatives were studied by thermogravimetric analysis. The method utilized shownd that after precipitation, washing and drying of precipitates at 150 o C, the resulting solid was weighed in the form of [M (RCH(OH)COO) 4 ] (M = Zr, Hf; R + C 6 H 5 , β-C 10 H 7 , p-BrC 6 H 4 ). (author)

  2. Development and validation of a method for the determination of folic acid in different pharmaceutical formulations using derivative spectrophotometry

    Directory of Open Access Journals (Sweden)

    Marcos Vinícius de Moura Ribeiro

    Full Text Available ABSTRACT Folic acid is a B complex water-soluble vitamin that is essential to humans, and its deficiency can cause problems including congenital malformations in the fetus as well as heart disease. Most countries affected by diseases associated with a lack of folic acid now supplement foods with the vitamin. There is therefore a need for the development of new analytical procedures able to determine folic acid present in different matrices. This work describes the development of zero order and first order derivative spectrophotometric methods for the determination of folic acid in different pharmaceutical formulations, using 0.1 mol L-1 NaOH as solvent. The methods are shown to be simple, selective, and robust. Good linearity was achieved, with correction coefficients ≥0.9996 and limits of detection and quantification ranging from 0.64 to 0.75 and from 1.80 to 2.85 mg L-1, respectively. Recoveries of 98-104% were obtained in accuracy tests, and precision (as RSD was between 0.2 and 4.8%. The methods can be used in routine analyses for quality control purposes, offering an alternative to the procedures already reported in the literature.

  3. Voltammetric Determination of Thiodiglycolic Acid in Urine

    Czech Academy of Sciences Publication Activity Database

    Dlasková, Z.; Navrátil, Tomáš; Heyrovský, Michael; Pelclová, D.; Novotný, Ladislav

    2003-01-01

    Roč. 375, - (2003), s. 164-168 ISSN 1618-2642 Institutional research plan: CEZ:AV0Z4040901 Keywords : urine * thioglycolic acid * voltammetry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.715, year: 2003

  4. Multielement Determination of Major-to Ultratrace Elements in a Cabbage, Spinach, and the Japanese Radish by ICP-AES After Acid Digestion

    OpenAIRE

    畑山, 友紀; 奴田原, 杏奈; 藤井, 和美; 西島, 基弘; ハタヤマ, ユキ; ヌタハラ, アンナ; フジイ, カズミ; ニシジマ, モトヒロ; Yuki, Hatayama; anna, Nutahara; Kazumi, Fujii; Motohiro, Nishijima

    2011-01-01

    A multi-element determination in a cabbage, spinach, and the Japanese radish was carried out by inductively coupled plasma atomic emission spectrometry (ICP). We investigated whether there was a difference in content according to the part of the vegetables. The dried vegetables (0.5g) were digested with nitric acid and with hydrogen peroxide acid in a resolution device As a result, about 9 elements were successfully determined. The values of the coefficient of variance for part interval by ea...

  5. Electrochemical Behavior and Determination of Chlorogenic Acid Based on Multi-Walled Carbon Nanotubes Modified Screen-Printed Electrode

    Directory of Open Access Journals (Sweden)

    Xiaoyan Ma

    2016-10-01

    Full Text Available In this paper, the multi-walled carbon nanotubes modified screen-printed electrode (MWCNTs/SPE was prepared and the MWCNTs/SPE was employed for the electrochemical determination of the antioxidant substance chlorogenic acids (CGAs. A pair of well-defined redox peaks of CGA was observed at the MWCNTs/SPE in 0.10 mol/L acetic acid-sodium acetate buffer (pH 6.2 and the electrode process was adsorption-controlled. Cyclic voltammetry (CV and differential pulse voltammetry (DPV methods for the determination of CGA were proposed based on the MWCNTs/SPE. Under the optimal conditions, the proposed method exhibited linear ranges from 0.17 to 15.8 µg/mL, and the linear regression equation was Ipa (µA = 4.1993 C (×10−5 mol/L + 1.1039 (r = 0.9976 and the detection limit for CGA could reach 0.12 µg/mL. The recovery of matrine was 94.74%–106.65% (RSD = 2.92% in coffee beans. The proposed method is quick, sensitive, reliable, and can be used for the determination of CGA.

  6. Rapid determination of ginkgolic acids in Ginkgo biloba kernels and leaves by direct analysis in real time-mass spectrometry.

    Science.gov (United States)

    Huang, Zhongping; Xu, Yueting; Huang, Yilei; Liu, Charles; Jiang, Kezhi; Wang, Lili

    2017-12-01

    A novel method based on direct analysis in real time integrated with mass spectrometry was established and applied into rapid determination of ginkgolic acids in Ginkgo biloba kernels and leaves. Instrument parameter settings were optimized to obtain the sensitive and accurate determination of ginkgolic acids. At the sample introduction speed of 0.2 mm/s, high intensity of [M-H] - ions for ginkgolic acids were observed in the negative ion mode by utilization of high-purity helium gas at 450°C. Two microliters of methanol extract of G. biloba kernels or leaves dropped on the surface of Quick-Strip module was analyzed after solvent evaporated to dryness. A series of standard solutions of ginkgolic acid 13:0 in the range of 2-50 mg/L were analyzed with a correlation coefficient r = 0.9981 and relative standard deviation (n = 5) from 12.5 to 13.7%. The limit of detection was 0.5 mg/L. The results of direct analysis in real time-mass spectrometry were in agreement with those observed by thermochemolysis gas chromatography. The proposed method demonstrated significant potential in the application of the high-throughput screening and rapid analysis for ginkgolic acids in dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Disintegration-Rate Determination by 4 {pi} Counting; Determination du taux de desintegrations par comptage 4 {pi}; Opredelenie skorosti raspada pri pomotsi 4 {pi} schetchikov; Determinacion de la velocidad de desintegracion por recuento 4 {pi}

    Energy Technology Data Exchange (ETDEWEB)

    Pate, Brian D [Chemistry Department, Washington University, St. Louis, MO (United States)

    1960-06-15

    The history of the development of the 4 {pi} counting method is reviewed. The unique properties of the 4 {pi} counter system are described and the criteria are specified which place disintegration rate measurements, made with the system, on an absolute basis. The types of radioactive decay process to which the method is applicable are outlined, together with the various errors to which a given measurement is liable. Departure of response probability from unity, absorption of radiation in the source-mounting system, and source self-absorption are discussed in detail. (author) [French] L'auteur fait l'historique des progres de la methode de comptage 4 {pi}. Il decrit les proprietes remarquables du dispositif de comptage 4 {pi} et precise les conditions dans lesquelles les mesures du taux de desintegration se font avec ce dispositif sur une base absolue. Il donne un apercu des types de processus de desintegration radioactive, ainsi que de diverses erreurs auxquelles est sujette une mesure donnee. Il examine en detail le cas ou la probabilite de reponse s'ecarte de l'unite, l'absorption des rayonnements dans le support de la source et l'autoabsorption de la source. (author) [Spanish] En la memoria el autor expone el desarrollo del metodo de recuento 4 {pi}. Describe las caracteristicas particulares de este metodo y explica las razones por las que las mediciones de la velocidad de desintegracion efectuadas segun ese procedimiento tienen un caracter absoluto. Se indican, asimismo, los tipos de procesos de desintegracion radiactiva a los que se puede aplicar el metodo, asi como los diferentes defectos de que puede adolecer una medicion determinada. Tambien se estudia detenidamente el caso en que la probabilidad de respuesta no es igual a la unidad, la absorcion de radiaciones en el soporte de la fuente y la autoabsorcion de la misma. (author) [Russian] Daetsya obzor istorii razvitiya metoda scheta s pomoshch'yu 4 {pi} schetchikov. Privoditsya opisanie unikal'nykh svojstv

  8. Simultaneous determination of flavonoids, isochlorogenic acids and triterpenoids in Ilex hainanensis Using high performance liquid chromatography coupled with diode array and evaporative light scattering detection.

    Science.gov (United States)

    Peng, Bo; Qiao, Chun-Feng; Zhao, Jing; Huang, Wei-Hua; Hu, De-Jun; Liu, Hua-Gang; Li, Shao-Ping

    2013-03-04

    A high performance liquid chromatography coupled with diode array and evaporative light scattering detection (HPLC-DAD-ELSD) method for simultaneous determination of eight major bioactive compounds including two flavonoids (rutin and eriodictyol-7-O-β-D-glucopyranoside), two isochlorogenic acids (isochlorogenic acid A and isochlorogenic acid C) and four triterpenoids (ilexhainanoside D, ilexsaponin A1, ilexgenin A and ursolic acid) in Ilex hainanensis has been developed for the first time. The 283 nm wavelength was chosen for determination of two flavonoids and two isochlorogenic acids. ELSD was applied to determine four triterpenoids. The analysis was performed on an Agilent Zorbax SB-C18 column (250 × 4.6 mm i.d., 5 µm) with gradient elution of 0.2% formic acid in water and acetonitrile. The method was validated for linearity, limit of detection, limit of quantification, precision, repeatability and accuracy. The proposed method has been successfully applied for simultaneous quantification of the analytes in four samples of Ilex hainanensis, which is helpful for quality control of this plant.

  9. Contributions te the study of methods and factors affecting the spectrophotometric determination of boron traces with carmin uranium compounds; Contribucion al estudio del metodo y factores que afectan a la determinacion espectrofotometrica de trazas de boro con Carmin en compuestos de uranio

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez Cellini, R; Gasco Sanchez, L

    1956-07-01

    The study of some factors affecting the spectrophotometric determination of boron traces with carmin is made; the influence of carmin from different origin, the stability of complex carmin-boric acid in relation with the sulphuric acid concentration, the interference produced by ion nitrate, and the ion uraline and light influence are discussed. (Author) 36 refs.

  10. A novel method for the determination of ascorbic acid and antioxidant capacity in Opuntia ficus indica using in vivo microdialysis.

    Science.gov (United States)

    Pretti, L; Bazzu, G; Serra, P A; Nieddu, G

    2014-03-15

    A simple and rapid method was developed for in vivo simultaneous determination of ascorbic-acid and antioxidant capacity in microdialysates from cladodes of Opuntia ficus-indica (L.) Miller. The method is verified in water-stressed plants, as compared with a well-watered test controls. The microdialysis probe construction and insertion procedure was specifically developed to minimise the tissue trauma of the plant and to obtain optimal dialysis performance. Microdialysis was performed using a flow rate of 3 μL/min and the samples were analysed by HPLC coupled to electrochemical detection of ascorbic-acid and DPPH-determined antioxidant capacity. Our data indicate exponential decay of the concentrations of the analysed compounds as a function of microdialysis sampling time. Water-stressed Opuntia show decreased ascorbic acid levels and increased the others antioxidants. Copyright © 2013 Elsevier Ltd. All rights reserved.

  11. Titrimetric application of 2-bromo-bis-1,10-phenanthroline-copper (II) bromide as a titrant in determination of ascorbic acid in pure form, fruits and vegetables

    International Nuclear Information System (INIS)

    Oladeji, O.

    2016-01-01

    Ascorbic acid is very important to man and the consumption has been linked to the prevention of degenerative diseases such as scurvy and serves as an antioxidants. There have been different approaches in the determination of ascorbic acid in fruits and vegetable. In recent times, new methods were introduced by scientists. Therefore, in order to prove the authenticity of these methods, the concentrations obtained were compared with the conventional methods. The results show that orange has maximum ascorbic acid content when compared to cashew and in vegetables Vermonia baldwinii has maximum and Solanium incanum has low ascorbic acid content. The amount of ascorbic acid determined by 2, 6-dichlorophenol-indophenol and copper (II) complex (2-bromo-bis-1, 10 phenanthroline-copper (II) bromide) are comparable.Therefore, 2-bromo-bis-1, 10-phenanthroline-copper (II) bromide can serve as a titrant in titrimetric determination of ascorbic acid in pure form, fruits and vegetables. (author)

  12. Differential pulse polarographic determination of trace antimony in standard biological samples after preconcentration using 2-nitroso-1-naphthol-4-sulfonic acid

    International Nuclear Information System (INIS)

    Taher, M. A.

    2003-01-01

    A highly selective, rapid and economical differential polarographic method has been developed for the determination of trace amounts of antimony in various standard alloys and biological samples after of its 2-naphthol-4 sulfonic acid tetradecyl dimethylbenzylammonium chloride on microcrystalline naphthalene in the ph range of 7.5-11.0. After filtration, the solid mass is shaken with 8-10 ml of 1 M hydrochloric acid (with preconcentration factor of 10) and antimony is determined by differential pulse polarography. Antimony can alternatively be quantitatively absorbed on 2-nitroso-1-naphthol-4-sulfonic acid tetradecyl dimethylbenzylammonium-naphthalene absorbed packed in a column (with preconcentration factor of 30) and determined similarly. In this case, 1.5 μg of antimony can be concentrated in a column from 300 ml of aqueous sample, where its concentration is as low as 5 ng/ml. Characterization of the electro active process included an examination of the degree of reversibility. The results show that the irreversibility of antimony. Various parameters such as the effect of ph, volume of aqueous phase, HCl concentration, reagent concentration, naphthalene concentration, shaking time and interference of a number of metal ions on the determination of antimony have been studied in detail to optimize the conditions for determination in standard alloys and standard biological samples

  13. Hollow Fiber Supported Liquid Membrane Extraction Combined with HPLC-UV for Simultaneous Preconcentration and Determination of Urinary Hippuric Acid and Mandelic Acid

    Directory of Open Access Journals (Sweden)

    Abdulrahman Bahrami

    2017-02-01

    Full Text Available This work describes a new extraction method with hollow-fiber liquid-phase microextraction based on facilitated pH gradient transport for analyzing hippuric acid and mandelic acid in aqueous samples. The factors affecting the metabolites extraction were optimized as follows: the volume of sample solution was 10 mL with pH 2 containing 0.5 mol·L−1 sodium chloride, liquid membrane containing 1-octanol with 20% (w/v tributyl phosphate as the carrier, the time of extraction was 150 min, and stirring rate was 500 rpm. The organic phase immobilized in the pores of a hollow fiber was back-extracted into 24 µL of a solution containing sodium carbonate with pH 11, which was placed inside the lumen of the fiber. Under optimized conditions, the high enrichment factors of 172 and 195 folds, detection limit of 0.007 and 0.009 µg·mL−1 were obtained. The relative standard deviation (RSD (% values for intra- and inter-day precisions were calculated at 2.5%–8.2% and 4.1%–10.7%, respectively. The proposed method was successfully applied to the analysis of these metabolites in real urine samples. The results indicated that hollow-fiber liquid-phase microextraction (HF-LPME based on facilitated pH gradient transport can be used as a sensitive and effective method for the determination of mandelic acid and hippuric acid in urine specimens.

  14. [Determination of fatty acids in natural cream and artificial cream by comprehensive two-dimensional gas chromatography-mass spectrometry].

    Science.gov (United States)

    Zhou, Ruize; Zhou, Ya; Mao, Ting; Jiang, Jie

    2018-01-08

    A method for the determination of 37 fatty acids in natural cream and artificial cream was developed by comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS). The samples were extracted with toluene and acetyl chloride-methanol (1:9,v/v) solution was added to the extract for fat esterification. Finally, the fatty acids were analyzed by GC×GC-MS. The GC conditions were as follows:a DB-5 column (30 m×0.25 mm×0.25 μm) was set as the 1st dimensional column and a BPX-50 column (2.5 m×0.1 mm×0.25 μm) was the 2nd dimensional column. The primary oven temperature was programmed from 50℃ (held for 2 min) to 180℃ at a rate of 20℃/min, followed by an increase to 250℃ at 2.5℃/min, then raised up to 300℃ (held for 5 min) at 3℃/min. The ion source temperature was 200℃ with auxiliary temperature of 300℃ in scan mode. All fatty acids were separated effectively and determined accurately while the modulation period was 5s and the scan range of MS was m/z 40-385. This procedure was applied to analyze the fatty acids in commercial natural cream and artificial cream from Chinese markets, among which we found the characteristic components in different kinds of samples. Compared with gas chromatography-flame ionization detector (GC-FID), GC×GC-MS method was more sensitive and more components of fatty acids were detected. Conclusively, this work suggests a new technical approach in analyzing fatty acids in natural cream and artificial cream, which is meaningful to ensure the quality identification and safety of natural cream.

  15. Determination of free fatty acids in pharmaceutical lipids by ¹H NMR and comparison with the classical acid value.

    Science.gov (United States)

    Skiera, Christina; Steliopoulos, Panagiotis; Kuballa, Thomas; Diehl, Bernd; Holzgrabe, Ulrike

    2014-05-01

    Indices like acid value, peroxide value, and saponification value play an important role in quality control and identification of lipids. Requirements on these parameters are given by the monographs of the European pharmacopeia. (1)H NMR spectroscopy provides a fast and simple alternative to these classical approaches. In the present work a new (1)H NMR approach to determine the acid value is described. The method was validated using a statistical approach based on a variance components model. The performance under repeatability and in-house reproducibility conditions was assessed. We applied this (1)H NMR assay to a wide range of different fatty oils. A total of 305 oil and fat samples were examined by both the classical and the NMR method. Except for hard fat, the data obtained by the two methods were in good agreement. The (1)H NMR method was adapted to analyse waxes and oleyloleat. Furthermore, the effect of solvent and in the case of castor oil the effect of the oil matrix on line broadening and chemical shift of the carboxyl group signal are discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Complexometric determination of trivalent rare earths and actinides with diethylene-triaminepentaacetic acid

    International Nuclear Information System (INIS)

    Timofeev, G.A.; Simakin, G.A.; Baklanova, P.F.; Kuznetsov, G.F.; Ivanov, V.I.

    1976-01-01

    Optimal conditions have been found for the separate quantitative determination of 200 to 500 mcg of trivalent Eu, La, Nd, Pr, Am and Cm by complexometric titration with diethylenetriaminepentaacetic acid. The final titration point (FTP) has been determined by using one of the following three methods, namely by visual inspection with the aid of xylene orange as an indicator, spectrophotometrically at pH 4.5-4.7 with xylene orange and potentiometrically at pH 4.0-5.5 through the backward titration of the excess complexone with the solution of Fe(3) in HNO 3 . The relative standard errors Ssub(r)=0.004 (Eu), 0.011 Cm with the visual indication of FTP; Ssub(r)=0.005 (Am) with the spectrophotometric indication of FTP; Ssub(r)=0.0O9 (Eu), 0.011 (Pr) and 0.02 (Am) with the potentiometric indication of FTP. Determination of trivalent lanthanides and actinoids is adversely affected by tetravalent actinoids, Zr, U(6), Hg(2) and Fe(3). Titration conditions chosen have been checked in the analysis of the mixture containing the sum of trivalent rare earths, Am and Cm [ru

  17. Determination of underivatized amino acids to evaluate quality of beer by capillary electrophoresis with online sweeping technique.

    Science.gov (United States)

    Luo, Tian; Ke, Jing; Xie, Yunfei; Dong, Yuming

    2017-10-01

    Capillary electrophoresis (CE) with ultraviolet detection was applied to determine underivatized amino acids in beer, based on the coordination interaction of copper ions and amino acids. An online sweeping technique was combined with CE to improve detection sensitivity. Using the United Nations Food Agriculture Organization/World Health Organization model of essential amino acid pattern and flavor of amino acids, the quality and taste in three kinds of beer were evaluated. It was found that Beer2 had higher quality than the other two kinds and the content of phenylalanine, proline, serine, and isoleucine was relatively large in all three kinds of beers with a great influence on beer flavor. Optimal conditions for separation were as follows: 50mM CuSO 4 at pH 4.40 as buffer; total length of fused silica capillary, 73 cm; effective length, 65 cm; separation voltage, 22.5 kV; and optimized sweeping condition, 70 seconds. In the appropriate range, linearity (r 2  > 0.9989), precision with a relative standard deviation amino acids in beer and to perform quantitative analysis directly without derivatization for the first time. Copyright © 2017. Published by Elsevier B.V.

  18. Polymorphisms in the fatty acid desaturase genes and diet are important determinants of infant docosahexaenoic acid status

    DEFF Research Database (Denmark)

    Lauritzen, L.; Harsløf, L.; Larsen, L.H.

    2013-01-01

    Tissue docosahexaenoic acid (DHA) accretion in early infancy is supported by DHA in breast-milk and may thus decrease once complementary feeding takes over. Endogenous synthesis of DHA from alphalinolenic acid is low and polymorphisms in the genes that encodes the fatty acid desaturases (FADS) ha...

  19. Spectrometric determination of clinically relevant fatty acids in the blood serum

    Science.gov (United States)

    Kalinin, A. V.; Krasheninnikov, V. N.; Sviridov, A. P.; Titov, V. N.

    2017-01-01

    The content of fatty acid (FA) triglycerides in food and biological media is predicting traditionally using gas and liquid chromatographic methods. Named techniques aren't available for clinical labs due to their complexity. So, our objective was to develop the method and apparatus for rapid assay of a few clinically important FA as the saturated palmitic, mono unsaturated oleic and others in serum using near infrared spectrometer. As a result, the applicability of the FT spectrometer in the wavelength range of 0.9 -1.8 μ to analyze these FA in serum without sample preparation was confirmed. Besides, measurement specifications were determined and a correlations of the absorption spectra and contents of total triglycerides and cholesterol, palmitic, oleic, linoleic and arachidonic FA in serum were established

  20. Determination of halogens, silicon, phosphorus, carbon, sulfur, tributyl phosphate and of free acid in uranyl nitrate solutions

    International Nuclear Information System (INIS)

    Chu Van Vinh

    2003-01-01

    High-purity uranium compounds are widely used in nuclear field in the form of uranyl nitrate or uranium oxides. In production of uranium material the estimation and the control of products quality is necessary and very important. Halogens was separated from uranium compounds by steam distillation and they were later determined by high performance liquid chromatography (HPLC) for Cl - , Br - , I - ions. Br - was also determined by spectrophotometric and iodide by the individual pulse polarography. Silicon and phosphorus in uranyl nitrate solutions were determined by the photometric method. Sulfur was determined as sulfate form by the measurement of turbidity by the titrimetry. TBP in kerosene and free acid in aqueous solution were determined by the titration. (author)

  1. A comparison of various modes of liquid-liquid based microextraction techniques: determination of picric acid.

    Science.gov (United States)

    Burdel, Martin; Šandrejová, Jana; Balogh, Ioseph S; Vishnikin, Andriy; Andruch, Vasil

    2013-03-01

    Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. The acidic functional groups of humic acid

    Energy Technology Data Exchange (ETDEWEB)

    Shanxiang, Li; Shuhe, Sun; Zhai Zongxi, Wu Qihu

    1983-09-01

    The acidic functional groups content, pK value, DELTAH and DELTAS of humic acid (HA) and nitro-humic acid (NHA) were determined by potentiometry, conductometry and calorimetric titration. The thermodynamic parameters of carboxylic groups and phenolic hydroxyl groups of humic acid are similar to that of simple hydroxy-benzoic acid. The configuration sites of acidic functional groups in humic acid from different coals are different. The carbonyl groups on aromatic rings are probably ortho to phenolic -OH for HA and NHA extracted from Huangxian's brown coal and Japanese lignite, while those from Lingshi's weathered coal are not. The weak -COOH groups of the latter possess higher chemical activity. The -COOH content in HA increases, phenolic -OH group decreases and the chemical acidity of acidic functional groups increases when HA is oxidized by nitric acid. (14 refs.)

  3. "Determination of mycophenolic acid in human plasma by high-performance liquid chromatography"

    Directory of Open Access Journals (Sweden)

    "Mehdi Ahadi Barzoki

    2005-05-01

    Full Text Available A simple, sensitive and reproducible HPLC method is presented for determination of mycophenolic acid(MPA in human plasma. Samples were prepared after precipitation of the plasma protein by addition of acetonitrile and naproxen was used as internal standard (I.S.. Separation was performed by reversedphase HPLC, using a Hamilton PRP-C18 Column, 51% acetonitrile and 49% potassium phosphate buffer (20 mM at pH 3.0 as mobile phase, flow rate of 1.0 ml/min, and UV detection at 215 nm. MPA and I.S. had retention times of 7.5 and 11.35 min, respectively. The method showed an acceptable linearity in the range of 0.1µg/ml-40µg/ml with r2 of .9992. The concentration of 0.1µg/ml was determined as quantification limit. Mean absolute recovery was 94.8%. The mean intra- and inter-day reproducibility of method was 4.6 and 11.4% respectively.

  4. Voltammetric Determination of Tumor Biomarkers for Neuroblastoma (Homovanillic Acid, Vanillylmandelic Acid, and 5-Hydroxyindole-3-acetic Acid) at Screen-printed Carbon Electrodes

    Czech Academy of Sciences Publication Activity Database

    Makrlíková, Anna; Ktena, E.; Economou, A.; Fischer, J.; Navrátil, Tomáš; Barek, J.; Vyskočil, V.

    2017-01-01

    Roč. 29, č. 1 (2017), s. 146-153 ISSN 1040-0397 Institutional support: RVO:61388955 Keywords : Homovanillic acid * Vanillylmandelic acid * 5-Hydroxyindole-3-acetic acid Subject RIV: CG - Electrochemistry OBOR OECD: Electrochemistry (dry cells, batteries, fuel cells, corrosion metals, electrolysis) Impact factor: 2.851, year: 2016

  5. Determination of buffering capacity of selected fermented feedstuffs and the effect of dietary acid-base status on ruminal fluid pH

    Directory of Open Access Journals (Sweden)

    Lukáš Bujňák

    2011-01-01

    Full Text Available The aim of this study was to evaluate the buffering capacity of some fermented feedstuffs and the effect of dietary acid-base status on ruminal fluid pH. The first experiment was performed with different types (n = 24 of wet and dry fermented feedstuffs to determine the buffering capacity and buffer value index. The buffer value index of wet corn silages was more negative than for dry corn silages account on acid loss during drying. In the second experiment, the effects of different concentrations of lactic acid on base-buffering capacity, buffer value index and indicators of fermentation process were studied in two groups of corn silages (n = 21. Two groups of analyzed values were compared using unpaired t-test. Differences among the groups in base-buffering capacity (P P P > 0.05 correlation was found between ruminal pH and dietary buffer value index. These results confirmed that dietary acid-base status alone is not adequate as a predictor of the need for buffers in the diet of lactating cows. It is the first report about using of buffering capacity determination methods for evaluation of feedstuffs and dietary acid-base status in dairy cows.

  6. Determination of flavonoids, phenolic acid and polyalcohol in Butea monosperma and Hedychium coronarium by semi-preparative HPLC Photo Diode Array (PDA Detector

    Directory of Open Access Journals (Sweden)

    Jignasu P. Mehta

    2014-12-01

    Full Text Available The semi preparative HPLC method with PDA Detector was proposed for the determination of one phenolic acid, three flavonoids and one polyalcohol from Butea monosperma and Hedychium coronarium in gradient elution system. The influence of composition of the mobile phase concentration of the mix modifier and temperature on the separation of gallic acid, quercetin, iso-butrin, butrin and eugenol for 90 min was studied. Two different gradient programmes were used to separate these components. The lower limit of quantification of phenolic acid, flavonoids and eugenol is 0.050–0.150 μg/mL and was determined by the least square method and a good correlation was obtained for all separated components.

  7. Determination of molar enthalpy of sublimation in case of orotic acid as obtained from experimental and computational data

    Science.gov (United States)

    Marochkin, Ilya I.; Altova, Ekaterina P.; Chilingarov, Norbert S.; Vilkova, Anna L.; Shishkov, Igor F.

    2018-03-01

    Saturated vapor pressure, ln(p/Pa) = (-21316 ± 511)/(T/K)+(41.64 ± 0.11), and enthalpy of sublimation of orotic acid, Δsub Hm0 (Tm) = 177 ± 4 kJ/mol, were determined by means of Knudsen effusion mass spectrometry in the temperature range of 423÷493 K. The computational approaches supported the experimental results reported. The theoretical estimation of the gas-phase enthalpy of formation for orotic acid was done with different working reactions used.

  8. Electrocatalytic simultaneous determination of ascorbic acid, uric acid and L-Cysteine in real samples using quercetin silver nanoparticles-graphene nanosheets modified glassy carbon electrode

    Science.gov (United States)

    Zare, Hamid R.; Jahangiri-Dehaghani, Fahime; Shekari, Zahra; Benvidi, Ali

    2016-07-01

    By immobilizing of quercetin at the surface of a glassy carbon electrode modified with silver nanoparticles and graphene nanosheets (Q-AgNPs-GNs-GCE) a new sensor has been fabricated. The cyclic voltammogram of Q-AgNPs-GNs-GCE shows a stable redox couple with surface confined characteristics. Q-AgNPs-GNs-GCE demonstrated a high catalytic activity for L-Cysteine (L-Cys) oxidation. Results indicated that L-Cys peak potential at Q-AgNPs-GNs-GCE shifted to less positive values compared to GNs-GCE or AgNPs-GCE. Also, the kinetic parameters such as the electron transfer coefficient,, and the heterogeneous electron transfer rate constant, k‧, for the oxidation of L-Cys at the Q-AgNPs-GNs-GCE surface were estimated. In differential pulse voltammetric determination, the detection limit of L-Cys was obtained 0.28 μM, and the calibration plots were linear within two ranges of 0.9-12.4 μM and 12.4-538.5 μM of L-Cys. Also, the proposed modified electrode is used for the simultaneous determinations of ascorbic acid (AA), uric acid (UA), and L-Cys. Finally, this study has demonstrated the practical analytical utility of the sensor for determination of AA in vitamin C tablet, L-Cys in a milk sample and UA in a human urine sample.

  9. The comparison of partial least squares and principal component regression in simultaneous spectrophotometric determination of ascorbic acid, dopamine and uric acid in real samples

    Directory of Open Access Journals (Sweden)

    Habiboallah Khajehsharifi

    2017-05-01

    Full Text Available Partial least squares (PLS1 and principal component regression (PCR are two multivariate calibration methods that allow simultaneous determination of several analytes in spite of their overlapping spectra. In this research, a spectrophotometric method using PLS1 is proposed for the simultaneous determination of ascorbic acid (AA, dopamine (DA and uric acid (UA. The linear concentration ranges for AA, DA and UA were 1.76–47.55, 0.57–22.76 and 1.68–28.58 (in μg mL−1, respectively. However, PLS1 and PCR were applied to design calibration set based on absorption spectra in the 250–320 nm range for 36 different mixtures of AA, DA and UA, in all cases, the PLS1 calibration method showed more quantitative prediction ability than PCR method. Cross validation method was used to select the optimum number of principal components (NPC. The NPC for AA, DA and UA was found to be 4 by PLS1 and 5, 12, 8 by PCR. Prediction error sum of squares (PRESS of AA, DA and UA were 1.2461, 1.1144, 2.3104 for PLS1 and 11.0563, 1.3819, 4.0956 for PCR, respectively. Satisfactory results were achieved for the simultaneous determination of AA, DA and UA in some real samples such as human urine, serum and pharmaceutical formulations.

  10. Determination of the limit of quantification of the calorimeter using a mixture of benzoic acid and silicon dioxide

    Directory of Open Access Journals (Sweden)

    Krstić Vesna R.

    2011-01-01

    Full Text Available In recent years quality control has received a great attention in laboratory work. Implementation of the international standard ISO/IEC 17025 is necessary for any laboratory that wishes to establish quality control in its work. One of the important factors for meeting the requirements of this standard is the usage of the certified reference materials (CRM in laboratory work. In order to determine the performance of the calorimeter, benzoic acid as CRM, from AlliedSignal Riedelda Haen, Ref.: 33045 and SiO2, Pro analyze, in various mass ratios was used. The results showed that benzoic acid can be successfully utilized for the control of the entire technical and instrumental measuring range and resolve the problem of determination of the limit of detection and quantification of the calorimeter.

  11. Influence of citric acid as chemical modifier for lead determination in dietary calcium supplement samples by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Cezar Paz de Mattos, Julio; Medeiros Nunes, Adriane; Figueiredo Martins, Ayrton; Luiz Dressler, Valderi; Marlon de Moraes Flores, Erico

    2005-01-01

    Citric acid was used as a chemical modifier for Pb determination by graphite furnace atomic absorption spectrometry in dietary supplement samples (calcium carbonate, dolomite and oyster shell samples) and its efficiency was compared to the use of palladium. Pyrolysis and atomization curves were established without use of chemical modifier, with the addition of 20, 100 and 200 μg of citric acid, and with 3 μg of palladium. The citric acid modifier made possible the interference-free Pb determination in the presence of high concentrations of Ca and Mg nitrates. Acid sample digestion involving closed vessels (microwave-assisted and conventional heating) and acid attack using polypropylene vessels at room temperature were compared. All digestion procedures presented similar results for calcium carbonate and dolomite samples. However, for oyster shell samples accurate results were obtained only with the use of closed vessel systems. Analyte addition and matrix-matched standards were used for calibration. The characteristic mass for Pb using citric acid and palladium were 16 and 25 pg, respectively. The relative standard deviation (RSD) was always less than 5% when citric acid was used. The relative and absolute limits of detection were 0.02 μg g -1 and 8 pg with citric acid and 0.1 μg g -1 and 44 pg with the Pd modifier, respectively (n = 10, 3σ). The recovery of Pb in spiked calcium supplement samples (10 μg l -1 ) was between 98% and 105%. With the use of 100 μg of citric acid as chemical modifier, problems such as high background absorption and high RSD values were minimized in comparison to the addition of 3 μg of palladium

  12. Development of a volumetric Analysis method to determine uranium in the loaded phosphoric acid and the loaded organic phase (DEHPA/TOPO)

    International Nuclear Information System (INIS)

    Shlewit, H.; Koudsi, Y.

    2003-01-01

    Rapid and reliable volumetric analysis method has been developed to determine uranium, on line, at uranium extraction unit from wet-process phosphoric acid, in aqueous and organic phases. This process enable up 300 mg of uranium to be determined in the presence of nitric acid, in a sample volume of up to at least 10 ml. The volume of the sample, the amounts of reagents added, the temperature of the reagents and the standing time of various stages were investigated to ensure that the conditions selected for the final procedure were reasonably non-critical

  13. Determination of haloacetic acids in water by ion chromatography--method development.

    Science.gov (United States)

    Lopez-Avila, V; Liu, Y; Charan, C

    1999-01-01

    The microextraction/ion chromatographic (IC) method developed in this study involves extraction of 9 haloacetic acids (HAAs) from aqueous samples (acidified with sulfuric acid to a pH of copper sulfate pentahydrate and sodium sulfate) with methyl tert-butyl ether (MTBE), back extraction into reagent water, and analysis by IC with conductivity detection. The separation column consists of an Ion Pac AG-11 (2 mm id x 50 mm length) guard column and an Ion Pac AS-11 (2 mm id x 250 mm length) analytical column, and the concentration column is a 4 mm id x 35 mm length Dionex TAC-LP column. Use of the 2 mm id Dionex AS-11 column improved detection limits especially for trichloracetic acid (TCAA), bromodichloroacetic acid (BDCAA), dibromochloroacetic acid (DBCAA), and tribromoacetic acid (TBAA). The peak interfering with BCAA elutes at the same retention time as nitrate; however, we have not confirmed the presence of nitrate. Stability studies indicate that HAAs are stable in water for at least 8 days when preserved with ammonium chloride at 100 mg/L and stored at 4 degrees C in the dark. At day 30, recoveries were still high (e.g., 92.1-106%) for dichloroacetic acid (DCAA), BCAA, dibromoacetic acid (DBAA), trichloroacetic acid (TCAA), BDCAA, and DBCAA. However, recoveries of monochloroacetic acid (MCAA), monobromoacetic acid (MBAA), and TBAA were only 54.6, 56.8, and 66.8%, respectively. Stability studies of HAAs in H2SO4-saturated MTBE indicate that all compounds except TBAA are stable for 48 h when stored at 4 degrees C in the dark. TBAA recoveries dropped to 47.1% after 6 h of storage and no TBAA was detected after 48 h of storage. The method described here is only preliminary and was tested in only one laboratory. Additional research is needed to improve method performance.

  14. Application of self-organising maps towards segmentation of soybean samples by determination of amino acids concentration.

    Science.gov (United States)

    Silva, Lívia Ramazzoti Chanan; Angilelli, Karina Gomes; Cremasco, Hágata; Romagnoli, Érica Signori; Galão, Olívio Fernandes; Borsato, Dionisio; Moraes, Larissa Alexandra Cardoso; Mandarino, José Marcos Gontijo

    2016-09-01

    Soybeans are widely used both for human nutrition and animal feed, since they are an important source of protein, and they also provide components such as phytosterols, isoflavones, and amino acids. In this study, were determined the concentrations of the amino acids lysine, histidine, arginine, asparagine, glutamic acid, glycine, alanine, valine, isoleucine, leucine, tyrosine, phenylalanine present in 14 samples of conventional soybeans and 6 transgenic, cultivated in two cities of the state of Paraná, Londrina and Ponta Grossa. The results were tabulated and presented to a self-organising map for segmentation according planting regions and conventional or transgenic varieties. A network with 7000 training epochs and a 10 × 10 topology was used, and it proved appropriate in the segmentation of the samples using the data analysed. The weight maps provided by the network, showed that all the amino acids were important in targeting the samples, especially isoleucine. Three clusters were formed, one with only Ponta Grossa samples (including transgenic (PGT) and common (PGC)), a second group with Londrina transgenic (LT) samples and the third with Londrina common (LC) samples. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  15. A simple one-step ultrasonic-assisted extraction and derivatization method coupling to high-performance liquid chromatographyfor the determination of ε-aminocaproic acid and amino acids in cosmetics.

    Science.gov (United States)

    Du, Yuanqi; Xia, Ling; Xiao, Xiaohua; Li, Gongke; Chen, Xiaoguang

    2018-06-15

    Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE

  16. Selective complexometric determination of titanium(IV) using sodium potassium tartrate or ascorbic acid as masking agent

    International Nuclear Information System (INIS)

    Sreekumar, N.V.; Bhat, N.G.; Narayana, B.; Nazareth, R.A.; Hegde, P.; Manjunatha, B.R.

    2003-01-01

    A simple, rapid and accurate complexometric method is proposed for the determination of titanium(IV) where sodium potassium tartrate or ascorbic acid were used as masking agents. In the presence of diverse metal ions, titanium is first complexed with excess of EDTA and surplus EDTA is then titrated at pH 5-6 with zinc sulfate, xylenol orange being used as indicator. An excess of 5 % aqueous sodium potassium tartrate is then added to displace the complexed EDTA from the Ti-EDTA complex quantitatively, which is titrated with zinc sulfate. Also, ascorbic acid may be used as the releasing agent. The methods work well in the range 1-53 mg of Ti(IV) for sodium potassium tartrate with relative errors ± 0.28 % and standard deviations 0.16 mg. For ascorbic acid the range is 1.00-30.00 mg of Ti(IV) with relative errors of ± 0.40 % and standard deviations of 0.05 mg. (author)

  17. Melamine and Cyanuric Acid do not interfere with Bradford and Ninhydrin assays for protein determination.

    Science.gov (United States)

    Field, Anjalie; Field, Jeffrey

    2010-08-01

    In the fall of 2007 pet food contaminated with melamine and cyanuric acid caused kidney stones in thousands of animals. In the summer of 2008, a more serious outbreak of adulterated dairy food caused the deaths of six infants and sickened about 290,000 children in China. In all cases, melamine was likely added to inflate the apparent protein content of the foods. To determine if we could measure protein without interference from melamine and cyanuric acid we tested these compounds in the Bradford and Ninhydrin assays, two common dye-based assays for protein, as well as by ammonia release, the most common assay used in the food industry. Neither compound was detected in the Ninhydrin and Bradford assays at concentrations of >100 μg/ml. The ammonia assay detected melamine but was inconclusive with respect to cyanuric acid. To develop an accurate test for food that would not detect either chemical as a protein, assays were run on cat food and reconstituted milk powder. The Bradford assay readily measured the protein content of each food, and importantly, the addition of melamine or cyanuric acid to reconstituted milk did not affect the readings. The protein concentrations obtained for reconstituted milk powder were as expected, but those for the cat food were 10 to 30-fold lower, due to its low solubility. We conclude that dye-binding assays can be employed to detect protein in food without interference from melamine and cyanuric acid, thus reducing the incentive to use them as additives.

  18. Quantitative determination of conjugated linoleic acid and polyunsaturated fatty acids in milk with C17 as internal marker – Evaluation of different methylation procedures

    DEFF Research Database (Denmark)

    Lashkari, Saman; Jensen, Søren Krogh

    2017-01-01

    in the methylation steps, as they are sensitive to pH changes and oxidation. The present study was carried out to determine the efficiency of different methylation procedures on quantitative determination of conjugated linoleic acid (CLA), PUFA and response of internal standard. The highest response of internal...... standard was observed for boron trifluoride (BF3)/methanol and methanolic HCl followed by NaOCH3, while cis-9, trans-11 CLA, total CLA and PUFA was higher with methanolic HCl followed by NaOCH3 compared with the BF3 method. These data can be useful for quantitating of milk FA....

  19. Prevalence of anaemia, deficiencies of iron and folic acid and their determinants in Ethiopian women.

    Science.gov (United States)

    Haidar, Jemal

    2010-08-01

    A cross-sectional community-based study with analytic component was conducted among Ethiopian women during June-July 2005 to assess the magnitude of anaemia and deficiencies of iron and folic acid and to compare the factors responsible for anaemia among anaemic and non-anaemic cases. In total, 970 women, aged 15-19 years, were selected systematically for haematological and other important parameters. The overall prevalence of anaemia, iron deficiency, iron-deficiency anaemia, deficiency of folic acid, and parasitic infestations was 30.4%, 50.1%, 18.1%, 31.3%, and 13.7% respectively. Women who had more children aged less than five years but above two years, open-field toilet habits, chronic illnesses, and having intestinal parasites were positively associated with anaemia. Women who had no formal education and who did not use contraceptives were negatively associated with anaemia. The major determinants identified for anaemia were chronic illnesses [adjusted odds ratio (AOR) = 1.1, 95% confidence interval (CI) 1.15-1.55), deficiency of iron (AOR = 0.4, 95% CI 0.35-0.64), and deficiency of folic acid (AOR = 0.5, 95% CI 0.50-0.90). The odds for developing anaemia was 1.1 times more likely among women with chronic illnesses, 60% more likely in the iron-deficient and 40% more likely in the folic acid-deficient than their counterparts. One in every three women had anaemia and deficiency of folic acid while one in every two had iron deficiency, suggesting that deficiencies of both folic acid and iron constitute the major micronutrient deficiencies in Ethiopian women. The risk imposed by anaemia to the health of women ranging from impediment of daily activities and poor pregnancy outcome calls for effective public-health measures, such as improved nutrient supplementation, health education, and timely treatment of illnesses.

  20. A Portable Parallel Implementation of the U.S. Navy Layered Ocean Model

    Science.gov (United States)

    1995-01-01

    Wallcraft, PhD (I.C. 1981) Planning Systems Inc. & P. R. Moore, PhD (Camb. 1971) IC Dept. Math. DR Moore 1° Encontro de Metodos Numericos...Kendall Square, Hypercube, D R Moore 1 ° Encontro de Metodos Numericos para Equacöes de Derivadas Parciais A. J. Wallcraft IC Mathematics...chips: Chips Machine DEC Alpha CrayT3D/E SUN Sparc Fujitsu AP1000 Intel 860 Paragon D R Moore 1° Encontro de Metodos Numericos para Equacöes

  1. Spectrographic determination of lanthanides in high-purity uranium compounds, after chromatographic separation by alumina-hydrofluoric acid

    International Nuclear Information System (INIS)

    Lordello, A.R.; Abrao, A.

    1979-01-01

    A method is presented for the determination of fourteen rare earth elements in high-purity uranium compounds by emission spectrography. The rare earths are chromatographically separated from uranium by using alumina-hydrofluoric acid. Lanthanum is used both as collector and internal standard. The technique of excitation involves a total consumption of the sample in a 17 ampere direct current arc. The range of determination is about 0.005 to 0.5 μg/g uranium. The coefficient of variation for Pr, Ho, Dy, Er, Tm, Lu, Gd and Tb amounts to 10%. (Author) [pt

  2. An Amperometric Biosensor for Uric Acid Determination Prepared From Uricase Immobilized in Polyaniline-Polypyrrole Film

    Directory of Open Access Journals (Sweden)

    Fatma Arslan

    2008-09-01

    Full Text Available A new amperometric uric acid biosensor was developed by immobilizing uricase by a glutaraldehyde crosslinking procedure on polyaniline-polypyrrole (pani-ppy composite film on the surface of a platinum electrode. Determination of uric acid was performed by the oxidation of enzymatically generated H2O2 at 0.4 V vs. Ag/AgCl. The linear working range of the biosensor was 2.5×10-6 – 8.5×10-5 M and the response time was about 70 s. The effects of pH, temperature were investigated and optimum parameters were found to be 9.0, 55 oC, respectively. The stability and reproducibility of the enzyme electrode have been also studied.

  3. Classical bile acids in animals, beta-phocaecholic acid in ducks.

    Science.gov (United States)

    Jirsa, M; Klinot, J; Klinotová, E; Ubik, K; Kucera, K

    1989-01-01

    1. Bile samples of different animals were analysed and the percentage content of classical bile acids was determined. 2. Herbivorous birds mostly excreted a large proportion of chenodeoxycholic acid. 3. The anteater (Myrmecophaga tridactyla) excreted deoxycholic acid most probably as a primary bile acid. 4. In the bile of ducks (Anas platyrhynchos) a large amount of (23R)3 alpha, 7 alpha, 23-trihydroxy-5 beta-cholan-24-oic acid (beta-phocaecholic acid) was found.

  4. Double-Sampling Method for Carrying Out Quality Control of a Fabrication Process; Methode du Double Echantillonnage pour le Controle de la Qualite d'un Procede de Fabrication; Metod dvukh obraztsov dlya osushchestvleniya kontrolya za kachestvom v protsesse izgotovleniya; Metodo de Muestreo Doble para el Control de Calidad de un Proceso de Fabricacion

    Energy Technology Data Exchange (ETDEWEB)

    Cerrolaza, J. A.; Lago, A.; Montojo, Rosa M. [Junta de Energia Nuclear, Madrid (Spain)

    1966-02-15

    taille des echantillons et le degre de controle sont determines en fonction des risques inherents a la premiere et a la deuxieme condition. Bien que cette methode soit applicable, elle est fort peu pratique quand il s'agit de controler des pieces de reacteurs, car les echantillons qu'elle exige sont de dimensions excessives. Le memoire expose une methode analogue a celle de Cave mais qui consiste a etablir un double echantillonnage dans lequel la taille moyenne de l'echantillon est beaucoup plus reduite. (author) [Spanish] La fabricacion de componentes que han de ser empleados en reactores nucleares presenta dos caracteristicas fundamentales que condicionan el proceso: la exigencia de una calidad muy elevada que limita a valores muy bajos el porcentaje de piezas defectuosas admisibles, y el coste muy alto de cada uno de los componentes. Estas dos condiciones obligan a que el control durante la fabricacion posea una curva de operacion con potencia muy elevada, y, por otra parte, a que el numero de piezas destruidas en cada inspeccion sea un pequeno como se pueda, siempre que se cumpla la condicion anterior. Los metodos usuales de control, basados en fijar el riesgo de primera especie, no son aplicables, ya que en general su eficacia no es suficiente. Cave ha desarrollado un metodo en que, tanto el tamano de las muestras como los limites de control, se fijan en funcion de los riesgos de primera y segunda especie. Este metodo, si bien es aplicable, resulta poco practico en el control de componentes para reactores, ya que se necesitan muestras de un tamano excesivamente grande. En el presente trabajo se desarrolla un metodo semejante al de Cave, pero en el que se establece un muestreo doble, con lo que el tamano medio de la muestra es mucho mas reducido. (author) [Russian] Pri izgotovlenii komponentov dlja ispol'zovanija v reaktorah reshajushhee znachenie imejut dva osnovnyh faktora, a imenno: neobhodimost' obespechit' ochen' vysokoe kachestvo, dopuskajushhee lish' ochen

  5. The determination of titratable acidity and total tannins in red wine

    OpenAIRE

    Rajković Miloš B.; Sredović Ivana D.

    2009-01-01

    Titration acidity and content of total tannins in mass-market red wines are analyzed in this paper. The content of total acids in wine, expressed through wine acid, was analyzed by potentiometric titration on 7.00 pH value. According to titratable acidity in analyzed wines, all wines (only) with analyzed parameters according to Regulations about wine quality. The analysis of differential potentiometric curves shows that these curves can give the answer to the question if non organic substance...

  6. Use of the ion exchange method for determination of stability constants of uranyl ions with three soil humic acids

    International Nuclear Information System (INIS)

    Tao Zuyi; Du Jinzhou

    1994-01-01

    The ion exchange equilibrium method proposed by Ardakani and Stevenson has not been widely used to determine the stability constants of metal-soil organic matter complexes. In this paper the Ardakani-Stevenson's method has been modified and the stability constants of uranyl ion complexes with three soil humic acids were determined by using the modified Ardakani-Stevenson's method. (orig.)

  7. A colourimetric method for the determination of the degree of chemical cross-linking in aspartic acid-based polymer gels

    Directory of Open Access Journals (Sweden)

    B. Gyarmati

    2015-02-01

    Full Text Available A 2,4,6-trinitrobenzenesulphonic acid (TNBS-based assay is developed to determine the degree of chemical cross-linking in aspartic acid-based polymer gels. The conventional colourimetric method for the quantitative determination of amine groups is difficult to use in polymer networks; thus, an improved method is developed to analyse polymer gels swollen in dimethyl sulfoxide (DMSO. Reaction products of the derivatizing reaction are examined by NMR. The chemical stability of the reagent is increased in DMSO, and the method shows satisfactory linearity and accuracy. The degree of chemical cross-linking in the investigated gels is close to its theoretical maximum, but the conversion of the pendant amine groups to cross-linking points is strongly dependent on the feed composition of the gels.

  8. A glassy carbon electrode modified with a polyaniline doped with silicotungstic acid and carbon nanotubes for the sensitive amperometric determination of ascorbic acid

    International Nuclear Information System (INIS)

    Zhang, X.; Lai, G.; Zhang, H.; Yu, A.

    2013-01-01

    We report on an electrochemical sensor for the sensitive amperometric determination of ascorbic acid (AA). Aniline containing suspended silicotungstic acid and carbon nanotubes was electropolymerized on the surface of a glassy carbon electrode in a single step which provides a simple and controllable method and greatly improves the electrocatalytic oxidation of AA. The effects of scan rate, solution pH and working potential were studied. A linear relationship exists between the current measured and the concentration of AA in the range from 1 μM to 10 μM and 0.01 mM to 9 mM, with a limit of detection as low as 0.51 μM (S/N = 3). The sensor is selective, stable and satisfyingly reliable in real sample experiments. In our eyes, it has a large potential for practical applications. (author)

  9. Fast and Simultaneous Determination of Pu(Ⅳ) and Nitric Acid in Spent Nuclear Fuel Reprocessing Sample by Near Infrared Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    LI; Ding-ming; ZHANG; Li-hua; WANG; Ling; GONG; Yan-ping; FAN; De-jun; YI; Bao-shan; CHEN; Qiang; JI; Yong-chao; WU; Ji-zong

    2013-01-01

    Determination of Pu(Ⅳ)and nitric acid plays significant role in nuclear fuel reprocessing plant to control process accurately and timely.Coupling C-T fixed-type grating with InGaAs detector,a new novel analytical system for simultaneous measurement of nitric acid and Pu(Ⅳ)was developed by our working group.After obtaining near infrared absorptive spectra by the spectroscopic instrument,the spectra data

  10. Influence of acid diffusion on the performance of lead-acid cells

    Energy Technology Data Exchange (ETDEWEB)

    Kappus, W.; Bohmann, J.

    1983-11-01

    A model for the discharge performance of the lead-acid cell is proposed. Diffusion of acid into the porous electrodes, which is connected with diffusional polarization, is considered as the principal factor in the transport process. The end of discharge is determined either by acid depletion inside the electrodes or by exhaustion of the active material, where utilization of the active material as a function of the acid density and the specific current is determined from empirical expressions. Curves of diffusional polarizations as a function of the discharge time are presented. Calculated discharge capacities show the influence of various parameters such as electrode thickness, current, and acid density. Tubular and pasted plates are considered.

  11. Plasma amino acids

    Science.gov (United States)

    Amino acids blood test ... types of methods used to determine the individual amino acid levels in the blood. ... test is done to measure the level of amino acids in the blood. An increased level of a ...

  12. Gas chromatographic determination of organic acids from fruit juices by combined resin mediated methylation and extraction in supercritical carbon dioxide.

    Science.gov (United States)

    Barden, T J; Croft, M Y; Murby, E J; Wells, R J

    1997-10-17

    A procedure in which anionic analytes, trapped on ion exchange resin, are simultaneously methylated and released using methyl iodide in either supercritical carbon dioxide or acetonitrile has been extended to polyfunctional organic acids. The combined SFE methylation of fruit juice acids trapped onto ion exchange resin proceeds in good yield producing the methyl esters of fumaric, succinic, malic, tartaric, isocitric and citric acids which are readily separated by GC. Using this procedure low concentrations of one acid can be detected and quantitated in the presence of very high concentrations of another. This new method detects tartaric acid at levels of 10 ppm in juices containing 10,000 ppm citric acid. Quantitation was performed either by using GC-FID with triethyl citrate or diethyl tartrate as internal standards or with the element specific calibration capability of the GC-AED. A simple new technique for the determination of citric/isocitric acid ratio is now available. Also, in contrast to HPLC methods, the identity of an analyte is readily confirmed by GC-MS.

  13. Quantitative determination of fatty acids in marine fish and shellfish from warm water of Straits of Malacca for nutraceutical purposes.

    Science.gov (United States)

    Abd Aziz, Nurnadia; Azlan, Azrina; Ismail, Amin; Mohd Alinafiah, Suryati; Razman, Muhammad Rizal

    2013-01-01

    This study was conducted to quantitatively determine the fatty acid contents of 20 species of marine fish and four species of shellfish from Straits of Malacca. Most samples contained fairly high amounts of polyunsaturated fatty acids (PUFAs), especially alpha-linolenic acid (ALA, C18:3 n3), eicosapentaenoic acid (EPA, C20:5 n3), and docosahexaenoic acid (DHA, C22:6 n3). Longtail shad, yellowstripe scad, and moonfish contained significantly higher (P < 0.05) amounts of eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and alpha-linolenic acid (ALA), respectively. Meanwhile, fringescale sardinella, malabar red snapper, black pomfret, Japanese threadfin bream, giant seaperch, and sixbar grouper showed considerably high content (537.2-944.1 mg/100 g wet sample) of desirable omega-3 fatty acids. The polyunsaturated-fatty-acids/saturated-fatty-acids (P/S) ratios for most samples were higher than that of Menhaden oil (P/S = 0.58), a recommended PUFA supplement which may help to lower blood pressure. Yellowstripe scad (highest DHA, ω - 3/ω - 6 = 6.4, P/S = 1.7), moonfish (highest ALA, ω - 3/ω - 6 = 1.9, P/S = 1.0), and longtail shad (highest EPA, ω - 3/ω - 6 = 0.8, P/S = 0.4) were the samples with an outstandingly desirable overall composition of fatty acids. Overall, the marine fish and shellfish from the area contained good composition of fatty acids which offer health benefits and may be used for nutraceutical purposes in the future.

  14. New synthesis of poly ortho-methoxyaniline nanostructures and its application to construct modified multi-wall carbon nanotube/graphite paste electrode for simultaneous determination of uric acid and folic acid

    Energy Technology Data Exchange (ETDEWEB)

    Rajabi, Hossein, E-mail: h.rajabi8086@gmail.com; Noroozifar, Meissam

    2017-06-01

    Uric acid (UA) and folic acid (FA) are compounds of biomedical interest. In humans, about 70% of daily uric acid disposal occurs via the kidneys, and in 5–25% of humans, impaired renal (kidney) excretion leads to hyperuricemia. Folate is another form folic acid of which is known as, is one of the B vitamins. It is used as a supplement by women to prevent neural tube defects developing during pregnancy. Polyortho-methoxyaniline nanostructures (POMANS) was synthesized with a new two phase (organic-water) synthesis method. The POMANS was characterized using transmission electron microscopy (TEM) and Fourier transform IR (FTIR). This polymer was used to construct a modified multi-wall carbon nanotube, graphite paste electrode (POMANS-MWCNT/GPE). Linear sweep voltammograms (LSV), cyclic voltammetry (CV) and chronoamperometry were used to investigate the suitability of polyortho-methoxyaniline with multi-wall carbon nanotubes paste electrode as a modifier for the electrocatalytic oxidation of UA and FA in aqueous solutions with various pHs. The results showed that POMANS-MWCNT/GPE had high anodic peak currents for the electrooxidation of UA and FA in pH 6.0.Under the optimized conditions, The catalytic peak currents obtained, was linearly dependent on the UA and FA concentrations in the range of 0.6–52 and 0.5–68 μM with two segments and the detection limits 0.157 and 0.113 μM for UA and FA were, respectively. Finally, the proposed method was also examined as a sensitive, simple and inexpensive electrochemical sensor for the simultaneous determination of UA and FA in real samples such as urine and serum. - Highlights: • For the first time, POMANS was synthesized with a new method of two-phase organic & water. • POMANS-MWCNT/GPE was used for simultaneous determination of UA and FA at optimum pH 6.0. • Parameters n and α were also determined for UA and FA. • Electrochemical simultaneous determination of UA and FA with modified electrode real samples.

  15. A digital image-based method for determining of total acidity in red wines using acid-base titration without indicator.

    Science.gov (United States)

    Tôrres, Adamastor Rodrigues; Lyra, Wellington da Silva; de Andrade, Stéfani Iury Evangelista; Andrade, Renato Allan Navarro; da Silva, Edvan Cirino; Araújo, Mário César Ugulino; Gaião, Edvaldo da Nóbrega

    2011-05-15

    This work proposes the use of digital image-based method for determination of total acidity in red wines by means of acid-base titration without using an external indicator or any pre-treatment of the sample. Digital images present the colour of the emergent radiation which is complementary to the radiation absorbed by anthocyanines present in wines. Anthocyanines change colour depending on the pH of the medium, and from the variation of colour in the images obtained during titration, the end point can be localized with accuracy and precision. RGB-based values were employed to build titration curves, and end points were localized by second derivative curves. The official method recommends potentiometric titration with a NaOH standard solution, and sample dilution until the pH reaches 8.2-8.4. In order to illustrate the feasibility of the proposed method, titrations of ten red wines were carried out. Results were compared with the reference method, and no statistically significant difference was observed between the results by applying the paired t-test at the 95% confidence level. The proposed method yielded more precise results than the official method. This is due to the trivariate nature of the measurements (RGB), associated with digital images. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Acid distribution in phosphoric acid fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Okae, I.; Seya, A.; Umemoto, M. [Fuji Electric Co., Ltd., Chiba (Japan)

    1996-12-31

    Electrolyte acid distribution among each component of a cell is determined by capillary force when the cell is not in operation, but the distribution under the current load conditions had not been clear so far. Since the loss of electrolyte acid during operation is inevitable, it is necessary to store enough amount of acid in every cell. But it must be under the level of which the acid disturbs the diffusion of reactive gases. Accordingly to know the actual acid distribution during operation in a cell is very important. In this report, we carried out experiments to clarify the distribution using small single cells.

  17. EXTRACTION AND QUANTITATIVE DETERMINATION OF ASCORBIC ACID FROM BANANA PEEL MUSA ACUMINATA ‘KEPOK’

    Directory of Open Access Journals (Sweden)

    Khairul Anwar Mohamad Said

    2016-04-01

    Full Text Available This paper discusses the extraction of an antioxidant compound, which is ascorbic acid or vitamin C, from a banana peel using an ultrasound-assisted extraction (UAE method. The type of banana used was Musa acuminata also known as “PisangKepok” in Malaysia. The investigation includes the effect of solvent/solid ratio (4.5, 5 g and 10  ml/g, sonication time (15, 30 and 45 mins and temperature variation (30 , 45  and 60oC on the extraction of ascorbic acid compounds from the banana peel to determine the best or optimum condition of the operation. Out of all extract samples analyzed by redox titration method using iodine solution, it was found that the highest yield was 0.04939 ± 0.00080 mg that resulted from an extraction at 30oC for 15 mins with 5 ml/g solvent-to-solute ratio.KEYWORDS:  Musa acuminata; ultrasound-assisted extraction; vitamin C; redox titration

  18. Determination of rat vertebral bone compressive fatigue properties in untreated intact rats and zoledronic-acid-treated, ovariectomized rats

    NARCIS (Netherlands)

    Brouwers, J.E.M.; Ruchselman, M.; Rietbergen, van B.; Bouxsein, M.L.

    2009-01-01

    Summary Compressive fatigue properties of whole vertebrae, which may be clinically relevant for osteoporotic vertebral fractures, were determined in untreated, intact rats and zoledronic-acid-treated, ovariectomized rats. Typical fatigue behavior was found and was similar to that seen in other

  19. Determination of aristolochic acids by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Wang, Yinan; Chan, Wan

    2014-06-25

    Nephrotoxic and carcinogenic aristolochic acids (AAs) are naturally occurring nitrophenanthrene carboxylic acids in the herbal genus Aristolochia. The misuse of AA-containing herbs in preparing slimming drugs has caused hundred of cases of kidney disease in Belgium women in a slimming regime in the early 1990s. Accumulating evidence also suggested that prolong dietary intake of AA-contaminated food is one of the major causes to the Balkan endemic nephropathy that was first observed in the late 1950s. Therefore, analytical methods of high sensitivity are extremely important for safeguarding human exposure to AA-containing herbal medicines, herbal remedies, and food composites. In this paper, we describe the development of a new high-performance liquid chromatography coupled fluorescence detector (HPLC-FLD) method for the sensitive determination of AAs. The method makes use of a novel cysteine-induced denitration reaction that "turns on" the fluorescence of AAs for fluorometric detections. Our results showed that the combination of cysteine-induced denitration and HPLC-FLD analysis allows for sensitive quantification of AA-I and AA-II at detection limits of 27.1 and 25.4 ng/g, respectively. The method was validated and has been successfully applied in quantifying AAs in Chinese herbal medicines.

  20. Determination of uranium in human hair by acid digestion and FIAS-ICPMS

    International Nuclear Information System (INIS)

    Gonnen, R.; Kol, R.; Laichter, Y.; Marcus, P.; Lorber, A.; Karpas, Z.; Halicz, L.

    2000-01-01

    The content of heavy metals in human hair may serve as an indicator of occupational or environmental exposure of metal compounds. However, before such exposure can be determined, the level of the element in a 'normal' population must be established. The concentration of uranium in human hair was measured by flow injection - inductively coupled plasma mass spectrometry (FIAS-ICPMS) after acid digestion of the hair samples. All hair samples were rinsed in order to remove external contamination prior to the digestion in a 2:1 solution of concentrated nitric acid and 30% hydrogen peroxide. The limit of detection of the method, for a 50 mg hair sample, was 0.015 μg/g, mainly due to the presence of impurities in the hydrogen peroxide. The range of uranium concentration in the initial test group was found to be 0.01-0.18 μg/g. The mean and median values of the entire study population were 0.062 and 0.050 μg U/g hair, respectively. Differences between the following sub-populations: male and female, smokers and non-smokers and people below and above 45 years of age were examined. The only statistically significant difference was found in the latter group (p=0.03). (author)

  1. Interference-Blind Microfluidic Sensor for Ascorbic Acid Determination by UV/vis Spectroscopy

    DEFF Research Database (Denmark)

    Bi, Hongyan; Oliveira Fernandes, Ana Carolina; Cardoso, Susana

    2016-01-01

    A microfluidic sensor is developed and targeted at specific ingredients determination in drug/food/beverage matrices. The surface of a serpentine polydimethylsiloxane (PDMS) microchannel is modified by enzyme via physisorption. When solutions containing target ingredients pass through...... the microfluidic channel, enzyme-catalyzed reaction occurs and only converts the target molecules to its products. The whole process is monitored by an end-channel UV/vis spectroscopic detection. Ascorbate oxidase and L-ascorbic acid (AA) are taken as enzyme-substrate model in this study to investigate......, specific, and accurate, and can be potentially used for fast quantification of ingredient in samples with complex matrix background. It is promising to be widely spread in food industry and quality control department...

  2. Rapid fluorometric determination of perfluorooctanoic acid by its quenching effect on the fluorescence of quantum dots

    International Nuclear Information System (INIS)

    Liu, Qi; Huang, Aizhen; Wang, Nan; Zheng, Guan; Zhu, Lihua

    2015-01-01

    Analysis of perfluorooctanoic acid (PFOA) usually requires a combination of high-performance liquid chromatography and mass spectrometry, which is expensive and time-consuming. In the present work, water-soluble CdS quantum dots (QDs) were employed to develop a simple and rapid fluorometric method for the determination of PFOA. Strongly fluorescent CdS QDs were prepared by using 3-mercaptopropionic acid (MPA) as a stabilizer. It was observed that PFOA strongly quenched the fluorescence emission of the MPA-CdS QDs because PFOA promotes the aggregation of MPA-CdS QDs through a fluorine–fluorine affinity interaction. Under optimum conditions, the fluorescence intensity of MPA-CdS QDs was observed to decrease linearly with an increase in the concentration of PFOA from 0.5 to 40 μmol L −1 , with a limit of detection of 0.3 μmol L −1 . This new method was successfully implemented for the analysis of PFOA-spiked textile samples, with recoveries ranging from 95% to 113%. - Highlights: • PFOA significantly quenched the fluorescence emission of quantum dots (QDs). • A rapid and simple fluorescence sensor was proposed for determining PFOA by QDs. • PFOA determination could be completed within approximately 10 min. • The developed method had a working range of 0.5 to 40 μmol L −1 and a detection limit of 0.3 μmol L −1

  3. [Acids in coffee. XI. The proportion of individual acids in the total titratable acid].

    Science.gov (United States)

    Engelhardt, U H; Maier, H G

    1985-07-01

    22 acids in ground roast coffees and instant coffees were determined by GLC of their silyl derivatives (after preseparation by gel electrophoresis) or isotachophoresis. The contribution to the total acidity (which was estimated by titration to pH 8 after cation exchange of the coffee solutions) was calculated for each individual acid. The mentioned acids contribute with 67% (roast coffee) and 72% (instant coffee) to the total acidity. In the first place citric acid (12.2% in roast coffee/10.7% in instant coffee), acetic acid (11.2%/8.8%) and the high molecular weight acids (8%/9%) contribute to the total acidity. Also to be mentioned are the shares of chlorogenic acids (9%/4.8%), formic acid (5.3%/4.6%), quinic acid (4.7%/5.9%), malic acid (3.9%/3%) and phosphoric acid (2.5%/5.2%). A notable difference in the contribution to total acidity between roast and instant coffee was found for phosphoric acid and pyrrolidonecarboxylic acid (0.7%/1.9%). It can be concluded that those two acids are formed or released from e.g. their esters in higher amounts than other acids during the production of instant coffee.

  4. HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC DETERMINATION OF CAFFEIC ACID AND ROSMARINIC ACID FROM THE LEAVES OF Orthosiphon stamineus

    Directory of Open Access Journals (Sweden)

    M. Amzad Hossain

    2010-06-01

    Full Text Available This paper presents the studies performed on extraction of Orthosiphon stamineus, Benth by using different solvent for the identification and quantification of the caffeic acid derivatives such as caffeic acid  and rosmarinic acid which confers to the leaves of this plant with remarkable pharmaceutical properties. High performance thin-layer chromatographic (HPTLC allows the identification and the quantification of more than 20 samples in the same chromatographic run. The analysis of the samples requires 15-30 min compared with more than 2 h using a typical HPLC method. Using the techniques of the HPTLC and the UV-VIS spectra we have found that the extraction of this herb plant contain, the caffeic acid and rosmarinic acid ranging between 0.029% up to 0.506% and up to 0.24% to 2.24% respectively.     Keywords: Caffice acid derivatives, quantification, Malaysian Orthosiphon stamineus, HPTLC

  5. Determination of the Cyanide Metabolite 2-Aminothiazoline-4-Carboxylic Acid in Urine and Plasma by Gas Chromatography-Mass Spectrometry

    National Research Council Canada - National Science Library

    Logue, Brian A; Kirschten, Nicholas P; Petrikovics, Ilona; Moser, Matthew A; Rockwood, Gary A; Baskin, Steven I

    2005-01-01

    The cyanide metabolite 2-aminothiazoline.4-carboxylic acid (ATCA) is a promising biomarker for cyanide exposure because of its stability and the limitations of direct determination of cyanide and more abundant cyanide metabolites...

  6. Simultaneous determination of nine kinds of dominating bile acids in various snake bile by ultrahigh-performance liquid chromatography with triple quadrupole linear iontrap mass spectrometry.

    Science.gov (United States)

    Zhang, Jie; Fan, Yeqin; Gong, Yajun; Chen, Xiaoyong; Wan, Luosheng; Zhou, Chenggao; Zhou, Jiewen; Ma, Shuangcheng; Wei, Feng; Chen, Jiachun; Nie, Jing

    2017-11-15

    Snake bile is one of the most expensive traditional Chinese medicines (TCMs). However, due to the complicated constitutes of snake bile and the poor ultraviolet absorbance of some trace bile acids (BAs), effective analysis methods for snake bile acids were still unavailable, making it difficult to solve adulteration problems. In present study, ultrahigh-performance liquid chromatography with triple quadrupole linear ion trap mass spectrometry (UHPLC-QqQ-MS/MS) was applied to conduct a quantitative analysis on snake BAs. The mass spectrometer was monitored in the negative ion mode, and multiple-reaction monitoring (MRM) program was used to determine the contents of BAs in snake bile. In all, 61 snake bile from 17 commonly used species of three families (Elapidae, Colubridae and Viperidae), along with five batches of commercial snake bile from four companies, were collected and detected. Nine components, Tauro-3α,12α-dihydroxy-7-oxo-5β-cholenoic acid (T1), Tauro-3α,7α,12α,23R-tetrahydroxy-5β-cholenoic acid (T2), taurocholic acid (TCA), glycocholic acid (GCA), taurochenodeoxycholic acid (TCDCA), taurodeoxycholic acid (TDCA), cholic acid (CA), Tauro-3α,7α-dihydroxy-12-oxo-5β-cholenoic acid (T3), and Tauro-3α,7α,9α,16α-tetrahydroxy-5β-cholenoic acid (T4) were simultaneously and rapidly determined for the first time. In these BAs, T1 and T2, self-prepared with purity above 90%, were first reported with their quantitative determination, and the latter two (T3 and T4) were tentatively determined by quantitative analysis multi-components by single marker (QAMS) method for roughly estimating the components without reference. The developed method was validated with acceptable linearity (r 2 ≥0.995), precision (RSD<6.5%) and recovery (RSD<7.5%). It turned out that the contents of BAs among different species were also significantly different; T1 was one of the principle bile acids in some common snake bile, and also was the characteristic one in Viperidae

  7. An Appraisal of Analytical Methods for Plutonium and their Applications to the Analysis of Nuclear Materials; Evaluation des Methodes Analytiques de Dosage du Plutonium et de Leur Application a l'Analyse des Matieres Nucleaires; Otsenka analiticheskikh metodov opredeleniya plutoniya i ikh primenenie dlya analiza yadernykh materialov; Metodos Analiticos de Determinacion del Plutonio y su Empleo en el Analisis de Materiales Nucleares

    Energy Technology Data Exchange (ETDEWEB)

    Milner, G. W.C.; Phillips, G. [Atomic Energy Research Establishment, Harwell, Berks. (United Kingdom)

    1966-02-15

    A variety of methods is available for the determination of the plutonium content of nuclear materials. For milligram amounts of plutonium the available methods include differential spectrophotometry using the colour of Pu (III), gravimetry based on PuO{sub 2} gamma counting, and redox methods including potentiometric and amperometric titrations and controlled-potential coulometry. Alpha counting, isotopic dilution, and polarographic methods are suitable for microgram amounts. Some methods are more suitable than others for certain types of sample and the analyst is faced with difficult selection problems to achieve the best results. The advantages and limitations of the above methods are described in the light of a varied experience with them over many years at AERE, together with comments on accuracy, precision, sensitivity and features of special interest. Some of the methods cannot be applied without some separation of the plutonium from other sample constituents, and comments are made from experience in the use of anion exchange and reverse-phase chromatographic techniques for this with emphasis on their suitability for radioactive samples. Consideration is given to the many problems that have arisen in the successful application of these methods to the analysis of plutonium alloys, ceramics and cermets in various systems containing uranium, thorium, iron, chromium, molybdenum, cerium and cobalt. Difficulties occurring in the dissolution of samples and in the adjustment of the plutonium to the required valency state are described. The respective merits of dissolving in mixtures of common mineral acids and with the aid of fusion techniques are commented upon with examples. Outlines of procedures, together with analytical results for typical samples, are given for the analysis of Pu-U, Pu-Ce-Co and Pu-U-Mo alloys, Pu-U oxides and carbides, and Pu-U carbide cermets with Fe, Mo and Cr. These materials have arisen from metallurgical research and development

  8. Direct complexonometric determination of thorium (IV), uranium (IV), neptunium (IV), plutonium (IV) by titration of diethylenetriaminepentaacetic acid with xylenol orange as indicator

    International Nuclear Information System (INIS)

    Rykov, A.G.; Piskunov, E.M.; Timofeev, G.A.

    1975-01-01

    The purpose of the present work was to develop a method of determining Th(IV), U(IV), Np(N) and Pu(IV) in acid solutions by titration with diethylenetriamine pentacetic acid, the indicator being xylenol orange. It has been established that Th, U, Np and Pu can be determined to within 0.5-1.5%. Th and U in quantities of tens of milligrams can be determined with greater accuracy, attaining hundredths of one per cent. During titration the determination is not hindered by singly- and doubly-charged metal ions, trivalent lanthanides and actinides, except plutonium. The proposed method can be used to determine U(IV) in the presence of considerable quantities of U(VI) and Np(IV) in the presence of Np(V). Total concentrations of uranium or neptunium are determined by reducing uranium (VI) or neptunium (V) by a standard method (for example, using metallic lead, cadmium or zinc amalgam) to the tetravalent state and applying the method described in the paper. (E.P.)

  9. Analytical methods for 2,4-D (Dichlorophenoxyacetic acid) determination; Metodos analiticos para la determinacion del 2,4-D (Acido diclorofenoxiacetico)

    Energy Technology Data Exchange (ETDEWEB)

    Martinez G, M.S.M

    1999-06-01

    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)

  10. [Determination of chlorogenic acid, caffeic acid and linarin in Flos Chrysanthemi Indici from different places by RP-hPLC].

    Science.gov (United States)

    Guo, Qiaosheng; Fang, Hailing; Shen, Haijin

    2010-05-01

    To evaluate the quality of Flos Chrysanthemi Indici which produced in twenty-two different producing places. Chlorogenic acid and caffeic acid were analyzed on a Shim-pack C8 colunm (4.6 mm x 250 mm, 5 microm) eluted with the mobile phase consisted of acetonitrile-0.5% phosphoric acid( 19:81). The detection wavelength was set at 326 nm. Linarin were eluted with the mobile phase consisted of methanol-water-acetic acid(26: 23: 1). The detection wavelength was set at 334 nm. The column temperature was 25 degrees C. The flow rate was 1.0 mL x min . The linear response ranged within 2.5-50 microg for chlorogenic acid (r = 0.998), 2.5-25 microg for caffeic acid (r = 0.998) and 4.97-41.47 microg for linarin (r = 0.999), respectively. Recoveries were 100.8% with RSD 2.1% for chlorogenic acid, 96.2% with RSD 2.3% for caffeic acid and 103.7% with RSD 1.8% for linarin. There was a significant difference in the content of chlorogenic acid, caffeic acid, linarin among the samples. The content of chlorogenic in the sample from Fengdou Chongqing city was the highest in those from other places. The content of caffeic acid in the all samples is very low. The content of linarin in the samples from Jiangsu province and Anhui province almost reached the national standard in pharmacopoeia.

  11. Determination of trace elements in acid rain by reversed phase extraction chromatography and neutron activation

    International Nuclear Information System (INIS)

    Rao, R.R.; Goski, D.G.; Chatt, A.

    1991-01-01

    A preconcentration neutron activation analysis (PNAA) method has been developed for the simultaneous determination of selected trace elements in acid rain and other water samples. The method consists of preconcentration of the elements by reversed phase extraction chromatography using oxine-loaded Amberlite XAD-2 resin. Nearly 100% recoveries were obtained for Co, Cu, Hg, V and Zn at pH 6.0 and for Cd at pH 7.0. Manganese gave incomplete recoveries at the pH range of 4.0-8.0 studies. Various factors that can influence preconcentration of the elements have been investigated in detail. The precision and accuracy of measurements have been evaluated by analyzing certified reference materials. The detection limits have been found to be of the order of ppb. The PNAA method has been applied to a number of acid rain and other water samples

  12. Modified gold electrodes based on thiocytosine/guanine-gold nanoparticles for uric and ascorbic acid determination

    International Nuclear Information System (INIS)

    Vulcu, Adriana; Grosan, Camelia; Muresan, Liana Maria; Pruneanu, Stela; Olenic, Liliana

    2013-01-01

    The present paper describes the preparation of new modified surfaces for electrodes based on guanine/thiocytosine and gold nanoparticles. The gold nanoparticles were analyzed by UV–vis spectroscopy and transmission electron microscopy (TEM) and it was found that they have diameters between 30 and 40 nm. The layers were characterized by specular reflectance infrared spectroscopy (FTIR-RAS) and by atomic force microscopy (AFM). The thickness of layers was found to be approximately 30 nm for TC layers and 300 nm for GU layers. Every layer was characterized as electrochemical sensor (by cyclic voltammetry) both for uric acid and ascorbic acid determinations, separately and in their mixture. The modified sensors have good calibration functions with good sensitivity (between 1.145 and 1.406 mA cm −2 /decade), reproducibility ( t hiocytosine (Au T C) and gold g uanine (Au G U) layers

  13. An investigation to compare the performance of methods for the determination of free acid in highly concentrated solutions of plutonium and uranium nitrate

    International Nuclear Information System (INIS)

    Crossley, D.

    1980-08-01

    An investigation has been carried out to compare the performance of the direct titration method and the indirect mass balance method, for the determination of free acid in highly concentrated solutions of uranium nitrate and plutonium nitrate. The direct titration of free acid with alkali is carried out in a fluoride medium to avoid interference from the hydrolysis of uranium or plutonium, while free acid concentration by the mass balance method is obtained by calculation from the metal concentration, metal valency state, and total nitrate concentration in a sample. The Gran plot end-point prediction technique has been used extensively in the investigation to gain information concerning the hydrolysis of uranium and plutonium in fluoride media and in other complexing media. The use of the Gran plot technique has improved the detection of the end-point of the free acid titration which gives an improvement in the precision of the determination. The experimental results obtained show that there is good agreement between the two methods for the determination of free acidity, and that the precision of the direct titration method in a fluoride medium using the Gran plot technique to detect the end-point is 0.75% (coefficient of variation), for a typical separation plant plutonium nitrate solution. The performance of alternative complexing agents in the direct titration method has been studied and is discussed. (author)

  14. Electrochemical determination of dopamine in the presence of ascorbic acid based on the gold nanorods/carbon nanotubes composite film

    Energy Technology Data Exchange (ETDEWEB)

    Deng Chunyan, E-mail: dengchunyan81@126.com [Key Laboratory of Resources Chemistry of Nonferrous Metals, Central South University, Changsha, 410083 (China); Chen Jinzhuo; Yang Minghui [Key Laboratory of Resources Chemistry of Nonferrous Metals, Central South University, Changsha, 410083 (China); Nie Zhou [State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University, Changsha 410082 (China); Si Shihui [Key Laboratory of Resources Chemistry of Nonferrous Metals, Central South University, Changsha, 410083 (China)

    2011-10-01

    Highlights: > The GNR/CNT/GC electrode was fabricated simply. It has higher catalytic activity towards the oxidation of DA and ascorbic acid (AA). The selective determination of DA was carried out with low detection limit (0.8 nM, S/N = 3). The proposed method was feasible to detect the concentration of DA in human blood serum. - Abstract: In this paper, the gold nanorods (GNRs)/multiwalled carbon nanotubes (CNT) composite film-modified glassy carbon (GC) electrode was fabricated simply by the electrostatic interaction between the positively charged GNRs and the negatively charged CNT. And the GNRs/CNT/GC electrode was used for the selective and sensitive determination of dopamine (DA) in the presence of ascorbic acid (AA). It was found that the GNRs/CNT/GC electrode had higher catalytic activity towards the oxidation of DA and ascorbic acid (AA) comparing with the bare GC and CNT/GC electrodes. It may be due to the synergic effect of GNRs and CNT, because the surface area of the GNRs/CNT/GC electrode increased, the edge plan sites presented on the CNT surface can improve the electron transfer between the modified electrode and DA, and the rod-shaped gold may be served as the mediator for the oxidation of dopamine and provided the electrocatalytic ability. Moreover, the voltammetric peaks of AA and DA were separated enough at the GNRs/CNT/GC electrode, which was sufficiently enough for the selective determination of DA. Thus, the selective determination of DA was carried out with low detection limit (0.8 nM, S/N = 3). Also it was obtained that the proposed method was feasible to detect the concentration of DA in human blood serum. Therefore, it can be concluded that the GNRs/CNT modified electrode may be advantageous for the DA determination.

  15. Determination of N metabolism parameters following 15N-amino acid infusion based on a mathematical model

    International Nuclear Information System (INIS)

    Pahle, T.; Koehler, R.; Souffrant, W.B.; Gebhardt, G.; Matkowitz, R.; Hartig, W.

    1983-01-01

    Two female pigs (25 kg live weight) received a continuous infusion of 15 N-glycine and 15 N-lysine solutions, resp., for 45 h and for further 72 h unlabelled amino acid solutions. The main protein and energy sources, however, were administered orally. The time course of the 15 N level and the differential urinary N excretion were determined from blood urea and urine. For the demonstration of synthesis and decay rates of the total body protein a mathematical model has been developed. The suitability of 15 N-lysine and 15 N-glycine for the determination of N metabolism parameters is discussed

  16. Influence of humic acids on the migration behavior of radioactive and non-radioactive substances under conditions close to nature. Synthesis, radiometric determination of functional groups, complexation

    International Nuclear Information System (INIS)

    Pompe, S.; Bubner, M.; Schmeide, K.; Heise, K.H.; Bernhard, G.; Nitsche, H.

    2000-04-01

    The interaction behavior of humic acids with uranium(VI) and the influence of humic substances on the migration behavior of uranium was investigated. A main focus of this work was the synthesis of four different humic acid model substances and their characterization and comparison to the natural humic acid from Aldrich. A radiometric method for the determination of humic acid functional groups was applied in addition to conventional methods for the determination of the functionality of humic acids. The humic acid model substances show functional and structural properties comparable to natural humic acids. Modified humic acids with blocked phenolic OH were synthesized to determine the influence of phenolic OH groups on the complexation behavior of humic acids. A synthesis method for 14 C-labeled humic acids with high specific activity was developed. The complexation behavior of synthetic and natural humic acids with uranium(VI) was investigated by X-ray absorption spectroscopy, laser-induced fluorescence spectroscopy and FTIR spectroscopy. The synthetic model substances show an interaction behavior with uranium(VI) that is comparable to natural humic acids. This points to the fact that the synthetic humic acids simulate the functionality of their natural analogues very well. For the first time the influence of phenolic OH groups on the complexation behavior of humic acids was investigated by applying a modified humic acid with blocked phenolic OH groups. The formation of a uranyl hydroxy humate complex was identified by laserspectroscopic investigations of the complexation of Aldrich humic acid with uranium(VI) at pH7. The migration behavior of uranium in a sandy aquifer system rich in humic substances was investigated in column experiments. A part of uranium migrates non-retarded through the sediment, bound to humic colloids. The uranium migration behavior is strongly influenced by the kinetically controlled interaction processes of uranium with the humic colloids

  17. Direct determination of mercury in cosmetic samples by isotope dilution inductively coupled plasma mass spectrometry after dissolution with formic acid

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Ying; Shi, Zeming; Zong, Qinxia; Wu, Peng; Su, Jing [Sichuan Provincial Key Laboratory of Nuclear Technology in Geology, College of Nuclear Technology and Automation Engineering, Chengdu University of Technology, Chengdu 610059 (China); Liu, Rui, E-mail: liur.ray@gmail.com [Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu 610059 (China)

    2014-02-17

    Graphical abstract: -- Highlights: •Simple, sensitive, and accurate method is established for mercury determination in cosmetics. •The sample preparation procedure is highly simplified. •Isotope dilution efficiently eliminates matrix effect. •First report of using formic acid based method in combination with PVG-ID-ICP MS for mercury quantitation in cosmetics. -- Abstract: A new method was proposed for the accurate determination of mercury in cosmetic samples based on isotopic dilution (ID)-photochemical vapor generation (PVG)-inductively coupled plasma mass spectrometry (ICP MS) measurement. Cosmetic samples were directly dissolved in formic acid solution and subsequently subjected to PVG for the reduction of mercury into vapor species following by ICP MS detection. Therefore, the risks of analyte contamination and loss were avoided. Highly enriched {sup 201}Hg isotopic spike is added to cosmetics and the isotope ratios of {sup 201}Hg/{sup 202}Hg were measured for the quantitation of mercury. With ID calibration, the influences originating from sample matrixes for the determination of mercury in cosmetic samples have been efficiently eliminated. The effects of several experimental parameters, such as the concentration of the formic acid, and the flow rates of carrier gas and sample were investigated. The method provided good reproducibility and the detection limits were found to be 0.6 pg mL{sup −1}. Finally, the developed method was successfully applied for the determination of mercury in six cosmetic samples and a spike test was performed to verify the accuracy of the method.

  18. Quantitative Determination of Fatty Acids in Marine Fish and Shellfish from Warm Water of Straits of Malacca for Nutraceutical Purposes

    Directory of Open Access Journals (Sweden)

    Nurnadia Abd Aziz

    2013-01-01

    Full Text Available This study was conducted to quantitatively determine the fatty acid contents of 20 species of marine fish and four species of shellfish from Straits of Malacca. Most samples contained fairly high amounts of polyunsaturated fatty acids (PUFAs, especially alpha-linolenic acid (ALA, C18:3 n3, eicosapentaenoic acid (EPA, C20:5 n3, and docosahexaenoic acid (DHA, C22:6 n3. Longtail shad, yellowstripe scad, and moonfish contained significantly higher (P<0.05 amounts of eicosapentaenoic acid (EPA, docosahexaenoic acid (DHA, and alpha-linolenic acid (ALA, respectively. Meanwhile, fringescale sardinella, malabar red snapper, black pomfret, Japanese threadfin bream, giant seaperch, and sixbar grouper showed considerably high content (537.2–944.1 mg/100g wet sample of desirable omega-3 fatty acids. The polyunsaturated-fatty-acids/saturated-fatty-acids (P/S ratios for most samples were higher than that of Menhaden oil (P/S=0.58, a recommended PUFA supplement which may help to lower blood pressure. Yellowstripe scad (highest DHA, ω-3/ω-6=6.4, P/S=1.7, moonfish (highest ALA, ω-3/ω-6=1.9, P/S=1.0, and longtail shad (highest EPA, ω-3/ω-6=0.8, P/S=0.4 were the samples with an outstandingly desirable overall composition of fatty acids. Overall, the marine fish and shellfish from the area contained good composition of fatty acids which offer health benefits and may be used for nutraceutical purposes in the future.

  19. Simultaneous determination of furfural and its degradation products, furoic acid and maleic acid, in transformer oil by the reversed-phase vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Yifan; Li, Haiyan; Yang, Zhen; Zhang, Weijie; Hua, Jia

    2017-12-01

    To explore why the use of furfural as a transformer oil-paper insulation aging characteristic is problematic in real world application, we developed a method for the simultaneous determination of furfural, furoic acid, and maleic acid in transformer oil by reversed-phase vortex-assisted liquid-liquid microextraction combined with high-performance liquid chromatography. The conditions for the proposed method were optimized, and the obtained extract can be directly analyzed by high-performance liquid chromatography. The detection limits (signal-to-noise ratio = 3) of the method ranged from 1.0 to 4.6 μg/L, the enrichment factors for furfural, furoic acid, maleic acid, and fumaric acid were 4.6, 25.1, 15.6, and 17.5, respectively, and the recovery rates for three analytes (fumaric acid was undetected) range from 82.1 to 106.2%. The contents of furfural, furoic acid, and maleic acid resulted from accelerated aging of transformer insulation oil-paper were measured using the present method for the first time, and the aging samples were analyzed by liquid chromatography with mass spectrometry for the identification of furoic acid and maleic acid in the aging transformer oil samples. Using the optimal method, the target products of samples at different aging time were tracked and measured. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Experimental determination of the (vapor + liquid) equilibrium data of binary mixtures of fatty acids by differential scanning calorimetry

    International Nuclear Information System (INIS)

    Matricarde Falleiro, Rafael M.; Meirelles, Antonio J.A.; Kraehenbuehl, Maria A.

    2010-01-01

    (Vapor + liquid) equilibrium (VLE) data for three binary mixtures of saturated fatty acids were obtained by differential scanning calorimetry (DSC). However, changes in the calorimeter pressure cell and the use of hermetic pans with holes (φ = 250 mm) in the lids were necessary to make it possible to apply this analytical technique, obtaining accurate results with smaller samples and shorter operational times. The systems evaluated in this study were: myristic acid (C 14:0 ) + palmitic acid (C 16:0 ), myristic acid (C 14:0 ) + stearic acid (C 18:0 ), and palmitic acid (C 16:0 ) + stearic acid (C 18:0 ), all measured at 50 mm Hg and with mole fractions between 0.0 and 1.0 in relation to the most volatile component of each diagram. The fugacity coefficients for the components in the vapor phase were calculated using the Hayden and O'Connell method [J.G. Hayden, J.P. O'Connell, Ind. Eng. Chem. Process Design Develop. 14 (3) (1975) 209-216] and the activity coefficients for the liquid phase were correlated with the traditional g E models (NRTL [H. Renon, J.M. Prausnitz, Aiche J. 14 (1968) 135-144], UNIQUAC [D.S. Abrams, J.M. Prausnitz, Aiche J. 21 (1975) 116-128], and Wilson [J.M. Prausnitz, N.L. Linchtenthaler, E.G. Azevedo, Molecular Thermodynamics of Fluid-phase Equilibria, River-Prentice Hall, Upper Saddle, 1999]). The sets of parameters were then compared in order to determine which adjustments best represented the VLE.

  1. Catalyzed oxidation reactions. IV. Picolinic acid catalysis of chromic acid oxidations

    International Nuclear Information System (INIS)

    Rocek, J.; Peng, T.Y.

    1977-01-01

    Picolinic acid and several closely related acids are effective catalysts in the chromic acid oxidation of primary and secondary alcohols; the oxidation of other substrates is accelerated only moderately. The reaction is first order in chromium-(VI), alcohol, and picolinic acid; it is second order in hydrogen ions at low acidity and approaches acidity independence at high perchloric acid concentrations. A primary deuterium kinetic isotope effect is observed at high but not at low acidities. At low acidity the reaction has a considerably lower activation energy and more negative activation entropy than at higher acidities. The reactive intermediate in the proposed mechanism is a negatively charged termolecular complex formed from chromic acid, picolinic acid, and alcohol. The rate-limiting step of the reaction changes with the acidity of the solution. At higher acidities the intermediate termolecular complex is formed reversibly and the overall reaction rate is determined by the rate of its decomposition into reaction products; at low acidities the formation of the complex is irreversible and hence rate limiting. Picolinic acids with a substituent in the 6 position show a greatly reduced catalytic activity. This observation is interpreted as suggesting a square pyramidal or octahedral structure for the reactive chromium (VI) intermediate. The temperature dependence of the deuterium isotope effect has been determined and the significance of the observed large values for E/sub a//sup D/ - E/sub a//sup H/ and A/sup D//A/sup H/ is discussed

  2. Determination of naphthenic acid profile in Ghana's Jubilee Oil using gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Osuteye, I.

    2015-01-01

    Crude oil is the life-blood of the global economy. Its importance stems from the fact that it is a base product for a wide variety of goods [Drugs, Plastics, Liquefied Petroleum Gas (LPG)]. The oil discovery (over 3 billion barrel reserves in hydrocarbon and gas), about 60 km offshore between the Deepwater Tano and Cape Three Points Block in South western Ghana is a valuable natural asset and it has the potential of boosting the Ghanaian economy. During petroleum processing, various waste products are generated. One of such products is Naphthenic acids (NA). Naphthenic acids are organic acids naturally occurring in crude oil and a constituent of waste associated with oil refinery. Naphthenic acids serve as biomarkers for identification of the source of crude oil. The presence of Naphthenic acid in the aquatic environment causes toxic effects due to their weak biodegradable nature; the toxicity of Naphthenic acids depends on the class of Naphthenic acids present in the crude oil. The study assessed the profile of Naphthenic acids in Ghana’s Jubilee crude oil using Low Resolution Electron Impact – Gas Chromatography Mass Spectrometry (LREI-GCMS) after isolation of Naphthenic acids in the Jubilee oil by a modified Kupchan’s Partitioning Process. The Mass Spectrometric (MS) Work Station Software was used for the identification of the Naphthenic acids present in the Jubilee crude oil. The quality of the Jubilee oil was also evaluated through the use of some key physico-chemical parameters [Total Acid Number (TAN), Sulphur Content, Viscosity, Pour Point, Flashpoint, Water Content and Densities] based on the American Standards for Testing and Materials (ASTM, 2007). The Total Acid Number was determined by Colorimetric Titration (ASTM D974); Sulphur Content by X-ray Fluorescent Spectrometry (ASTM D4294); Pour Point by the use of the SETA cloud and Pour Point Refrigerator Technique (ASTM D97); Viscosity by Gravity Timed Method (ASTM D445); Density by the Hydrometer

  3. Simultaneous Determination of Seven Phenolic Acids in Rat Plasma Using UHPLC-ESI-MS/MS after Oral Administration of Echinacea purpurea Extract

    Directory of Open Access Journals (Sweden)

    Yan Du

    2017-09-01

    Full Text Available A rapid and sensitive Ultra High Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry (UHPLC-ESI-MS/MS method was developed and validated to simultaneously determine the concentration of seven phenolic acids (syringic acid, ferulic acid, caffeic acid, vanillic acid, p-coumaric acid, 3,4-dihydroxybenzoic acid and 4-hydroxybenzoic acid in rat plasma after oral administration of Echinacea purpurea extract. After mixing with the internal standard (IS, butylparaben, plasma samples were prepared by liquid–liquid extraction with ethyl acetate. The separation was performed using the Agilent Eclipse Plus C18 column (1.8 μm, 2.1 mm × 50 mm with a gradient system consisting of solution A (0.1% acetic acid in water and solution B (methanol at a flow rate of 0.3 mL/min. The detection was accomplished by a multiple reaction monitoring (MRM mode with electrospray ionization (ESI. The method was validated in terms of linearity, precision, accuracy, extraction recovery, matrix effect and stability. This method was successfully applied to study the pharmacokinetic properties of the seven compounds after oral administration of Echinacea purpurea extract in rats.

  4. Determination of free amino acids and 18 elements in freeze-dried strawberry and blueberry fruit using an Amino Acid Analyzer and ICP-MS with micro-wave digestion.

    Science.gov (United States)

    Zhang, Hua; Wang, Zhen-Yu; Yang, Xin; Zhao, Hai-Tian; Zhang, Ying-Chun; Dong, Ai-Jun; Jing, Jing; Wang, Jing

    2014-03-15

    The objective of this study was to investigate the level of 18 trace elements of two freeze-dried samples from the Blueberry (Vaccinium corymbosum) and the Strawberry (Fragaria × Ananassa). The total free amino acid composition in the blueberry and strawberry was determined by an Amino Acid Analyzer. Eleven free amino acids were found in both berries. The trace elements in each dried fruit sample were determined by ICP-MS with microwave digestion. The linearity range of the standard curves was 0-1250.0 μg L(-1) (Mg, P, K, Ca),while in all cases, except for B, Na, Al, Cr, Mn, Fe, Ni, Cu, Zn, Se, Cd, Pb, Ge and As, which was 125.0 μg mL(-1), all related coefficients were above 0.9999; recovery was in the range of 79.0-106.8%. Minor concentrations of nutritional elements were found in each freeze-dried berry. In sum, the toxic trace element analysis found the content of toxic trace elements in each freeze-dried berry sample was safe for human consumption and that the overall quality of the blueberry surpassed that of the strawberry. The results certify that the two freeze-dried berries have potential for human consumption in value-added products and have a certain theoretical and practical significance. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

  5. Identifying a base in a nucleic acid

    Science.gov (United States)

    Fodor, Stephen P. A.; Lipshutz, Robert J.; Huang, Xiaohua

    2005-02-08

    Devices and techniques for hybridization of nucleic acids and for determining the sequence of nucleic acids. Arrays of nucleic acids are formed by techniques, preferably high resolution, light-directed techniques. Positions of hybridization of a target nucleic acid are determined by, e.g., epifluorescence microscopy. Devices and techniques are proposed to determine the sequence of a target nucleic acid more efficiently and more quickly through such synthesis and detection techniques.

  6. determination of TOC value (sugar, organic acid and pesticides) in sewage waste water in Damascus city

    International Nuclear Information System (INIS)

    Takriti, S.; Odah, A.

    2000-03-01

    The determination and radiation degradation of organic pollutant existing in municipal sewage wastewater of Damascus plant were investigated. The wastewater samples were analyzed using TOC, HPLC, and GC techniques, and irradiation was carried out using gamma radiation with dose rate 3.5 kGy/h. The results have shown that the TOC value increases in hot season. Some of pesticides have been noticed in wastewater. These pesticides need 2.5 kGy to be degraded. The variation of TOC gives the raison to determined the existence of organic acids as function of gamma doses. Therefore, the concentration of the citric, malic, oxalic and acitic acids was increased with the increase of gamma dose. it is clear that the high value of TOC need high dose to be degraded. It is shown that with low dose the value of TOC increased and then started to be decreased. This remark may be due to the radiation reactions in aqueous phase. Significant decrease of organic pollutants degradation is caused by the presence of very small amount of hydroxyl group which known as effective scavenger for radicals. (Author)

  7. A Modified Fluorimetric Method for Determination of Hydrogen Peroxide Using Homovanillic Acid Oxidation Principle

    Directory of Open Access Journals (Sweden)

    Biswaranjan Paital

    2014-01-01

    Full Text Available Hydrogen peroxide (H2O2 level in biological samples is used as an important index in various studies. Quantification of H2O2 level in tissue fractions in presence of H2O2 metabolizing enzymes may always provide an incorrect result. A modification is proposed for the spectrofluorimetric determination of H2O2 in homovanillic acid (HVA oxidation method. The modification was included to precipitate biological samples with cold trichloroacetic acid (TCA, 5% w/v followed by its neutralization with K2HPO4 before the fluorimetric estimation of H2O2 is performed. TCA was used to precipitate the protein portions contained in the tissue fractions. After employing the above modification, it was observed that H2O2 content in tissue samples was ≥2 fold higher than the content observed in unmodified method. Minimum 2 h incubation of samples in reaction mixture was required for completion of the reaction. The stability of the HVA dimer as reaction product was found to be >12 h. The method was validated by using known concentrations of H2O2 and catalase enzyme that quenches H2O2 as substrate. This method can be used efficiently to determine more accurate tissue H2O2 level without using internal standard and multiple samples can be processed at a time with additional low cost reagents such as TCA and K2HPO4.

  8. Gas chromatographic determination of acid herbicides in surface water samples with electron-capture detection and mass spectrometric confirmation

    NARCIS (Netherlands)

    Vink, M.; Poll, J.M. van der

    1996-01-01

    The development of a multi-residue method for the determination of eight polar acidic herbicides (MCPA, MCPB, mecoprop, 2,4-D, dichlorprop, bentazone, dicamba and dikegulac) in surface water is described. The method involves an off-line solid-phase extraction (SPE) procedure prior to instrumental

  9. Rapid and simple clean-up and derivatizaton procedure for the gas chromatographic determination of acidic drugs in plasma

    NARCIS (Netherlands)

    Roseboom, H.; Hulshoff, A.

    1979-01-01

    A rapid and simple clean-up and derivatization procedure that can be generally applied to the gas chromatographie (GC) determination of acidic drugs of various chemical and therapeutic classes is described. The drugs are extracted from acidified plasma with chloroform containing 5% of isopropanol,

  10. Fabrication and characterisation of high performance polypyrrole modified microarray sensor for ascorbic acid determination

    Energy Technology Data Exchange (ETDEWEB)

    Samseya, J. [Alagappa University, Karaikudi, Tamil Nadu (India); Srinivasan, R., E-mail: sivarunjan@gmail.com [Central Electro Chemical Research Insititute, Karaikudi, Tamil Nadu (India); Chang, Yu-Tsern; Tsao, Cheng-Wen [Department of Cosmetic Applications, Taoyuan Innovation Institute of Technology, Taiwan (China); Vasantha, V.S. [Madurai Kamaraj University, Madurai, Tamil Nadu (India)

    2013-09-02

    Graphical abstract: -- Highlights: •Gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. •Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared. •Ppy/Au/MEA used for ascorbic acid determination in the presence of different neurotransmitters. •The micro array exhibited wide linear range, very high sensitivity and very low LOD than the earlier reports. •It was used successfully to test ascorbic acid in different types real samples. -- Abstract: In this study, gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared by cyclic voltammetry technique. The deposition potential range and number of cycles were optimised in order to get optimum thickness of Ppy film. Scanning Electron Microscope and Atomic Force Microscope investigations reveal that Ppy coating formed at 3 cycles is porous with thickness of 1.5 μm which exhibiting high catalytic current for ascorbic acid (AA) in square wave technique (SWV). In contrast to earlier sensors designs, these Ppy/Au/MEA sensors exhibits lower detection limit (LOD) of 10 nm towards AA at physiological conditions. It also exhibits enhanced sensitivity (2.5 mA cm{sup −2} mM{sup −1}) and long range of linear detection limit from 10 nm to 2.8 mM. In the same way, polypyrrole modified macro Au (Ppy/Au/MA) biosensor was also fabricated and its electro catalytic property towards AA was compared with that of Ppy/Au/MEA. The Ppy/Au/MA exhibits sensitivity of only 0.27 mA cm{sup −2} mM{sup −1}, LOD of 5 μM and linear range of 10 μM to 2.2 mM. Hence, our investigations indicate that the Ppy/Au/MEA could serve as highly sensitive sensor for AA than any of the earlier designs. So, the Ppy/Au/MEA electrode was utilised for determination AA in a wide variety of real samples.

  11. Fabrication and characterisation of high performance polypyrrole modified microarray sensor for ascorbic acid determination

    International Nuclear Information System (INIS)

    Samseya, J.; Srinivasan, R.; Chang, Yu-Tsern; Tsao, Cheng-Wen; Vasantha, V.S.

    2013-01-01

    Graphical abstract: -- Highlights: •Gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. •Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared. •Ppy/Au/MEA used for ascorbic acid determination in the presence of different neurotransmitters. •The micro array exhibited wide linear range, very high sensitivity and very low LOD than the earlier reports. •It was used successfully to test ascorbic acid in different types real samples. -- Abstract: In this study, gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared by cyclic voltammetry technique. The deposition potential range and number of cycles were optimised in order to get optimum thickness of Ppy film. Scanning Electron Microscope and Atomic Force Microscope investigations reveal that Ppy coating formed at 3 cycles is porous with thickness of 1.5 μm which exhibiting high catalytic current for ascorbic acid (AA) in square wave technique (SWV). In contrast to earlier sensors designs, these Ppy/Au/MEA sensors exhibits lower detection limit (LOD) of 10 nm towards AA at physiological conditions. It also exhibits enhanced sensitivity (2.5 mA cm −2 mM −1 ) and long range of linear detection limit from 10 nm to 2.8 mM. In the same way, polypyrrole modified macro Au (Ppy/Au/MA) biosensor was also fabricated and its electro catalytic property towards AA was compared with that of Ppy/Au/MEA. The Ppy/Au/MA exhibits sensitivity of only 0.27 mA cm −2 mM −1 , LOD of 5 μM and linear range of 10 μM to 2.2 mM. Hence, our investigations indicate that the Ppy/Au/MEA could serve as highly sensitive sensor for AA than any of the earlier designs. So, the Ppy/Au/MEA electrode was utilised for determination AA in a wide variety of real samples

  12. Determination of trace elements in biological samples treated with formic acid by inductively coupled plasma mass spectrometry using a microconcentric nebulizer

    International Nuclear Information System (INIS)

    Tormen, Luciano; Gil, Raul A.; Frescura, Vera L.A.; Dante Martinez, Luis; Curtius, Adilson J.

    2010-01-01

    A simple a