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Sample records for acid determination metodos

  1. 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.

  2. 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

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    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)

  3. 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

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    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.

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

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    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.

  5. 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)

  6. Determination of polycyclic aromatic hydrocarbons (PAHs). gas chromatographic method; Determinazione degli idrocarburi policiclici aromatici (IPA). Metodo gascaromatografico

    Energy Technology Data Exchange (ETDEWEB)

    Menichini, E; Viviano, G [Istituto Superiore di Sanita` , Rome (Italy). Lab. di Igiene Ambientale

    1997-12-01

    The method enables the determination of 4- to 6- ring PAHs and particularly of carcinogenic PAHs regulated in Italy. This revision is based on the results of a national collaborative study. Sample extract, obtained by a method described in a previous report (Rapporto ISTISAN: 90/33) is cleaned up by thin layer chromatography and analysed by gas chromatography; identification is confirmed by mass spectrometry. An intralaboratory quality control program is described.

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

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    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.

  8. 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

  9. Determination of the response time of pressure transducers using the direct method; Determinacao do tempo de resposta de transdutores de pressao utilizando o metodo de medida direta

    Energy Technology Data Exchange (ETDEWEB)

    Perillo, S R.P.

    1994-12-31

    The available methods to determine the response time of nuclear safety related pressure transducers are discussed, with emphasis to the direct method. In order to perform the experiments, a Hydraulic Ramp Generator was built. The equipment produces ramp pressure transients simultaneously to a reference transducer and to the transducer under test. The time lag between the output of the two transducers, when they reach a predetermined setpoint, is measured as the time delay of the transducer under test. Some results using the direct method to determine the time delay of pressure transducers (1 E Class Conventional) are presented. (author). 18 refs, 35 figs, 12 tabs.

  10. Validation of a method to determine methylmercury in fish tissues using gas chromatography; Validacion de un metodo para determinar metilmercurio en tejido de pescado por cromatografia de gases

    Energy Technology Data Exchange (ETDEWEB)

    Vega Bolannos, Luisa O; Arias Verdes, Jose A; Beltran Llerandi, Gilberto; Castro Diaz, Odalys; Moreno Tellez, Olga L [Instituto de Nutricion e Higiene de los Alimentos, La Habana (Cuba)

    2000-07-01

    We validated a method to determine methylmercury in fish tissues using gas chromatography with an electron capture detector as described by the Association of Official Analytical Chemist (AOAC) International. The linear curve range was 0.02 to 1 g/ml and linear correlation coefficient was 0.9979. A 1 mg/kg methylmercury-contaminated fish sample was analyzed 20 times to determine repeatability of the method. The quantification limit was 0.16 mg/kg and detection limit was 0.06 ppm. Fish samples contaminated with 0.2 to 10 mg/kg methylmercury showed recovery indexes from 94.66 to 108.8%.

  11. Method to determine the activity concentration and total activity of radioactive waste; Metodo para determinar la concentracion de actividad y actividad total de desechos radiactivos

    Energy Technology Data Exchange (ETDEWEB)

    Angeles C, A

    2001-02-15

    A characteristic system of radioactive waste is described to determine the concentration of radionuclides activity and the total activity of bundles of radioactive waste. The system this integrated by three subsystems: - Elevator of drums. - Electromechanics. - Gamma spectroscopy. In the system it is analyzed waste of issuing gamma specifically, and this designed for materials of relative low density and it analyzes materials of cylindrical recipients.

  12. Analytical Comparison of Miniaturized Methods for Selected PAH Determination in Clean Waters; Comparacion Analitica de 4 Metodos Miniaturizados de Determinacion de PAHs mediante HPLC en Aguas

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, S.; Perez, R. M.; Fernandez, O.

    2012-04-11

    A study on the comparison and evaluation of 4 miniaturized extraction methods for the determination of selected PAHs in clear waters is presented. Four types of liquid-liquid extraction were used for chromatographic analysis by HPLC/ FD. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the scope of the methods developed at low and high levels of concentration. (Author) 13 refs.

  13. In-situ gamma spectrometry method for determination of environmental gamma dose; Metodo de espectrometria gamma in situ para determinacao de dose gama ambiental

    Energy Technology Data Exchange (ETDEWEB)

    Conti, Claudio de Carvalho

    1995-07-15

    This work tries to establish a methodology for germanium detectors calibration, normally used for in situ gamma ray spectrometry, for determining the environmental exposure rate in function of the energy of the incident photons. For this purpose a computer code has been developed, based on the stripping method, for the computational spectra analysis to calculate the contribution of the partial absorption of the gamma rays (Compton effect) in the active and nonactive parts of the detector. The resulting total absorption spectrum is then converted to fluence distribution in function of the energy for the photons reaching the detector, which is then used to calculate the exposure rate or kerma in air. The unfolding and fluency convention parameters are determined by detector calibration using point gamma sources. The method is validated by comparison of the results against the calculated exposure rate at a point of interest for the standards. This method is used for the direct measurement of the exposure rate distribution in function of the energy at the site, in situ measurement technic, leading to rapid results during an emergency situation and also used for indoor measurements. (author)

  14. Doses determination in UCCA treatments with LDR brachytherapy using Monte Carlo methods; Determinacion de dosis en tratamientos de CaCU con braquiterapia LDR usando metodos Monte Carlo

    Energy Technology Data Exchange (ETDEWEB)

    Benites R, J. L. [Centro Estatal de Cancerologia de Nayarit, Comite de Investigacion, Calz. de la Cruz 118 sur, 63000 Tepic, Nayarit (Mexico); Vega C, H. R., E-mail: neutronesrapidos@gmail.com [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Cipres No. 10, Fracc. La Penuela, 98068 Zacatecas, Zac. (Mexico)

    2017-10-15

    Using Monte Carlo methods, with the code MCNP5, a gynecological mannequin and a vaginal cylinder were modeled. The spatial distribution of absorbed dose rate in uterine cervical cancer (UCCA) treatments was determined under the modality of manual brachytherapy of low dose rate (B-LDR). The design of the model included the gynecological liquid water mannequin, a vaginal cylinder applicator of Lucite (PMMA) with hemisphere termination. The applicator was formed by a vaginal cylinder 10.3 cm long and 2 cm in diameter. This cylinder was mounted on a stainless steel tube 15.2 cm long by 0.6 cm in diameter. A linear array of four radioactive sources of Cesium 137 was inserted into the tube. 13 water cells of 0.5 cm in diameter were modeled around the vaginal cylinder and the absorbed dose was calculated in these. The distribution of the fluence of gamma photons in the mesh was calculated. It was found that the distribution of the absorbed dose is symmetric for cells located in the upper and lower part of the vaginal cylinder. The values of the absorbed dose rate were estimated for the date of manufacture of the sources. This result allows the use of the law of radioactive decay to determine the dose rate at any date of a gynecological treatment of B-LDR. (Author)

  15. Studies of trace element determinations in nails by neutron activation analysis method; Estudo de elementos traco em unhas pelo metodo de analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Aguiar, Amilton Reinaldo; Saiki, Mitiko [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

    1996-07-01

    The purpose of this work was to develop the neutron activation analysis for trace element determinations in nails in order to apply this method to the study of the cystic fibrosis disease. It was verified that the elements Al, As, Br, Ca, Cd, Cl, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Se and Zn can be determined by using short and long irradiations with thermal neutron flux from 10{sup 11} to 10{sup 13} n.cm{sup -2}.{sup -1} at the IEA-R1 nuclear research reactor. The washing solutions of triton-X100, NH{sub 4} OH and acetone were tested in order to eliminate external contaminants from the nail samples. The nail analyses of the individual fingers from both of hands showed that the samples must be collected from all the fingers from both of hands to have a representative sample. The precision and the accuracy of the results were also examined by analyzing NIES 10C Rice Flour, IUPAC Bowen's Kale and NIST 1572 Citrus Leaves reference materials. (author)

  16. Determination of Sn in 99{sup m}Tc Radiopharmaceutical Kits by Polarographic Methods; Determinacion de Estano en Radiofarmacos de 99{sup m}Tc mediante Metodos Polarograficos

    Energy Technology Data Exchange (ETDEWEB)

    Castro, M; Cruz, J; Sanchez, M

    2009-07-01

    Kits of 99{sup m}Tc radiopharmaceuticals are used in nuclear medicine for diagnosis of different diseases. Sn (II) is one of the essential components in their formulations, which is used for reduction 99{sup m}Tc-pertechnetate in cold kits for on-site preparation 99{sup m}Tc-pertechnetate radiopharmaceuticals. Usually, these cold kits contain different additives (complexing agents, antioxidants, buffers, etc.) and the amount of Sn (II) varies from kit to kit. The determination of Sn in these products is essential in assessing their quality. We report here the development of a new polarographic method for the determination of Sn (II) and total Sn in representative radiopharmaceuticals kits (for the content of Sn and chemical composition) produced at the Center of Isotopes of Cuba (CENTIS). These methods were validated by analysis of variance and recovery techniques. From the results of the validation, the characteristic functions of uncertainties and fits are considered for the established methods, which give the necessary evidences to demonstrate the usefulness of these methods according to the current trends in Analytical Chemistry. This work provides practical results of great importance for CENTIS. After the speciation of Sn in the MAG3 radiopharmaceuticals kit is inferred that the production process is affected by uncontrolled factors that influence in the product stability, which demonstrates the necessity for analytical tools for the characterization of products and processes. (Author) 57 refs.

  17. Determination of bacterial endotoxin (pyrogen) in radiopharmaceuticals by the gel clot method. Validation; Determinacao de endotoxina bacteriana (pirogenio) em radiofarmacos pelo metodo de formacao de gel. Validacao

    Energy Technology Data Exchange (ETDEWEB)

    Fukumori, Neuza Taeko Okasaki

    2008-07-01

    Before the Limulus amebocyte lysate (LAL) test, the only available means of pirogenicity testing for parenteral drugs and medical devices was the United States Pharmacopoeia (USP) rabbit pyrogen test. Especially for radiopharmaceuticals, the LAL assay is the elective way to determine bacterial endotoxin. The aim of this work was to validate the gel clot method for some radiopharmaceuticals without measurable interference. The FDA's LALTest guideline defines interference as a condition that causes a significant difference between the endpoints of a positive water control and positive product control series using a standard endotoxin. Experiments were performed in accordance to the USP bacterial endotoxins test in the {sup 131}I- m-iodobenzylguanidine; the radioisotopes Gallium-67 and Thallium-201; the lyophilized reagents DTPA, Phytate, GHA, HSA and Colloidal Tin. The Maximum Valid Dilution (MVD) was calculated for each product based upon the clinical dose of the material and a twofold serial dilution below the MVD was performed in duplicate to detect interferences. The labeled sensitivity of the used LAL reagent was 0.125 EU mL{sup -1} (Endotoxin Units per milliliter). For validation, a dilution series was performed, a twofold dilution of control standard endotoxin (CSE) from 0.5 to 0.03 EU mL{sup -1}, to confirm the labeled sensitivity of the LAL reagent being tested in sterile and non pyrogenic water, in quadruplicate. The same dilution series was performed with the CSE and the product in the 1:100 dilution factor, in three consecutive batches of each radiopharmaceutical. The products {sup 131}I-m-iodobenzylguanidine, Gallium-67, Thallium-201, DTPA, HSA and Colloidal Tin were found compatible with the LAL test at a 1:100 dilution factor. Phytate and GHA showed some interference in the gel clot test. Other techniques to determine endotoxins as the chromogenic (color development) and the turbidimetric test (turbidity development), were also assessed to get valuable

  18. Trace element determination study in human hair by neutron activation analysis; Estudo da determinacao de elementos traco em cabelos humanos pelo metodo de analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Frazao, Selma Violato

    2008-07-01

    Human hair analysis studies have been subject of continuous interest due to the fact that they can be used as an important tool to evaluate trace element levels in the human body. These determinations have been carried out to use hair for environmental and occupational monitoring, to identify intoxication or poisoning by toxic metals, to assess nutritional status, to diagnose and to prevent diseases and in forensic sciences. Although hair analysis presents several advantages over other human tissue or fluid analyses, such as organ tissue, blood, urine and saliva, there are some controversies regarding the use of hair analysis data. These controversies arise from the fact that it is difficult to establish reliable reference values for trace elements in hair. The purpose of this study was to evaluate the factors that affect element concentrations in hair samples from a population considered healthy and residing in the Sao Paulo metropolitan area. The collected human head hair was cut in small pieces, washed, dried and analyzed by neutron activation analysis (NAA). Aliquots of hair samples and synthetic elemental standards were irradiated at the IEA-R1 nuclear research reactor for 16 h under a thermal neutron flux of about 5x10{sup 12} n cm{sup -2} s{sup -1} for As, Br, Ca, Co, Cr, Cs, Cu, Fe, K, La, Na, Sb, Sc, Se and Zn determinations. The induced gamma activities of the standards and samples were measured using a gamma ray spectrometer coupled to an hiperpure Ge detector. For quality control of the results, IAEA- 85 Human Hair and INCT-TL-1 Tea Leaves certified reference materials (CRMs) were analyzed. Results obtained in these CRMs presented for most of elements, good agreement with the values of the certificates (relative errors less than 10%) and good precision (variation coefficients less than 13.6%). Results of replicate hair sample analysis showed good reproducibility indicating homogeneity of the prepared sample. Results obtained in the analyses of dyed and

  19. Determination of bacterial endotoxin (pyrogen) in radiopharmaceuticals by the gel clot method. Validation; Determinacao de endotoxina bacteriana (pirogenio) em radiofarmacos pelo metodo de formacao de gel. Validacao

    Energy Technology Data Exchange (ETDEWEB)

    Fukumori, Neuza Taeko Okasaki

    2008-07-01

    Before the Limulus amebocyte lysate (LAL) test, the only available means of pirogenicity testing for parenteral drugs and medical devices was the United States Pharmacopoeia (USP) rabbit pyrogen test. Especially for radiopharmaceuticals, the LAL assay is the elective way to determine bacterial endotoxin. The aim of this work was to validate the gel clot method for some radiopharmaceuticals without measurable interference. The FDA's LALTest guideline defines interference as a condition that causes a significant difference between the endpoints of a positive water control and positive product control series using a standard endotoxin. Experiments were performed in accordance to the USP bacterial endotoxins test in the {sup 131}I- m-iodobenzylguanidine; the radioisotopes Gallium-67 and Thallium-201; the lyophilized reagents DTPA, Phytate, GHA, HSA and Colloidal Tin. The Maximum Valid Dilution (MVD) was calculated for each product based upon the clinical dose of the material and a twofold serial dilution below the MVD was performed in duplicate to detect interferences. The labeled sensitivity of the used LAL reagent was 0.125 EU mL{sup -1} (Endotoxin Units per milliliter). For validation, a dilution series was performed, a twofold dilution of control standard endotoxin (CSE) from 0.5 to 0.03 EU mL{sup -1}, to confirm the labeled sensitivity of the LAL reagent being tested in sterile and non pyrogenic water, in quadruplicate. The same dilution series was performed with the CSE and the product in the 1:100 dilution factor, in three consecutive batches of each radiopharmaceutical. The products {sup 131}I-m-iodobenzylguanidine, Gallium-67, Thallium-201, DTPA, HSA and Colloidal Tin were found compatible with the LAL test at a 1:100 dilution factor. Phytate and GHA showed some interference in the gel clot test. Other techniques to determine endotoxins as the chromogenic (color development) and the turbidimetric test (turbidity development), were also assessed to get

  20. An Optimised Method to Determine PAHs in a Contaminated Soil; Metodo Optimizado para la Determinacion de PAHs en un Suelo Contaminado

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.; Sevillano castano, M. L.; Escolano Segovia, O.; Garcia Frutos, F. J.

    2007-07-20

    An analytical study is presented based on an optimised method to determine selected polycyclic aromatic hydrocarbons (PAHs) by High Performance Liquid Chromatography (HPLC) with fluorescence detection. The work was focused to obtain reliable measurements of PAH in a gas work contaminated soil and was performed in the frame of the project 'Assessment of natural remediation technologies for PAHs in contaminated soils' (Spanish Plan Nacional l+D+i, CTM 2004-05832-CO2-01): First assays were focused to evaluate an initial proposed procedure by sonication extraction in the contaminated soil. Afterwards to extend the efficiency and reduce solvent and time consuming of extraction procedures, the more relevant parameters that affect the extraction step were investigated. A comparison between sonication and microwave procedures was done, and the influence of sample grinding was studied. In general, both extraction techniques led on comparable results, although sonication procedure needs to be more carefully optimised. Finally, as a final application of the optimised method, the effect of particle size on relative distribution of selected PAHs in the contaminated soil was investigated. Relative abundance of more volatile PAHs showed a decreasing according to lower grain size, while relative abundance of less volatile compounds indicated an increasing of concentration levels for lower grain size. (Author) 10 refs.

  1. Determination of the fast neutrons spectra by the Elastic scattering method (n, p); Determinacion del espectro de neutrones rapidos por el metodo de la dispersion elastica (n, p)

    Energy Technology Data Exchange (ETDEWEB)

    Elizalde D, J

    1973-07-01

    This work consists in determining the fast neutron spectra emitted by a Pu-Be isotopic source. The implemented technique is based in the spectrometry (n, p). This consists in making to fall on a fast neutrons beams (polyenergetic) over a thin film of hydrogenated material, detecting the spectra of emitted protons at a fix angle. The polyethylene film and the used solid state detector are inside of a vacuum chamber. The detector is placed at 30 degree with respect to direction of the incident neutrons beam. The protons spectra is stored in a multichannel. the energy is obtained with the prior calibration of the system. The data processing involves the transformation of the protons spectra observed at the falling on neutrons spectra over the film. The energy of the neutrons is related with that of the protons, according to the collision kinematical equations. The cross section of elastic collision of the neutrons with the hydrogen atoms is obtained from literature. Applying these relations to the observed spectra it is obtained the falling on neutron spectra over the film. (Author)

  2. Optimization of a radiochemistry method for plutonium determination in biological samples; Optimizacion del metodo radioquimico para determinar plutonio en muestras biologicas

    Energy Technology Data Exchange (ETDEWEB)

    Cerchetti, Maria L; Arguelles, Maria G [Comision Nacional de Energia Atomica, Ezeiza (Argentina). Laboratorio de Dosimetria Personal y de Area

    2005-07-01

    Plutonium has been widely used for civilian an military activities. Nevertheless, the methods to control work exposition have not evolved in the same way, remaining as one of the major challengers for the radiological protection practice. Due to the low acceptable incorporation limit, the usual determination is based on indirect methods in urine samples. Our main objective was to optimize a technique used to monitor internal contamination of workers exposed to Plutonium isotopes. Different parameters were modified and their influence on the three steps of the method was evaluated. Those which gave the highest yield and feasibility were selected. The method involves: 1-) Sample concentration (coprecipitation); 2-) Plutonium purification; and 3-) Source preparation by electrodeposition. On the coprecipitation phase, changes on temperature and concentration of the carrier were evaluated. On the ion-exchange separation, changes on the type of the resin, elution solution for hydroxylamine (concentration and volume), length and column recycle were evaluated. Finally, on the electrodeposition phase, we modified the following: electrolytic solution, pH and time. Measures were made by liquid scintillation counting and alpha spectrometry (PIPS). We obtained the following yields: 88% for coprecipitation (at 60 C degree with 2 ml of CaHPO{sub 4}), 71% for ion-exchange (resins AG 1x8 Cl{sup -} 100-200 mesh, hydroxylamine 0.1N in HCl 0.2N as eluent, column between 4.5 and 8 cm), and 93% for electrodeposition (H{sub 2}SO{sub 4}-NH{sub 4}OH, 100 minutes and pH from 2 to 2.8). The expand uncertainty was 30% (NC 95%), the decision threshold (Lc) was 0.102 Bq/L and the minimum detectable activity was 0.218 Bq/L of urine. We obtained an optimized method to screen workers exposed to Plutonium. (author)

  3. 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).

  4. 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)

  5. 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.

  6. 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)

  7. 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.

  8. 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.

  9. 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

  10. 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...

  11. 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 ...

  12. 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

  13. 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

  14. 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

  15. [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.

  16. 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, ...

  17. 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)

  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. 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...

  20. 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

  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. 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

  3. 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.

  4. Use of radioanalytical methods for determination of uranium, neptunium, plutonium, americium and curium isotopes in radioactive wastes; Utilizacao de metodos radioanaliticos para a determinacao de isotopos de uranio, plutonio, americio e curio em rejeitos radioativos

    Energy Technology Data Exchange (ETDEWEB)

    Geraldo, Bianca

    2012-07-01

    Activated charcoal is a common type of radioactive waste that contains high concentrations of fission and activation products. The management of this waste includes its characterization aiming the determination and quantification of the specific radionuclides including those known as Difficult-to-Measure Radionuclides (RDM). The analysis of the RDM's generally involves complex radiochemical analysis for purification and separation of the radionuclides, which are expensive and time-consuming. The objective of this work was to define a methodology for sequential analysis of the isotopes of uranium, neptunium, plutonium, americium and curium present in a type of radioactive waste, evaluating chemical yield, analysis of time spent, amount of secondary waste generated and cost. Three methodologies were compared and validated that employ ion exchange (TI + EC), extraction chromatography (EC) and extraction with polymers (ECP). The waste chosen was the activated charcoal from the purification system of primary circuit water cooling the reactor IEA-R1. The charcoal samples were dissolved by acid digestion followed by purification and separation of isotopes with ion exchange resins, extraction and chromatographic extraction polymers. Isotopes were analyzed on an alpha spectrometer, equipped with surface barrier detectors. The chemical yields were satisfactory for the methods TI + EC and EC. ECP method was comparable with those methods only for uranium. Statistical analysis as well the analysis of time spent, amount of secondary waste generated and cost revealed that EC method is the most effective for identifying and quantifying U, Np, Pu, Am and Cm present in charcoal. (author)

  5. 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

  6. 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.

  7. Determination of Selected Perfluorinated Alkyl Acids in ...

    Science.gov (United States)

    The 1996 amendments to the Safe Drinking Water Act (SDWA) required EPA to establish a Contaminant Candidate List (CCL), that contains a list of drinking water contaminants that the Agency will consider for future regulation. EPA must make a regulatory determination on a minimum of five contaminants every five years. The first CCL was published in 1998, and updates were anticipated every five years thereafter. One of the key pieces of information that must be available in order to make a regulatory determination is nationwide occurrence data for the chemical contaminants under consideration. Historically, EPA has collected the necessary occurrence data under its Unregulated Contaminant Monitoring Regulations (UCMR). Under the UCMR, monitoring is conducted at selected drinking water utilities for specific contaminants of interest. The chemical analyses are usually performed by the utilities or by commercial laboratories. To meet the requirements of monitoring under the UCMR program, the analytical methods developed should be specific, sensitive, and practical enough for application in commercial laboratories. This task will focus on the development of analytical methods for chemicals identified on future CCLs or emerging contaminants not yet listed on the CCL. These methods will be used for the collection of occurrence data under future UCMRs. The objective of this research effort is to develop analytical methods to be used to measure the occurrence of

  8. 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 ...

  9. Evaluation of human dental loss caused by carbamide peroxide bleacher compared with phosphoric acid conditioning - radioactive method; Avaliacao da perda dental humana com o uso do clareador peroxido de carbamida comparado ao condicionamento com acido fosforico - metodo radiometrico

    Energy Technology Data Exchange (ETDEWEB)

    Adachi, Eduardo Makoto; Yousseff, Michel Nicolau [Sao Paulo Univ., SP (Brazil). Faculdade de Odontologia. Dept. de Dentistica; Saiki, Mitiko [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil). Lab. de Analise por Ativacao Neutronica

    2002-07-01

    The radiometric method was applied to the evaluation of dental loss caused by carbamide peroxide when it is applied on the surface layers of enamel and dentin tissues. Also the dental loss caused by the etching with 37% phosphoric acid procedure used in aesthetic restoration was assessed for comparison with those results obtained. The tooth samples irradiated with a P standard in a thermal neutron flux of the nuclear reactor were placed in contact with 10% carbamide peroxide or with 37% phosphoric acid solution. The radioactivity of {sup 32} P transferred from the radioactive teeth to the bleaching gel or to etching acid was measured using a Geiger Muller detector to calculate the mass of P removed in this treatment and losses were calculated after obtaining their P concentrations. Results obtained indicated that enamel and dentin exposed to carbamide peroxide bleaching agent lose phosphorus. The extent of enamel loss was smaller than that obtained for dentin. In the case of acid etching, there was no difference between the results obtained for enamel and dentin loss. Also the dentin loss obtained after a treatment of 30 applications of 10% carbamide peroxide was the same magnitude of that one application of 37% phosphoric acid. (author)

  10. 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.

  11. 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)

  12. 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)

  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. 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

  15. 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

    Energy Technology Data Exchange (ETDEWEB)

    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

  16. Influence of reason citric acid/ metal cations in the synthesis of mullite by Pechini Method; Iinfluencia da razao acido citrico/cations metalicos na sintese de mulita pelo Metodo Pechini

    Energy Technology Data Exchange (ETDEWEB)

    Braga, A.N.S.; Costa, D.L.; Farias, R.M.C.; Neves, G.A.; Lira, H.L.; Menezes, R.R., E-mail: Alluskynha@homail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Departamento de Engenharia de Materiais

    2014-07-01

    Mullite is a ceramic material with high technological applications. Its synthesis has been extensively studied due to their excellent properties. Thus, this paper proposes to obtain mullite by Pechini method. The amount of acid citric/metal cations in proportions of 3:1 and 1:1 were investigated in order to understand their influence in obtaining the mullite phase. The synthesized samples were characterized by X-ray diffraction (XRD) and thermal analysis (TG/DTG and DTA). The results showed that the ratio citric acid/metal cations influence on the formed phase with the mullite obtained only in proportion 1:1. With the increase of the ratio to 3:1 was observed the formation of the alumina layer. (author)

  17. Two new methods to determine the adhesion by means of internal friction in materials covered with films; Dos nuevos metodos para determinar la adhesion mediante friccion interna en materiales recubiertos con peliculas

    Energy Technology Data Exchange (ETDEWEB)

    Colorado, H. A.; Ghilarducci, A. A.; Salva, H. R.

    2006-07-01

    Two new models are proposed to determine the adhesion energy be means of the internal friction technique (IF) in thin films layered materials. for the first method is necessary to determine enthalpy by means of the IF technique, for which the adhesion work has been determined with experimental data. In the second method are necessary to perform IF tests at constant temperature. (Author)

  18. 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.

  19. 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

  20. 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)

  1. Scienza e conoscenza: sul valore del metodo scientifico

    Directory of Open Access Journals (Sweden)

    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.

  2. Method for determining the wedge angle from the daily measurements made with the measurement enabled devices DC6; Metodo para la determinacion del angulo de cuna a partir de las medidas diarias realizadas con el dispositio de medida QC6

    Energy Technology Data Exchange (ETDEWEB)

    Marques Fraguela, E.; Suero Rodrigo, M. A.

    2011-07-01

    The aim of this paper is to present a method for determining the angle of the wedges virtual electron linear accelerator (ALE) Siemens Primus, from the daily measurements made with the measurement system PTW-QC6Plus and found to be sufficiently sensitive to determine variations of {+-} 1 of this parameter. In addition, we study the behavior statistically CUFLE angle over a year.

  3. Molecular structure determination of cyclooctane by Ab Initio and electron diffraction methods in the gas phase; Determinacao da estrutura molecular do ciclooctano por metodos Ab Initio e difracao de eletrons na fase gasosa

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Wagner B. de [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Quimica

    2000-10-01

    The determination of the molecular structure of molecules is of fundamental importance in chemistry. X-rays and electron diffraction methods constitute in important tools for the elucidation of the molecular structure of systems in the solid state and gas phase, respectively. The use of quantum mechanical molecular orbital ab initio methods offer an alternative for conformational analysis studies. Comparison between theoretical results and those obtained experimentally in the gas phase can make a significant contribution for an unambiguous determination of the geometrical parameters. In this article the determination for an unambiguous determination of the geometrical parameters. In this article the determination of the molecular structure of the cyclooctane molecule by electron diffraction in the gas phase an initio calculations will be addressed, providing an example of a comparative analysis of theoretical and experimental predictions. (author)

  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. 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)

  6. Analytical method of Kr-85 determination, using cryogenic concentration and separation and liquid scintillation counting; Desarrollo del metodo de concentracion y se paracion criogenica cromatografica y medida radiactiva por centelleo liquido de Kr-85

    Energy Technology Data Exchange (ETDEWEB)

    Heras, M C; Perez, M M; Grau, A

    1983-07-01

    The method used in the Laboratory of the JEN for the determination of Kr-85 levels in gaseous effluents of nuclear power and in the atmosphere is described. Samples of air, collected in metallic cylinders, are introduced into a gas-solid chromatographic separation system which resolves Kr from the other air components. The separated Kr ia dissolved in a toluene based scintillation cocktail, and the Kr-85 content is determined by liquid scintillation counting. (Author)

  7. The two means method for the attenuation coefficient determination of archaeological ceramics from the North of Parana; Metodo dos dois meios para a determinacao do coeficiente de atenuacao de ceramicas arqueologicas do norte do Parana

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Richard Maximiliano Cunha e

    1998-12-31

    This work reports an alternative methodology for the linear attenuation coefficient determination ({mu} {rho}) of irregular form samples, in such a way that is not necessary to consider the sample thickness. With this methodology, indigenous archaeological ceramics fragments from the region of Londrina, north of Parana, were studied. These ceramics fragments belong to the Kaingaing and Tupiguarani traditions. The equation for the {mu} {rho} determination employing the two mean method was obtained and it was used for {mu} {rho} determination by the gamma ray beam attenuation if immersed ceramics, by turns, in two different means with known linear attenuation coefficient. By the other side, {mu} theoretical value was determined with the XCOM computer code. This code uses as input the ceramics chemistry composition and provides an energy versus mass attenuation coefficient table. In order to validate the two mean method validation, five ceramics samples of thickness 1.15 cm and 1.87 cm were prepared with homogeneous clay. Using these ceramics, {mu} {rho} was determined using the attenuation method, and the two mean method. The result obtained for {mu} {rho} and its respective deviation were compared for these samples, for the two methods. With the obtained results, it was concluded that the two means method is good for the linear attenuation coefficient determination of materials of irregular shape, what is suitable, specially, for archaeometric studies. (author) 25 refs., 29 figs., 28 tabs.

  8. The two means method for the attenuation coefficient determination of archaeological ceramics from the North of Parana; Metodo dos dois meios para a determinacao do coeficiente de atenuacao de ceramicas arqueologicas do norte do Parana

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Richard Maximiliano Cunha e

    1997-12-31

    This work reports an alternative methodology for the linear attenuation coefficient determination ({mu} {rho}) of irregular form samples, in such a way that is not necessary to consider the sample thickness. With this methodology, indigenous archaeological ceramics fragments from the region of Londrina, north of Parana, were studied. These ceramics fragments belong to the Kaingaing and Tupiguarani traditions. The equation for the {mu} {rho} determination employing the two mean method was obtained and it was used for {mu} {rho} determination by the gamma ray beam attenuation if immersed ceramics, by turns, in two different means with known linear attenuation coefficient. By the other side, {mu} theoretical value was determined with the XCOM computer code. This code uses as input the ceramics chemistry composition and provides an energy versus mass attenuation coefficient table. In order to validate the two mean method validation, five ceramics samples of thickness 1.15 cm and 1.87 cm were prepared with homogeneous clay. Using these ceramics, {mu} {rho} was determined using the attenuation method, and the two mean method. The result obtained for {mu} {rho} and its respective deviation were compared for these samples, for the two methods. With the obtained results, it was concluded that the two means method is good for the linear attenuation coefficient determination of materials of irregular shape, what is suitable, specially, for archaeometric studies. (author) 25 refs., 29 figs., 28 tabs.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  10. 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 ...

  11. 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 ...

  12. Two media method for linear attenuation coefficient determination of irregular soil samples; Metodo dos dois meios para a determinacao do coeficiente de atenuacao linear de amostras irregulares de solos

    Energy Technology Data Exchange (ETDEWEB)

    Vici, Carlos Henrique Georges

    2004-07-01

    In several situations of nuclear applications, the knowledge of gamma-ray linear attenuation coefficient for irregular samples is necessary, such as in soil physics and geology. This work presents the validation of a methodology for the determination of the linear attenuation coefficient ({mu}) of irregular shape samples, in such a way that it is not necessary to know the thickness of the considered sample. With this methodology irregular soil samples (undeformed field samples) from Londrina region, north of Parana were studied. It was employed the two media method for the {mu} determination. It consists of the {mu} determination through the measurement of a gamma-ray beam attenuation by the sample sequentially immersed in two different media, with known and appropriately chosen attenuation coefficients. For comparison, the theoretical value of {mu} was calculated by the product of the mass attenuation coefficient, obtained by the WinXcom code, and the measured value of the density sample. This software employs the chemical composition of the samples and supplies a table of the mass attenuation coefficients versus the photon energy. To verify the validity of the two media method, compared with the simple gamma ray transmission method, regular pome stone samples were used. With these results for the attenuation coefficients and their respective deviations, it was possible to compare the two methods. In this way we concluded that the two media method is a good tool for the determination of the linear attenuation coefficient of irregular materials, particularly in the study of soils samples. (author)

  13. A Simple Analytical Method Using HPLC with Fluorescence Detection to Determine Selected Polycyclic Aromatic Compounds in Filter Samples; Metodo Analitico Sencillo para la Determinacion de Compuestos Aromaticos Policiclicos en Muestras de Filtros mediante HPLC con Detector de Fluorescencia

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, S.; Perez, R. M.

    2014-06-01

    A study on the comparison and evaluation of a miniaturized extraction method for the determination of selected PACs in sample filters is presented. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the intermediate precision. (Author)

  14. 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)

  15. 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.

  16. Study of the precision and trueness of the Brazilian method for ethanol and gasoline determination; Estudo da precisao e exatidao do metodo brasileiro para determinacao de etanol e gasolina

    Energy Technology Data Exchange (ETDEWEB)

    Zucchini, Ricardo R.; Hinata, Patricia [Instituto de Pesquisas Tecnologicas (IPT), Sao Paulo, SP (Brazil); Gioseffi, Carla S.; Franco, Joao B.S. [Instituto Brasileiro de Petroleo, Gas e Biocombustiveis (IBP), Rio de Janeiro, RJ (Brazil); Nascimento, Cristina R.; Torres, Eduardo S. [Agencia Nacional do Petroleo, Gas Natural e Biocombustiveis (ANP), Rio de Janeiro, RJ (Brazil)

    2008-07-01

    The determination of repeatability and reproducibility standard deviations of an analytical method, s{sub r} and s{sub R}, obtained by Interlaboratory program, makes it possible to calculate many kinds of precision limits of the method, which are needed in every laboratory's routine result comparisons and also in between-laboratories comparisons. This paper presents the results of the first interlaboratory trial, accomplished in the Brazilian petroleum sector, performed to define the trueness and precision of the Brazilian standard method for the determination of fuel anhydrous ethylic alcohol content in gasoline, that was performed by 34 experienced laboratories. The r and R values were 0,7 and 2,3 and main factors that would improve and optimize the method are presented. (author)

  17. Determination of rare earth and uranium in reference biological materials certified by the method of neutron activation analysis; Determinacao de terras raras e de uranio em materiais biologicos de referencia certificados pelo metodo de analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Lais H.P.; Saiki, Mitiko, E-mail: laispaciulli@gmail.com, E-mail: mitiko@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    The objective of this study was to evaluate the precision and accuracy of the determinations of Sc, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and U in certified reference materials (CRMs). To solve the problem of interference from fission products of U in the determination of lanthanides were obtained correction factors for this interference for {sup 140}La, {sup 141}Ce, {sup 143}Ce, {sup 153}Sm and {sup 147}Nd. The experimental procedure of Neutron Activation Analysis consisted of irradiating aliquots of each of the CRMs with synthetic standards of elements under thermal neutron flux of the IEA-R1 nuclear reactor, followed by gamma-ray spectrometry using a high-resolution hyperpurity GE detector. The analyzes of CRMs indicate good accuracy and precision of results, demonstrating the feasibility of applying of established procedure in NAA of elements studied in organic vegetable matrices.

  18. Contribution to the spectrographic determination of impurities in uranium by the carrier distillation method; Nuevas aportaciones a la determinacion espectrografica de impurezas en materiales de uranio por el metodo de distilacion fraccionada con portador

    Energy Technology Data Exchange (ETDEWEB)

    Capdevila, C

    1967-07-01

    The carrier distillation method for the determination of impurities in uranium has been modified in order to get a greater sensitivity. Electrodes 9.5 mm. diam. with a crater 7 mm. diam. and 10 mm. deep have been used, being the weigh of charge 300 mg.. The elements considered were: Al, As, B, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, P, Pb, Si, Sn, Ti and V, over the range 0.01 to 30 ppm. (Author) 13 refs.

  19. Semi-empirical determination of the diffusion coefficient of the Fricke Xylenol Gel dosimeter through finite difference methods; Determinacao semi-empirica do coeficiente de difusao do dosimetro Fricke Xilenol Gel atraves do metodo de diferencas finitas

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, E.O.; Oliveira, L.N., E-mail: lucas@ifg.edu.br [Instituto Federal de Educacao, Ciencia e Tecnologia de Goias (IFG), Goiania, GO (Brazil)

    2014-11-01

    Partial Differential Equations (PDE) can model natural phenomena, such as related to physics, chemistry and engineering. For these classes of equations, analytical solutions are difficult to be obtained, so a computational approach is indicted. In this context, the Finite Difference Method (FDM) can provide useful tools for the field of Medical Physics. In this study, is described the implementation of a computational mesh, in order to be used in determining the Diffusion Coefficient (DC) of the Fricke Xylenol Gel dosimeter (FXG). The initial and boundary conditions both referred by experimental factors are modelled in FDM, thus making a semi-empirical study in determining the DC. Together, the method of Reflection and Superposition (SRM) and the analysis of experimental data, served as first validation for the simulation. Such methodologies interface generated concordant results for a range of error of 3% in concentration lines for small times when compared to the analytical solution. The result for the DC was 0.43 mm{sup 2} /h. This value is in concordance with measures parameters range found in polymer gels dosimeters: 0.3-2.0 mm{sup 2} /h. Therefore, the application of computer simulation methodology supported by the FDM may be used in determining the diffusion coefficient in FXG dosimeter. (author)

  20. 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)

  1. 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.

  2. Analysis of a calculation method for the determination of the value of safety or control bars; Analisis de un metodo de calculo para la determinacion del valor de barras de seguridad o control

    Energy Technology Data Exchange (ETDEWEB)

    Aguilar H, F; Torres A, C; Filio L, C [ININ, Gcia. de Reactores, 52045 Ocoyoacac, Estado de Mexico (Mexico)

    1982-09-15

    Due to the control or safety bars in a nuclear reactor are constituted by strongly absorbent materials, the Diffusion Theory like tool for the calculation of bar values is not directly applicable, should it use the Transport Theory. However the speed and economy of the Diffusion codes for the reactors calculation, those make attractiveness and by this reason its are used in the determination of characteristic parameters and even in the determination of bar values, not without before to make some theoretical developments that allow to make applicable this theory. The application of the Diffusion Theory in strongly absorbent media is based on the use of some effective cross sections distinct from the real ones obtained when imposing the reason that among the flow and it gradient in the external surface of such media (control element in general, bar type or flagstone) be similar to the one obtained using Transport Theory in all the control region (multiplicative and absorbent media) with those real cross sections. The effective cross sections were obtained of the Leopard-NUMICE cell code which has incorporate the respective calculation theory of effective cross sections. Later these constants its were used in the bidimensional diffusion code Exterminator-II, simulating in it, the distribution of safety or control bars. From the cell code its were also obtained the respective constants of the homogeneous fuel cell. The results as soon as those obtained bar values of the diffusion code, its were compared with some experimental results obtained in the R{phi} Swedish reactor of natural uranium and heavy water. In this work an analysis of the bar value of one of them, trying to determine the applicability of the method is made. (Author)

  3. 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.

  4. Analytical Evaluation to Determine Selected PAHs in a Contaminated Soil With Type II Fuel; Metodo Optimizado de Extraccion por Ultrasonidos para la Determinacion de PAHs Seleccionados en un Suelo Contaminado con Fuel de Tipo II

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.; Sevillano Castano, M. L.; Garcia Frutos, F. J.

    2010-10-21

    A study on the optimization of an ultrasonic extraction method for selected PAHs determination in soil contaminated by type II fuel and by using HPLC with fluorescence detector is presented. The main objective was optimize the analytical procedure, minimizing the volume of solvent and analysis time and avoiding possible loss by evaporation. This work was carried out as part of a project that investigated a remediation process of agricultural land affected by an accidental spillage of fuel (Plan Nacional I + D + i, CTM2007-64 537). The paper is structured as: Optimization of wavelengths in the chromatographic conditions to improve resolution in the analysis of fuel samples. Optimization of the main parameters affecting in the extraction process by sonication. Comparison of results with those obtained by accelerated solvent extraction. (Author) 3 refs.

  5. Analytical Evaluation to Determine Selected PAHs by HPLC in a Type 2 Fuel; Evaluacion Analitica de 4 Metodos de Determinacion de PAHs medianteHPLC en un Fuel de Tipo II

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.; Sevillano Castano, M. L.; Escolano Segovia, O.; Garcia Frutos, F. J.

    2009-05-21

    An evaluation of analytical parameters to determine selected PAHs in a fuel oil type II by HPLC coupled to fluorescence and diode detectors is presented. The study was focused on four conventional treatments of these kinds of oil samples and the main objective was giving a measure of confidence level of PAH results in the fuel oil. This study was performed in the frame of the project Assessment of natural attenuation of PAHs in agricultural soil contaminated with fuel from an accidental spill (Spanish National Plain I+D+I, CTM2007-64537). This paper is presented as follows: Analysis of reference material 1582 (NIST) by using the four kinds of sample treatments of interest. Application of variance analysis to compare results obtained from type II fuel by using each sample treatment and chromatographic detector. Finally, a statistic calculation was performed to measure uncertainty components in chromatographic analysis. (Author)

  6. Uncertainty Evaluation and Influence of Gran Size to Determine PAHs in a Contaminated Soil; Influencia del Tamano de Particula de un Suelo Contaminado en las Incertidumbres Asociadas al Metodo de Determinacion de PAHs

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Alonso, S.; Perez Pastor, R. M.; Escolano Segoviano, O.; Garcia Frutos, F. J.

    2007-07-20

    An evaluation of uncertainty associated to PAH determination in a contaminated soil is presented. The work was focused to measure the influence of grain size on concentration deviations and give a measure of result confidence of PAHs in the gasworks contaminated soil. This study was performed in the frame of the project 'Assessment of natural remediation technologies for PAHs in contaminated soils'(Spanish Plan Nacional I+D+i, CTM 2004-05832-CO2-01). This paper is presented as follows: A brief introduction which describes the main uncertainty contributions associated to chromatographic analysis. Afterwards, a statistic calculation was performed to measure each uncertainty component. Finally, a global uncertainty was calculated and the influence of grain size and distribution of compounds according to volatility was evaluated. (Author) 10 refs.

  7. Determination of viscosity of fayalite slags for kv model and measurements by means of inclined plane; Estimacion de la viscosidad de escorias fayaliticas utilizando el modelo de calculo kv y el metodo experimental del plano inclinado

    Energy Technology Data Exchange (ETDEWEB)

    Bazan, V.; Goni, C.; Castella, L.; Brandaleze, E.; Verdeja, L. F.; Parra, R.

    2006-07-01

    The viscosity of the lands represents one of the most relevant variables of most of the processes metallurgical and kinetics of the refine operations, since it is one of the decisive factors of the efficiency in the reactions between metal and lag, as much as slag-refractory. In the last decades, the mathematical models of different metallurgical processes have established methods to predict viscosity of mixtures of oxides fused to high temperatures in function of the chemical composition. The model developed by Toguri, based on the data reported by Johasen and Winterhager et al has proposed the Kv model. The used index it is similar to the relationship used in the steel industry like the basicity index. It is presented in this work values determined of viscosity in experimental form by means of the technique of inclined plane. (Author)

  8. Use of activation analysis method for determining trace elements in human nail clippings; Aplicacao do metodo de analise por ativacao a determinacao de elementos tracos em aparas de unhas humanas

    Energy Technology Data Exchange (ETDEWEB)

    Aguiar, Amilton Reinaldo; Saiki, Mitiko [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

    1999-11-01

    This work presents results obtained in nail clipping samples analyses. These nail samples were collected from healthy group of individuals and from patients with cystic fibrosis disease. Irradiation of nail clippings was carried out with a thermal neutron flux from 10{sup 11} to 10{sup 13} n.cm{sup -2}.s{sup -1} at the IEA-R1m nuclear research reactor and the elements Al, As, Br, Ca, cd, Cl, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Se and Zn were determined. The results obtained for healthy group were within the range of concentrations published, for normal population. However for several elements, the group of patients presented higher concentrations than those presented for healthy individuals. The precision and the accuracy of the results were evaluated by analyzing reference materials NIST 1577b Bovine Liver and 1566a Oyster Tissue. (author) 6 refs., 4 tabs.

  9. 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)

  10. 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.

  11. Neutron activation analysis applied to the determination of trace elements in human nails; Aplicacao do metodo de analise por ativacao com neutrons a determinacao de elementos traco em unhas humanas

    Energy Technology Data Exchange (ETDEWEB)

    Aguiar, Amilton Reinaldo

    2001-07-01

    There is a considerable interest in the determination of trace elements in human nails in order to use this tissue as a monitor of nutritional and healthy status of individuals, of occupational exposure diseases and of the environmental contamination. In this work, instrumental neutron activation analysis was applied to determine trace elements in finger nail clippings to make comparisons between the elemental concentrations obtained in nails from healthy individuals of a control group and those from cystic fibrosis (CF) patients. Firstly, a protocol for sample collection and preparation for analysis was established. Finger and toe nail samples from CF patients were collected at the Instituto da Crianca of Medicine School, University of Sao Paulo, SP. The nail samples from control group were collected from healthy adults and from children living in Sao Paulo city, SP. These samples were cleaned by stirring them witha a diluted Triton X100 solution and then by washing with distilled water and acetone. The analytical procedure consisted of irradiation nail samples and elemental standards in the IEA-R1m nuclear reactor under thermal neutro flux of about 10{sup 12} n cm{sup -2} s{sup -1}, for short and long period irradiations. The activities of the radionuclides were measured using a gamma-ray spectrometer comprising an hyperpure Ge detector and associated electronic system. The biological reference materials Bovine Liver 1577b and Oyster Tissue 1566a, both from National Institute of Standards and Technology, USA were analysed in order to evaluate the accuracy and precision of the results. The analysis of variance (ANOVA) and F-test at the significance level of 5% were used to make a comparison between the sets of results obtained in this work. In the comparison of the results obtained for finger and toe nails from CF patients, the Br concentrations were higher in finger nails that those obtained for toe nails. For the control group of children, the finger nails

  12. A study on chemical element determinations in human nails by neutron activation analysis; Estudo sobre determinacao de elementos quimicos em unhas humanas pelo metodo de analise por ativacao com neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Sanches, Thalita Pinheiro

    2012-07-01

    Nail analyses have been the object of study in order to assess the levels of elements accumulated in the human organism and to use this tissue to monitor environmental and occupational exposure, to evaluate the nutritional status, to verify intoxication by toxic metals and to diagnose or to prevent diseases. Nail analyses present advantages due to easy sample collection, storage, transportation and this tissue provides element level accumulation over time. However, there is controversy regarding the application of nail analysis data due to difficulties to establish reliable reference values or element concentration ranges as control values. The objective of this study was to evaluate the factors that can affect nail element concentrations for further sample analyses of a group of individuals by applying neutron activation analysis (NAA). Fingernails and toenails collected from adult individuals of both genders, aged 18 to 71 years, living in the Sao Paulo Metropolitan Region were cut in small fragments, cleaned and dried for analyses. Samples and element standards were irradiated for 16 h under a thermal neutron flux of about 4.5 x 10{sup 12} n cm{sup -2} s{sup -1} at the IEA-R1 nuclear research reactor followed by gamma ray spectrometry. Element concentrations for As, Br, Ca, Co, Cr, Cs, Fe, K, La, Na, Rb, Sb, Sc, Se and Zn were determined. For quality control of the analytical results, certified reference materials were analysed and the results showed good accuracy and precision with relative errors and relative standard deviations lower than 5.1 % and 11.6 %, respectively. Preliminary assays indicated that the contribution due to impurities from plastic involucres used in the irradiation as well as those from nail polishes is very low and could be considered negligible. Results from the nail sample cleaning process using distinct procedures indicated that HNO{sub 3} solution may cause sample dissolution. Sample homogeneity was verified by analysis of a sample in

  13. 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

  14. 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.

  15. 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

  16. 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.

  17. 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)

  18. 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

  19. 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

  20. 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.

  1. 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.

  2. 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

  3. 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.

  4. 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

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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, ...

  17. 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.

  18. Determination of free amino acids of porcine serum responsible for ...

    African Journals Online (AJOL)

    The 1H NMR spectra of serum metabolites at 600 MHz showed that free amino acids such as alanine, leucine, phenylalanine, and valine were qualitatively higher in the HpHG than in the LpHG. The relative abundance of three amino acids was quantitatively verified by HPLC: Phenylalanine and valine (P<0.01) and leucine ...

  19. 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)

  20. 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.

  1. 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)

  2. 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)

  3. 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

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

    African Journals Online (AJOL)

    user user

    2012-07-10

    Jul 10, 2012 ... Neural tube defects (NTDs) are severe but common congenital malformations. Neonates who ... malformations that affect the central nervous system. NTDs are costly .... protective effect of folic acid supplementation on NTD.

  5. Determination of Carboxylic Acids and Water-soluble Inorganic Ions ...

    African Journals Online (AJOL)

    NICO

    radiation balance.4,5 Major water-soluble inorganic ions are associated with atmospheric ... molecular weight carboxylic acids in aerosol samples collected from a rural ... include biomass burning, agriculture, livestock and soil dust. Tropical ...

  6. 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)

  7. Method for determining microamounts of uranium in solutions from copper ores, by liquid-liquid extraction and spectrophotometry with arsenazo III.; Metodo para determinar microcantidades de uranio en disoluciones de minerales de cobre, por extraccion liquido-liquido y espectrofotometria con arsenazo III

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez, B.

    1972-07-01

    A spectrophotometric method is described for determining small amounts of uranium in aqueous solutions from copper ores. Uranium is quantitatively separated in a single extraction by a solution of tri-n-octylphosphine oxide in benzene, using ethylendiaminetetracetic acid and sodium fluoride as complexing agents, for improving the selectivity of the procedure. An aliquot of the extract is diluted with a hydrocolloidal solution of arsenazo III. Optical density is measured at 650 nm. (Author) 3 refs.

  8. 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.

  9. Radioimmunoassay for the determination of free and conjugated abscisic acid

    International Nuclear Information System (INIS)

    Weiler, E.W.

    1979-01-01

    The characterization and application of a radioimmunoassay specific for free and conjugated abscisic acid (ABA) is reported, The antibodies produced against a bovine serum albumin-(+-)-ABA conjugate have a high affinity for ABA (Ka= 1.3 x 10 9 l mol -1 ). Trans, trans-ABA and related compounds, such as xanthoxin, phaseic acid, dihydrophaseic acid, vomifoliol or violaxanthin do not interfere with the assay. The detection limit of this method is 0.25 x 10 -12 mol ABA, the measuring range extends to 20 x 10 -12 mol, and average recoveries are 103%. Because of the high specificity of this immunoassay, no extract purification steps are required prior to analysis. Several hundred plants can be analyzed per day in a semi-automatic assay performance. ABA has been detected in all higher plant families examined, but was absent in the blue-green alga, Spirulina platensis, the liverwort Marchantia polymorpha, and two species of fungi. (orig.) [de

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

    Directory of Open Access Journals (Sweden)

    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.

  11. 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…

  12. 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

  13. Determination of ferulic acid and related compounds by thin layer ...

    African Journals Online (AJOL)

    The analysis of certain phenolic compounds from plants, and their chemical transformation with microorganisms or isolated enzymes, has application in the food and pharmaceutical industry. The rapid quantitative estimation of ferulic acid by thin layer chromatography is described by measurement of the area of the ...

  14. Quick and sensitive determination of gene expression of fatty acid ...

    African Journals Online (AJOL)

    User

    2011-05-16

    May 16, 2011 ... from fatty acid synthase (FAS) with a different glucose level in ... By using the following formula, this study was able to quantify the mRNA expression of ... hypertension, heart disease and diabetes. ... regulation of gene expression has emerged in recent ... stages of adipocyte meta-bolism are relatively well.

  15. Determination of Carboxylic Acids and Water-soluble Inorganic Ions ...

    African Journals Online (AJOL)

    Atmospheric aerosol samples of PM2.5 and PM10 were collected in April–May 2011 from a rural site in Tanzania and analyzed for water-soluble inorganic ions and low molecular weight carboxylic acids using ion chromatography. PM2.5 and PM10 low-volume samplers with quartz fibre filters were deployed and aerosol ...

  16. Bioavailability of ferulic acid is determined by its bioaccessibility

    NARCIS (Netherlands)

    Mateo Anson, N.; Berg, R. van den; Havenaar, R.; Bast, A.; Haenen, G.R.M.M.

    2009-01-01

    Epidemiological studies have linked whole grain consumption to prevention of several chronic diseases. Whole grain is a source of important phytochemicals, such as ferulic acid (FA). FA is the most abundant phenolic and major contributor to the in vitro antioxidant capacity of wheat grain. Several

  17. On-line Determination of Hydrochloric Acid in Process Effluent ...

    African Journals Online (AJOL)

    Prof Van Staden

    The sample is sandwiched between two titrants in a holding coil, with the volume of the first base being twice to that of the second one and channeled by flow reversal through a reaction coil to the potentiometric sensor. A linear relationship between peak width and logarithm of the hydrochloric acid concentration was.

  18. Quick and sensitive determination of gene expression of fatty acid ...

    African Journals Online (AJOL)

    Obesity results from an imbalance between energy intake and energy expenditure, which leads to a pathological accumulation of adipose tissue, but the underlying mechanism at gene level, is far from being elucidated. The objective of this study was to investigate the correlation between mRNA express from fatty acid ...

  19. 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...

  20. Determination of perfluoroalkyl carboxylic, sulfonic, and phosphonic acids in food.

    Science.gov (United States)

    Ullah, Shahid; Alsberg, Tomas; Vestergren, Robin; Berger, Urs

    2012-11-01

    A sensitive and accurate method was developed and validated for simultaneous analysis of perfluoroalkyl carboxylic acids, sulfonic acids, and phosphonic acids (PFPAs) at low picograms per gram concentrations in a variety of food matrices. The method employed extraction with acetonitrile/water and cleanup on a mixed-mode co-polymeric sorbent (C8 + quaternary amine) using solid-phase extraction. High-performance liquid chromatographic separation was achieved on a C18 column using a mobile phase gradient containing 5 mM 1-methyl piperidine for optimal chromatographic resolution of PFPAs. A quadrupole time-of-flight high-resolution mass spectrometer operating in negative ion mode was used as detector. Method detection limits were in the range of 0.002 to 0.02 ng g(-1) for all analytes. Sample preparation (extraction and cleanup) recoveries at a spiking level of 0.1 ng g(-1) to a baby food composite were in the range of 59 to 98 %. A strong matrix effect was observed in the analysis of PFPAs in food extracts, which was tentatively assigned to sorption of PFPAs to the injection vial in the solvent-based calibration standard. The method was successfully applied to a range of different food matrices including duplicate diet samples, vegetables, meat, and fish samples.

  1. 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

  2. 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)

  3. 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)

  4. 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...

  5. 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.

  6. 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.

  7. Specificity determinants for the abscisic acid response element ?

    OpenAIRE

    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 interac...

  8. 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

  9. 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.

  10. 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

  11. 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 ...

  12. Plutonium determination in solution with excess hydrofluoric acid

    International Nuclear Information System (INIS)

    Krtil, J.; Kuvik, V.; Spevackova, V.

    1975-01-01

    The determination is described of plutonium in solutions in the presence of fluoride ions resulting from the hydrolysis of PuF 6 . The method is based on reduction of Pu(VI) by excess of Fe(II) and on re-titration of Fe(II) with ceric salt. The effect of fluoride ions on plutonium determination was studied. It was found that a 3 mole excess of HF with respect to Pu decreased the results of Pu determination. The interference of fluoride ions was eliminated by a two-fold evaporation of the solution to be titrated with HNO 3 to dryness or by complex formation with boric arid. The amount of 20.50 mg Pu in the presence of a 10 mole excess of fluoride ions (17 mg HF) was determined with an error of +- 0.09 mg ). (author)

  13. 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...

  14. Microbiological aspects of determination of trichloroacetic acid in soil

    International Nuclear Information System (INIS)

    Matucha, M.; Rohlenová, J.; Forczek, S.T.; Gryndler, M.; Uhlířová, H.; Fuksová, K.; Schroder, P.

    2004-01-01

    Soils have been shown to possess a strong microbial trichloroacetic acid (TCA)-degrading activity. High TCA-degradation rate was also observed during soil extraction with water. For correct measurements of TCA levels in soil all TCA-degrading activities have to be inhibited immediately after sampling before analysis. We used rapid freezing of soil samples (optimally in liquid nitrogen) with subsequent storage and slow thawing before analysis as an efficient technique for suppressing the degradation. Frozen soil samples stored overnight at −20 °C and then thawed slowly exhibited very low residual TCA-degrading activity for several hours. Omitting the above procedure could lead to the confusing differences between the TCA levels previously reported in the literature

  15. 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.

  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. 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.

  18. 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.

  19. 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…

  20. 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....

  1. 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.

  2. 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

  3. 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.

  4. 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

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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).

  12. 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).

  13. 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).

  14. 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)

  15. [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.

  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. 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.

  18. 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

  19. 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.

  20. A modification of the method for determining current efficiency of aluminium electrolytic cells; Modification de la methode permettant de determiner le rendement des cuves dans la production d'aluminium par electrolyse; Izmenenie metoda opredeleniya ehffektivnosti toka v alyuminievykh ehlektroliticheskikh bakakh; Modificacion del metodo para determinar el rendimiento de las celdas utilizadas en la produccion de aluminio por electrolisis

    Energy Technology Data Exchange (ETDEWEB)

    Pradzynski, A [Institute of Basic Technical Problems, Polish Academy of Sciences. Warsaw (Poland); Orman, Z [Institute of Nonferrous Metals, Gliwice (Poland)

    1962-01-15

    The method for determining the current efficiency of aluminium electrolytic cells described first by REMPEL et al. was improved by BOZOKY et al. by using the radioisotope Au{sup 198}. In that work, master alloys of aluminium with Au{sup 198} were made, and samples of this were measured by means of a G-M tube with a lead absorber inserted between the tube and the sample. In this work the specific activity of the master alloy was reduced by diluting with a known quantity of pure aluminium. In that way samples of diluted master alloy and samples taken from the electrolytic cell were of the same order of specific activity and could be measured without any absorber. Radioactivation analysis was employed in order to facilitate the application of the above method in aluminium plants and to avoid all restrictions and dangers connected with the handling of unsealed radioactive sources outside special radioisotope laboratories. Inactive gold was introduced into the master alloy and into the smelting bath in the electrolytic cell. The concentration of gold in samples of both the master alloy and the smelt was then measured after irradiating the samples in a nuclear reactor. (author) [French] La methode permettant de determiner le rendement des cuves a aluminium, exposee tout d'abord par Rempel et al., a ete perfectionnee par Bozoky et al. qui ont utilise a cet effet le radioisotope or-198. Des alliages types d'aluminium et d'or-198 ont ete prepares et des echantillons mesures au moyen d'un tube Geiger-Muller, un absorbeur en plomb etant insere entre le tube et l'echantillon. Les auteurs du memoire ont mesure l'activite specifique de l'alliage type apres dilution dans une quantite connue d'aluminium pur. Les echantillons d'alliage type ainsi dilue et les echantillons preleves dans la cuve electrolytique ayant alors une activite specifique du meme ordre, il a ete possible de la mesurer sans aucun absorbeur. Les auteurs ont procede a des essais d'analyse par radioactivation afin

  1. 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

  2. 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

  3. 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.

  4. 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

  5. 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

  6. [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.

  7. 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.

  8. 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

  9. 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

  10. 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.

  11. 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)

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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.

  20. [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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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)

  8. 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.

  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. 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.

  11. 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.

  12. 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)

  13. [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.

  14. 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.

  15. 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.

  16. 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

  17. 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.

  18. 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.

  19. 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

  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. 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)

  3. 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

  4. 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.

  5. 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...

  6. 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...

  7. 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

  8. 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...

  9. 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

  10. 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

  11. [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.

  12. 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

  13. 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.

  14. 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).

  15. [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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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)

  6. 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.

  7. 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...

  8. 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.

  9. 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.

  10. 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.

  11. 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...

  12. 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)

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. 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.

  1. [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.

  2. 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 .

  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. 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)

  5. 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

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. Synthesis of aluminum oxide by the polymer precursor method (Pechini) in 4: 1 ratio of citric acid: metal cation: calcination temperature effect; Sintese do oxido de aluminio pelo metodo dos precursores polimericos (Pechini) na relacao 4:1 de acido citrico: cation metalico: efeito da temperatura de calcinacao

    Energy Technology Data Exchange (ETDEWEB)

    Silva, M.C.; Lira, H.L.; Ribeiro, P.C.; Freitas, N.L., E-mail: mirelecsilva@hotmail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Engenharia de Materiais

    2014-07-01

    The technology field is nanopowders prominent in science since these materials fall in various sectors regarding their applications. This work aims at the synthesis of aluminum oxide by polymeric precursors in 4:1 ratio of citric acid:metal cation and evaluate the influence of calcination temperature on their structural and morphological characteristics. The samples after reaction were characterized by XRD and thermal analysis. After calcination 500-1200°C the samples were characterized by XRD, SEM and particle size distribution. The results showed that the variation of the calcination temperature is sufficient to achieve a same material with different structural and morphological characteristics. The most stable phase aluminum oxide arose only after calcination at 1100°C, below 900°C, the amorphous material appeared. As regards the morphology, the change was not as significant as compared to the structure. (author)

  11. 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.

  12. 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.

  13. Determination of complex formation constants by phase sensitive alternating current polarography: Cadmium-polymethacrylic acid and cadmium-polygalacturonic acid.

    Science.gov (United States)

    Garrigosa, Anna Maria; Gusmão, Rui; Ariño, Cristina; Díaz-Cruz, José Manuel; Esteban, Miquel

    2007-10-15

    The use of phase sensitive alternating current polarography (ACP) for the evaluation of complex formation constants of systems where electrodic adsorption is present has been proposed. The applicability of the technique implies the previous selection of the phase angle where contribution of capacitive current is minimized. This is made using Multivariate Curve Resolution by Alternating Least Squares (MCR-ALS) in the analysis of ACP measurements at different phase angles. The method is checked by the study of the complexation of Cd by polymethacrylic (PMA) and polygalacturonic (PGA) acids, and the optimal phase angles have been ca. -10 degrees for Cd-PMA and ca. -15 degrees for Cd-PGA systems. The goodness of phase sensitive ACP has been demonstrated comparing the determined complex formation constants with those obtained by reverse pulse polarography, a technique that minimizes the electrode adsorption effects on the measured currents.

  14. 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.

  15. 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)

  16. 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

  17. 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.

  18. 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)

  19. 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)

  20. 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%.

  1. 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.

  2. 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.

  3. [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.

  4. 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

  5. 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)

  6. 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

  7. 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.)

  8. 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

  9. 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)

  10. 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

  11. Determination of uranium in urine samples for workers in the phosphoric acid purification using fluorimetry technique

    International Nuclear Information System (INIS)

    Kharita, M. H.; Sakhita, Kh.; Aldalal, Z.

    2003-10-01

    There is probability of exposure to uranium for workers in the phosphoric acid purification (internal exposure) by inhalation, and the deposition of this uranium in organs and tissues, and the consequence excreation out of the body by perspiration or urine. This study focuses on the determination of uranium in urine samples of workers. All results seem to be under the detection limit of the method, therefore no routine monitoring is required. (author)

  12. 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.

  13. Multi-elemental analysis of atmospheric pollutants and determination of particle size using the PIXE method, a cascade impactor and a filter unit constructed in Mexico; Analisis multielemental de contaminantes atmosfericos y determinacion de tamano de particula utilizando el metodo PIXE, un impactor de cascada y una unidad de filtro construidos en Mexico

    Energy Technology Data Exchange (ETDEWEB)

    Aldape U, F [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)

    1989-01-15

    This work presents: 1) The methodology and the experimental conditions of the PIXE technique so that it is used as a better option inside the analytical methods in aerosols studies, 2) The development, tests and applications of a cascade impactor of the Batelle type built to determine particle size to use it jointly with the mentioned technique in the determination of the elements concentration according to its size.By this way is fulfilled with the first goal of this extensive project. (Author)

  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. 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

  16. 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…

  17. 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…

  18. 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.

  19. 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.

  20. 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

  1. Determination of Kr-85 in environmental samples and gaseous effluents from nuclear industries using the standard method; Aplicacion del metodo de concentracion separacion y medida radiactiva por centelleo liquido de Kr-85 en muestras ambientales y en efluentes gaseosos de la industria nuclear

    Energy Technology Data Exchange (ETDEWEB)

    Heras, M c; Perez, M M

    1983-07-01

    The determination of the Kr-85 activity in environmental samples and gaseous effluents from Spanish Nuclear Power Stations is described. The method employed has been published elsewhere. The determinations has been carried out in environmental samples token at JEN Laboratories (Madrid) and the Nuclear Power Stations, Jose Cabrera (Zorita), Garona and Vandellos. Also samples of gaseous effluents of the three plants has been analyzed. Values of the Kr-85 environmental background activity in the Almaraz Nuclear Power Stations, has been determined, before the beginning of its nuclear activity. In this paper the sampling equipment used is described and the values found of Kr-85 activity in all the samples in given. (Author) 29 refs.

  2. 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

  3. 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...

  4. Determination of furan precursors and some thermal damage markers in baby foods: ascorbic acid, dehydroascorbic acid, hydroxymethylfurfural and furfural.

    Science.gov (United States)

    Mesías-García, Marta; Guerra-Hernández, Eduardo; García-Villanova, Belén

    2010-05-26

    The presence of ascorbic acid (AA), vitamin C (AA + dehydroascorbic acid (DHAA)) and furfural as potential precursors of furan in commercial fruit and vegetable jarred baby food was studied. Hydroxymethylfurfural (HMF) was also determined and used, together with furfural levels, as markers of thermal damage. AA, calculated DHAA and vitamin C values ranged between 22.4 and 103, 2.9 and 13.8, and 32.1 and 113.2 mg/100 g, respectively, in fruit-based baby food. However, no trace of AA was found in the vegetable-based baby food samples tested, probably because these samples are not enriched in vitamin C and the content of this vitamin in fresh vegetables is destroyed during processing. Furfural values ranged from not detected to 236 microg/100 g, being higher in vegetable samples than in fruit samples possibly because of greater AA degradation favored by a higher pH in the vegetable samples. HMF values (range: not detected-959 microg/100 g), however, were higher in the fruit samples, probably due to greater carbohydrate content degradation and as a consequence of the Maillard reaction, favored by a lower pH in these samples. According to these results, HMF would be the optimum indicator of thermal treatment for fruits, and furfural for vegetables. The higher furfural content of vegetable baby food could be considered an index of greater AA degradation and, therefore, the furan content might be higher in this kind of sample than in fruit-based baby food.

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. [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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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

  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. 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.

  4. 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.

  5. 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

  6. [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.

  7. 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.

  8. 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.

  9. 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.

  10. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media

    International Nuclear Information System (INIS)

    Popov, L.

    2016-01-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials. - Highlights: • The method allows cost-effective determination of U isotopes. • High amounts of environmental samples can be analyzed. • High chemical yields, energy resolution and decontamination factors were achieved. • Uranium isotope concentrations in mineral waters from Bulgaria are presented.

  11. 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.

  12. 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.

  13. 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)

  14. Determination of ingestion levels of arsenic, antimony, cadmium, thorium and uranium in children diets by duplicate portion method; Determinacao dos niveis de ingestao dietetica dos elementos arsenio, antimonio, cadmio, torio, tungstenio e uranio em dietas de criancas pelo metodo da porcao em duplicata

    Energy Technology Data Exchange (ETDEWEB)

    Maihara, Vera T.; Vasconcellos, Marina B.A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil). Supervisao de Radioquimica

    1996-07-01

    A study was made with a group of 19 pre-school children at the central nursery of the University of Sao Paulo with the aim of evaluating the toxic elements contents present in diets of this group. The diet samples were collected by duplicate portion method. A radiochemical was applied to the determination of Cd, Sb, Th, U and W by means of retention of these elements in the chelating resin Chelex 100, in 0,1 M H Ac-NH{sub 4}Ac medium, followed by retention of As in the inorganic exchanger tin dioxide, in HCl 6 M medium. (author)

  15. Study of an X-ray fluorescence thin film method for the determination of uranium in low activity solutions; Estudio de un metodo de fluorescencia de rayos X en capa delgada para la determinacion del uranio en soluciones de baja actividad

    Energy Technology Data Exchange (ETDEWEB)

    Diaz-Guerra, J P

    1980-07-01

    The application of the X-ray fluorescence thin film technique to the uranium determination in nitric solutions for a concentration range from 1 g/l to 100 g/l and activity levels under 5 mCi/ml is studied. The most suited excitation and measurement conditions are also studied and the uranium matrix effect correction, which is performed through the double dilution, {alpha}{sub U}U interaction coefficient calculation and internal standard methods, is discussed. The specimen preparation is satisfactorily accomplished by using P.V.C. filters fixed on aluminium supports. (Author) 18 refs.

  16. Optimization of the Analytical Method Using HPLC with Fluorescence Detection to Determine Selected Polycyclic Aromatic Compounds in Clean Water Samples; Optimizacion del Metodo Analitico mediante HPLC con Detector de Fluorescencia para la Determinacion de Ciertos Compuestos Aromaticos Policiclicos en Muestras de Aguas Limpias

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-10-01

    A study on the comparison and evaluation of 3 miniaturized extraction methods for the determination of selected PACs in clear waters is presented. Three types of liquid-liquid extraction were used for chromatographic analysis by HPLC with fluorescence detection. The main objective was the optimization and development of simple, rapid and low cost methods, minimizing the use of extracting solvent volume. The work also includes a study on the scope of the methods developed at low and high levels of concentration and intermediate precision. (Author)

  17. Determination of {sup 60} Co by means of Neutron Activation Analysis in the sorption of Co in synthesized porous oxides by the combustion method; Determinacion de {sup 60} Co por medio de AAN en la sorcion de Co en oxidos porosos sintetizados por metodo de combustion

    Energy Technology Data Exchange (ETDEWEB)

    Lugo, V.; Bulbulian, S.; Urena, F. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)]. e-mail: violelugo@yahoo.es

    2005-07-01

    Recently inorganic materials are investigating as sorbent of radioactive pollutants present in water. The inorganic oxides belong to this group of materials. A quick method exists for the obtaining of inorganic oxides, denominated combustion method that could be used to produce porous oxides successfully with good properties for the sorption of radioactive ions. In this investigation, iron oxides, magnesium and zinc were synthesized obtained by the combustion method, comparing them with those synthesized by the calcination method, using two different synthesis temperatures. The obtained solids were characterized by scanning electron microscopy (Sem), by X-ray diffraction (XRD) and by semiquantitative elemental analysis (EDS). After the characterization, the crystalline oxides synthesized by both methods, to temperature of 800 C, were evaluated as sorbents in the removal of Co{sup 2+} ions, through experiments in batch, and using neutron activation analysis, determining the sorption percentage, with this it was concluded that the magnesium oxide produced by combustion it is more effective in the removal of Co{sup 2+} ions than that synthesized by calcination. It was determined the surface area of the magnesium oxides, obtaining a surface area greater for the synthesized oxide by combustion method. (Author)

  18. 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

  19. 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

  20. 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

  1. Comparison among physical and mathematical simulation methods to calibrate the scintillating detector to determine the high energy radionuclides in human body; Comparacao entre metodos de simulacao fisica e matematica para calibracao de detetor de cintilacao, visando a determinacao de radionuclideos de alta energia no corpo humano

    Energy Technology Data Exchange (ETDEWEB)

    Mello, J.Q.; Dantas, A.L.A.; Almeida, A.P.F.; Hunt, J.G.; Dantas, B.M., E-mail: jquince@bolsista.ird.gov.br [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2015-07-01

    In vivo monitoring of photon emitters requires prior calibration of the detectors in order to obtain factors relate the count rate obtained in measuring the individual with this activity in the body. In this work were compared two calibration methods of a Nal scintillation detector (Tl) 3 x 3 for determination in vivo of {sup 40}K: (1) Experimental method using a physical-anthropomorphic simulator called BOMAB and (2) mathematical method using the VMC software (Visual Monte Carlo). Both methods aim at simulation of radionuclide distribution in the human body geometry and interaction of photons with the detector. The obtained results show the similarities and limitations of the evaluated methods for the measurement conditions used.

  2. Development of an analytical method for the direct determination of uranium isotopes in occupationally exposed personnel urine samples using Icp-SFMS; Desarrollo de un metodo analitico para la determinacion directa de isotopos de uranio en muestras de orina de personal ocupacionalmente expuesto (POE) usando ICP-SFMS

    Energy Technology Data Exchange (ETDEWEB)

    Torres C, C. O.; Hernandez M, H.; Romero G, E. T. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Vega C, H. R., E-mail: hector.hernandez@inin.gob.mx [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Cipres No. 10, Fracc. La Penuela, 98060 Zacatecas, Zac. (Mexico)

    2016-09-15

    The development of an analytical method for measuring actinides in radioactive waste, environmental and biological samples has been a major challenge in institutions dedicated to the nuclear sector. Is for this reason that the developed and validated methods to measure isotopes of elements belonging to the actinide family have as main objective the characterization of radioactive wastes, the monitoring of radioactive installations and the dosimetric evaluation of occupationally exposed personnel, this for the purpose to prevent incidents or radiological accidents and to safeguard workers. This research work is focused on determining isotopes of uranium (U) and obtaining isotope ratios in urine samples of occupationally exposed personnel using a Magnetic Sector Mass Spectrometer with Inductively Coupled Plasma Source (Icp-SFMS), which is a versatile and promising technique for a large number of applications. The urine samples are acidified in order to favor the dissolution of the analytes in the samples, minimizing as much as possible their loss by sorption in the walls of the sampling bottle. For the determination of U in urine samples, dilution was performed, taking 2 ml of the urine samples and weighing it to 100 ml with 2% ultra pure HNO{sub 3} and finally performing the measurement by Icp-SFMS. The results obtained in the measurements of U show an order of magnitude in terms of sensitivity offered by Icp-SFMS. The isotopic ratios {sup 234}U/{sup 238}U, {sup 235}U/{sup 238}U are very close to the results reported by the literature and the quantification of the isotopes of said element show be within the concentration range of U, indicating that is exposed to depleted U. Additionally, Limit of Detection and Quantification Limit calculations were performed, which are of the order of pg mL{sup -1}. (Author)

  3. [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.

  4. Highly sensitive spectrophotometric kinetic determination of vanadium by catalysis of the gallic acid-bromate reaction

    International Nuclear Information System (INIS)

    Fukasawa, Tsutomu; Kawakubo, Susumu; Yamanouchi, Tatsuo

    1985-01-01

    Conditions are described for improving the speed and sensitivity of this catalytic determination of vanadium. The reaction of 0.018 M gallic acid with 0.96 M sodium bromate at pH 3.8 and double-beam spectrophotometric measurement at 380 nm are recommended. The highest practical sensitivity at 22-30 0 C was ca. 40 pg for an absorbance change of 0.0005, 50 times better than previously. The detection limit was ca. 0.5 ng of vanadium. Reaction at 50 0 C gave even better sensitivity. (Auth.)

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

    Directory of Open Access Journals (Sweden)

    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.

  6. 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)

  7. Determination of trace vanadium using its catalytic effect on the oxidation of gallic acid by bromate

    International Nuclear Information System (INIS)

    Yamane, Takeshi; Fukasawa, Tsutomu

    1976-01-01

    The oxidation of gallic acid by bromate with trace vanadium as catalyst was followed spectrophotometrically by measurements of absorbance change at 420 nm. The reaction rate was obtained graphically from the absorbance vs. time curve in the range of about 15 to 40 min. reaction time. The reaction rate was proportional to the concentration of vanadium(V) in the range 0--120 ng (under the conditions of 5.3x10 -3 M gallic acid, 6.0x10 -3 M potassium bromate, pH 3.8) and 0--30 ng (1.1x10 -2 M gallic acid, 2.7x10 -2 M potassium bromate, pH 3.8). Using this relationship, the concentration of vanadium as low as 0.1 ng/ml can be determined. The relative standard deviations at 50 ng and 20 ng of vanadium were 3.5% (n=14) and 4.0% (n=10), respectively. Iron(III) interfered seriously even when present in 20 times the amounts of vanadium. Up to 60 times, W(VI), Mo(VI) and iodide did not interfere. Many of the other ions examined were found to have no effect or slight effect even when present in 1000 times the amounts of vanadium. Other factors affecting the reaction rate were also studied. (auth.)

  8. 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.

  9. 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

  10. 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.

  11. Validation of methods for WDXRF and OES-spark techniques in steel analysis. Determination of the uncertainty of measurements for API steel plant sample; Validacao de metodos para as tecnicas de WDXRF e OES-spark na analise de acos. Calculo de incerteza de medicao para amostras de processo, aco classe API

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Carlos Eduardo da

    2009-07-01

    The increase of gas and petroleum demanding in the national and international markets, the specification and certification of the chemical analysis results of gas and oil pipe-line have became more and more challenging. A continuous development has been outlined to improve API grade alloy steels (American Petroleum Institute). The steel properties depend on the chemical composition control and process parameters during its manufacturing. In this work, a comparison of the measurement uncertainty between X-ray fluorescence (WD system) and Optical Emission (OES-spark) spectrometry, for API grade steel plant samples analysis, was outlined. Usually, this kind of analyze requires less than 40 seconds for full chemical characterization for adjustment in the process parameters production. The main influence source in the chemical analysis was evaluated for design of experiments. The constituents and trace elements such as Al, Si, P, S, Ti, V, Cr, Mn, Co, Ni, Cu, As, Nb, Mo and Sn were determined using the ASTM E-322, E-415, E-1009 and E-1085 standard methodologies. The 185A and 187A certified reference materials from CMI (Czech Metrology Institute) were used for evaluation of the methods. The uncertainty of the measurement, precision, accuracy, repeatability and reproducibility of the measurements were obtained applying statistic tests, recommended by ISO/IEC 17025. The uncertainty of measurement for each element is discussed for both techniques. (author)

  12. Quantitative determination of phases in ZrO{sub 2} (MgO) (Y{sub 2}O{sub 3}) using the Rietveld method; Determinacao quantitativa de fases em ZrO{sub 2} - MgO - Y{sub 2}O{sub 3} utilizando o metodo de Rietveld

    Energy Technology Data Exchange (ETDEWEB)

    Castro, Antonio Carlos de

    2007-07-01

    The key objective of this work is the crystallographic characterization of the zircon co-doped with Yttria and magnesium with the application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon monoclinic, tetragonal, and cubic). Samples of zircon polymorph were obtained from zircon doped with Yttria and magnesium at defined molar concentrations. The zircon polymorph stability during subeutetoid aging at 1350 deg C were investigated to determine ZrO{sub 2} - MgO - Y{sub 2}0{sub 3} phases degradation and to define the solid solutions stability environment. ZrO{sub 2} powders doped with 8 mol por cent of MgO and 1 mol por cent of Y{sub 2}O{sub 3}, and 9 mol por cent of MgO and 0 mol por cent of Y{sub 2}O{sub 3} have been prepared by chemical route using the co-precipitation method. These samples have been calcinate at 550 deg C, sintered at 1500 deg C and characterized by the Rietveld method using the X-ray diffraction data. The variation of the lattice parameter, changes in the phase composition and their microstructures are discussed. The application of the Rietveld method for quantitative phase analysis of zircon polymorph (zircon tetragonal and cubic) reveals no formation of tetragonal phase and indicating that the matrix is the cubic phase with low concentration of monoclinic phase.(author)

  13. Is the fatty acid composition of Daphnia galeata determined by the fatty acid composition of the ingested diet?

    NARCIS (Netherlands)

    Weers, P.M.M.; Siewertsen, K.; Gulati, R.D.

    1997-01-01

    1. The fatty acid (FA) composition of Daphnia galeata and their algal food was analysed and showed many similarities, however, some significant differences were also found in the relative abundance of the FA C16:4 omega 3 and docosahexaenoic acid (DHA). Their relative abundances were much lower in

  14. 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)

  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. Implementation of a constant load method, for determination of crack growth velocities in MEX-03 system of National Institute of Nuclear Research; Implementacion de un metodo de carga constante, para la determinacion de velocidades de crecimiento de grieta en el sistema MEX-03 del ININ

    Energy Technology Data Exchange (ETDEWEB)

    Diaz S, A.; Fuentes C, P.; Merino C, F. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico)], e-mail: angeles.diaz@inin.gob.mx

    2009-10-15

    Whit the objective of to complete the existent techniques for susceptibility evaluation to phenomenon of stress corrosion cracking in laboratories of Applied Sciences Area of National Institute of Nuclear Research; was realized and documented the modification of a high pressure and temperature equipment, identified as MEX-03 to carry out the implementation of a growth and crack propagation assay, using a constant load method. The assay was realized to a specimen of stainless steel AISI 304l type CT of an inch, which was previously thermally sensitize, simulating the typical degradation of this materials type below operation conditions in a BWR. The MEX-03 system, consist from an annexed auto key to a load system which originally was controlled by displacement; therefore were carried out modifications to achieve the control by load. The realized adjustments allowed to maintain a constant load during all the experiment, and as much the temperature conditions (T = 288 C) as of pressure (P = 8 Mpa) were controlled during the assay realization. The steel was exposed to a conditioned ambient with hydrogen gas addition; simulating a well-known alternative chemistry as hydrogen water chemistry that is used to mitigate the phenomenon of stress corrosion cracking, main degradation mechanism of austenitic stainless steels. The continuation of the crack behavior was realized by means of electric potential fall technique and later was validated of visual form through the fractographic analysis of cracked surface. The modification and control of equipment for realization of this experiment is necessary, for what should be carried out new assays, whose results will allow to establish the effect of dynamic and static methods in velocity determination of crack growth to laboratory level; to be considered in the existent models of crack propagation in systems and components in operation. (Author)

  18. 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%

  19. Empirical equations for viscosity and specific heat capacity determination of paraffin PCM and fatty acid PCM

    Science.gov (United States)

    Barreneche, C.; Ferrer, G.; Palacios, A.; Solé, A.; Inés Fernández, A.; Cabeza, L. F.

    2017-10-01

    Phase change materials (PCM) used in thermal energy storage (TES) systems have been presented, over recent years, as one of the most effective options in energy storage. Paraffin and fatty acids are some of the most used PCM in TES systems, as they have high phase change enthalpy and in addition they do not present subcooling nor hysteresis and have proper cycling stability. The simulations and design of TES systems require the knowledge of the thermophysical properties of PCM. Thermal conductivity, viscosity, specific heat capacity (Cp) can be experimentally determined, but these are material and time consuming tasks. To avoid or to reduce them, and to have reliable data without the need of experimentation, thermal properties can be calculated by empirical equations. In this study, five different equations are given to calculate the viscosity and specific heat capacity of fatty acid PCM and paraffin PCM. Two of these equations concern, respectively, the empirical calculation of the viscosity and liquid Cp of the whole paraffin PCM family, while the other three equations presented are for the corresponding calculation of viscosity, solid Cp, liquid Cp of the whole fatty acid family of PCM. Therefore, this study summarize the work performed to obtain the main empirical equations to measure the above mentioned properties for whole fatty acid PCM family and whole paraffin PCM family. Moreover, empirical equations have been obtained to calculate these properties for other materials of these PCM groups and these empirical equations can be extrapolated for PCM with higher or lower phase change temperatures within a lower relative error 4%.

  20. 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

  1. 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.

  2. 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.

  3. Determination of thymine glycol residues in irradiated or oxidized DNA by formation of methylglyceric acid

    International Nuclear Information System (INIS)

    Schellenberg, K.A.; Shaeffer, J.

    1986-01-01

    Treatment of DNA solutions with X-irradiation various oxidants including hydrogen peroxide plus ferrous ion, hydrogen peroxide plus copper ion and ascorbate, permanganate, or sonication in the presence of dissolved oxygen all produced varying amounts of thymine glycol residues. After denaturing the DNA with heat, the glycol residues were reduced and labeled at the 6 position with tritium- labeled sodium borohydride. Subsequent reaction with anhydrous methanolic HCl gave a quantitative yield of the methyl ester of methylglyceric acid, which was determined by thin layer chromatography. The method, developed using thymidine as a model, was used to ascertain the requirements for glycol formation in DNA. It was shown that hydroxyl radical generating systems, permanganate, X-irradiation, or sonication in presence of oxygen were required, but hydrogen peroxide in the absence of iron or copper and ascorbate was inactive. Application to determination of DNA damage in vivo is being explored

  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. 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.

  6. Simultaneous determination of Magnolol and Honokiol by amino acid ionic liquid synchronous fluorescence spectrometry

    Science.gov (United States)

    Liu, Wei; Zhu, Xiashi

    2018-05-01

    A novel method based on amino acid ionic liquids (AAILs) as an additive synchronous fluorescence spectrometry is proposed for simultaneous determination of magnolol (MN) and honokiol (HN) in traditional Chinese medicine Houpu. The overlapping fluorescence spectrum of MN and HN could be completely separated in the AAILs medium. Experiment parameters (the type and concentration of AAILs, pH values and temperature) were discussed. The detection limits of MN and HN reached 1.46 ng/mL, 0.92 ng/mL and the recovery rates ranged from 98.6%-100.7%, 99.7%-100.6%, respectively. This methods was successfully employed for simultaneously determination of MN and HN in real samples. No significant differences could be found in the results of this method and the pharmacopoeia of People's Republic of China 2015 (Ch.P.2015). The experiment mechanisms were discussed by the Gaussian simulation and fluorescence quantum yield.

  7. Determination of binding constants of cyclodextrin inclusion complexes with amino acids and dipeptides by potentiometric titration.

    Science.gov (United States)

    Kahle, Claudia; Holzgrabe, Ulrike

    2004-10-01

    Cyclodextrins are well known for their ability to separate enantiomers of drugs, natural products, and other chiral substances using HPLC, GC, or CE. The resolution of the enantiomers is due to the formation of diastereomeric complexes between the cyclodextrin and the pairs of enantiomers. The aim of this study was to determine the binding constants of the complexes between alpha- and beta-cyclodextrin and the enantiomers of a series of aliphatic and aromatic amino acids, and dipeptides, using a potentiometric titration method. The results of this method are compared to other methods, and correlated to findings in cyclodextrin-modified capillary electrophoresis and possible complex structures. Potentiometric titration was found to be an appropriate tool to determine the binding constants of cyclodextrin inclusion complexes.

  8. A method for determining an indicator of effective dose calculation due to inhalation of Radon and its progeny from in vivo measurements; Um metodo para determinar um indicador para calcular dose efetiva devida a inalacao de Radonio e seus descendentes utilizando medicoes in vivo

    Energy Technology Data Exchange (ETDEWEB)

    Estrada, Julio Jose da Silva

    1994-07-01

    Direct measurement of the absolved dose to lung tissue from inhalation of radon and its progeny is not possible and must be calculated using dosimetric models, taking into consideration the several parameters upon which the dose calculation depends. To asses the dose due to inhalation of radon and its progeny, it is necessary to estimate the cumulative exposure. Historically, this has been done using WLM values estimated with measurements of radon concentration in air. The radon concentration in air varies significantly, however, in space with time, and the exposed individual is also constantly moving around. This makes it almost impossible to obtain a precise estimate of an individual's inhalation exposure. This work describes a pilot study to calculate lung dose from the deposition of radon progeny, via estimates of cumulative exposure derived from in vivo measurements of {sup 210} Pb, in subjects exposed to above-average radon and its progeny concentrations in their home environments. The measurements were performed in a whole body counter. With this technique, the exposed individuals become, in affect, their own samplers and dosimeters and the estimate of cumulative exposure is not affected by the variation of the atmospheric concentration of radon and its progeny in time and space. Forty individuals identified as living in homes with radon levels ranging from about 740 Bq/m{sup 3} to 150.000 Bq/m{sup 3} were measured. Also, additional 34 measurements were made on personnel from NYUMC/NIEM who live in a residential area surrounding the laboratory in which the levels of radon have been shown to be at below average values. To realize these measurements a methodology was developed to determine the subject's background, using a head phantom made with a cubic plastic container containing known amounts of potassium and calcium dissolved in four liters of water. The effective doses calculated from the in vivo measurements are compared to effective doses estimated, for

  9. A method for determining an indicator of effective dose calculation due to inhalation of Radon and its progeny from in vivo measurements; Um metodo para determinar um indicador para calcular dose efetiva devida a inalacao de Radonio e seus descendentes utilizando medicoes in vivo

    Energy Technology Data Exchange (ETDEWEB)

    Estrada, Julio Jose da Silva

    1994-07-01

    Direct measurement of the absolved dose to lung tissue from inhalation of radon and its progeny is not possible and must be calculated using dosimetric models, taking into consideration the several parameters upon which the dose calculation depends. To asses the dose due to inhalation of radon and its progeny, it is necessary to estimate the cumulative exposure. Historically, this has been done using WLM values estimated with measurements of radon concentration in air. The radon concentration in air varies significantly, however, in space with time, and the exposed individual is also constantly moving around. This makes it almost impossible to obtain a precise estimate of an individual's inhalation exposure. This work describes a pilot study to calculate lung dose from the deposition of radon progeny, via estimates of cumulative exposure derived from in vivo measurements of {sup 210} Pb, in subjects exposed to above-average radon and its progeny concentrations in their home environments. The measurements were performed in a whole body counter. With this technique, the exposed individuals become, in affect, their own samplers and dosimeters and the estimate of cumulative exposure is not affected by the variation of the atmospheric concentration of radon and its progeny in time and space. Forty individuals identified as living in homes with radon levels ranging from about 740 Bq/m{sup 3} to 150.000 Bq/m{sup 3} were measured. Also, additional 34 measurements were made on personnel from NYUMC/NIEM who live in a residential area surrounding the laboratory in which the levels of radon have been shown to be at below average values. To realize these measurements a methodology was developed to determine the subject's background, using a head phantom made with a cubic plastic container containing known amounts of potassium and calcium dissolved in four liters of water. The effective doses calculated from the in vivo measurements are compared to effective doses

  10. 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%.

  11. Different Chromatographic Methods for Simultaneous Determination of Mefenamic Acid and Two of Its Toxic Impurities.

    Science.gov (United States)

    Morcoss, Martha M; Abdelwahab, Nada S; Ali, Nouruddin W; Elsaady, Mohammed T

    2017-08-01

    Two sensitive, accurate and precise chromatographic methods mentioned as TLC-densitometric method and RP-HPLC-DAD method, were developed and validated for the simultaneous determination of mefenamic acid (MEF) and its two toxic impurities, benzoic acid (BA) and 2,3-dimethylaniline (DMA). In the proposed TLC-densitometric method a developing system consisting of chloroform:acetone:acetic acid:ammonia solution(70:30:2:2, v/v/v/v) was used, TLC aluminum plates 60 F254 was used as a stationary phase and the separated bands were UV-scanned at 225 nm. While the proposed RP-HPLC-DAD method depended on chromatographic separation on C18 column using 0.05 M KH2PO4 buffer: acetonitrile (40:60, v/v) as a mobile phase at constant flow rate of 1 mL/min with UV detection at 225 nm. Linear relationships were obtained in the ranges of 0.3-2, 0.3-2 and 0.3-1.8 μg/band (for TLC-densitometric method) and in the ranges of 7-50, 10-50 and 7-50 μg/mL (for HPLC-DAD method) for MEF, BA and DMA, respectively. Factors affecting the developed methods have been studied and optimized. Moreover ,the proposed methods were successfully applied for determination of the studied drug in its pharmaceutical dosage form. The methods showed no significance difference when compared with the reported method using F-test and Student's-t test. The low of detection and quantization limits of the proposed methods get them suitable for quality control and stability studies of MEF in pharmaceutical formulation. The developed methods have advantages of being more selective and sensitive than the published methods. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. Capillary electrophoresis determination of glucosamine in nutraceutical formulations after labeling with anthranilic acid and UV detection.

    Science.gov (United States)

    Volpi, Nicola

    2009-04-05

    A new robust CE method for the determination of the glucosamine (GlcN) content in nutraceutical formulations is described after its derivatization with anthranilic acid (2-aminobenzoic acid, AA). The CE separation of derivatized GlcN with AA was performed on an uncoated fused-silica capillary tube (50 microm I.D.) using an operating pH 7.0 buffer of 150 mM boric acid/50 mM NaH2PO4 and UV detection at 214 nm. The method was validated for specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The detector response for GlcN was linear over the selected concentration range from 240 to 2400 pg (40-400 microg/mL) with a correlation coefficient greater than 0.980. The intra- and inter-day variations (CV%) were between 0.5 and 0.9 for migration time, and between 2.8 and 4.3 for peak area, respectively. The LOD and the LOQ of the method were approximately 200 and 500 pg, respectively. The intra- and inter-day accuracy was estimated to range from 2.8% to 5.1%, while the percent recoveries of GlcN in formulations were calculated to be about 100% after simple centrifugation for 10 min, lyophilization and derivatization with AA. The CE method was applied to the determination of GlcN content, in the form of GlcN-hydrochloride or GlcN-sulfate, of several nutraceutical preparations in the presence of other ingredients, i.e. chondroitin sulfate, vitamin C and/or methylsulfonylmethane (MSM) as well as salts and other agents. The quantitative results obtained were in total conformity with the label claims.

  13. 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.

  14. 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.

  15. A sol-gel based molecular imprint incorporating carbon dots for fluorometric determination of nicotinic acid

    International Nuclear Information System (INIS)

    Zuo, Pengli; Gao, Junfa; Liu, Jianha; Zhao, Mingming; Zhao, Jiahong; Peng, Jun; Zuo, Pengjian; He, Hua

    2016-01-01

    We are introducing functionalized carbon dots (C-dots) coated with a shell of molecularly imprinted sol-gel as a new tool in molecular imprint-based detection. Specifically, an imprint recognizing nicotinic acid (NA) was prepared in two steps. The first involves pyrolytic decomposition of citric acid in the presence of aminopropyltriethoxysilane to yield triethoxysilyl-modified C-dots with a typical size of 2.8 ± 1.1 nm. These are then polycondensed in the presence of tetraethoxysilane and NA at room temperature to give spherical silica nanoparticles (SiNPs) with a typical size of ∼300 nm and containing C-dots and NA in the silica matrix. NA was then removed by extraction. The resulting SiNPs are well permeable to NA, photostable, display strong blue luminescence and can bind NA fairly selectively. The fluorometric detection scheme is based on the finding that increasing concentrations of NA quench the fluorescence of the C-dots in the SiNPs. NA can be determined by this method in the 0.5 to 10.5 μM concentration range, with a 12.6 nM detection limit. The composite was successfully utilized as a fluorescent probe for the determination of NA in spiked human urine samples. The method is believed to have a wider scope in being applicable to other analytes that are capable of quenching the fluorescence of C-dots. (author)

  16. 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)

  17. Determination of glyphosate and aminomethylphosphonic acid for assessing the quality tap water using SPE and HPLC

    Directory of Open Access Journals (Sweden)

    Eduardo Luiz Delmonico

    2014-02-01

    Full Text Available The use of pesticides in agriculture is one of the current problems that may result in contamination of both ground and surface water and groundwater. Considering the environmental importance and the increasing use of herbicides in Maringá region, in the present work methods for extraction and determination of glyphosate (GLYP and aminomethylphosphonic acid (AMPA using solid phase extraction (SPE and high performance liquid chromatography (HPLC were developed. For SPE, anion exchange resin was used and elution was done with hydrochloric acid 50.0 mmol L-1, achieving recovery rates of 82.5-116.2% and 67.1-104.0% for AMPA and GLYP, respectively. For HPLC determination the analytes were derivatized and injected in the HPLC with a C18 column and using mobile phase consisting of phosphate buffer 0.20 mol L-1 at pH 3.0 and acetonitrile (85:15; the monitoring was done at 240 nm. The analysis was performed in 8 min with the same limit of detection and limit of quantification for AMPA and GLYP of 0.09 and 0.20 mg L-1, respectively. The methods were applied to analysis of public water supply samples and concentrations from 2.1 up to 2.9 µg L-1 for AMPA and from 2.3 up to 3.3 µg L-1 for glyphosate were found.

  18. 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.

  19. 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

  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. 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

  2. Method by chromatography of gases for the determination of made up of alcoholic fermentation in pineapple fruits (Ananas comosus [L.] Merr); Metodo por cromatografia de gases para la determinacion de compuestos de fermentacion alcoholica en frutos de pina (Ananas comosus [L.] Merr)

    Energy Technology Data Exchange (ETDEWEB)

    Murillo Williams, A

    2001-07-01

    The pineapple (Ananas comosus) it is used in the entire world for the fresh consumption or for processed products (canned, frozen, dehydrated). it is cultivated in a wide range of countries and in extreme latitudes.The factors of quality include: maturity, stability, size uniformity, absence of microbial deterioration, absence of burns for the sun, absence of blows, damage for insects and breaking, crowns, color, longitude and integrity. The factors that determine the longevity of a product can be physiologic or pathological. The physiologic conditions refer to the processes of degradation of the fabrics after the crop, while the pathological ones involve the attack of mushrooms and bacteria. In the case of the pineapple, a physiologic problem exists, called black heart, internal brewing (IB), brown endogenic stain ({sup m}ancha cafe endogena{sup ,} MCE) or chilling injury (CI) that can happen in any part of the world where it is cultivated. This problem has associated to the exhibition from the pineapple to low temperatures, so it is a challenge to manage a fruit like the pineapple that it cannot tolerate low temperatures without problems. In studies made about the physiologic changes that happen during the storage in controlled atmospheres in fruits, it has been observed that the ethanol and the acetaldehyde are volatile compounds associated with metabolic post-crop changes and that they have implication in the quality of the product. (author) [Spanish] La pina (Ananas comosus) se utiliza en todo el mundo para el consumo fresco o para productos procesados (enlatados, congelados, deshidratados). Se cultiva en un amplio rango de paises y en latitudes extremas. Los factores de calidad incluyen: madurez, firmeza, uniformidad de tamano, ausencia de deterioro microbiano, ausencia de quemaduras por el sol, ausencia de golpes, dano por insectos y quebraduras, corona, color, longitud e integridad. Los factores que determinan la longevidad de un producto pueden ser

  3. 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

  4. [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.

  5. Novel Spectrophotometric Methods for Determination of Salicylamide and Ascorbic acid in their binary mixture

    International Nuclear Information System (INIS)

    Ali, N.W.; Zaazaa, H.E.S.; Abdelrahman, M.M.

    2014-01-01

    Simple, selective and precise four spectrophotometric methods were developed and validated for quantitative determination of Salicylamide (SAD) and Ascorbic acid (ASC, Vitamin C) in their binary mixture. Method A is Area under curve spectrophotometry, in which the area under curve in the wavelength ranges 225-245 nm and 265-285 nm were selected for determination of SAD and ASC. Method B is based on dual wavelength spectrophotometry, where ASC can be determined by difference in absorbance at 249.8 and 285.8 nm. On the same way; SAD is measured by difference in absorbance at 240.4 and 286.4 nm. Method C utilizes isoabsorptive point spectrophotometry where total concentration of SAD and ASC was calculated at their isoabsorptive points at 246.4 and 287 nm, while SAD concentration alone can be determined by first derivative spectrophotometry (1D) at 315.4 nm, then ASC concentration can be determined by subtraction. Method D is ratio subtraction spectrophotometry, where ASC can be determined by dividing the spectrum of the mixture by the spectrum of the SAD (as a divisor) followed by subtracting the constant absorbance value of the plateau region, then finally multiplying the obtained spectrum by the spectrum of the divisor. The developed methods have been successfully applied for determination of the studied drugs in different laboratory prepared mixtures and in their pharmaceutical formulation. Statistical comparison between the results obtained by applying the proposed methods and the reported HPLC method was done, and it was found that there was no significant difference between them regarding both accuracy and precision. (author)

  6. Determination of tetrahydrophtalimide and 2-thiothiazolidine-4-carboxylic acid, urinary metabolites of the fungicide captan, in rats and humans

    NARCIS (Netherlands)

    van Welie, R.T.H.; van Duyn, P; Lamme, E K; Jäger, P; van Baar, B L; Vermeulen, N P

    1991-01-01

    Capillary gas chromatographic (GC) methods using sulphur and mass selective detection for the qualitative and quantitative determination of tetrahydrophtalimide (THPI) and 2-thiothiazolidine-4-carboxylic acid (TTCA), urinary metabolites of the fungicide captan in rat and humans, were developed.

  7. 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...

  8. 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

  9. O-Anisidine as Indicator in Titrimetric Determination of Ascorbic Acid and Isonicotinic Acid Hydrazide in Pharmaceutical Formulations

    OpenAIRE

    B.S.A.Andrews; B.Sreenivas Rao; Som Shankar Dubey; B.Venkata Kiran

    2010-01-01

    Inspite of the beautiful red coloured oxidized product of O-anisidine, the studies on its application in analytical techniques are scanty. So, authors have taken up the investigation on the utility of O-anisidine as a new Analytical reagent in the bromatometric-Indicator reaction. The detailed reaction on the potassium bromate and OAnisidine has enabled the authors to utilize O-Anisidine in titration of Ascorbic Acid and Isonicitonic Acid Hydrazide. Suitable conditions has been established wi...

  10. 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...

  11. 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.)

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

    Directory of Open Access Journals (Sweden)

    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.:

  13. Rapid fluorometric determination of perfluorooctanoic acid by its quenching effect on the fluorescence of quantum dots

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Qi; Huang, Aizhen; Wang, Nan, E-mail: nwang@hust.edu.cn; Zheng, Guan; Zhu, Lihua

    2015-05-15

    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{sup −1}, with a limit of detection of 0.3 μmol L{sup −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{sup −1} and a detection limit of 0.3 μmol L{sup −1}.

  14. 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.

  15. 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.

  16. 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

  17. Determination of organic acids evolution during apple cider fermentation using an improved HPLC analysis method

    NARCIS (Netherlands)

    Zhang, H.; Zhou, F.; Ji, B.; Nout, M.J.R.; Fang, Q.; Zhang, Z.

    2008-01-01

    An efficient method for analyzing ten organic acids in food, namely citric, pyruvic, malic, lactic, succinic, formic, acetic, adipic, propionic and butyric acids, using HPLC was developed. Boric acid was added into the mobile phase to separate lactic and succinic acids, and a post-column buffer

  18. 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.

  19. 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.

  20. 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.

  1. Phenylboronic acid immunoaffinity reactor coupled with flow injection chemiluminescence for determination of {alpha}-fetoprotein

    Energy Technology Data Exchange (ETDEWEB)

    Wu Yafeng [Jiangsu Provincial Key Lab of Biomaterials and Biodevices, School of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096 (China); Zhuang Yafeng [Department of Chemistry, Changzhou Institute of Technology, Changzhou 213022 (China); Liu Songqin [Jiangsu Provincial Key Lab of Biomaterials and Biodevices, School of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096 (China)], E-mail: liusq@seu.edu.cn; He Lin [Department of Chemistry, North Carolina State University, Raleigh, NC 27695-8204 (United States)

    2008-12-23

    A reusable and sensitive immunoassay based on phenylboronic acid immunoaffinity reactor in combination with flow injection chemiluminescence (CL) for determination of glycoprotein was described. The reactor was fabricated by immobilizing 3-aminophenylboronic acid (APBA) on glass microbeads with {gamma}-glycidoxypropyltrimethoxysilane (GPMS) as linkage. The {alpha}-fetoprotein (AFP) could be easily immobilized on the APBA coated beads through sugar-boronic interaction. After an off-line incubation, the mixture of the analyte AFP with horseradish peroxidase-labeled AFP antibody (HRP-anti-AFP) was injected into the reactor. This led the trapping of free HRP-anti-AFP by the surface coated AFP on glass beads. The trapped HRP-anti-AFP was detected by chemiluminescence due to its sensitizing effect on the reaction of luminol and hydrogen peroxide. Under optimal conditions, the chemiluminescent signal was proportional to AFP concentration in the range of 10-100 ng mL{sup -1}. The whole assay process including regeneration of the reactor could be completed within 31 min. The proposed system showed acceptable detection and fabrication reproducibility, and the results obtained with the present method were in acceptable agreement with those from parallel single-analyte test of practical clinical sera. The described method enabled a low-cost, time saving and was potential to detect the serum AFP level in clinical diagnosis.

  2. Spectrophotometric Determination of Gemifloxacin Mesylate, Moxifloxacin Hydrochloride, and Enrofloxacin in Pharmaceutical Formulations Using Acid Dyes

    Directory of Open Access Journals (Sweden)

    Ayman A. Gouda

    2014-01-01

    Full Text Available Simple, rapid, and extractive spectrophotometric methods were developed for the determination of some fluoroquinolones antibiotics: gemifloxacin mesylate (GMF, moxifloxacin hydrochloride (MXF, and enrofloxacin (ENF in pure forms and pharmaceutical formulations. These methods are based on the formation of ion-pair complexes between the basic drugs and acid dyes, namely, bromocresol green (BCG, bromocresol purple (BCP, bromophenol blue (BPB, bromothymol blue (BTB, and methyl orange (MO in acidic buffer solutions. The formed complexes were extracted with chloroform and measured at 420, 408, 416, 415, and 422 nm for BCG, BCP, BPB, BTB, and MO, respectively, for GMF; at 410, 415, 416, and 420 nm for BCP, BTB, BPB, and MO, respectively, for MXF; and at 419 and 414 nm for BCG and BTB, respectively, in case of ENF. The analytical parameters and their effects are investigated. Beer’s law was obeyed in the ranges 1.0–30, 1.0–20, and 2.0–24 μg mL−1 for GMF, MXF, and ENF, respectively. The proposed methods have been applied successfully for the analysis of the studied drugs in pure forms and pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent agreement and indicated no significant difference in accuracy and precision.

  3. 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

  4. 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.

  5. 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)

  6. 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

  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. Electrochemistry and analytical determination of lysergic acid diethylamide (LSD) via adsorptive stripping voltammetry.

    Science.gov (United States)

    Merli, Daniele; Zamboni, Daniele; Protti, Stefano; Pesavento, Maria; Profumo, Antonella

    2014-12-01

    Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1-90 ng L(-1) for deposition times of 50s. LOD of 1.4 ng L(-1) and LOQ of 4.3 ng L(-1) were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. 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...

  10. Electrochemical Determination of Uric Acid at CdTe Quantum Dot Modified Glassy Carbon Electrodes.

    Science.gov (United States)

    Pan, Deng; Rong, Shengzhong; Zhang, Guangteng; Zhang, Yannan; Zhou, Qiang; Liu, Fenghai; Li, Miaojing; Chang, Dong; Pan, Hongzhi

    2015-01-01

    Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical behavior of uric acid (UA) at a CdTe quantum dot (QD) modified the glassy carbon electrode (GCE). CdTe QDs, as new semiconductor nanocrystals, can greatly improve the peak current of UA. The anodic peak current of UA was linear with its concentration between 1.0×10(-6) and 4.0×10(-4) M in 0.1 M pH 5.0 phosphate buffer solution. The LOD for UA at the CdTe electrode (1.0×10(-7) M) was superior to that of the GCE. In addition, we also determined the effects of scan rate, pH, and interferences of UA for the voltammetric behavior and detection. The results indicated that modified electrode possessed excellent reproducibility and stability. Finally, a new and efficient electrochemical sensor for detecting UA was developed.

  11. 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

  12. Determination of the Acidity of Oils Using Paraformaldehyde as a Thermometric End-Point Indicator

    Directory of Open Access Journals (Sweden)

    Carneiro Mário J. D.

    2002-01-01

    Full Text Available The determination of the acidity of oils by catalytic thermometric titrimetry using paraformaldehyde as the thermometric end-point indicator was investigated. The sample solvent was a 1:1 (v/v mixture of toluene and 2-propanol and the titrant was 0.1 mol L-1 aqueous sodium hydroxide. Paraformaldehyde, being insoluble in the sample solvent, does not present the inconvenience of other indicators that change the properties of the solvent due to composition changes. The titration can therefore be done effectively in the same medium as the standard potentiometric and visual titration methods. The results of the application of the method to both non-refined and refined oils are presented herein. The proposed method has advantages in relation to the potentiometric method in terms of speed and simplicity.

  13. [Development of the determination methods of fatty acid esters of chloropropanediols in fat-rich foods].

    Science.gov (United States)

    Yan, Xiaobo; Wu, Shaoming; Li, Nan; Lü, Huadong; Fu, Wusheng

    2013-02-01

    Fatty acid esters of chloropropanediols are a kinds of newly emerged food contaminants, especially 3-monochloropropane-1,2-diol (3-MCPD) esters that have been detected in many foodstuffs such as infant formula and edible oils at relatively high levels. Based on the Tolerable Dose Intake (TDI) of 3-MCPD, the intake of 3-MCPD from 3-MCPD esters may cause the health risk to human beings. The researches for the analysis of 3-MCPD esters have been carried out in some institutes abroad, but there were only a few in China. This paper reviews the methods for the determination of 3-MCPD esters in fat-rich foods, including the extraction, hydrolysis, the derivatization of 3-MCPD esters, the total amount of 3-MCPD esters and the amounts of monoesters and diesters of 3-MCPD.

  14. Electrochemical Determination of Glycoalkaloids Using a Carbon Nanotubes-Phenylboronic Acid Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Huiying Wang

    2013-11-01

    Full Text Available A versatile strategy for electrochemical determination of glycoalkaloids (GAs was developed by using a carbon nanotubes-phenylboronic acid (CNTs-PBA modified glassy carbon electrode. PBA reacts with α-solanine and α-chaconine to form a cyclic ester, which could be utilized to detect GAs. This method allowed GA detection from 1 μM to 28 μM and the detection limit was 0.3 μM. Affinity interaction of GAs and immobilized PBA caused an essential change of the peak current. The CNT-PBA modified electrodes were sensitive for detection of GAs, and the peak current values were in quite good agreement with those measured by the sensors.

  15. Neural networks applied to determine the thermophysical properties of amino acid based ionic liquids.

    Science.gov (United States)

    Cancilla, John C; Perez, Ana; Wierzchoś, Kacper; Torrecilla, José S

    2016-03-14

    A series of models based on artificial neural networks (ANNs) have been designed to estimate the thermophysical properties of different amino acid-based ionic liquids (AAILs). Three different databases of AAILs were modeled using these algorithms with the goal set to estimate the density, viscosity, refractive index, ionic conductivity, and thermal expansion coefficient, and requiring only data regarding temperature and electronic polarizability of the chemicals. Additionally, a global model was designed combining all of the databases to determine the robustness of the method. In general, the results were successful, reaching mean prediction errors below 1% in many cases, as well as a statistically reliable and accurate global model. Attaining these successful models is a relevant fact as AAILs are novel biodegradable and biocompatible compounds which may soon make their way into the health sector forming a part of useful biomedical applications. Therefore, understanding the behavior and being able to estimate their thermophysical properties becomes crucial.

  16. 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)

  17. Factors affecting variations in the detailed fatty acid profile of Mediterranean buffalo milk determined by 2-dimensional gas chromatography.

    Science.gov (United States)

    Pegolo, S; Stocco, G; Mele, M; Schiavon, S; Bittante, G; Cecchinato, A

    2017-04-01

    Buffalo milk is the world's second most widely produced milk, and increasing attention is being paid to its composition, particularly the fatty acid profile. The objectives of the present study were (1) to characterize the fatty acid composition of Mediterranean buffalo milk, and (2) to investigate potential sources of variation in the buffalo milk fatty acid profile. We determined the profile of 69 fatty acid traits in 272 individual samples of Mediterranean buffalo milk using gas chromatography. In total, 51 individual fatty acids were identified: 24 saturated fatty acids, 13 monounsaturated fatty acids, and 14 polyunsaturated fatty acids. The major individual fatty acids in buffalo milk were in the order 16:0, 18:1 cis-9, 14:0, and 18:0. Saturated fatty acids were the predominant fraction in buffalo milk fat (70.49%); monounsaturated and polyunsaturated fatty acids were at 25.95 and 3.54%, respectively. Adopting a classification based on carbon-chain length, we found that medium-chain fatty acids (11-16 carbons) represented the greater part (53.7%) of the fatty acid fraction of buffalo milk, whereas long-chain fatty acids (17-24 carbons) and short-chain fatty acids (4-10 carbons) accounted for 32.73 and 9.72%, respectively. The n-3 and n-6 fatty acids were 0.46 and 1.77%, respectively. The main conjugated linoleic acid, rumenic acid, represented 0.45% of total milk fatty acids. Herd/test date and stage of lactation were confirmed as important sources of variation in the fatty acid profile of buffalo milk. The percentages of short-chain and medium-chain fatty acids in buffalo milk increased in early lactation (+0.6 and +3.5%, respectively), whereas long-chain fatty acids decreased (-4.2%). The only exception to this pattern was butyric acid, which linearly decreased from the beginning of lactation, confirmation that its synthesis is independent of malonyl-CoA. These results seem to suggest that in early lactation the mobilization of energy reserves may have less

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. Determination model for cetane number of biodiesel at different fatty acid composition: a review

    Directory of Open Access Journals (Sweden)

    Michal Angelovič

    2014-05-01

    Full Text Available The most accepted definition of biodiesel is stated at the EU technical regulation EN 14214 (2008 or in the USA in ASTM 6751-02. As a result of this highly strict description only methyl esters of fatty acids conform to these definitions, nevertheless the term ‘‘biodiesel’’ is spread out to other alkyl fatty esters. Some countries have adopted bioethanol for replacement of methanol in biodiesel transesterification and thus assuring a fully biological fuel. Of course, such position brings some problems in fulfilling technical requirements of EN 14214 or ASTM 6751-02. Biodiesel is actually a less complex mixture than petrodiesel, but different feedstock origins and the effect of seasonality may impose difficulties in fuel quality control. Since biodiesel is an alternative diesel fuel derived from the transesterification of triacylglycerol comprised materials, such as vegetable oils or animal fats, with simple alcohols to furnish the corresponding mono-alkyl esters, its composition depends on the raw material used, the cultivated area location, and harvest time. The choice of the raw material is usually the most important factor for fluctuations of biodiesel composition, because different vegetable oils and animal fats may contain different types of fatty acids. Important properties of this fuel vary significantly with the composition of the mixture. Cetane number, melting point, degree of saturation, density, cloud point, pour point, viscosity, and nitrogen oxides exhaust emission (NOx, for instance, deserve to be mentioned. One of the most important fuel quality indicators is the cetane number; however its experimental determination may be an expensive and lengthy task. To weaken situation concerning biodiesel, the availability of data in the literature is also scarce. In such scenario, the use of reliable models to predict the cetane number or any other essential characteristic may be of great utility. We reviewed available literature to

  3. Effect of hydrofluoric acid on acid decomposition mixtures for determining iron and other metallic elements in green vegetables

    International Nuclear Information System (INIS)

    Dogbe, S.A.; Afful, S.; Debrah, C.

    2007-01-01

    The efficiency of acid mixtures, HNO 3 - HCI0 4 -HF, HNO 3 - HCI - HF, HNO 3 - HCIO 4 and HNO 3 - HCI in the decomposition of four edible green vegetables, Gboma (Solanum macrocarpon), Aleefu (Amaranttius hibiridus), Shoeley (Hibiscus sabdariffa) and Ademe (Corchorus olitorius), for flame Atomic Absorption Spectrometer analysis of Fe, Mn, Mg, Cu, Zn and Ca was studied. The concentrations of Fe were higher (120.61 -710.10 mg/kg), while the values of Cu were lower (2.31 - 4.84 mg/kg) in all the samples. The values of concentration for Fe were more reproducible when HF was included in the decomposition mixtures. There were no significant differences in the concentrations of the other elements when HF was included in the acid mixture as compared to the acid mixtures without HF. Therefore, the inclusion of HF in the acid decomposition mixtures would ensure total and precise estimation of Fe in plant materials, but not critical for analysis of Mn, Mg, Cu, Zn and Ca. Performance of the decomposition procedures was verified by applying the methods to analyse Standard Reference Material IAEA-V-10 Hay Powder. (au)

  4. Polymorphism in the fatty acid desaturase genes and diet are important determinants of infant n-3 fatty acid status

    DEFF Research Database (Denmark)

    Harsløf, L.B.S.; Larsen, L.H.; Ritz, C.

    and polymorphism in the genes that encodes the fatty acid desaturases (FADS) has little effect on DHA-status in adults. It is however unclear to what extent endogenous DHA-synthesis contributes to infant DHA-status. Aim: To investigate the role of diet and FADS polymorphism on DHA-status at 9 months and 3 years...... breastfeeding was obtained by questionnaires and fish intake was assessed by 7-day pre-coded food diaries. Results: FADS-genotype, breastfeeding, and fish intake were found to explain 25% of the variation in infant RBC DHA-status (mean±SD: 6.6±1.9% of the fatty acids (FA%)). Breastfeeding was the most important......Background and objectives: Tissue docosahexaenoic acid (DHA) accretion in early infancy has been shown to be supported by the DHA-content of breast-milk and thus may decrease once complementary feeding takes over. Endogenous synthesis of DHA from alpha-linolenic acid has been shown to be very low...

  5. 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.)

  6. 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)

  7. Linear sweep polarographic determination of nucleic acids using acridine orange as a bioprobe

    Directory of Open Access Journals (Sweden)

    WEI SUN

    2007-11-01

    Full Text Available The interaction of acridine orange (AO with double-stranded (ds DNA in aqueous solution was investigated by linear sweep polarography (LSP on a dropping mercury working electrode (DME. In pH 2.5 Britton–Robinson (B–R buffer solution, AO had a sensitive linear sweep polarographic reductive peak at –0.89 V (vs. SCE, which could be greatly inhibited by the addition of dsDNA, with a positive shift of the peak potential. Based on the decrease of the reductive peak current, a new quantitative electrochemical determination method for dsDNA was developed with a linear range of 2.0−20.0 mg l-1 and the linear regression equation: ΔIp” (nA = 111.90 C (mg l-1+125.32 (n = 9, γ = 0.997. The influences of commonly co-existing substances, such as metal ions, amino acid, etc., on the determination were also investigated. The method is sensitive, rapid and simple with good selectivity. The new proposed method was further applied to the detection of RNA and three synthetic samples containing dsDNA with satisfactory results. The binding number and the equilibrium constant between dsDNA and AO were calculated by an electrochemical method.

  8. "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.

  9. Precise equilibrium structure determination of hydrazoic acid (HN3) by millimeter-wave spectroscopy

    International Nuclear Information System (INIS)

    Amberger, Brent K.; Esselman, Brian J.; Woods, R. Claude; McMahon, Robert J.; Stanton, John F.

    2015-01-01

    The millimeter-wave spectrum of hydrazoic acid (HN 3 ) was analyzed in the frequency region of 235-450 GHz. Transitions from a total of 14 isotopologues were observed and fit using the A-reduced or S-reduced Hamiltonian. Coupled-cluster calculations were performed to obtain a theoretical geometry, as well as rotation-vibration interaction corrections. These calculated vibration-rotation correction terms were applied to the experimental rotational constants to obtain mixed theoretical/experimental equilibrium rotational constants (A e , B e , and C e ). These equilibrium rotational constants were then used to obtain an equilibrium (R e ) structure using a least-squares fitting routine. The R e structural parameters are consistent with a previously published R s structure, largely falling within the uncertainty limits of that R s structure. The present R e geometric parameters of HN 3 are determined with exceptionally high accuracy, as a consequence of the large number of isotopologues measured experimentally and the sophisticated (coupled-cluster theoretical treatment (CCSD(T))/ANO2) of the vibration-rotation interactions. The R e structure exhibits remarkable agreement with the CCSD(T)/cc-pCV5Z predicted structure, validating both the accuracy of the ab initio method and the claimed uncertainties of the theoretical/experimental structure determination

  10. Simultaneous determination of isoniazid and p-aminosalicylic acid by capillary electrophoresis using chemiluminescence detection.

    Science.gov (United States)

    Zhang, Xinfeng; Xuan, Yuelan; Sun, Aimin; Lv, Yi; Hou, Xiandeng

    2009-01-01

    It was found that isoniazid (ISO) or p-aminosalicylic acid (PAS) could enhance the chemiluminescence (CL) emission from Cu (II)-luminol-hydrogen peroxide system, and the increased chemiluminescence signals were proportional to their concentrations, respectively. Based on this phenomenon, a chemiluminescence method coupled to capillary electrophoresis (CE) was established for simultaneous determination of ISO and PAS. The CE conditions including running buffer and running voltage were investigated in detail. The effects of the pH of H(2)O(2) solution and the concentrations of luminol, H(2)O(2) and Cu (II) on the CL signal were also investigated carefully. Under the optimized conditions, the analysis could be accomplished within 10 min, with the limits of detection of 0.3 microg mL(-1) for ISO and 1.1 microg mL(-1) for PAS, corresponding to 7.2 and 26.4 pg per injection (24 nL), respectively. Finally, the method was validated by determining the two analytes in pharmaceutical preparation and spiked human serum samples. The results of pharmaceutical tablet analysis were in good agreement with the labeled amounts. The recoveries for ISO and PAS in human serum were in the range of 92-104% and 90-113%, respectively. Copyright 2008 John Wiley & Sons, Ltd.

  11. Electrochemical determination of ascorbic acid at p-phenylenediamine film-holes modified glassy carbon electrode

    Directory of Open Access Journals (Sweden)

    Olana Bikila Nagasa

    2015-01-01

    Full Text Available In this work the determination of ascorbic acid (AA at glassy carbon electrode (GCE modified with a perforated film produced by reduction of diazonium generated in situ from p-phenylenediamine (PD is reported. Holes were intentionally created in the modifier film by stripping a pre-deposited gold nanoparticles. The modified electrodes were electrochemically characterized by common redox probes: hydroquinone, ferrocyanide and hexamineruthenium(III. The cyclic voltammetric and amperometric response of AA using the modified electrodes was compared with that of bare GCE. The bare GCE showed a linear response to AA in the concentration range of 5 mM to 45 mM with detection limit of 1.656 mM and the modified GCE showed a linear response to AA in the concentration range of 5 μM to 45 μM with detection limit of 0.123 μM. The effect of potential intereferents on amperometric signal of AA at the modified GCE was examined and found to be minimal. The inter-electrode reproducibility, stability, and accuracy were determined. The modified electrode showed excellent inter-electrode reproducibility, accuracy and stability. The modified electrode reported is a promising candidate for use in electroanalysis of AA.

  12. Sensitive Electrochemical Determination of Gallic Acid: Application in Estimation of Total Polyphenols in Plant Samples

    Directory of Open Access Journals (Sweden)

    Mohammad Ali Sheikh-Mohseni

    2016-12-01

    Full Text Available A modified electrode was prepared by modification of the carbon paste electrode (CPE with graphene nano-sheets. The fabricated modified electrode exhibited an electrocatalytic activity toward gallic acid (GA oxidation because of good conductivity, low electron transfer resistance and catalytic effect. The graphene modified CPE had a lower overvoltage and enhanced electrical current respect to the bare CPE for the oxidation of GA. The oxidation potential of GA decreased more than 210 mV by the modified electrode. The modified electrode responded to the GA in the concentration range of 3.0 × 10-5-1.5 × 10-4 M with high sensitivity by the technique of differential pulse voltammetry. Also, detection limit of 1.1 × 10-7 M was obtained by this modified electrode for GA. This electrode was used for the successful determination of GA in plant samples. Therefore, the content of total polyphenols in plant samples can be determined by the proposed modified electrode based on the concentration of GA in the sample.

  13. Hybrid unscented particle filter based state-of-charge determination for lead-acid batteries

    International Nuclear Information System (INIS)

    Shen, Yanqing

    2014-01-01

    Accurate prediction of cell SOC (state of charge) is important for the safety and functional capabilities of the battery energy storage application system. This paper presents a hybrid UPF (unscented particle filter) based SOC determination combined model for batteries. To simulate the entire dynamic electrical characteristics of batteries, a novel combined state space model, which takes current as a control input and let SOC and two constructed parameters as state variables, is advanced to represent cell behavior. Besides that, an improved UPF method is used to evaluate cell SOC. Taking lead-acid batteries for example, we apply the established model for test. Results show that the evolved combined state space cell model simulates battery dynamics robustly with high accuracy and the prediction value based on the improved UPF method converges to the real SOC very quickly within the error of±2%. - Highlights: • This paper introduces a hybrid UPF based SOC determination model for batteries. • The evolved model takes SOC and two constructed parameters as state variables. • The combined state space cell model simulates battery dynamics robustly. • NLMS based method is employed to lessen search space and fasten convergence process. • Novel model converges to the real SOC robustly and quickly with fewer particles

  14. 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...

  15. Determination of stability constants of lanthanides (III) with amino acids (Preprint No. AL-07)

    International Nuclear Information System (INIS)

    Patel, N.M.; Patel, P.M.; Patel, M.N.; Joshi, J.D.

    1989-01-01

    The present paper reports the stability constants of La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) with amino acids valine, serine, threonine, methionine and aspartic acid. The coordination of valine and aspartic acid have been discussed. The stability constants of trivalent lanthanide amino acid complexes were found to be in the order, La < Ce < Pr < Nd < Sm < Gd. (author). 5 refs

  16. The Determination of Sub-Microgram Quantities, of Amino Acids with H{sup 3}- and C{sup 1}4-Labelled 1-Fluoro-2.4 Dinitrobenzene; Determination d'acides amines en quantites inferieures au microgramme a l'aide de 1-fluoro-2,4-dinitrobenzen e marque au {sup 3}H et au {sup 14}C; Podschet submikrogrammnykh kolichestv aminokislot pri pomoshchi 2 : 4 dinitroftor'enzola, mechennogo H{sup 3} i C{sup 14}; Determinacion de cantidades de aminoacidos inferiores al microgramo por medio de 1-fluoro-2,4-dinitrobenceno marcado con {sup 3}H y {sup 14}C

    Energy Technology Data Exchange (ETDEWEB)

    Beale, D; Whitehead, J K [Middlesex Hospital Medical School, London (United Kingdom)

    1962-01-15

    A method of isotope derivation analysis is described for the estimation of amino acids at levels as low as 10{sup -5} {mu}M in protein hydrolysates. 1-fluoro-2.4-dinitrobenzene-H{sup 3} (G) was synthesized from bromobenzene-H{sup 3} (G), and 1-fluoro- 2.4-dinitrobenzene-C{sup 14} (G) was prepared from chlorobenzene-C{sup 14} (G). The method of analysis involves the treatment of the mixture of amino acids with the tritiated reagent (specific activity 12,8{mu}c/{mu}-equivalent) in alkaline solution followed by the addition of known activities (6000 dpm) of C{sup 14}-labelled 2.4-dinitto phenyl derivatives. After solvent extraction the reaction mixture is separated into its constituent dinitro phenyl derivatives by two-way paper chromatography, and the H{sup 3} and C{sup 14} contente of each spot are determined by combustion and gas counting. The H{sup 3} count gives a measure of the amount of DNP derivative of amino acid isolated from the original mixture, and the C{sup 14} count gives a measure pf losses ihcurred during the analysis. The results obtained from the analysis of ({mu}g of hydrolyzed insulin are in good agreement with values obtained by derivative analysis with H{sup 3} and C{sup 14}-labelled acetic anhydride and by ion exchange resin chromatography. [French] Les auteurs decrivent une methode d'analyse par derivation isotopique permettant d'evaluer des quantites d'acides amines aussi faibles que 10{sup -5} {mu}M dans des hydrolysats de proteine. Le 1-fluoro-2,4-dinitrobenzene-{sup 3}H (G) a ete prepare par synthese a partir du bromobenzene-{sup 3}H (U), et le 1-fluoro-2,4-dinitrobenzene-{sup 14}C (G) a partir du chlorobenzene-{sup 14}C (U). Cette methode d'analyse implique le traitement du melange d'acides amines par le reactif tritie (activite specifique: 12,8 p.c par microequivalent) en solution alcaline, suivi.de l'addition de derives du dinitro-2,4-phenyl e marque au {sup 14}C d'activite connue (6000 dpm). Apres extraction par solvant, les derives du

  17. 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.

  18. Hierarchical nanoporous platinum-copper alloy for simultaneous electrochemical determination of ascorbic acid, dopamine, and uric acid

    International Nuclear Information System (INIS)

    Zhao, Dianyun; Fan, Dawei; Wang, Jinping; Xu, Caixia

    2015-01-01

    A hierarchical nanoporous PtCu alloy was fabricated by two-step dealloying of a PtCuAl precursor alloy followed by annealing. The new alloy possesses interconnected hierarchical network architecture with bimodal distributions of ligaments and pores. It exhibits high electrochemical activity towards the oxidation of ascorbic acid (AA), dopamine (DA), and uric acid (UA) at working potentials of 0.32, 0.47 and 0.61 V (vs. a mercury sulfate reference electrode), respectively. The new alloy was placed on a glassy carbon electrode and then displayed a wide linear response to AA, DA, and UA in the concentration ranges from 25 to 800 μM, 4 to 20 μM, and 10 to 70 μM, respectively. The lower detection limits are 17.5 μM, 2.8 µM and 5.7 μM at an S/N ratio of 3. (author)

  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. 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)

  1. Determination of the conjugated linoleic acid-containing triacylglycerols in New Zealand bovine milk fat.

    Science.gov (United States)

    Robinson, N P; MacGibbon, A K

    2000-07-01

    Reversed-phase high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection at 233 nm was used to separate, quantify, and identify the triacylglycerols (TAG) of milk fat that contain conjugated linoleic acid (CLA). The absorbance at 233 nm was substantially due to CLA-TAG (chromatography of some representative TAG devoid of CLA, such as tripalmitin and triolein, showed poor responses at 233 nm, 1/800th that of CLA-TAG). A CLA molar extinction coefficient at 233 nm of 23,360 L mol(-1) cm(-1) and an HPLC UV response factor were obtained from a commercially available cis-9,trans-11-CLA standard. This molar extinction coefficient was only 86% of reported literature values. Summation of all chromatographic peaks absorbing at 233 nm using the corrected response factor gave good agreement with independent determinations of total CLA by gas chromatography and UV spectrophotometry. This agreement allowed quantification of individual CLA-TAG peaks in the HPLC separation of a typical New Zealand bovine milk fat. Three CLA-containing TAG, CLA-dipalmitin, CLA-oleoyl-palmitin and CLA-diolein, were prepared by interesterification of tripalmitin with the respective fatty acid methyl esters and used to assign individual peaks in the reversed-phase chromatography of total milk fat, of which CLA-oleoyl-palmitin was coincident with the largest UV peak. Band fractions from argentation thin-layer chromatography of total milk fat were similarly employed to identify five predominant CLA-TAG groups in total milk fat: CLA-disaturates, CLA-oleoyl-saturates, CLA-vaccenyl-saturates, CLA-vaccenyl-olein, and CLA-diolein.

  2. Determination of glycated albumin using boronic acid-derived agarose beads on paper-based devices.

    Science.gov (United States)

    Ko, Euna; Tran, Van-Khue; Geng, Yanfang; Kim, Min Ki; Jin, Ga Hyun; Son, Seong Eun; Hur, Won; Seong, Gi Hun

    2018-01-01

    Self-monitoring of glycated albumin (GA), a useful glycemic marker, is an established method for preventing diabetes complications. Here, the paper-based lateral flow assay devices were developed for the sensitive detection of GA and the total human serum albumin (tHSA) in self-monitoring diabetes patients. Boronic acid-derived agarose beads were packed into a hole on a lateral flow channel. These well-coordinated agarose beads were used to capture GA through specific cis-diol interactions and to enhance the colorimetric signals by concentrating the target molecules. The devices exhibited large dynamic ranges (from 10  μ g/ml to 10 mg/ml for GA and from 10 mg/ml to 50 mg/ml for tHSA) and low detection limits (7.1  μ g/ml for GA and 4.7 mg/ml for tHSA), which cover the range of GA concentration in healthy plasma, which is 0.21-1.65 mg/ml (0.6%-3%). In determining the unknown GA concentrations in two commercial human plasma samples, the relative percentage difference between the values found by a standard ELISA kit and those found by our developed devices was 2.62% and 8.80%, which are within an acceptable range. The measurements of GA and tHSA were completed within 20 min for the total sample-to-answer diagnosis, fulfilling the demand for rapid analysis. Furthermore, the recovery values ranged from 99.4% to 110% in device accuracy tests. These results indicate that the developed paper-based device with boronic acid-derived agarose beads is a promising platform for GA and tHSA detection as applied to self-monitoring systems.

  3. 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.

  4. Simultaneous determination of rutin and ascorbic acid in a sequential injection lab-at-valve system.

    Science.gov (United States)

    Al-Shwaiyat, Mohammed Khair E A; Miekh, Yuliia V; Denisenko, Tatyana A; Vishnikin, Andriy B; Andruch, Vasil; Bazel, Yaroslav R

    2018-02-05

    A green, simple, accurate and highly sensitive sequential injection lab-at-valve procedure has been developed for the simultaneous determination of ascorbic acid (Asc) and rutin using 18-molybdo-2-phosphate Wells-Dawson heteropoly anion (18-MPA). The method is based on the dependence of the reaction rate between 18-MPA and reducing agents on the solution pH. Only Asc is capable of interacting with 18-MPA at pH 4.7, while at pH 7.4 the reaction with both Asc and rutin proceeds simultaneously. In order to improve the precision and sensitivity of the analysis, to minimize reagent consumption and to remove the Schlieren effect, the manifold for the sequential injection analysis was supplemented with external reaction chamber, and the reaction mixture was segmented. By the reduction of 18-MPA with reducing agents one- and two-electron heteropoly blues are formed. The fraction of one-electron heteropoly blue increases at low concentrations of the reducer. Measurement of the absorbance at a wavelength corresponding to the isobestic point allows strictly linear calibration graphs to be obtained. The calibration curves were linear in the concentration ranges of 0.3-24mgL -1 and 0.2-14mgL -1 with detection limits of 0.13mgL -1 and 0.09mgL -1 for rutin and Asc, respectively. The determination of rutin was possible in the presence of up to a 20-fold molar excess of Asc. The method was applied to the determination of Asc and rutin in ascorutin tablets with acceptable accuracy and precision (1-2%). Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Ruminal bacteria and protozoa composition, digestibility, and amino acid profile determined by multiple hydrolysis times.

    Science.gov (United States)

    Fessenden, S W; Hackmann, T J; Ross, D A; Foskolos, A; Van Amburgh, M E

    2017-09-01

    Microbial samples from 4 independent experiments in lactating dairy cattle were obtained and analyzed for nutrient composition, AA digestibility, and AA profile after multiple hydrolysis times ranging from 2 to 168 h. Similar bacterial and protozoal isolation techniques were used for all isolations. Omasal bacteria and protozoa samples were analyzed for AA digestibility using a new in vitro technique. Multiple time point hydrolysis and least squares nonlinear regression were used to determine the AA content of omasal bacteria and protozoa, and equivalency comparisons were made against single time point hydrolysis. Formalin was used in 1 experiment, which negatively affected AA digestibility and likely limited the complete release of AA during acid hydrolysis. The mean AA digestibility was 87.8 and 81.6% for non-formalin-treated bacteria and protozoa, respectively. Preservation of microbe samples in formalin likely decreased recovery of several individual AA. Results from the multiple time point hydrolysis indicated that Ile, Val, and Met hydrolyzed at a slower rate compared with other essential AA. Singe time point hydrolysis was found to be nonequivalent to multiple time point hydrolysis when considering biologically important changes in estimated microbial AA profiles. Several AA, including Met, Ile, and Val, were underpredicted using AA determination after a single 24-h hydrolysis. Models for predicting postruminal supply of AA might need to consider potential bias present in postruminal AA flow literature when AA determinations are performed after single time point hydrolysis and when using formalin as a preservative for microbial samples. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  6. 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.

  7. 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.

  8. 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.

  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

    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

  10. 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.

  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 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.

  13. 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

  14. 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

  15. 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.

  16. 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

  17. 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

  18. Identification of crucial amino acids in mouse aldehyde oxidase 3 that determine substrate specificity.

    Directory of Open Access Journals (Sweden)

    Martin Mahro

    Full Text Available In order to elucidate factors that determine substrate specificity and activity of mammalian molybdo-flavoproteins we performed site directed mutagenesis of mouse aldehyde oxidase 3 (mAOX3. The sequence alignment of different aldehyde oxidase (AOX isoforms identified variations in the active site of mAOX3 in comparison to other AOX proteins and xanthine oxidoreductases (XOR. Based on the structural alignment of mAOX3 and bovine XOR, differences in amino acid residues involved in substrate binding in XORs in comparison to AOXs were identified. We exchanged several residues in the active site to the ones found in other AOX homologues in mouse or to residues present in bovine XOR in order to examine their influence on substrate selectivity and catalytic activity. Additionally we analyzed the influence of the [2Fe-2S] domains of mAOX3 on its kinetic properties and cofactor saturation. We applied UV-VIS and EPR monitored redox-titrations to determine the redox potentials of wild type mAOX3 and mAOX3 variants containing the iron-sulfur centers of mAOX1. In addition, a combination of molecular docking and molecular dynamic simulations (MD was used to investigate factors that modulate the substrate specificity and activity of wild type and AOX variants. The successful conversion of an AOX enzyme to an XOR enzyme was achieved exchanging eight residues in the active site of mAOX3. It was observed that the absence of the K889H exchange substantially decreased the activity of the enzyme towards all substrates analyzed, revealing that this residue has an important role in catalysis.

  19. Flow injection chemiluminescence determination of loxoprofen and naproxen with the acidic permanganate-sulfite system

    Directory of Open Access Journals (Sweden)

    Li-Juan Wang

    2011-02-01

    Full Text Available A novel flow injection chemiluminescence (CL method for the determination of loxoprofen and naproxen was proposed based on the CL system of KMnO4, and Na2SO3 in acid media. The CL intensity of KMnO4-Na2SO3 was greatly enhaneed in the presence of loxoprofen and naproxen. The mechanism of the CL reaction was studied by the kinetic proecss and UV-vis absorption and the conditions were optimized. Under optimized conditions, the CL intensity was linear with loxoprofen and naproxen concentration in the range of 7.0 × 10−8 – 1.0 × 10−5 g/mL and 2.0 × 10−7 – 4.0 × 10−6 g/mL with the detection limit of 2.0 × 10−8 g/mL and 3.0 × 10−8 g/mL (S/N = 3, respectively. Thc relative standard deviations were 2.39% and 1.37% for 5.0 × 10−7 g/mL naproxen and 5.0 × 10−7 g/mL loxoprofen (n = 10, respectively. The proposed method was satisfactorily applied to thc determination of loxoprofen and naproxen in pharmaceutical preparations. Keywords: chemiluminescence, KMnO4, loxoprofen, naproxen

  20. Determination of lipoic acid in human urine by capillary zone electrophoresis.

    Science.gov (United States)

    Kubalczyk, Paweł; Głowacki, Rafał

    2017-07-01

    Fast, simple, and accurate CE method enabling determination of lipoic acid (LA) in human urine has been developed and validated. LA is a disulfide-containing natural compound absorbed from the organism's diet. Due to powerful antioxidant activity, LA has been used for prevention and treatment of various diseases and disorders, e.g. cardiovascular diseases, neurodegenerative disorders, and cancer. The proposed analytical procedure consists of liquid-liquid sample extraction, reduction of LA with tris(2-carboxyethyl)phosphine, derivatization with 1-benzyl-2-chloropyridinium bromide (BCPB) followed by field amplified sample injection stacking, capillary zone electrophoresis separation, and ultraviolet-absorbance detection of LA-BCPB derivative at 322 nm. Effective baseline electrophoretic separation was achieved within 6 min under the separation voltage of 20 kV (∼80 μA) using a standard fused-silica capillary (effective length 51.5 cm, 75 μm id) and BGE consisted of 0.05 mol/L borate buffer adjusted to pH 9. The experimentally determined limit of detection for LA in urine was 1.2 μmol/L. The calibration curve obtained for LA in urine showed linearity in the range 2.5-80 μmol/L, with R 2 0.9998. The relative standard deviation of the points of the calibration curve was lower than 10%. The analytical procedure was successfully applied to analysis of real urine samples from seven healthy volunteers who received single 100 mg dose of LA. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Functionalized-graphene modified graphite electrode for the selective determination of dopamine in presence of uric acid and ascorbic acid.

    Science.gov (United States)

    Mallesha, Malledevaru; Manjunatha, Revanasiddappa; Nethravathi, C; Suresh, Gurukar Shivappa; Rajamathi, Michael; Melo, Jose Savio; Venkatesha, Thimmappa Venkatarangaiah

    2011-06-01

    Graphene is chemically synthesized by solvothermal reduction of colloidal dispersions of graphite oxide. Graphite electrode is modified with functionalized-graphene for electrochemical applications. Electrochemical characterization of functionalized-graphene modified graphite electrode (FGGE) is carried out by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The behavior of FGGE towards ascorbic acid (AA), dopamine (DA) and uric acid (UA) has been investigated by CV, differential pulse voltammetry (DPV) and chronoamperommetry (CA). The FGGE showed excellent catalytic activity towards electrochemical oxidation of AA, DA and UA compared to that of the bare graphite electrode. The electrochemical oxidation signals of AA, DA and UA are well separated into three distinct peaks with peak potential separation of 193mv, 172mv and 264mV between AA-DA, DA-UA and AA-UA respectively in CV studies and the corresponding peak potential separations in DPV mode are 204mv, 141mv and 345mv. The FGGE is successfully used for the simultaneous detection of AA, DA and UA in their ternary mixture and DA in serum and pharmaceutical samples. The excellent electrocatalytic behavior of FGGE may lead to new applications in electrochemical analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Determination of proteins induced in response to jasmonic acid and salicylic acid in resistant and susceptible cultivars of tomato.

    Science.gov (United States)

    Afroz, Amber; Khan, Muhammad Rashid; Komatsu, Setsuko

    2010-07-01

    Jasmonic acid (JA) and salicylic acid (SA) are signaling molecules that play key roles in the regulation of metabolic processes, reproduction, and defense against pathogens. The proteomics approach was used to identify proteins that are induced by JA and SA in the tomato cultivars Roma and Pant Bahr, which are susceptible and resistant to bacterial wilt, respectively. Threonine deaminase and leucine amino peptidase were upregulated, and ribulose-1,5-bisphosphate carboxylase/oxygenase small chain was downregulated by time-course application of JA. Translationally controlled tumor protein was upregulated by time-course application of SA. Protein disulfide isomerase was upregulated by application of either JA or SA. Proteins related to defense, energy, and protein destination/storage are suspected to be responsible for the susceptibility or resistance of the cultivars. Furthermore, in Roma, iron ABC transporter was upregulated by JA and down-regulated by SA. Iron ABC transporter plays a part in the signal transduction of both JA and SA in cultivars of tomato that are resistant to bacterial wilt.

  3. Determination of homovanillic acid and vanillylmandelic acid in urine of autistic children by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Kałuzna-Czaplińska, Joanna; Socha, Ewa; Rynkowski, Jacek

    2010-09-01

    Studies suggest dopamine nervous systems are involved in the pathogenesis of autistic disorder. Quantification of urinary homovanillic acid (HVA) and vanillylmandelic acid (VMA) can be a very important tool in the study of disorders of dopamine metabolism in autistic children. The urine specimens were collected from 20 autistic children and 36 neurologically normal children. Urinary HVA and VMA were simultaneously analyzed by gas chromatography-mass spectrometry. The method involves extraction of HVA and VMA from urinary samples and derivatization to N,O-bis(trimethylsilyl)trifluoroacetamide derivatives. The detection limits are 0.15 microg/mL and 0.23 microg/mL for VMA and HVA, respectively. The levels of HVA and VMA were higher in the urine of autistic children (28.8+/-15.5 micromol/mmol creatinine and 22.2+/-13.0 micromol/mmol creatinine, respectively) compared with those of the generally healthy children (4.6+/-0.7 micromol/mmol creatinine for HVA and 3.8+/-0.6 micromol/mmol creatinine for VMA). We proposed a simple, rapid method for a routine analysis of human urine to detect HVA and VMA related to an abnormal functional imbalance of the dopamine system, and showed our experience of application of this method to patients with a diagnosis of autism spectrum disorders. These results suggest significant differences in the levels of HVA and VMA between autistic and healthy children.

  4. [Determination of residual solvents in 7-amino-3-chloro cephalosporanic acid by gas chromatography].

    Science.gov (United States)

    Ma, Li; Yao, Tong-wei

    2011-01-01

    To develop a gas chromatography method for determination of residual solvents in 7-amino-3-chloro cephalosporanic acid (7-ACCA). The residual levels of acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine and toluene in 7-ACCA were measured by gas chromatography using Agilent INNOWAX capillary column (30 m × 0.32 mm,0.5 μm). The initial column temperature was 70° maintained for 6 min and then raised (10°C/min) to 160°C for 1 min. Nitrogen gas was used as carrier and FID as detector. The flow of carrier was 1.0 ml/min, the temperature of injection port and detector was 200°C and 250°C, respectively. The limits of detection for acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine, toluene in 7-ACCA were 2.5 μg/ml, 1.5 μg/ml, 15 μg/ml, 2.5 μg/ml, 2.5 μg/ml, 2.5 μg/ml and 11 μg/ml, respectively. Only acetone was detected in the sample, and was less than the limits of Ch.P. The method can effectively detect the residual solvents in 7-ACCA.

  5. Determination of cobalt-60 in seawater by solvent extraction with pyrrolidinedithiocarbamic acid

    International Nuclear Information System (INIS)

    Tseng, C.L.; Lo, J.M.

    1978-01-01

    Cobalt-60 was extracted from a large volume of seawater and concentrated in a small volume of organic solution of pyrrolidinedithiocarbamic acid (HPDC) in chloroform. All foreign nuclides in the organic phase were stripped completely with 12N HCl and 2N HNO 3 successively. By this procedure, a chemically pure Co-60 chelate, 60 Co(PDC) 3 , in chloroform was obtained. The recovery of Co-60 activity was found to average 99%. Cobalt-60 in seawater can thus be simply, rapidly and accurately determined by direct NaI(Tl) scintillation counting. The time for a single analysis, for example, exclusive of the counting operation, is about 40 min. The effects of various foreign nuclides on the extraction of Co-60 were examined by the use of 42 radiotracers and the results are tabulated. The nuclides Ag + , Mn 2+ , Ni 2+ , Cu 2+ , Zn 2+ , Cd 2+ , Pb 2+ , Hg 2+ , Fe 3+ , Ga 3+ , In 3+ , As 3+ , Sn 4+ , and Cr 6+ were extracted almost completely into chloroform with cobalt as the pyrrolidinedithiocarbamates. The extraction yield of Sb 3+ was close to 90%. Appreciable fractions of Cs + , Ba 2+ , Cr 3+ , Zr 4+ and Np 5+ were also found in the organic phase. (T.I.)

  6. Determination of amino acid and protein peroxides by the xylenol orange-Fe(III) complex

    International Nuclear Information System (INIS)

    Collins, J.; Craig, G.; Gebicki, J.

    1996-01-01

    Oxidative stress imposed on living organisms is believed to lead to the depletion of their antioxidant defences, followed by chemical changes in the cell constituents. These may ultimately develop into pathological conditions such as cancer or cardiovascular disease. An assay of peroxides which could be applied to tissues or simple tissue extracts would prove extremely useful in the studies of the phenomenon of oxidative stress. With this purpose, the authors have tested the ability of two peroxide assay techniques to measure the formation of amino acid and protein peroxides in aqueous solutions irradiated with gamma rays, using a modification of the method based on the oxidation of Fe(II)) by peroxides and complexing of the Fe(III) produced by xylenol orange. The molar extinction coefficients of the peroxides tested were determined by comparison with the well-tested iodometric assay. This work was extended to the detection of all organic peroxides in human blood plasma or serum subjected to oxidative stress, where the iodometric assay proved difficult to apply and unreliable because of the binding of iodine to the blood components. Preliminary results suggest that exposure of serum to gamma radiation leads to immediate peroxidation of the proteins, with a delay before generation of lipid peroxides

  7. Simultaneous spectrophotometric determination of trimethoprim and sulphamethoxazole following charge-transfer complexation with chloranilic acid

    Directory of Open Access Journals (Sweden)

    Olajire A. Adegoke

    2017-05-01

    Full Text Available A simple, accurate and precise simultaneous spectrophotometric method has been developed for the analysis of trimethoprim–sulphamethoxazole combination in pure and tablet dosage forms. The method involves direct charge transfer complexation of trimethoprim (TMP with chloranilic acid (CAA in acetonitrile–dioxane solvent mixture and complexation of sulphamethoxazole (SMZ after its hydrolysis in dilute H2SO4. Optimization of temperature and time revealed the superiority of room temperature and 20 and 30 min respectively for TMP and SMZ. Optimal detector responses were obtained at 520 and 440 nm and were therefore selected as working wavelength maxima for SMZ and TMP respectively. TMP and hydrolysed SMZ were combined with CAA at mole ratios of 1:1 and 1:3 respectively. Accuracies were generally less than 4% (estimated as degree of inaccuracy or error with a precision of the order of less than 2% on a three-day assessment. Physicochemical factors responsible for complex stability were estimated and related to the observed data. The method was successfully applied to the determination of TMP and SMZ in tablet dosage forms with accuracies comparable to the official BP method. There were no interferences from common tablet excipients and TMP complex did not interfere with the assay of SMZ. The developed method could find application in routine quality control of TMP–SMZ combination. It is the first reported full simultaneous colorimetric assay of TMP and SMZ using the same analytical reagent.

  8. Applications of Tandem Mass Spectrometry in the Structure Determination of Permethylated Sialic Acid-containing Oligosaccharides

    International Nuclear Information System (INIS)

    Yoo, Eun Sun; Yoon, In Mo

    2005-01-01

    Sets of sialic acid-containing trisaccharides having different internal and terminal linkages have been synthesized to develop a sensitive method for analysis of the reducing terminal linkage positions. The trisaccharides, sialyl(α 2-3)Gal(β 1-3)GalNAc and sialyl(α 2-3)Gal(β 1-X)GlcNAc where X=3, 4 and 6, were synthesized and examined using electrospray ionization (ESI)-collision induced dissociation (CID) tandem mass spectrometry (MS/MS). The compounds chosen for this study are related to terminal groups likely to be found on polylactosamine-like glycoproteins and glycolipids which occur on the surface of mammalian cells. The purpose of this study is to develop tandem mass spectrometral methods to determine detailed carbohydrate structures on permethylated or partially methylated oligosaccharides for future applications on biologically active glycoconjugates and to exploit a faster method of synthesizing a series of structural isomeric oligosaccharides to be used for further mass spectrometry and instrumental analysis

  9. Determination of trifluoroacetic acid in 1996--1997 precipitation and surface waters in California and Nevada

    Energy Technology Data Exchange (ETDEWEB)

    Wujcik, C.E.; Cahill, T.M.; Seiber, J.N. [Univ. of Nevada, Reno, NV (United States)

    1999-05-15

    The atmospheric degradation of three chlorofluorocarbon (CFC) replacement compounds, namely HFC-134a, HCFC-123, and HCFC-124, results in the formation of trifluoroacetic acid (TFA). Concentrations of TFA were determined in precipitation and surface water samples collected in California and Nevada during 1996--1997. Terminal lake systems were found to have concentrations 4--13 times higher than their calculated yearly inputs, providing evidence for accumulation. The results support dry deposition as the primary contributor of TFA to surface waters in arid and semiarid environments. Precipitation samples obtained from three different locations contained 20.7--1530 ng/L with significantly higher concentrations in fogwater over rainwater. Elevated levels of TFA were observed for rainwater collected in Nevada over those collected in California, indicating continual uptake and concentration as clouds move from a semiarid to arid climate. Thus several mechanisms exist, including evaporative concentration, vapor-liquid phase partitioning, lowered washout volumes of atmospheric deposition water, and dry deposition, which may lead to elevated concentrations of TFA in atmospheric and surface waters above levels expected from usual rainfall washout.

  10. 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

  11. 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

  12. Determination of Dornic acidity as a method to select donor milk in a milk bank.

    Science.gov (United States)

    Vázquez-Román, Sara; Garcia-Lara, Nadia Raquel; Escuder-Vieco, Diana; Chaves-Sánchez, Fernando; De la Cruz-Bertolo, Javier; Pallas-Alonso, Carmen Rosa

    2013-02-01

    Dornic acidity may be an indirect measurement of milk's bacteria content and its quality. There are no uniform criteria among different human milk banks on milk acceptance criteria. The main aim of this study is to report the correlation between Dornic acidity and bacterial growth in donor milk in order to validate the Dornic acidity value as an adequate method to select milk prior to its pasteurization. From 105 pools, 4-mL samples of human milk were collected. Dornic acidity measurement and culture in blood and McConkey's agar cultures were performed. Based on Dornic acidity degrees, we classified milk into three quality categories: top quality (acidity pasteurize in a human milk bank based in quality and safety criteria.

  13. Gender and oral contraceptive steroids as determinants of drug glucuronidation: effects on clofibric acid elimination.

    OpenAIRE

    Miners, J O; Robson, R A; Birkett, D J

    1984-01-01

    The disposition of clofibric acid, a drug metabolised largely by glucuronidation, was studied in eight males, eight females and eight females receiving oral contraceptive steroids (OCS). Clofibric acid plasma clearance was not significantly different in males compared to the control female group but was 48% greater (P less than 0.01) in women receiving OCS compared to non-pill using females. This difference was due to an alteration in clofibric acid metabolic clearance as there were no differ...

  14. 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.

  15. Eicosapentaenoic acid and docosahexaenoic acid have distinct membrane locations and lipid interactions as determined by X-ray diffraction.

    Science.gov (United States)

    Sherratt, Samuel C R; Mason, R Preston

    2018-01-31

    Eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) differentially influence lipid oxidation, signal transduction, fluidity, and cholesterol domain formation, potentially due in part to distinct membrane interactions. We used small angle X-ray diffraction to evaluate the EPA and DHA effects on membrane structure. Membrane vesicles composed of 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine (POPC) and cholesterol (C) (0.3C:POPC mole ratio) were prepared and treated with vehicle, EPA, or DHA (1:10 mol ratio to POPC). Electron density profiles generated from the diffraction data showed that EPA increased membrane hydrocarbon core electron density over a broad area, up to ± 20 Å from the membrane center, indicating an energetically favorable extended orientation for EPA likely stabilized by van der Waals interactions. By contrast, DHA increased electron density in the phospholipid head group region starting at ± 12 Å from the membrane center, presumably due to DHA-surface interactions, with coincident reduction in electron density in the membrane hydrocarbon core centered ± 7-9 Å from the membrane center. The membrane width (d-space) decreased by 5 Å in the presence of vehicle as the temperature increased from 10 °C to 30 °C due to increased acyl chain trans-gauche isomerizations, which was unaffected by addition of EPA or DHA. The influence of DHA on membrane structure was modulated by temperature changes while the interactions of EPA were unaffected. The contrasting EPA and DHA effects on membrane structure indicate distinct molecular locations and orientations that may contribute to observed differences in biological activity. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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.

  1. 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.

  2. 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)

  3. 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.

  4. Determination of fusaric acid in maize using molecularly imprinted SPE clean-up

    Science.gov (United States)

    A new liquid chromatography method to detect fusaric acid in maize is reported based on molecularly imprinted polymer solid phase extraction clean-up (MISPE) using mimic-templated molecularly-imprinted polymers. Picolinic acid was used as a toxin analog for imprinting polymers during a thermolytic s...

  5. Genetic determinism of oil acidity among some DELI oil palm (Elaeis ...

    African Journals Online (AJOL)

    USER

    2016-08-24

    Aug 24, 2016 ... Key words: Elaeis guineensis Jacq., free fatty acid content, crude palm oil, inheritance. INTRODUCTION. The oil palm (Elaeis ... of world's production of vegetable oils. The highest palm oil producing countries ... Without prior refining, acidic palm oil is improper for human consumption (Anonymous, 2005).

  6. 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

  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. Chromatographic determination of silicon and phosphorus as molybdic heteropoly acids with preconcentration

    International Nuclear Information System (INIS)

    Tikhomirova, T.I.; Krokhin, O.V.; Dubovik, D.B.; Ivanov, A.V.; Shpigun, O.A.

    2002-01-01

    Chromatographic behaviour of silicon and phosphorus as molybdic heteropoly acids with preconcentration as ion associations of heteropoly acid with tributylammonium bromide was studied. The technique of simultaneous analysis of silicon and phosphorus was developed. During investigation into the effect of acetonitril content in the probe on the form of chromatographic peak of molybdosilicic acid the negative influence of acetonitril on the form of peak was ascertained. This effect may be eliminated by the lowering of acetonitril content up to 50 %. It was found that under these conditions the chromatographic peak practically was absent, because of the heteropoly acid of the Mo(VI) abundance transformed in the MoO 2 2+ cation form without reaction with tributylammonium cation during concentration of heteropoly acid [ru

  9. 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.

  10. 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....

  11. 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

  12. Valproic acid treatment response in vitro is determined by TP53 status in medulloblastoma.

    Science.gov (United States)

    Mascaro-Cordeiro, Bruna; Oliveira, Indhira Dias; Tesser-Gamba, Francine; Pavon, Lorena Favaro; Saba-Silva, Nasjla; Cavalheiro, Sergio; Dastoli, Patrícia; Toledo, Silvia Regina Caminada

    2018-05-22

    Histone deacetylate inhibitors (HDACi), as valproic acid (VA), have been reported to enhance efficacy and to prevent drug resistance in some tumors, including medulloblastoma (MB). In the present study, we investigated VA role, combined to cisplatin (CDDP) in cell viability and gene expression of MB cell lines. Dose-response curve determined IC 50 values for each treatment: (1) VA single, (2) CDDP single, and (3) VA and CDDP combined. Cytotoxicity and flow cytometry evaluated cell viability after exposure to treatments. Quantitative PCR evaluated gene expression levels of AKT, CTNNB1, GLI1, KDM6A, KDM6B, NOTCH2, PTCH1, and TERT, before and after treatment. Besides, we performed next-generation sequencing (NGS) for PTCH1, TERT, and TP53 genes. The most effective treatment to reduce viability was combined for D283MED and ONS-76; and CDDP single for DAOY cells (p AKT genes were overexpressed after treatments with VA. D283MED and ONS-76 cells presented variants in TERT and PTCH1, respectively and DAOY cell line presented a TP53 mutation. MB tumors belonging to SHH molecular subgroup, with TP53 MUT , would be the ones that present high risk in relation to VA use during the treatment, while TP53 WT MBs can benefit from VA therapy, both SHH and groups 3 and 4. Our study shows a new perspective about VA action in medulloblastoma cells, raising the possibility that VA may act in different patterns. According to the genetic background of MB cell, VA can stimulate cell cycle arrest and apoptosis or induce resistance to treatment via signaling pathways activation.

  13. 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,

  14. 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

  15. 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

  16. 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

  17. Optimized Analytical Method to Determine Gallic and Picric Acids in Pyrotechnic Samples by Using HPLC/UV (Reverse Phase)

    International Nuclear Information System (INIS)

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

    2013-01-01

    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)

  18. Determining a Robust D-Optimal Design for Testing for Departure from Additivity in a Mixture of Four Perfluoroalkyl Acids.

    Science.gov (United States)

    Our objective is to determine an optimal experimental design for a mixture of perfluoroalkyl acids (PFAAs) that is robust to the assumption of additivity. PFAAs are widely used in consumer products and industrial applications. The presence and persistence of PFAAs, especially in ...

  19. 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).

  20. Determination of major boswellic acids in plasma by high-pressure liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Gerbeth, Kathleen; Meins, Juergen; Kirste, Simon; Momm, Felix; Schubert-Zsilavecz, Manfred; Abdel-Tawab, Mona

    2011-12-15

    Until now, dexamethasone is the medication of choice to reduce peritumoral edema associated with primary and secondary brain tumors. Because of the severe side effects accompanying such a treatment the interest in alternative agents that may be co-administered with glucocorticoids and help to reduce the required dose is constantly increasing. Boswellia serrata gum resin extracts (BSE), which have been designated an orphan drug status by the European Medicines Agency (EMA) in 2002 for the treatment of peritumoral edema, may represent a promising supplemental herbal remedy. However, clinical studies on the effect of BSE on brain edema as well as analyzes of serum levels are very scarce. Based on that background a prospective, placebo controlled, and double blind clinical pilot trial was conducted on 14 patients applying for the first time a high dose of 4200 mg BSE per day and 13 patients receiving placebo. For monitoring the serum levels of all major boswellic acids (BAs) a highly sensitive HPLC-MS method has been developed that allows the determination of KBA and AKBA from 5.0 ng/ml to 3000 ng/ml and of αBA, βBA, AαBA and AβBA from 0.5 ng/ml to 12,000 ng/ml. It is the first validated method that covers such a wide concentration range, which makes it suitable to be used as standard method in clinical trials as it compensates for the great pharmacokinetic variability in the plasma levels of BAs observed in clinical practice. Average steady concentrations (ng/ml) in the range of 6.4-247.5 for KBA, 0-15.5 for AKBA, 36.7-4830.1 for αBA, 87.0-11948.5 for βBA, 73.4-2985.8 for AαBA and 131.4-6131.3 for AβBA were determined in the verum group. The here quantified steady state levels suggest βBA to be a possible candidate for the anti-inflammatory and anti-edemateous effects of BSE. In general, the serum level analysis underlines the promising clinical results of BSE on cerebral edema. Copyright © 2011 Elsevier B.V. All rights reserved.