WorldWideScience

Sample records for alpha spectrometric determination

  1. Improved analytical procedure for the determination of 210Pb and 210Po using alpha-spectrometric isotope dilution

    International Nuclear Information System (INIS)

    Urnezis, P.W.; Holtzman, R.B.

    1981-01-01

    An isotope dilution method has been incorporated into the 210 Pb- 210 Po analysis. A known amount of 209 Po is added to the sample before analysis. Then both 209 Po and 210 Po are deposited on a silver planchet which is assayed in an alpha spectrometer to determine the activities of each isotope. The recoveries generally range from 70% to 90%

  2. Spectrometric determination of ammonium-nitrogen with quinol in ...

    African Journals Online (AJOL)

    Quinol is proposed as a reagent for the spectrometric determination of ammonium-nitrogen (NH4+-N) in aqueous medium. Quinol forms a pink complex with ammonium salt in aqueous medium. Hydrogen peroxide is needed for colour accentuation. The quinol/ammonium charge transfer complex has absorption maximum ...

  3. Partial least squares−near infrared spectrometric determination of ...

    African Journals Online (AJOL)

    Partial least squares−near infrared spectrometric determination of ethanol in distilled alcoholic beverages. ... Derivative, mean centering and subtracting minimum value were used as data treatment techniques for noise reduction and baseline correction. Mean centering has given the best partial least squares model with ...

  4. Graphite furnace atomic absorption spectrometric determination of ...

    African Journals Online (AJOL)

    A method for the determination of trace amount of cadmium ion after preconcentration by extracting its dithizone complex into molten naphthalene was developed. Several experimental conditions such as pH of the solution, stirring time, the amounts of naphthalene, standing time and volume of the solution were optimized.

  5. Photometric and emission-spectrometric determination of boron in steels

    International Nuclear Information System (INIS)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated. (orig.) [de

  6. Photometric and emission-spectrometric determination of boron in steels

    Energy Technology Data Exchange (ETDEWEB)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated.

  7. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal...... of calibration samples, including complex formation and the mass spectrometric methodology, is described and discussed....

  8. Determination of iodine to compliment mass spectrometric measurements

    International Nuclear Information System (INIS)

    Hohorst, F.A.

    1994-11-01

    The dose of iodine-129 to facility personnel and the general public as a result of past, present, and future activities at DOE sites is of continuing interest, WINCO received about 160 samples annually in a variety of natural matrices, including snow, milk, thyroid tissue, and sagebrush, in which iodine-129 is determined in order to evaluate this dose, Currently, total iodine and the isotopic ratio of iodine-127 to iodine-129 are determined by mass spectrometry. These two measurements determine the concentration of iodine-129 in each sample, These measurements require at least 16 h of mass spectrometer operator time for each sample. A variety of methods are available which concentrate and determine small quantities of iodine. Although useful, these approaches would increase both time and cost. The objective of this effort was to determine total iodine by an alternative method in order to decrease the load on mass spectrometry by 25 to 50%. The preparation of each sample for mass spectrometric analysis involves a common step--collection of iodide on an ion exchange bed. This was the focal point of the effort since the results would be applicable to all samples

  9. Atomic absorption spectrometric determination of mineral elements in mammalian bones

    International Nuclear Information System (INIS)

    Udoh, Anthony P.

    2000-01-01

    The phosphorus content of the major bones of male and female selected mammals was determined using the yellow vanadomolybdate colorimetric method. For each animal, the bone with the highest phosphorus content was used as pilot sample. Varying concentrations of strontium were added to solutions of the ashed pilot samples to minimize phosphorus interference in the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 6,000 ppm (0.6%) of strontium was required to give optimum results for calcium. The amount of magnesium obtained from the analysis was not affected by the addition of strontium. With the incorporation of strontium in the sample solution, all elements of interest can be determined in the same sample solution. Based on this, a procedure is proposed for the determination of calcium and other elements in bones. Average recoveries of spiked calcium and magnesium were 97.85% and 98.16%, respectively at the 95% confidence level. The coefficients of variation obtained for replicate determinations using one of the samples were 0.00% for calcium, lead and sodium, 2.93% for magnesium, 3.27% for iron and 3.92% for zinc at the concentration levels found in that sample. Results from the proposed procedure compared well with those from classical chemical methods at the 95% confidence level. It is evident that calcium phosphorus, magnesium and sodium which are the most abundant elements in the bones are distributed in varying amounts both in the different types of bones and different animal species, although the general trend is Ca > P > Na > Mg for each bone considered. The calcium - phosphorus ratio is generally 3:1. The work set out to propose an atomic absorption spectrometric method for the multi-element analysis of mammalian bones with a single sample preparation and to study the distribution pattern of these elements in the bones. (Author)

  10. The determination of $\\alpha_s$ by the ALPHA collaboration

    CERN Document Server

    Bruno, Mattia

    2016-01-01

    We review the ALPHA collaboration strategy for obtaining the QCD coupling at high scale. In the three-flavor effective theory it avoids the use of perturbation theory at $\\alpha > 0.2$ and at the same time has the physical scales small compared to the cutoff $1/a$ in all stages of the computation. The result $\\Lambda_\\overline{MS}^{(3)}=332(14)$~MeV is translated to $\\alpha_\\overline{MS}(m_Z)=0.1179(10)(2)$ by use of (high order) perturbative relations between the effective theory couplings at the charm and beauty quark "thresholds". The error of this perturbative step is discussed and estimated as $0.0002$.

  11. Determination of uranium enrichment by using gamma-spectrometric methods

    International Nuclear Information System (INIS)

    Kutnyj, D.V.; Telegin, Yu.N.; Odejchuk, N.P.; Mikhailov, V.A.; Tovkanets, V.E.

    2009-01-01

    By using commercial analysis programs MGAU (LLNL, USA) and FRAM (LANL, USA) the summary error of gamma-spectrometric uranium enrichment measurements was investigated. Uranium samples with enrichments of 0,71; 4,46 and 20,1 % were measured. The coaxial high purity germanium detector (type GC) and the planar germanium detector (type LEGe) were used as gamma-radiation detectors. It was shown that experimental equipment and mathematical software available in NSC KIPT allow us to measure uranium enrichment by nondestructive method with accuracy of not worse than 2%.

  12. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    International Nuclear Information System (INIS)

    Doyle, Adriana; Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N.; Aucélio, Ricardo Q.

    2013-01-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated

  13. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    Energy Technology Data Exchange (ETDEWEB)

    Doyle, Adriana [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil); Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N. [Leopoldo Américo Miguez de Mello Research Center — Petrobras (CENPES), Cidade Universitária, Quadra 7, Ilha do Fundão, Rio de Janeiro 21949-900 (Brazil); Aucélio, Ricardo Q., E-mail: aucelior@puc-rio.br [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil)

    2013-08-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated.

  14. Application of isotopic dillution techniques by alpha and mass spechometry for determining uranium and evaluated its distributIon in geological materials

    International Nuclear Information System (INIS)

    Shihomatsu, H.M.

    1987-01-01

    Determination of uranium in the concentration range of 2 to 4000 ppm in nuclear raw materials by mass spectrometric (MSID) and alpha spectrometric isotope dilution techniques (ASID), using the isotope tracer enriched in 233 U, is presented. An investigation on the nature of the thermoionic emission in various types of filament arrangements like, single plane rhenium, single boat and double, are carried out for the isotope analysis by mass spectrometry. In the preparation of the sources for alpha spectrometry by electrodeposition the experimental parameters such as: current density, pH of the mixed solution containing sample and electrolyte, concentration of the electrolyte solution, time of deposition and distance between electrodes are optimised. The accuracy of the technique is discussed based on the determination of uranium in the same samples by other research workers employing various analytical techniques including mass spectrometric and alpha spectrometric isotope dilution techniques (MSID and ASID). (author) [pt

  15. Studying of isotope structure of uranium by alpha-spectrometric method

    International Nuclear Information System (INIS)

    Sattarov, G.S.; Muzafarov, A.M.; Petukhov, O.F.; Petrenko, V.Z.

    2004-01-01

    Full text: The knowledge of isotope structure of uranium in waters, in minerals and in finished goods gives the helpful information on the radiation and nuclear-physical processes occurring in natural environments. Besides, customers put a question before uranium producing enterprises on the control of limiting concentration of an isotope 234 U in finished goods (uranium protoxide-oxide). For these reasons studying and development of techniques of definition of isotope structure of uranium is an actual task. In this connection for researches alpha - spectrometers 'PROGRESS-ALPHA' produced by R and D 'DOZE' Russia and firms 'Canberra' the USA were used. The isotope structure of uranium ( 234 U, 235 U, 238 U) was determined on a known ratio 234 U/ 238 U, which is equal to 53,41micrograms/gram. Identification of isotopes carried out by 4198 keV ( 235 U), 4395 keV ( 234 U) and 4773 keV ( 238 U). The technique of radiochemical preparation of samples to the analysis included: clearing of organic chemistry and preventing natural isotopes; drawing by a method electrolytic sedimentation on a metal substrate (d=24mm) an active stain, the area 4,5 cm 2 , with isotropy distribution of ions 234 U, 235 U, 238 U. As standards, the international and All-Russian standards with known contents 234 U were used. The isotope structure of uranium in uranium protoxide-oxide, chemical concentrates, technological solutions is determined. Infringements of isotope balance 234 U/ 238 U on separate sites of fulfilled uranium deposits and in technological products are found out

  16. Determination of pyrethroid pesticide residues in processed fruits and vegetables by gas chromatography with electron capture and mass spectrometric detection.

    Science.gov (United States)

    Sannino, Anna; Bandini, Mirella; Bolzoni, Luciana

    2003-01-01

    A gas chromatographic method was developed for the simultaneous determination of 12 pyrethroids (tefluthrin, bifenthrin, fenpropathrin, cyhalothrin, permethrin, cyfluthrin, cypermethrin, alpha-cypermethrin, flucythrinate, fenvalerate, fluvalinate, and deltamethrin) in tomato puree, peach nectar, orange juice, and canned peas. A miniaturized extraction-partition procedure requiring small amounts of nonchlorinated solvents is used. Samples are extracted with acetone, partitioned with ethyl acetate-cyclohexane (50 + 50, v/v), and cleaned up on a Florisil cartridge. The final extract is analyzed by gas chromatography with both electron capture and mass spectrometric detection modes. Studies at fortification levels of 0.010-0.100 mg/kg gave mean recoveries ranging from 70.2 to 96.0% and coefficients of variation between 4.0 and 13.9% for all compounds. Quantitation limits were < 0.010 mg/kg for electron capture detection.

  17. [Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

    Science.gov (United States)

    Zhong, L X; Ding, B M; Jiang, D; Liu, D Y; Yu, B; Zhu, B L; Ding, L

    2016-05-20

    To establish a method to determine cobalt in human urine by graphite furnace atomic absorption spectrometry. Urine with 2% nitric acid diluted two-fold, to quantify the curve, graphite furnace atomic absorption spectrometric detection. Co was linear within 2.5~40.0 ng/ml with r>0.999. Spike experiment showed that Co received good recovery rate, which was 90.8%~94.8%. Intra-assay precisions were 3.2%~5.1% for Co, inter-assay precisions were 4.4%~5.2% for Co. The method by using graphite furnace atomic absorption spectrometr to determine urine Co was fast, accurate and with low matrix effect. It could meet the requirement in GBZ/T 210.5-2008.

  18. New miniaturized alpha/beta spectrometric system for the surface contamination monitoring and radon personal dosimeter

    International Nuclear Information System (INIS)

    Streil, T.; Oeser, V.; Holfeld, G.

    1998-01-01

    The heart of the new miniaturized alpha/beta spectroscopic system is a Smart Card MCA having a 12 bit resolution and a 32 bit memory for each channel with the size of a cheque card. The system consists of a single or up to 12 alpha spectrometers in a battery powered casing with connectors for direct detector/amplifier module plugging. Surface contamination in the order of 1 Bq/cm 2 of 239 Pu can be measured. (M.D.)

  19. Uranium determination using atomic spectrometric techniques: An overview

    International Nuclear Information System (INIS)

    Santos, Juracir S.; Teixeira, Leonardo S.G.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Godoy, Jose M.; Ferreira, Sergio L.C.

    2010-01-01

    This review focuses on the determination of uranium using spectroanalytical techniques that are aimed at total determination such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), inductively coupled plasma optical emission spectrometry (ICP-OES); and inductively coupled plasma mass spectrometry (ICP-MS) that also enables the determination of uranium isotopes. The advantages and shortcomings related to interferences, precision, accuracy, sample type and equipment employed in the analysis are taken into account, as well as the complexity and costs (i.e., acquisition, operation and maintenance) associated with each of the techniques. Strategies to improve their performance that employ separation and/or preconcentration steps are considered, with an emphasis given to solid-phase extraction because of its advantages compared to other preconcentration procedures.

  20. Gamma spectrometric determination of depleted Uranium in Yugoslavia

    International Nuclear Information System (INIS)

    Pantelic, G.; Eremic Savkovic, M.; Javorina, L.; Tanaskovic, I.; Vuletic, V.; Milacic, S.

    2002-01-01

    The radiation protection is very important interdisciplinary research field due to the presence of the radiation in daily life. The systematic examination of radioactive contamination of various environmental samples was established forty years ago in the Institute of Occupational and Radiological Health Dr Dragomir Karajovic for the sake of preventive protection of population and environment from the harmful effect of ionizing radiation. The global sources of radionuclide contamination in our country are the fallout due to previous nuclear testing and the deposition of radionuclides from the region of Chernobyl accident. The contents of radionuclides were determined in aerosol, soil, fallout (wet and dry deposition), rivers, lakes, drinking water, human and animal food. The samples were collected in several locations of the Republic of Serbia and in regular time intervals, according to methods determined by the regulation. The regulations and the monitoring programs were updated after the Chernobyl accident. In the recent time, after the NATO aggression, we analyzed depleted uranium content in the environmental samples. We used high-resolution gamma spectrometry measurements, because of their simplicity and accuracy. Aims of the control were to asses the increase of radioactivity above the natural levels in the immediate and near vicinity of the bomb craters, to asses the corresponding effect of changed natural radioactivity on the health of the population living in these places and finding unexploded depleted uranium bullets

  1. ALPHA SPECTROMETRIC EVALUATION OF SRM-995 AS A POTENTIAL URANIUM/THORIUM DOUBLE TRACER SYSTEM FOR AGE-DATING URANIUM MATERIALS

    Energy Technology Data Exchange (ETDEWEB)

    Beals, D.

    2011-12-06

    Uranium-233 (t{sub 1/2} {approx} 1.59E5 years) is an artificial, fissile isotope of uranium that has significant importance in nuclear forensics. The isotope provides a unique signature in determining the origin and provenance of uranium-bearing materials and is valuable as a mass spectrometric tracer. Alpha spectrometry was employed in the critical evaluation of a {sup 233}U standard reference material (SRM-995) as a dual tracer system based on the in-growth of {sup 229}Th (t{sub 1/2} {approx} 7.34E3 years) for {approx}35 years following radiochemical purification. Preliminary investigations focused on the isotopic analysis of standards and unmodified fractions of SRM-995; all samples were separated and purified using a multi-column anion-exchange scheme. The {sup 229}Th/{sup 233}U atom ratio for SRM-995 was found to be 1.598E-4 ({+-} 4.50%) using recovery-corrected radiochemical methods. Using the Bateman equations and relevant half-lives, this ratio reflects a material that was purified {approx} 36.8 years prior to this analysis. The calculated age is discussed in contrast with both the date of certification and the recorded date of last purification.

  2. Gamma Spectrometric Determination of U, Th, K and Some Geochemical Applications

    International Nuclear Information System (INIS)

    Dodona, A.; Tashko, A.

    2001-01-01

    The application of 'in situ' gamma-spectrometric method (''infinite'' environment), made possible the simultanious determination of U, Th and K. 4 channel gamma-spectrometric analyser with NaI(TI) scintilation counter crystal detector (103 cm 3 φ=50x50mm) was used to determin U, Th(more than 1-2 ppm) and K (more than 1%) in laboratory conditions. The detector was inserted into a lead camera and calibrated for measurement geometry with vessel of ''Marineli'' type of a 17o cm 3 volume. The study of main factors, which influence in the gamma spectrometric measurements, (the technical, physical, geometrical and time parameters) has been carried out. International standards of U, Th, K and internal monitoring standard samples are used for the calibration. External analytical control has been realized by other radiometric and chemical methods. The detection limits ( 1 ppm Th, 2ppm U and 1% K) and the relative errors (17-20% for 1-10 ppm U, Th and 10-15% for more than 10 ppm U, Th and more than 1% K) guarantee a quantitative analysis that may be used successfully in the geochemical studies. Some geochemical applications, based on the content of Th, U and Th/U ratio in rocks samples that we have we have analyzed with this method, are shown in this paper. U, Th and their ratio are used as trace elements to indicate the differences between the acidic magmatic rocks of Albania (Th/U ratio=2-6 and>10). The bimodal character of Th/U scattering in ignimbrides and monzonites (Korabi zone) shows that in addition to the ''normal'' rocks, there are also some ones enriched with Th, So, the differential analysis of Th, U, and K may be used as geochemical exploration criteria for the radioactive and non-radioactive mineralization, such as REE (Rare Earth Elements), phospghorites, bauxites, placers etc. (authors)

  3. Fully Automated Spectrometric Protocols for Determination of Antioxidant Activity: Advantages and Disadvantages

    Directory of Open Access Journals (Sweden)

    Marketa Ryvolova

    2010-11-01

    Full Text Available The aim of this study was to describe behaviour, kinetics, time courses and limitations of the six different fully automated spectrometric methods - DPPH, TEAC, FRAP, DMPD, Free Radicals and Blue CrO5. Absorption curves were measured and absorbance maxima were found. All methods were calibrated using the standard compounds Trolox® and/or gallic acid. Calibration curves were determined (relative standard deviation was within the range from 1.5 to 2.5 %. The obtained characteristics were compared and discussed. Moreover, the data obtained were applied to optimize and to automate all mentioned protocols. Automatic analyzer allowed us to analyse simultaneously larger set of samples, to decrease the measurement time, to eliminate the errors and to provide data of higher quality in comparison to manual analysis. The total time of analysis for one sample was decreased to 10 min for all six methods. In contrary, the total time of manual spectrometric determination was approximately 120 min. The obtained data provided good correlations between studied methods (R = 0.97 – 0.99.

  4. Determination of plutonium-241 half-life by mass spectrometric measurement

    International Nuclear Information System (INIS)

    Hiyama, Takashi; Wada, Yukio; Onishi, Koichi

    1982-01-01

    Much data for Pu-241 half-life have been reported, but these values range from 13.8 years to 15.1 years depending on investigators. In order to define the half-life of Pu-241, the half-life was calculated by analyzing the mass spectrometry data obtained in the author's laboratory over the past six years on Plutonium Isotopic Standard Reference Materials prepared at the National Bureau of Standards (NBS). The sample used for this work consisted of SRM-947 and SRM-948 prepared at NBS. Before mass spectrometric analysis, the plutonium aliquot was separated from its Am-241 daughter by anion exchange chromatography, since Am-241 is not distinguished from Pu-241 in the mass spectrometer. 241 Pu/ 239 Pu and 241 Pu/ 240 Pu ratios were calculated from the values of mass spectrometric measurement. From the relation of log N to time, the half-life of Pu-241 was determined, based on the slope using a least squares fit. The half-life of Pu-241 was estimated to be 14.29+-0.15 years. (Yoshitake, I.)

  5. Determination of alpha radionuclides in fish

    International Nuclear Information System (INIS)

    Pernicka, L.; Matel, L.; Rosskopfova, O.

    2001-01-01

    In atmospheric water, external water and undercurrent the occurrence of radionuclides is usual. It is an important factor of quality of the environment. Plants ingest radionuclides from water and with they everyone. And it arises radioactivity infest food-chain. Radiotoxicity of this radionuclides is very deer sometimes. The sensitive radiochemical procedures for their determination are necessarily important. The poster presents the combined procedure used at our laboratory for determination of alpha radionuclides in biological samples. (authors)

  6. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  7. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    International Nuclear Information System (INIS)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H.

    2005-12-01

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here

  8. Determination of isotope fractionation effect using a double spike (242Pu+240Pu) during the mass spectrometric analysis of plutonium

    International Nuclear Information System (INIS)

    Chitambar, S.A.; Parab, A.R.; Khodade, P.S.; Jain, H.C.

    1986-01-01

    Isotope fractionation effect during the mass spectrometric analysis of plutonium has been investigated using a double spike ( 242 Pu+ 240 Pu) and the determination of concentration of plutonium in dissolver solution of irradiated fuel is reported. (author). 6 refs., 2 tables

  9. Electrospray ionization mass spectrometric analysis of newly synthesized alpha,beta-unsaturated gamma-lactones fused to sugars.

    Science.gov (United States)

    Madeira, Paulo J Amorim; Rosa, Ana Margarida; Xavier, Nuno M; Rauter, Amélia P; Florêncio, M Helena

    2010-04-15

    Knowledge of the fragmentation mechanisms of lactones and their behaviour under electrospray ionization (ESI) conditions can be extended to larger and more complex natural products that contain an alpha,beta-unsaturated gamma-lactone moiety in their structure. Moreover, little is known about the gas-phase behaviour of alpha,beta-unsaturated gamma-lactones linked or fused to sugars. Therefore, five alpha,beta-unsaturated gamma-lactones (butenolides) fused to a pyranose ring, recently synthesized compounds with potential relevance regarding their biological properties, were investigated using ESI-MS and ESI-MS/MS in both positive and negative ion modes. Their fragmentation mechanisms and product ion structures were compared. It was observed that two isomers could be unambiguously distinguished in the negative ion mode by the fragmentation pathways of their deprotonated molecules as well as in the positive ion mode by the fragmentation pathways of either the protonated or the sodiated molecule. Fragmentation mechanisms are proposed taking into account the MS/MS data and semi-empirical calculations using the PM6 Hamiltonean. The semi-empirical calculations were also very useful in determining the most probable protonation and cationization sites. 2010 John Wiley & Sons, Ltd.

  10. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements

    DEFF Research Database (Denmark)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin

    2014-01-01

    This paper reports an analytical method for the determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation......, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference...... counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5×105 for 20 g soil compared to the level reported in the literature...

  11. Review of procedures involving separation and preconcentration for the determination of cadmium using spectrometric techniques

    International Nuclear Information System (INIS)

    Ferreira, Sergio L.C.; Andrade, Jailson B. de; Korn, Maria das Gracas A.; Pereira, Madson de G.; Lemos, Valfredo A.; Santos, Walter N.L. dos; Rodrigues, Frederico de Medeiros; Souza, Anderson S.; Ferreira, Hadla S.; Silva, Erik G.P. da

    2007-01-01

    Spectrometric techniques for the analysis of trace cadmium have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, such as electrochemical deposition, precipitation, coprecipitation, solid phase extraction, liquid-liquid extraction (LLE) and cloud point extraction (CPE), and consider the features of the their application with several spectrometric techniques

  12. Precise timing of the last interglacial period from mass spectrometric determination of thorium-230 in corals

    Science.gov (United States)

    Chen, J. H.; Wasserburg, G. J.; Ku, T.-L.; Edwards, R. Lawrence

    1987-01-01

    The development of mass spectrometric techniques for determination of Th-230 abundance has made it possible to reduce analytical errors in (U-238)-(U-234)-(Th-230) dating of corals even with very small samples. Samples of 6 x 10 to the 8th atoms of Th-230 can be measured to an accuracy of + or - 3 percent (2sigma), and 3 x 10 to the 10th atoms of Th-230 can be measured to an accuracy of + or - 0.2 percent. The time range over which useful age data on corals can be obtained now ranges from about 50 to about 500,000 years. For young corals, this approach may be preferable to C-14 dating. The precision with which the age of a coral can now be determined should make it possible to critically test the Milankovitch hypothesis concerning Pleistocene climate fluctuations. Analyses of a number of corals that grew during the last interglacial period yield ages of 122,000 to 130,000 years. The ages coincide with, or slightly post-date, the summer solar insolation high at 65 deg N latitude which occurred 128,000 years ago. This supports the idea that changes in Pleistocene climate can be the result of variations in the distribution of solar insolation caused by changes in the geometry of the earth's orbit and rotation axis.

  13. Determination of platinum originated from antitumoral drugs in human urine by atomic absorption spectrometric methods.

    Science.gov (United States)

    da Costa, Anilton Coelho; Vieira, Mariana Antunes; Luna, Aderval Severino; de Campos, Reinaldo Calixto

    2010-10-15

    Cisplatin and carboplatin are the most common platinum-based drugs used in cancer treatment. Pharmacokinetic investigations, the evaluation of the body burden during the treatment, as well as baseline levels of platinum in humans have attracted great interest. Thus, accurate analytical methods for fast and easy Pt monitoring in clinical samples become necessary. In the present study atomic absorption spectrometric methods for the determination of platinum in the forms of cisplatin and carboplatin in human urine were investigated. Platinum, in these different forms, could be determined in urine, after simple sample dilution. Regarding electrothermal atomic absorption spectrometry, the optimum parameters were defined by a central composite design optimization. Multiplicative matrix effects were overcome by using a mixture of HCl and NaCl as modifier. The limit of detection (LOD) was 0.004 mgL(-1) of platinum in the original sample. For the analysis of more concentrated samples, high resolution continuous source flame atomic absorption spectrometry was also investigated. Flame conditions were optimized by a multivariate D-optimal design, using as response the sum of the analyte addition calibration slopes and their standard deviations. Matrix matched external calibration with PtCl(2) calibration solutions, was possible, and the LOD was 0.06 mgL(-1) in the original sample. The results obtained by the proposed procedures were also in good agreement with those obtained by an independent comparative procedure. Copyright © 2010 Elsevier B.V. All rights reserved.

  14. Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples.

    Science.gov (United States)

    Taher, Mohammad Ali; Pourmohammad, Fatemeh; Fazelirad, Hamid

    2015-12-01

    In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra-trace amounts of rhodium after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015-0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Determination of ractopamine in pig hair using liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Wu, Junlin; Liu, Xiaoyun; Peng, Yunping

    2014-01-01

    A quantitative analytical procedure for the determination of ractopamine in pig hair has been developed and validated. The hair samples were washed and incubated at 75°C with isoxuprine and hair extraction buffer. The drug present was quantified using mixed solid-phase extraction and liquid chromatography with tandem mass spectrometric detection. The limit of quantization (LOQ) was 10pg/mg and the intra-day precision at 25pg/mg and 750pg/mg was 0.49% and 2.8% respectively. Inter-day precision was 0.88% and 3.52% at the same concentrations. The hair extraction percentage recovery at 25pg/mg and 50ng/mL was 99.47% and 103.83% respectively. The extraction percentage recovery at 25pg/mg and 50ng/mg was 93.52% and 100.26% respectively. Our results showed that ractopamine residues persist in hair in 24days of withdrawal and also showed the possibility to test ractopamine from pig hair samples. Copyright © 2014 Elsevier Inc. All rights reserved.

  16. Determination of plutonium-238 in plutonium by alpha spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jain, H.C.; Mathews, C.K.; Ramaniah, M.V.

    1975-01-01

    A method is presented for the determination of 238 Pu in plutonium samples by alpha spectrometry. Various factors attributing towards the energy degradation, a problem usually encountered in alpha spectrometry, are discussed. A computer programme is given for the evaluation of peak areas when the alpha spectrum is degraded. The results are compared with those obtained by mass spectrometry. (author)

  17. Comparison of accelerator mass spectrometric measurement with liquid scintillation counting measurement for the determination of 14C in environmental samples

    International Nuclear Information System (INIS)

    Yasuike, Kaeko; Yamada, Yoshimune; Amano, Hikaru

    2010-01-01

    The concentrations of organically-bound 14 C in tree-ring cellulose of a Japanese Black Pine grown in Shika-machi (37.0 deg. N, 136.8 deg. E) and those of a Japanese Cedar grown in Kanazawa (36.5 deg. N, 136.7 deg. E), Japan, were analyzed for the ring-years from 1989 to 1998 by the accelerator mass spectrometric measurement. The results were compared with those of the same samples analyzed by the liquid scintillation counting measurement to determine the reliability of liquid scintillation counting measurement. An important result of this study is that the sensitivity and reproducibility of accelerator mass spectrometric measurement was almost equal to that of liquid scintillation counting measurement.

  18. Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

    Energy Technology Data Exchange (ETDEWEB)

    Karadjova, Irina B. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria); Lampugnani, Leonardo [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy)]. E-mail: lampugnani@ipcf.cnr.it; Onor, Massimo [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy); D' Ulivo, Alessandro [C.N.R. Istituto per i processi chimico-fisici, Area della Ricerca di Pisa, Via Moruzzi 1, 56124 Pisa (Italy); Tsalev, Dimiter L. [Faculty of Chemistry, University of Sofia, 1 James Bourchier Blvd., Sofia 1164 (Bulgaria)

    2005-07-15

    Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 {mu}g l{sup -1} As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 {mu}g l{sup -1}. Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l{sup -1} acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l{sup -1} HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 {mu}g l{sup -1} for As(III) and 0.3 {mu}g l{sup -1} for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 {mu}g l{sup -1} (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non

  19. Considering the determination of an alpha value

    International Nuclear Information System (INIS)

    Lorenz, B.

    1987-01-01

    Following an outline of the most important international methods of evaluating an alpha value (the monetary equivalent of one man-sievert) and an approach deemed suitable for use in the GDR, it is recommended that alpha be taken as 30,000 Mark per man-sievert in national cost-benefit analyses. This value should be revisited every five to ten years. (author)

  20. Partial vapor-phase hydrolysis of peptide bonds: A method for mass spectrometric determination of O-glycosylated sites in glycopeptides

    DEFF Research Database (Denmark)

    Mirgorodskaya, E; Hassan, H; Wandall, H H

    1999-01-01

    In this study we present a method for determination of O-glycosylation sites in glycopeptides, based on partial vapor-phase acid hydrolysis in combination with mass spectrometric analysis. Pentafluoropropionic acid and hydrochloric acid were used for the hydrolysis of glycosylated peptides....... The reaction conditions were optimized for efficient polypeptide backbone cleavages with minimal cleavage of glycosidic bonds. The glycosylated residues were identified by mass spectrometric analysis of the hydrolytic cleavage products. Although glycosidic bonds are partially cleaved under acid hydrolysis...

  1. Rapid in situ gamma spectrometric determination of fallout radioactivity in the environment. Progress report

    International Nuclear Information System (INIS)

    Zombori, Peter

    1995-01-01

    layers. Though fresh fallout is often assumed to be distributed completely on the ground surface recent studies revealed that a certain penetration of the radioactivity into the soil can occur already in the first instance. The improper estimation of the distribution parameter can result in a deviation of the determined activity concentration from the true value by a factor of 2 or more. This way the reliability of the method is limited due to the lack of information on the depth profile of the activity concentration. The main objective of our study is to find a method (or more, if possible) to estimate the penetration character of the fallout radioactivity by using only spectral information obtained by the in situ spectrometric measurement thus avoiding the need for a long and tiresome sampling and sample analysis procedure

  2. $\\alpha_s$ determinations from ATLAS (status and plans)

    CERN Document Server

    Malaescu, Bogdan

    2015-01-01

    The determinations of the strong coupling constant using ATLAS data at √ s = 7 TeV, from the inclusive jet cross section, multi-jet cross section ratios and transverse energy-energy cor- relations in multi-jet events are presented.

  3. Determination of hCG-alpha subunit in threatened pregnancy

    International Nuclear Information System (INIS)

    Talas, M.; Pohanka, J.; Fingerova, H.; Janouskova, M.; Krikal, Z.; Prasilova, J.; Zupkova, H.

    1987-01-01

    Radioimmunoassay of the hCG-alpha subunit was made using an antibody anti hCG-alpha serum, highly purified hCG-alpha for 125 I-labelling and the standard hCG-alpha. Sera of healthy pregnant women sampled throughout the whole pregnancies were used to determine x-bar±S.D. of hCG-alpha for 14-day intervals. Included in the study were groups of women with high risk of premature labor, late toxemia of pregnancy, twins and fetal hypotrophy. It was shown that increased hCG-alpha is found in pregnant women in whom signs of late toxemia of pregnancy are combined with high risk of premature labor, or with twin pregnancies, while in those with fetal hypotrophy hCG-alpha is within normal limits. (author). 3 figs., 7 refs

  4. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  5. Gas chromatographic-mass spectrometric determination of levodropropizine plasma levels in healthy volunteers.

    Science.gov (United States)

    Zaratin, P; De Angelis, L; Cattabeni, F

    1988-08-01

    A gas chromatographic-mass spectrometric method for the qualitative and quantitative analysis of levodropropizine (S(-)-3-(4-phenyl-piperazin-1-yl)-propane-1,2-diol, DF 526) in plasma is described. The method proved to be highly selective and sensitive. Drug concentrations as low as 5 ng/ml could be measured. Levodropropizine plasma levels were measured in 6 healthy volunteers after administration of an acute 60 mg dose. Peak concentrations were reached between 40 and 60 min and measurable amounts of drug were present till 8 h after administration.

  6. Application of a Gas Chromatography/Mass Spectrometric Method for the Determination of Butyltin Compounds in Sediment

    International Nuclear Information System (INIS)

    Chung, Min Young; Kim, Byung Joo; Yim, Yong Heon; So, Hun Young; Won, Yong Il; Jung, Pyong Gil; Kim, Yong Seong

    2004-01-01

    A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry

  7. LC-APCI mass spectrometric method development and validation for the determination of atovaquone in human plasma.

    Science.gov (United States)

    Gurule, Sanjay; Goswami, Dipanjan; Khuroo, Arshad H; Monif, Tausif

    2010-05-01

    A newly developed LC-APCI mass spectrometric method is described for human plasma determination of atovaquone using lapachol internal standard. A single-step protein precipitation technique for plasma extraction of atovaquone achieving mean recovery of 94.17% (CV 8%) without compromising sensitivity (limit of quantitation 50.3 ng/mL) or linearity (50.3 ng/mL-23924.6 ng/mL) is delineated in this paper. Heated nebulizer in negative multiple reaction monitoring mode was employed with transitions m/z 365.2 --> m/z 337.1 and m/z 240.9 --> m/z 185.7 for atovaquone and lapachol respectively in this liquid chromatographic-tandem mass spectrometric method. Excellent chromatographic separation on a Synergi 4 micro Polar-RP 80A (150 x 2.0 mm) column, using 100 microL of plasma extraction volume along with 10 microL of injection load, completing analysis run-time within 2.5 min, highlights this simple yet unique bioanalytical method. The developed method can be successfully applied to pharmacokinetic studies on atovaquone suspension administered in healthy volunteers or HIV-infected patients. Moreover full method validation results not published before are presented and discussed in detail for the first time in this article. 2009 John Wiley & Sons, Ltd.

  8. Application and evaluation of the mass spectrometric isotope dilution technique in the determination of rare earths in geological materials

    International Nuclear Information System (INIS)

    Moraes, N.M.P. de.

    1988-01-01

    Establishment of the experimental procedures employed in the rare earth element determination of geological samples by mass spectrometric isotope dilution analysis is discussed in the present work. The procedures involve preparation and calibration of the isotope tracers isotope dilution, dissolution in a teflon pressure vessel, chemical separation and isotope analysis using a fully automated Micromass VG ISOTOPES model 354 thermal ionization mass spectrometer. For the initial chemical separation of total rare earths the cationic resin was employed and HC1 and HNO 3 acids as eluents. In the second step rare earths elements were separated into individual (La, Ce and Nd) and subgroups (Sm-Eu-Gd, Yb-Er-Dy) fractions using the same cationic resin and α-HIBA as eluent. Nine elements La, Ce, Nd, Sm, Eu, Gd, Dy, Er and Yb are determined by this method in the ''United States Geological Survey'' (USGS) standard samples GSP-1, AGV-1 and G-2, with an overall precision of +- 1 to 2% and an accuracy of 5%. The concentration of rare earth element determined in the standard sample PCC-1 showed that the total analytical blanks are in submicrogram levels. The concentration of rare earth elements in the same USGS standard samples were also determined by Instrumental neutron activation analysis, neutron activation analysis with chemical separation before irradiation and inductively coupled argon plasma spectroscopy. The chemical procedures employed for these methods are the same as that used for mass spectrometric isotope dilution. Based on the results obtained, each method was evaluated pointing out their merits and defects. The study clearly showed that the chemical procedure employed for all these techniques was satisfactory. (author) [pt

  9. Determination of radium-226 in fresh water, using alpha spectroscopy

    International Nuclear Information System (INIS)

    Byrakdar, M. E.

    2006-12-01

    Four radium isotopes are present in nature, i.e. Ra-223, Ra-224, Ra-226, and Ra-228. The first three are alpha emitters while the last is a beta emitter. Because of the importance of the determination of Alpha isotope emitters in pure water (drinking water), this work focuses on the determination of radium-226 as it has the longest half-life (1600 years, in comparison to 11.4 day, 3.66 days for Ra-223 and Ra-224, respectively) using Alpha spectroscopy. This method has the capability to be applied in sampling fields and low detection limit which in turn makes the analysis of low-level radioactive environmental water samples, with hardness does not exceed 40 French Degree, satisfying for health and environment control programmes. However, counting the samples using Alpha spectroscopy has to be immediate (or within 48 hours). (author)

  10. Development of an Isotope-Dilution Liquid Chromatography/Mass Spectrometric Method for the Accurate Determination of Acetaminophen in Tablets

    Energy Technology Data Exchange (ETDEWEB)

    Shin, Hyun Ju; Kim, Byung Joo; Lee, Joon Hee; Hwang, Eui Jin [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2010-12-15

    Acetaminophen (N-acetyl-p-aminophenol) is one of the most popular analgesic and antipyretic drugs. An isotope dilution mass spectrometric method based on LC/MS was developed as a candidate reference method for the accurate determination of acetaminophen in pharmaceutical product. After spiking an isotope labeled acetaminophen (acetyl-{sup 13}C{sub 2}, {sup 15}Nacetaminophen) as an internal standard, tablet extracts were analyzed by LC/MS in a selected reaction monitoring (SRM) mode to detect ions at m/z 152→110 and m/z 155→111 for acetaminophen and acetyl-{sup 13}C{sub 2}, {sup 15}N-acetaminophen, respectively. The repeatability and reproducibility of the developed ID/LC-MS method were tested for the validation and assessment of metrological quality of the method.

  11. Determination of $\\alpha_{s}$ via the Differential 2-Jet-Rate with ATLAS at LHC

    CERN Document Server

    Lichtnecker, Markus

    The first determination of the strong coupling constant alpha_s via the differential 2-jet-rate in pp collisions at the LHC (at a center-of-mass-energy of 7 TeV) is presented. Data gathered by the ATLAS experiment are fitted by next-to-leading order (NLO) perturbative QCD predictions from calculations with the program NLOJET++. As an observable, the jet-flip-parameter from 3 to 2 reconstructed jets is investigated, using the infrared and collinear safe kT jet algorithm in the exclusive reconstruction mode. The jet-flip-parameters from real data are compared to simulated data from Monte Carlo generators. For the determination of alpha_s, real data have been corrected for the jet-energy-scale, whereas the calculations from NLOJET++ have been corrected for the influence of hadronization effects as well as the impact of the Underlying Event by applying bin-by-bin corrections. The fit between real data and the calculations from NLOJET++ yields a value of alpha_s(M_Z)=0.120 +/-0.001(stat.) +/-0.005(syst.), which is...

  12. Determination of $\\alpha_{s}$ using Jet Rates at LEP with the OPAL detector

    CERN Document Server

    Abbiendi, G.; Akesson, P.F.; Alexander, G.; Anagnostou, G.; Anderson, K.J.; Asai, S.; Axen, D.; Bailey, I.; Barberio, E.; Barillari, T.; Barlow, R.J.; Batley, R.J.; Bechtle, P.; Behnke, T.; Bell, Kenneth Watson; Bell, P.J.; Bella, G.; Bellerive, A.; Benelli, G.; Bethke, S.; Biebel, O.; Boeriu, O.; Bock, P.; Boutemeur, M.; Braibant, S.; Brown, Robert M.; Burckhart, H.J.; Campana, S.; Capiluppi, P.; Carnegie, R.K.; Carter, A.A.; Carter, J.R.; Chang, C.Y.; Charlton, D.G.; Ciocca, C.; Csilling, A.; Cuffiani, M.; Dado, S.; De Roeck, A.; De Wolf, E.A.; Desch, K.; Dienes, B.; Donkers, M.; Dubbert, J.; Duchovni, E.; Duckeck, G.; Duerdoth, I.P.; Etzion, E.; Fabbri, F.; Ferrari, P.; Fiedler, F.; Fleck, I.; Ford, M.; Frey, A.; Gagnon, P.; Gary, John William; Geich-Gimbel, C.; Giacomelli, G.; Giacomelli, P.; Giunta, Marina; Goldberg, J.; Gross, E.; Grunhaus, J.; Gruwe, M.; Gunther, P.O.; Gupta, A.; Hajdu, C.; Hamann, M.; Hanson, G.G.; Harel, A.; Hauschild, M.; Hawkes, C.M.; Hawkings, R.; Hemingway, R.J.; Herten, G.; Heuer, R.D.; Hill, J.C.; Horvath, D.; Igo-Kemenes, P.; Ishii, K.; Jeremie, H.; Jovanovic, P.; Junk, T.R.; Kanzaki, J.; Karlen, D.; Kawagoe, K.; Kawamoto, T.; Keeler, R.K.; Kellogg, R.G.; Kennedy, B.W.; Kluth, S.; Kobayashi, T.; Kobel, M.; Komamiya, S.; Kramer, T.; Krasznahorkay, A.; Krieger, P.; von Krogh, J.; Kuhl, T.; Kupper, M.; Lafferty, G.D.; Landsman, H.; Lanske, D.; Lellouch, D.; Lettso, J.; Levinson, L.; Lillich, J.; Lloyd, S.L.; Loebinger, F.K.; Lu, J.; Ludwig, A.; Ludwig, J.; Mader, W.; Marcellini, S.; Martin, A.J.; Mashimo, T.; Mattig, Peter; McKenna, J.; McPherson, R.A.; Meijers, F.; Menges, W.; Merritt, F.S.; Mes, H.; Meyer, Niels T.; Michelini, A.; Mihara, S.; Mikenberg, G.; Miller, D.J.; Mohr, W.; Mori, T.; Mutter, A.; Nagai, K.; Nakamura, I.; Nanjo, H.; Neal, H.A.; Nisius, R.; O'Neale, S.W.; Oh, A.; Oreglia, M.J.; Orito, S.; Pahl, C.; Pasztor, G.; Pater, J.R.; Pilcher, J.E.; Pinfold, J.; Plane, David E.; Pooth, O.; Przybycien, M.; Quadt, A.; Rabbertz, K.; Rembser, C.; Renkel, P.; Roney, J.M.; Rossi, A.M.; Rozen, Y.; Runge, K.; Sachs, K.; Saeki, T.; Sarkisyan, E.K.G.; Schaile, A.D.; Schaile, O.; Scharff-Hansen, P.; Schieck, J.; Schorner-Sadenius, T.; Schroder, Matthias; Schumacher, M.; Seuster, R.; Shears, T.G.; Shen, B.C.; Sherwood, P.; Skuja, A.; Smith, A.M.; Sobie, R.; Soldner-Rembold, S.; Spano, F.; Stahl, A.; Strom, David M.; Strohmer, R.; Tarem, S.; Tasevsky, M.; Teuscher, R.; Thomson, M.A.; Torrence, E.; Toya, D.; Tran, P.; Trigger, I.; Trocsanyi, Z.; Tsur, E.; Turner-Watson, M.F.; Ueda, I.; Ujvari, B.; Vollmer, C.F.; Vannerem, P.; Vertesi, R.; Verzocchi, M.; Voss, H.; Vossebeld, J.; Ward, C.P.; Ward, D.R.; Watkins, P.M.; Watson, A.T.; Watson, N.K.; Wells, P.S.; Wengler, T.; Wermes, N.; Wilson, G.W.; Wilson, J.A.; Wolf, G.; Wyatt, T.R.; Yamashita, S.; Zer-Zion, D.; Zivkovic, Lidija

    2006-01-01

    Hadronic events produced in e+e- collisions by the LEP collider and recorded by the OPAL detector were used to form distributions based on the number of reconstructed jets. The data were collected between 1995 and 2000 and correspond to energies of 91 GeV, 130-136 GeV and 161-209 GeV. The jet rates were determined using four different jet-finding algorithms (Cone, JADE, Durham and Cambridge). The differential two-jet rate and the average jet rate with the Durham and Cambridge algorithms were used to measure alpha(s) in the LEP energy range by fitting an expression in which order alpah_2s calculations were matched to a NLLA prediction and fitted to the data. Combining the measurements at different centre-of-mass energies, the value of alpha_s (Mz) was determined to be alpha(s)(Mz)=0.1177+-0.0006(stat.)+-0.0012$(expt.)+-0.0010(had.)+-0.0032

  13. Simultaneous determination of oxygen, nitrogen and hydrogen in metals by pulse heating and time of flight mass spectrometric method.

    Science.gov (United States)

    Shen, Xuejing; Wang, Peng; Hu, Shaocheng; Yang, Zhigang; Ma, Hongquan; Gao, Wei; Zhou, Zhen; Wang, Haizhou

    2011-05-30

    The inert gas fusion and infrared absorption and thermal conductivity methods are widely used for quantitative determination of oxygen(O), nitrogen(N) and hydrogen(H) in metals. However, O, N and H cannot be determined simultaneously with this method in most cases and the sensitivity cannot meet the requirement of some new metal materials. Furthermore, there is no equipment or method reported for determination of Argon(Ar) or Helium(He) in metals till now. In this paper, a new method for simultaneous quantitative determination of O, N, H and Ar(or He) in metals has been described in detail, which combined the pulse heating inert gas fusion with time of flight mass spectrometric detection. The whole analyzing process was introduced, including sample retreatment, inert gas fusion, mass spectral line selection, signal acquisition, data processing and calibration. The detection limit, lower quantitative limit and linear range of each element were determined. The accuracy and precision of the new method have also been verified by measurements of several kinds of samples. The results were consistent with that obtained by the traditional method. It has shown that the new method is more sensitive and efficient than the existing method. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. 226Ra determination in phosphogypsum by alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Aguado, J.L.; Bolivar, J.P.; Garcia-Tenorio, R.

    1999-01-01

    A radiochemical method for 226 Ra determination by alpha-particle spectrometry in environmental samples has been developed in our laboratory. The method has been validated by measurements in samples with known concentrations of this radionuclide and it has been applied in studies related to 226 Ra behaviour in phosphogypsum (the main by-product of producing phosphoric acid from phosphate rocks). (author)

  15. 226Ra determination in phosphogypsum by alpha-particle spectrometry

    Science.gov (United States)

    Aguado, J. L.; Bolívar, J. P.; García-Tenorio, R.

    1999-01-01

    A radiochemical method for226Ra determination by alpha-particle spectrometry in environmental samples has been developed in our laboratory. The method has been validated by measurements in samples with known concentrations of this radionuclide and it has been applied in studies related to226Ra behaviour in phosphogypsum (the main by-product of producing phosphoric acid from phosphate rocks).

  16. Mass spectrometric determination of magnesium isotopic ratios and its corrections for electron multiplier discrimination and mass fractionation

    International Nuclear Information System (INIS)

    Deng Zhongguo

    1989-01-01

    The mass spectrometric determination of magnesium isotopic ratios by the use of uranyl nitrate added to magnesium samples to act as a binding agent is reported. Prebaking empty filaments and preheating filaments with deposited magnesium samples on its surface in a vacuum are employed to reduce the Na signal from the thenium-ribbon. Methods for correcting magnesium isotopic ratios for electron multiplier discrimination and mass fractionation are described in detail. The results of the determination of natural magnesium isotopic ratios are 25 Mg/ 24 Mg = 0.12660 (1±0.01%) and 26 Mg/ 24 Mg = 0.13938 (1±0.10%). The magnesium isotopic ratios of rich - 26 Mg-2 sample and rich- 25 Mg-1 sample are 24 Mg/ 26 Mg = 0.003463 (1±0.2%), 25 Mg/ 26 Mg = 0.001656 (±0.2%) and 24 Mg/ 25 Mg = 0.006716 (1±0.2%), 26 Mg/ 25 Mg = 0.007264 (1±0.2%) respectively

  17. Atomic-absorption spectrometric determination of cobalt, nickel, and copper in geological materials with matrix masking and chelation-extraction

    Science.gov (United States)

    Sanzolone, R.F.; Chao, T.T.; Crenshaw, G.L.

    1979-01-01

    An atomic-absorption spectrometric method is reported for the determination of cobalt, nickel, and copper in a variety of geological materials including iron- and manganese-rich, and calcareous samples. The sample is decomposed with HP-HNO3 and the residue is dissolved in hydrochloric acid. Ammonium fluoride is added to mask iron and 'aluminum. After adjustment to pH 6, cobalt, nickel, and copper are chelated with sodium diethyl-dithiocarbamate and extracted into methyl isobutyl ketone. The sample is set aside for 24 h before analysis to remove interferences from manganese. For a 0.200-g sample, the limits of determination are 5-1000 ppm for Co, Ni, and Cu. As much as 50% Fe, 25% Mn or Ca, 20% Al and 10% Na, K, or Mg in the sample either individually or in various combinations do not interfere. Results obtained on five U.S. Geological Survey rock standards are in general agreement with values reported in the literature. ?? 1979.

  18. Burnup determination of a high burnup PWR fuel by neodymium and cesium isotope monitor methods based on isotope dilution mass spectrometric measurements

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jung Suk; Jeon, Young Shin; Park, Soon Dal; Han, Sun Ho; Ha, Yeong Keong; Song, Kyu Seok [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2008-11-15

    Destructive methods were used for the burnup determination of a PWR nuclear fuel irradiated to a high burnup in power reactors. The total burnup was determined from a measurement of the Nd and Cs isotope burnup monitors. The methods included U, Pu, {sup 148}Nd, {sup 145}Nd+{sup 146}Nd, total of the Nd isotopes, and {sup 133}Cs and {sup 137}Cs determinations by the isotope dilution mass spectrometric method (IDMS) by using quadrupole spikes ({sup 233}U, {sup 242}Pu, {sup 150}Nd and {sup 133}Cs). The methods involved two sequential anion exchange resin (AG 1X8 and 1X4) separation procedures and a Cs purification with a cation exchange resin (AG 50WX4) separation procedure. The effective fission yield was calculated from the weighted fission yields averaged over the irradiation period. The results obtained by the Nd and Cs isotopes from the mass spectrometric measurement were compared with those by the ORIGEN code.

  19. Alpha spectrometry of thick sources. I. Application to alpha emitters determination

    International Nuclear Information System (INIS)

    Acena, M.L.; Garcia-Torano, E.; Rivero, M.C.

    1977-01-01

    A method for determining alpha emitters by silicon surface barrier detector spectroscopy using thick sources is studied. Two types of spectra have been obtained. They have different shapes of line according to the procedure used for preparing the sources. For both spectra a computing least square programme has been developed. In this way it is possible to calculate line intensities with accuracy better than 20 percent. (author) [es

  20. Microdiffusion-based UV-LED spectrometric setup for determining low levels of ethanol in fruit juice.

    Science.gov (United States)

    Gros, Nataša

    2011-12-15

    A novel setup is described in which we combined the separation of a volatile substance from a sample with a complex matrix on the basis of a microdiffusion process with a kinetic on-line spectrometric monitoring of the reaction in the receptive medium at 365 nm. The fruit juice was selected as a model for testing the performance of the setup in real-life applications. The ethanol content in fruit juice can be considered as an indicator of the fruit-juice quality and should not exceed the regulatory limiting values. After optimising the microdiffusion process, blackcurrant, orange and two varieties of apple juice were analysed. The sample analysis lasted 15 min at 35°C. The ethanol concentrations were found to be between 0.9 and 4.0 mmol/L, and were comparable to the results obtained using the SIST:ISO 2448:1998 standard method, which is time consuming, labour intensive and requires high sample volumes. The setup can easily be adapted for determining other volatile substances in low concentrations in complicated samples of different types by introducing different chemistry and replacing the light source if the light of a different wavelength is required. The measuring characteristics of the setup were critically assessed, the main sources of uncertainty recognised and the possibilities for further improvements of the setup and the procedure considered. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Gas chromatography-mass spectrometric determination of traces of ether-type icing inhibitors in free-floating fuels

    Energy Technology Data Exchange (ETDEWEB)

    Shin, H.S. [Dept. of Environmental Education, Kongju National Univ., Kongju (Korea); Abuse Drug Research Center, Kongju National Univ., Kongju (Korea); Ahn, H.S. [Dept. of Environmental Science, Kongju National Univ., Kongju (Korea)

    2004-08-01

    A gas chromatographic-mass spectrometric (GC-MS) assay method has been developed for simultaneous determination of ethylene glycol monomethyl ether (EGME) and diethylene glycol monomethly ether (DEGME) in spilled aviation fuels. Ethylene glycol monobutyl ether (EGBE) and ethylene glycol monoethyl ether (EGEE) were used as internal standard and surrogate, respectively. Sample preparation consisted of back-extraction with 7 mL dichloromethane after extraction of 50 mL of fuel with 2 mL of water. The extract was concentrated to dryness, dissolved in 100 {mu}L methanol, and analyzed by GC-MS with selected-ion monitoring (SIM). The peaks had good chromatographic properties on a semi-polar column. EGME and DEGME were extracted from fuel with high recovery of 75 and 85%, with small variations, respectively. Method detection limits were 1.3 and 1.0 ng mL{sup -1} for EGME and DEGME, respectively, in spilled fuel. DEGME was detected at concentrations of 22.6 and 19.7 ng mL{sup -1} in two samples from among five free-floating samples collected in a tunnel of a subway station located in the vicinity of an army base in Korea. The method might be useful for differentiation between the fuel-types kerosene and JP-8, which might originate from a storage tank. (orig.)

  2. Gas Chromatographic-Selected Ion Monitoring-Mass Spectrometric Determination of Cigarette Mainstream Smoke Components with Sensory Attributes

    Directory of Open Access Journals (Sweden)

    Coleman WM

    2014-12-01

    Full Text Available A new method has been developed that detects significant quantitative differences in the amounts of pyrazines, pyridines, furfurals, carboxylic acids, b-damascenone, sclareolide, and megastigmatrienones in the mainstream smoke of a series of five commercial cigarettes. This new quantitative method is based on the gas chromatographic-selected ion monitoring-mass spectrometric (GC-SIM-MS determination of the selected smoke constituents. The accuracy and precision of the approach were well within acceptable parameters with the majority of cases relative standard deviation (RSD values consistently around 5%. Sample preparation was simple requiring only the dissolution of the trapped particulate material in a known volume of methanol followed by injection of this clear dark colored solution into the gas chromatograph. This approach represents an advance in the technology in terms of higher sample throughput and less sample workup. Certain products demonstrated consistent trends in concentration of specific chemical classes. The mainstream smoke from a University of Kentucky reference cigarette, 2R4F, was included for reference purposes. These results are applicable in the overall evaluation of the components responsible for the taste associated with cigarette products.

  3. Determination of nuclear fuel burn-up using mass spectrometric techniques

    International Nuclear Information System (INIS)

    Saha, B.; Bagyalakshmi, R.; Periaswami, G.; Kavimandan, V.D.; Chitambar, S.A.; Jain, H.C.; Mathews, C.K.

    1977-01-01

    Determination of burn-up using a stable fission product monitor such as 148 Nd and heavy elements, determined by isotope dilution mass spectrometry gives the most accurate data. This report describes the work carried out to standardise the conditions for burn-up determination. Some typical results are given. (author)

  4. Determination of Ra in environmental samples by. alpha. -particle spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hancock, G.J.; Martin, P. (Alligator Rivers Region Research Inst., Jabiru, N.T. (Australia))

    1991-01-01

    A method of determining Ra isotopes by {alpha}-particle spectrometry using {sup 225}Ra as a yield tracer has been developed. Radium is coprecipitated with lead sulphate, purified using ion exchange techniques, and electrodeposited from an aqueous/ethanol solution. The procedure can be easily completed in 1 day. Tracer recoveries are typically 80%, and the resolution obtained is typically 40 keV FWHM. (author).

  5. X-ray spectrometric determination of glass content of melts incorporating radioactive waste: a feasibility study

    International Nuclear Information System (INIS)

    Slates, R.V.

    1978-09-01

    X-ray fluorescence spectrometry was evaluated for the determination of glass content and homogeneity of glass incorporating high-level radioactive waste. Accuracy and precision were determined for analyses of Al 2 O 3 , SiO 2 , CaO, TiO 2 , MnO, Fe 2 O 3 , and NiO in specimens of known composition. These specimens were prepared by fusing powdered glass with nonradioactive synthetic waste. Matrix effects of sodium on these analyses were specifically evaluated. X-ray fluorescence spectrometry was shown to be applicable to the proposed determinations by comparing the known glass contents of 14 glass waste compositions with those calculated from experimentally determined concentrations of SiO or TiO 2

  6. Gas Chromatographic-Mass Spectrometric Determination of British Anti-Lewisite in Plasma

    National Research Council Canada - National Science Library

    Byers, C. E; Holloway, E. R; Korte, W. D; Smith, J. R; Clarkson, E. D; Platoff, G. E; Capacio, B. R

    2004-01-01

    British anti-Lewisite (BAL) (2,3-dimercapto-1-propanol) is a potential therapeutic compound when used against the effects of cutaneous sulfur mustard, and a method for its determination in plasma has been developed...

  7. Alpha spectrometric characterization of process-related particle size distributions from active particle sampling at the Los Alamos National Laboratory uranium foundry

    Energy Technology Data Exchange (ETDEWEB)

    Plionis, Alexander A [Los Alamos National Laboratory; Peterson, Dominic S [Los Alamos National Laboratory; Tandon, Lav [Los Alamos National Laboratory; Lamont, Stephen P [Los Alamos National Laboratory

    2009-01-01

    Uranium particles within the respirable size range pose a significant hazard to the health and safety of workers. Significant differences in the deposition and incorporation patterns of aerosols within the respirable range can be identified and integrated into sophisticated health physics models. Data characterizing the uranium particle size distribution resulting from specific foundry-related processes are needed. Using personal air sampling cascade impactors, particles collected from several foundry processes were sorted by activity median aerodynamic diameter onto various Marple substrates. After an initial gravimetric assessment of each impactor stage, the substrates were analyzed by alpha spectrometry to determine the uranium content of each stage. Alpha spectrometry provides rapid nondestructive isotopic data that can distinguish process uranium from natural sources and the degree of uranium contribution to the total accumulated particle load. In addition, the particle size bins utilized by the impactors provide adequate resolution to determine if a process particle size distribution is: lognormal, bimodal, or trimodal. Data on process uranium particle size values and distributions facilitate the development of more sophisticated and accurate models for internal dosimetry, resulting in an improved understanding of foundry worker health and safety.

  8. Gas Chromatographic Mass Spectrometric Determination of Myo-inositol in Humans Utilizing a Deuterated Internal Standard

    DEFF Research Database (Denmark)

    Andersen, Jan Rud; Larsen, Elfinn; Harbo, Helge

    1982-01-01

    The isotopic dilution technique was used for determining the content of myo-inositol in human urine, plasma and haemolysed erythrocyte samples. A deuterated myo-inositol, synthesized from inosose-2 by base-catalysed exchange of hydrogens by deuterium, followed by reduction of the inosose with 2H2...

  9. Gamma spectrometric determination of naturally occurring elements in sediment samples of Egypt

    International Nuclear Information System (INIS)

    EL-Sayed, A.A.

    2006-01-01

    Determination of the naturally occurring elements 238 U( 226 Ra), 40 K, 232 Th( 228 Ra) and the fission product 137 Cs in sediments and water in two environmental systems in southern and northern parts of Egypt was made. These ecological systems represent main surface water system, supply drinking water to eastern part of Egypt, and the other is brackish water

  10. Simultaneous determination of U and Pu isotopes by alpha spectrometry

    International Nuclear Information System (INIS)

    Equillor, H.E.; Campos, J.M.

    2011-01-01

    Determination of actinides by alpha spectrometry is usually carried out after full separation of each of the components of the sample. The procedure presented in this paper permits U and Pu isotopes to be measured together allowing faster sample processing and measurement. The method consists in the extraction with tributyl phosphate of U and Pu isotopes from the rest of the matrix, followed by a cathodic electrodeposition to obtain alpha spectrometry suitable pieces. It can be applied to various environmental samples, such as water, filters and soil (about 0.5 g of solid sample for the described conditions). High-quality electroplated discs are essential for simultaneous processing, so a technique to achieve this requirement is also explained. (authors) [es

  11. 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

  12. Fragment Formula Calculator (FFC): Determination of Chemical Formulas for Fragment Ions in Mass Spectrometric Data

    OpenAIRE

    Wegner, André; Weindl, Daniel; Jäger, Christian; Sapcariu, Sean C.; Dong, Xiangyi; Stephanopoulos, Gregory; Hiller, Karsten

    2014-01-01

    The accurate determination of mass isotopomer distributions (MID) is of great significance for stable isotope-labeling experiments. Most commonly, MIDs are derived from gas chromatography/electron ionization mass spectrometry (GC/EI-MS) measurements. The analysis of fragment ions formed during EI, which contain only specific parts of the original molecule can provide valuable information on the positional distribution of the label. The chemical formula of a fragment ion is usually applied to ...

  13. On-line Incorporation of Cloud Point Extraction in Flame Atomic Absorption Spectrometric Determination of Silver

    OpenAIRE

    DALALI, Nasser; JAVADI, Nasrin; AGRAWAL, Yadvendra KUMAR

    2008-01-01

    A cloud point extraction method was incorporated into a flow injection system, coupled with flame atomic absorption spectrometry, for determination of trace amounts of silver. The analyte in the aqueous solution was acidified with 0.2 mol L-1 sulfuric acid and complexed with dithizone. The cloud point extraction was performed using the non-ionic surfactant Triton X-114. After obtaining the cloud point, the surfactant-rich phase containing the dithizonate complex was collected in a m...

  14. Microwave plasma atomic emission spectrometric determination of Ca, K and Mg in various cheese varieties.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-02-01

    Microwave plasma-atomic emission spectrometry (MP-AES) was used to determine calcium, magnesium and potassium in various Turkish cheese samples. Cheese samples were dried at 100 °C for 2 days and then digested in a mixture of nitric acid/hydrogen peroxide (3:1). Good linearities (R(2) > 0.999) were obtained up to 10 μg mL(-1) of Ca, Mg and K at 445.478 nm, 285.213 nm and 766.491 nm, respectively. The analytes in a certified reference milk powder sample were determined within the uncertainty limits. Moreover, the analytes added to the cheese samples were recovered quantitatively (>90%). All determinations were performed using aqueous standards for calibration. The LOD values for Ca, Mg and K were 0.036 μg mL(-1), 0.012 μg mL(-1) and 0.190 μg mL(-1), respectively. Concentrations of Ca, K and Mg in various types of cheese samples produced in different regions of Turkey were found between 1.03-3.70, 0.242-0.784 and 0.081-0.303 g kg(-1), respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. A mass spectrometric method to determine activities of enzymes involved in polyamine catabolism

    International Nuclear Information System (INIS)

    Moriya, Shunsuke; Iwasaki, Kaori; Samejima, Keijiro; Takao, Koichi; Kohda, Kohfuku; Hiramatsu, Kyoko; Kawakita, Masao

    2012-01-01

    Highlights: ► Compounds in polyamine catabolic pathway were determined by a column-free ESI-TOF MS. ► N 1 - and N 8 -acetylspermidine were determined by a column-free ESI-MS/MS. ► The method was applied to determine activities of APAO, SMO, and SSAT in the pathway. ► The assay method contained stable isotope-labeled natural substrates. ► It is applicable to biological samples containing natural substrate and product. - Abstract: An analytical method for the determination of three polyamines (putrescine, spermidine, and spermine) and five acetylpolyamines [N 1 -acetylspermidine (N 1 AcSpd), N 8 -acetylspermidine (N 8 AcSpd), N 1 -acetylspermine, N 1 ,N 8 -diacetylspermidine, and N 1 ,N 12 -diacetylspermine] involved in the polyamine catabolic pathway has been developed using a hybrid tandem mass spectrometer. Heptafluorobutyryl (HFB) derivatives of these compounds and respective internal standards labeled with stable isotopes were analyzed simultaneously by TOF MS, based on peak areas appearing at appropriate m/z values. The isomers, N 1 AcSpd and N 8 AcSpd were determined from their fragment ions, the acetylamidopropyl and acetylamidobutyl groups, respectively, using MS/MS with 13 C 2 -N 1 AcSpd and 13 C 2 -N 8 AcSpd which have the 13 C 2 -acetyl group as an internal standard. The TOF MS method was successfully applied to measure the activity of enzymes involved in polyamine catabolic pathways, namely N 1 -acetylpolyamine oxidase (APAO), spermine oxidase (SMO), and spermidine/spermine N 1 -acetyltransferase (SSAT). The following natural substrates and products labeled with stable isotopes considering the application to biological samples were identified; for APAO, [4,9,12- 15 N 3 ]-N 1 -acetylspermine and [1,4,8- 15 N 3 ]spermidine ( 15 N 3 -Spd), respectively; for SMO, [1,4,8,12- 15 N 4 ]spermine and 15 N 3 -Spd, respectively; and for SSAT, 15 N 3 -Spd and [1,4,8- 15 N 3 ]-N 1 -acetylspermidine, respectively.

  16. A mass spectrometric method to determine activities of enzymes involved in polyamine catabolism

    Energy Technology Data Exchange (ETDEWEB)

    Moriya, Shunsuke; Iwasaki, Kaori [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan); Samejima, Keijiro, E-mail: samejima-kj@igakuken.or.jp [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan); Takao, Koichi [Faculty of Pharmaceutical Sciences, Josai University, 1-1 Keyakidai, Sakado, Saitama 350-0295 (Japan); Kohda, Kohfuku [Research Institute of Pharmaceutical Sciences, Musashino University, 1-1-20 Shinmachi, Nishitokyo, Tokyo 202-8585 (Japan); Hiramatsu, Kyoko; Kawakita, Masao [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan)

    2012-10-20

    Highlights: Black-Right-Pointing-Pointer Compounds in polyamine catabolic pathway were determined by a column-free ESI-TOF MS. Black-Right-Pointing-Pointer N{sup 1}- and N{sup 8}-acetylspermidine were determined by a column-free ESI-MS/MS. Black-Right-Pointing-Pointer The method was applied to determine activities of APAO, SMO, and SSAT in the pathway. Black-Right-Pointing-Pointer The assay method contained stable isotope-labeled natural substrates. Black-Right-Pointing-Pointer It is applicable to biological samples containing natural substrate and product. - Abstract: An analytical method for the determination of three polyamines (putrescine, spermidine, and spermine) and five acetylpolyamines [N{sup 1}-acetylspermidine (N{sup 1}AcSpd), N{sup 8}-acetylspermidine (N{sup 8}AcSpd), N{sup 1}-acetylspermine, N{sup 1},N{sup 8}-diacetylspermidine, and N{sup 1},N{sup 12}-diacetylspermine] involved in the polyamine catabolic pathway has been developed using a hybrid tandem mass spectrometer. Heptafluorobutyryl (HFB) derivatives of these compounds and respective internal standards labeled with stable isotopes were analyzed simultaneously by TOF MS, based on peak areas appearing at appropriate m/z values. The isomers, N{sup 1}AcSpd and N{sup 8}AcSpd were determined from their fragment ions, the acetylamidopropyl and acetylamidobutyl groups, respectively, using MS/MS with {sup 13}C{sub 2}-N{sup 1}AcSpd and {sup 13}C{sub 2}-N{sup 8}AcSpd which have the {sup 13}C{sub 2}-acetyl group as an internal standard. The TOF MS method was successfully applied to measure the activity of enzymes involved in polyamine catabolic pathways, namely N{sup 1}-acetylpolyamine oxidase (APAO), spermine oxidase (SMO), and spermidine/spermine N{sup 1}-acetyltransferase (SSAT). The following natural substrates and products labeled with stable isotopes considering the application to biological samples were identified; for APAO, [4,9,12-{sup 15}N{sub 3}]-N{sup 1}-acetylspermine and [1,4,8-{sup 15}N{sub 3

  17. Mass spectrometric determination of the thermodynamic excess properties of ternary Fe-Co-Cr melts

    International Nuclear Information System (INIS)

    Schmidt, Harald; Tomiska, Josef

    2004-01-01

    Computer-aided Knudsen cell mass spectrometry is used for the thermodynamic investigations on ternary Fe-Co-Cr melts over the entire range of composition. The thermodynamic mixing behavior has been determined by means of the 'digital intensity-ratio' (DIR) method. The ternary thermodynamically adapted power (TAP) series concept is used for the algebraic representation of the molar excess properties. The corresponding TAP parameters, and the values of the molar excess quantities Z E (T, x) (Z is the Gibbs energy G, heat of mixing H, entropy S) as well as the thermodynamic activities of all three constituents at 1950 K are presented

  18. Determination of cilnidipine, a new calcium antagonist, in human plasma using high performance liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Zhang, Xianhua; Zhai, Suodi; Zhao, Rongsheng; Ouyang, Jin; Li, Xiaoguang; Baeyens, Willy R G

    2007-09-26

    A rapid, sensitive and reliable high performance liquid chromatographic method coupled with tandem mass spectrometry (HPLC-MS/MS) has been developed and validated for the determination of cilnidipine, a relatively new calcium antagonist, in human plasma. The reversed-phase chromatographic system was interfaced with a TurboIonSpray (TIS) source. Nimodipine was employed as the internal standard (IS). Sample extracts following protein precipitation were injected into the HPLC-MS/MS system. The analyte and IS were eluted isocratically on a C18 column, with a mobile phase consisting of CH(3)OH and NH(4)Ac (96:4, v/v). The ions were detected by a triple quadrupole mass spectrometric detector in the negative mode. Quantification was performed using multiple reaction monitoring (MRM) of the transitions m/z 491.2-->122.1 and m/z 417.1-->122.1 for cilnidipine and for the IS, respectively. The analysis time for each run was 3.0 min. The calibration curve fitted well over the concentration range of 0.1-10 ngmL(-1), with the regression equation Y=(0.103+/-0.002)X+(0.014+/-0.003) (n=5), r=0.9994. The intra-day and inter-day R.S.D.% were less than 12.51% at all concentration levels within the calibration range. The recoveries were between 92.71% and 97.64%. The long-term stability and freeze-thaw stability were satisfying at each level. The present method provides a modern, rapid and robust tool for pharmacokinetic studies of cilnidipine.

  19. Mass spectrometric determination of the predominant adrenergic protoalkaloids in bitter orange (Citrus aurantium).

    Science.gov (United States)

    Nelson, Bryant C; Putzbach, Karsten; Sharpless, Katherine E; Sander, Lane C

    2007-11-28

    The predominant adrenergic protoalkaloid found in the peel and fruit of bitter orange, Citrus aurantium, is synephrine. Synephrine is reputed to have thermogenic properties and is used as a dietary supplement to enhance energy and promote weight loss. However, there exists some concern that the consumption of dietary supplements containing synephrine or similar protoalkaloids may contribute to adverse cardiovascular events. This study developed and validated a positive-ion mode liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the quantitative determination of the major (synephrine) and minor (tyramine, N-methyltyramine, octopamine, and hordenine) adrenergic protoalkaloids in a suite of National Institute of Standards and Technology (NIST) bitter orange Standard Reference Materials (SRMs): SRM 3258 Bitter Orange Fruit, SRM 3259 Bitter Orange Extract, and SRM 3260 Bitter Orange Solid Oral Dosage Form. The limit of quantitation (LOQ) for all protoalkaloids is approximately 1 pg on-column, except for octopamine (20 pg on-column). Additionally, the method has a linear dynamic range of > or =3 orders of magnitude for all of the protoalkaloids. Individual, as well as "total", protoalkaloid levels (milligrams per kilogram) in the NIST SRMs were determined and compared to the levels measured by an independent liquid chromatography/fluorescence detection (LC/FD) method. Satisfactory concordance between the LC/MS/MS and LC/FD protoalkaloid measurements was demonstrated. LC/MS/MS analysis of the protoalkaloids in the SRMs resulted in mean measurement imprecision levels of < or =10% coefficient of variation (% CV).

  20. An indirect atomic absorption spectrometric determination of ciprofloxacin, amoxycillin and diclofenac sodium in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    MAHMOUD MOHAMED ISSA

    2008-05-01

    Full Text Available A highly sensitive indirect atomic absorption spectrophotometric (AAS method has been developed for the determination of very low concentrations of ciprofloxacin, amoxycillin and diclofenac sodium. The method is based on the oxidation of these drugs with iron(III. The excess of iron(III was extracted into diethyl ether and then the iron(II in the aqueous layer was aspirated into an air–acetylene flame and determined by AAS. The linear concentration ranges were 25–400, 50–500 and 60–600 ng ml-1 for ciprofloxacin, amoxycillin and diclofenac sodium, respectively. The results were statistically compared with the official method using t- and f-test at p < 0.05. There were insignificant interferences from most of the excipients present. The intra- and inter-day assay coefficients of variation were less than 6.1 % and the recoveries ranged from 95 to 103 %. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

  1. A computer program for nuclear fuel burnup determination using gamma spectrometric methods

    International Nuclear Information System (INIS)

    Dobrin, Relu; Pavelescu, Margarit

    2010-01-01

    In the end of its service life in the reactor, the fuel needs to be characterized for reasons relating both to safety and economy. The main investigations carried out are oriented towards verifying the fuel cladding integrity and determining the fissile content and the fuel burnup. A computer program for fast burnup evaluation was developed at the Post-Irradiation Examination Laboratory (PIEL) from INR Pitesti, the only laboratory of this kind in Romania. The input data consists, on one hand, of axial and radial gamma-scanning profiles (for the experimental evaluation of the number of nuclei of a given fission product - selected as burnup monitor - in the end of irradiation) and, on the other hand, of the history of irradiation (the time length and relative value of the neutron flux for each step of irradiation). Using the equation for the build-up and decay of the burnup monitor during irradiation the flux value is iteratively adjusted until the calculated number of nucleus is equal to the experimental one. Then the flux value is used in the equations of evolution of the fissile and fertile nuclei to determine the number of fissions and consequently the fuel burnup. The program was successfully used in the analysis of more then one hundred of TRIGA and CANDU-type fuel rods. An experimental result is reported in some details. (authors)

  2. Technique for mass-spectrometric determination of moisture content in fuel elements and fuel element claddings

    International Nuclear Information System (INIS)

    Kurillovich, A.N.; Pimonov, Yu.I.; Biryukov, A.S.

    1988-01-01

    A technique for mass-spectroimetric determination of moisture content in fuel elements and fuek claddings in the 2x10 -4 -1.5x10 -2 g range is developed. The relative standard deviation is 0.13. A character of moisture extraction from oxide uranium fuels in the 20-700 deg C temperature range is studied. Approximately 80% of moisture is extracted from the fuels at 300 deg C. The moisture content in fuel elements with granular uranium oxide fuels is measured. Dependence of fuel element moisture content on conditions of hot vacuum drying is shown. The technique permits to optimize the fuel element fabrication process to decrease the moisture content in them. 4 refs.; 3 figs.; 2 tabs

  3. Determination of sirolimus in rabbit arteries using liquid chromatography separation and tandem mass spectrometric detection.

    Science.gov (United States)

    Zhang, Jun; Rodila, Ramona; Watson, Pamela; Ji, Qin; El-Shourbagy, Tawakol A

    2007-10-01

    Sirolimus, an effective immunosuppressive agent, is used for drug eluting stents. During stent development, an analytical method for the determination of sirolimus in tissue needs to be established. Normally, tissue samples are homogenized and then analyzed against the calibration standards prepared in a tissue homogenate. This approach provides insufficient control of the homogenization process. In this paper, tissue quality control samples were introduced for the optimization of the homogenization process during method development, but also allowance for the performance evaluation of the entire analytical process. In addition, a new approach using rabbit blood as a homogenization medium was developed to stabilize sirolimus in rabbit tissue homogenates. Calibration standards and quality controls were prepared by spiking different sirolimus working solutions into rabbit blood. Homogenization quality control samples were prepared by injecting other sirolimus working solutions into empty test tubes and pre-cut arteries within pre-defined masses. A high-throughput homogenization procedure was optimized based on the specific chemical properties of sirolimus. The linear dynamic range was between 49.9 pg/mL and 31.9 ng/mL to accommodate the expected artery homogenate concentrations. Additionally, quality controls in rabbit blood were also used in the extraction to support the calibration standards. The accuracy and precision of the quality controls in rabbit blood reflect the extraction performance and the accuracy and precision of the homogenization tissue quality controls reflect the overall performance of the method. The mean bias was between -4.5 and 0.2% for all levels of quality controls in the blood and between 4.8 and 14.9% for all levels of the homogenization tissue quality controls. The CVs of all concentration levels were < or =5.3% for the quality controls in blood and < or =9.2% for the homogenization tissue quality controls. The method was successfully

  4. A comparison of reliability of soil Cd determination by standard spectrometric methods

    Science.gov (United States)

    McBride, M.B.

    2015-01-01

    Inductively coupled plasma emission spectrometry (ICP-OES) is the most common method for determination of soil Cd, yet spectral and matrix interferences affect measurements at the available analytical wavelengths for this metal. This study evaluated the severity of the interference over a range of total soil Cd by comparing ICP-OES and ICP-MS measurements of Cd in acid digests. ICP-OES using the emission at 226.5 nm generally unable to quantify soil Cd at low (near-background) levels, and gave unreliable values compared to ICP-MS. Using the line at 228.nm, a marked positive bias in Cd measurement (relative to the 226.5 nm measurement) was attributable to As interference even at soil As concentrations below 10 mg/kg. This spectral interference in ICP-OES was severe in As-contaminated orchard soils, giving a false value for soil total Cd near 2 mg kg−1 when soil As was 100–150 mg kg−1. In attempting to avoid these ICP emission-specific interferences, we evaluated a method to estimate total soil Cd using 1 M HNO3 extraction followed by determination of Cd by flame atomic absorption (FAA), either with or without pre-concentration of Cd using an Aliquat-heptanone extractant. The 1 M HNO3 extracted an average of 82% of total soil Cd. The FAA method had no significant interferences, and estimated the total Cd concentrations in all soils tested with acceptable accuracy. For Cd-contaminated soils, the Aliquat-heptanone pre-concentration step was not necessary, as FAA sensitivity was adequate for quantification of extractable soil Cd and reliable estimation of total soil Cd. PMID:22031569

  5. Pharmacological dose of alpha-tocopherol induces cardiotoxicity in Wistar rats determined by echocardiography and histology

    Science.gov (United States)

    The effect of pharmacological dose of alpha-tocopherol on heart health was determined in Wistar rats. Animals were randomly assigned to either C (control, n = 11) or E (alpha-tocopherol, n = 11) group. Animals received corn oil (C) or alpha-tocopherol dissolved in corn oil (250 mg alpha-tocopherol/[...

  6. Fragment Formula Calculator (FFC): Determination of Chemical Formulas for Fragment Ions in Mass Spectrometric Data

    Science.gov (United States)

    Wegner, André; Weindl, Daniel; Jäger, Christian; Sapcariu, Sean C.; Dong, Xiangyi; Stephanopoulos, Gregory; Hiller, Karsten

    2015-01-01

    The accurate determination of mass isotopomer distributions (MID) is of great significance for stable isotope-labeling experiments. Most commonly, MIDs are derived from gas chromatography/electron ionization mass spectrometry (GC/EI-MS) measurements. The analysis of fragment ions formed during EI, which contain only specific parts of the original molecule can provide valuable information on the positional distribution of the label. The chemical formula of a fragment ion is usually applied to derive the correction matrix for accurate MID calculation. Hence, the correct assignment of chemical formulas to fragment ions is of crucial importance for correct MIDs. Moreover, the positional distribution of stable isotopes within a fragment ion is of high interest for stable isotope-assisted metabolomics techniques. For example, 13C-metabolic flux analyses (13C-MFA) are dependent on the exact knowledge of the number and position of retained carbon atoms of the unfragmented molecule. Fragment ions containing different carbon atoms are of special interest, since they can carry different flux information. However, the process of mass spectral fragmentation is complex, and identifying the substructures and chemical formulas for these fragment ions is nontrivial. For that reason, we developed an algorithm, based on a systematic bond cleavage, to determine chemical formulas and retained atoms for EI derived fragment ions. Here, we present the fragment formula calculator (FFC) algorithm that can calculate chemical formulas for fragment ions where the chemical bonding (e.g., Lewis structures) of the intact molecule is known. The proposed algorithm is able to cope with general molecular rearrangement reactions occurring during EI in GC/MS measurements. The FFC algorithm is able to integrate stable isotope labeling experiments into the analysis and can automatically exclude candidate formulas that do not fit the observed labeling patterns.1 We applied the FFC algorithm to create a

  7. [Flame atomic absorption spectrometric determination of H2O2 using (Au) core (Ag) shell nanoparticles].

    Science.gov (United States)

    Jiang, Zhi-Liang; Tang, Ya-Fang; Liang, Ai-Huiz; Gong, Qi

    2009-07-01

    The 10 nm gold nanoparticles were prepared by Frens procedure. Using tri-sodium citrate as reducer of AgNO3, and 10 nm gold nanoparticles as seed, the (Au)core(Ag)shell nanoparticles the size of about 30 nm were prepared at 90 degrees C for 10 min. Then it was separated by centrifuge at 10000 r x min(-1) for 15 min to obtain pure (Au)core(Ag)shell nanoparticles. In pH 3.8 sodium acetate-acetic acid buffer solution, hydroxyl free radical from Fenton reaction between Fe(II)-H2O2 oxidized (Au)core(Ag)shell nanoparticles to form silver ions. The silver ions in the centrifugal solutions can be measured by flame atomic absorption spectrometry at 328.1 nm. The silver ions in the centrifugal solutions increased with the H2O2 concentration increasing, and the absorption value at 328. 1 nm was enhanced linearly. The influence factors such as pH value, buffer solution volume, concentration of (Au)core(Ag)shell and Fe(II), reaction temperature and time, and centrifuging velocity and time were considered, respectively. Under the conditions of 0.20 mL pH 3.8 sodium acetate-acetic acid buffer solution, 50 microL of 2.0 mmol x L(-1) FeSO4, 60 microL of 2.94 x 10(-4) mol x L(-1) (Au)core(Ag)shell nanoparticle solution, reaction time of 20 min at 60 degrees C, and centrifugalization at 14 000 rpm for 10 min, the increased value deltaA is proportional to the H2O2 concentration (c) from 2. 64 to 42.24 micromol x L(-1), with a detection limit of 0.81 micromol x L(-1). The regress equation was deltaA = 0.014c-0.013 1, with a coefficient of 0.998 4. The effect of foreign substances such as 100-times glucose, Cu2+, Mg2+, Ca2+, 50-times urea, bovine serum albumin, Mn2+, Pb2+, and 30-times Cr3+ on the determination of 13.2 micromol x L(-1) H2O2 was examined respectively, with a relative error of +/- 10%. Results showed that there was no interference. This assay showed high sensitivity and good selectivity for quantitative determination of H2O2 in waste water samples, with satisfactory

  8. Determination of long-lived radionuclides at ultratrace level using advanced mass spectrometric techniques

    International Nuclear Information System (INIS)

    Zoriy, M.

    2005-11-01

    Determination of long-lived radionuclides at sub-fg concentration level is a challenging task in analytical chemistry. Inductively coupled plasma mass spectrometry (ICP-MS) with its ability to provide the sensitive and fast multielemental analysis is one of the most suitable method for the measurements of long lived radionuclides in the trace and ultra trace concentration range. In present the Ph.D. study a variety of procedures have been developed permitting the sub fg ml-1 determination of long-lived radionuclides (e.g. U, Th, Pu) as well as 226 Ra (T 1/2 = 1600 y) and 90 Sr (T 1/2 = 28.1 y) in different samples. In order to avoid isobaric interferences, to increase the sensitivity, precision and accuracy of the methods the application of different techniques: pre-concentration of the sample, off-line separation on the crown resin, measurements under cold plasma conditions, using microconcentric nebulizers (e.g DIHEN, DS-5) or the application of LA-ICP-MS for sample introduction have been studied. The limits of detection for different radionuclides was significantly improved in comparison to the ones reported in the literature, and, depending on the method applied, was varied from 10 -15 to 10 -18 g ml -1 concentration range. In addition to the analysis of long lived radionuclides, some other elements, that can present potential interest to the analyzed sample, were measured within the framework of the present study. Laser ablation inductively coupled plasma mass spectrometry (LAICP- MS) was used to produce images of element distribution in 20μm m thin sections of human brain tissue. The sample surface was scanned (raster area ∝80 mm 2 ) with a focused laser beam (wavelength 213 nm, diameter of laser crater 50μm, and laser power density 3x10 9 W cm -2 ) in a cooled laser ablation chamber developed for these measurements. Cross sections of human brain samples - hippocampus as well as brain tissues infected and non-infected with Glioblastoma Multiforme (tumor

  9. Fragment formula calculator (FFC): determination of chemical formulas for fragment ions in mass spectrometric data.

    Science.gov (United States)

    Wegner, André; Weindl, Daniel; Jäger, Christian; Sapcariu, Sean C; Dong, Xiangyi; Stephanopoulos, Gregory; Hiller, Karsten

    2014-02-18

    The accurate determination of mass isotopomer distributions (MID) is of great significance for stable isotope-labeling experiments. Most commonly, MIDs are derived from gas chromatography/electron ionization mass spectrometry (GC/EI-MS) measurements. The analysis of fragment ions formed during EI, which contain only specific parts of the original molecule can provide valuable information on the positional distribution of the label. The chemical formula of a fragment ion is usually applied to derive the correction matrix for accurate MID calculation. Hence, the correct assignment of chemical formulas to fragment ions is of crucial importance for correct MIDs. Moreover, the positional distribution of stable isotopes within a fragment ion is of high interest for stable isotope-assisted metabolomics techniques. For example, (13)C-metabolic flux analyses ((13)C-MFA) are dependent on the exact knowledge of the number and position of retained carbon atoms of the unfragmented molecule. Fragment ions containing different carbon atoms are of special interest, since they can carry different flux information. However, the process of mass spectral fragmentation is complex, and identifying the substructures and chemical formulas for these fragment ions is nontrivial. For that reason, we developed an algorithm, based on a systematic bond cleavage, to determine chemical formulas and retained atoms for EI derived fragment ions. Here, we present the fragment formula calculator (FFC) algorithm that can calculate chemical formulas for fragment ions where the chemical bonding (e.g., Lewis structures) of the intact molecule is known. The proposed algorithm is able to cope with general molecular rearrangement reactions occurring during EI in GC/MS measurements. The FFC algorithm is able to integrate stable isotope labeling experiments into the analysis and can automatically exclude candidate formulas that do not fit the observed labeling patterns.1 We applied the FFC algorithm to create

  10. Separation methods for radiometric and mass-spectrometric (ICP-MS) determination of technetium

    International Nuclear Information System (INIS)

    Bartosova, A.

    2005-01-01

    Declaration of specific activities of important radionuclides arisen by liquidation low-level nuclear waste represents an actual problem by decommissioning of NPP Jaslovske Bohunice. 99 Tc is an anthropological, long term half life radionuclide and belongs to the significant beta emitter with the influence on the radionuclides composition of the radwastes produced in NPP A-1 Jaslovske Bohunice. 99 Tc was determined in samples of soils, solid and liquid radioactive wastes from NPP Jaslovske Bohunice. 1. Several sorbents for Tc-99 separation were prepared. The prepared extraction materials were based on: Aliquat-336/ Polymer 7K1195, Aliquat-336/Teflon, Aliquat-336/hydrophobized silica gel with different concentrations of anchored quaternary amine (Aliquat-336), TOA/silica gel and TOA/Teflon. Prepared sorbents anchored on Teflon and polymer were not suitable as chromatographic bed material because of their non porously surface. Prepared sorbents based on TOA/Teflon Alq./ Teflon were viscously in the concentration range of amines (30%-60%), in concentration in the range (10%-20%) were amines sorbed with low yields - bounded Aliquat-336 on the prepared sorbent were about 4%-18%. It was found out: - By Tc desorption using prepared sorbents based on Aliquat-336/Polymer 7K1195 and Aliquat-336/Teflon were not reached satisfying recoveries - Organic phase - TOA was eluted with 99 mTcO 4 - by Tc desorption using sorbents TOA/silica gel and TOA/Teflon. 2. The best for effective separation of Tc-99 was found out the chromatographic material based on Aliquat-336 and hydrophobized silica gel. The highest retention of pertechnate was obtained in 0.1 mol.dm -3 HNO 3 media - chemical recovery of the sorption was nearly 100%. The elution of 99 mTcO 4 - was also tested with nitric acid concentration in the range 0.1-8 mol.dm -3 . The highest yields were using 20 ml of 8 mol.dm -3 HNO 3 - R=96.4%. The highest K D value of 99m TcO 4 - 2778 ml.g -1 were obtained in 0.1 mol. dm -3 HNO 3

  11. Honeybee Venom Proteome Profile of Queens and Winter Bees as Determined by a Mass Spectrometric Approach

    Science.gov (United States)

    Danneels, Ellen L.; Van Vaerenbergh, Matthias; Debyser, Griet; Devreese, Bart; de Graaf, Dirk C.

    2015-01-01

    Venoms of invertebrates contain an enormous diversity of proteins, peptides, and other classes of substances. Insect venoms are characterized by a large interspecific variation resulting in extended lists of venom compounds. The venom composition of several hymenopterans also shows different intraspecific variation. For instance, venom from different honeybee castes, more specifically queens and workers, shows quantitative and qualitative variation, while the environment, like seasonal changes, also proves to be an important factor. The present study aimed at an in-depth analysis of the intraspecific variation in the honeybee venom proteome. In summer workers, the recent list of venom proteins resulted from merging combinatorial peptide ligand library sample pretreatment and targeted tandem mass spectrometry realized with a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR MS/MS). Now, the same technique was used to determine the venom proteome of queens and winter bees, enabling us to compare it with that of summer bees. In total, 34 putative venom toxins were found, of which two were never described in honeybee venoms before. Venom from winter workers did not contain toxins that were not present in queens or summer workers, while winter worker venom lacked the allergen Api m 12, also known as vitellogenin. Venom from queen bees, on the other hand, was lacking six of the 34 venom toxins compared to worker bees, while it contained two new venom toxins, in particularly serine proteinase stubble and antithrombin-III. Although people are hardly stung by honeybees during winter or by queen bees, these newly identified toxins should be taken into account in the characterization of a putative allergic response against Apis mellifera stings. PMID:26529016

  12. Honeybee venom proteome profile of queens and winter bees as determined by a mass spectrometric approach.

    Science.gov (United States)

    Danneels, Ellen L; Van Vaerenbergh, Matthias; Debyser, Griet; Devreese, Bart; de Graaf, Dirk C

    2015-10-30

    Venoms of invertebrates contain an enormous diversity of proteins, peptides, and other classes of substances. Insect venoms are characterized by a large interspecific variation resulting in extended lists of venom compounds. The venom composition of several hymenopterans also shows different intraspecific variation. For instance, venom from different honeybee castes, more specifically queens and workers, shows quantitative and qualitative variation, while the environment, like seasonal changes, also proves to be an important factor. The present study aimed at an in-depth analysis of the intraspecific variation in the honeybee venom proteome. In summer workers, the recent list of venom proteins resulted from merging combinatorial peptide ligand library sample pretreatment and targeted tandem mass spectrometry realized with a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR MS/MS). Now, the same technique was used to determine the venom proteome of queens and winter bees, enabling us to compare it with that of summer bees. In total, 34 putative venom toxins were found, of which two were never described in honeybee venoms before. Venom from winter workers did not contain toxins that were not present in queens or summer workers, while winter worker venom lacked the allergen Api m 12, also known as vitellogenin. Venom from queen bees, on the other hand, was lacking six of the 34 venom toxins compared to worker bees, while it contained two new venom toxins, in particularly serine proteinase stubble and antithrombin-III. Although people are hardly stung by honeybees during winter or by queen bees, these newly identified toxins should be taken into account in the characterization of a putative allergic response against Apis mellifera stings.

  13. Liquid Chromatography-Tandem Mass Spectrometric Assay for Determination of Stavudine in Human Plasma

    Directory of Open Access Journals (Sweden)

    Fengdan Jin

    2014-01-01

    Full Text Available A LC-MS/MS method for determination of stavudine in human plasma was established and validated, and it was applied to the pharmaceutical formulations bioequivalence study. 0.5 mL plasma sample was extracted by liquid-liquid extraction. Stavudine was detected by a LC-MS/MS system. The pharmacokinetic parameters of stavudine in different formulations were calculated by noncompartment model statistics. The method was linear over the concentration ranges 5.00–1000 ng/mL in plasma. The intra- and interassay relative standard deviation (RSD was <10%. The average accuracies for the assay at three concentrations (5.00, 80.0, and 900 ng/mL were from 100.2% to 102.5%. Pharmacokinetic parameters of stavudine reference formulation were obtained as follows: Tmax was 0.6±0.2 h, Cmax was 480.7±150.9 g/L, t1/2 was 1.7±0.4 h, and AUC0-t was 872.8±227.8 g·h/L, and pharmacokinetic parameters of stavudine test formulation were obtained as follows: Tmax was 0.5±0.2 h, Cmax was 537.5±178.5 g/L, t1/2 was 1.7±0.3 h, and AUC0-t was (914.1±284.5 g·h/L. Calculated with AUC0-t, the bioavailability of two formulations was 105.0%.

  14. Determination of radium-226 by high-resolution alpha spectrometry

    International Nuclear Information System (INIS)

    Sill, C.W.

    1983-01-01

    The determination of radium-226 by alpha spectrometry has been investigated critically to determine experimental conditions under which high resolution and accurate and reliable results can be obtained. Refractory solids such as soils, ores, and tailings from uranium mills are dissolved completely by fusion with potassium fluoride in the presence of barium-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion with simultaneous volatilization of all silica and fluoride. Radium is precipitated with barium already present in the sample by addition of lead perchlorate to a dilute hydrochloric acid solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of diethylenetriaminepentaacetic acid, and the radium and barium sulfates are reprecipitated with acetic acid. The precipitate is mounted on a membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution of the subsequent alpha spectra is much better than has been achieved previously from barium sulfate, and is almost as good as is obtainable with actinides electrodeposited on polished steel plates. The resolution is about 60 keV full-width-half-maximum with 100 μg of barium on a 1-inch filter with a 450 mm 2 detector at 20% counting efficiency. Recovery is about 97% and accuracy is generally as good as the counting statistics obtained will permit. Grossly inaccurate results can be obtained under certain conditions when barium-133 tracer is used to determine the chemical yield of radium-226. Severe contamination of the surface-barrier detector by polonium-210 and by recoil products of the radium isotopes being counted is demonstrated, amd methods for virtual elimination of both problems are discussed

  15. Determination of {sup 227}Ac by {alpha}-particle spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martin, P. [Environmental Research Inst. of the Supervising Scientist, Jabiru, NT (Australia); Hancock, G.J. [Commonwealth Scientific and Industrial Research Organization, Canberra, ACT (Australia). Div. of Water Resources; Paulka, S. [Australian Radiation Lab., Yallambie, VIC (Australia); Akber, R.A. [Queensland Univ. of Technology, Brisbane, QLD (Australia)

    1995-10-01

    A method is described for the determination of {sup 227}Ac concentration in environmental samples. Actinium is separated from the sample digest by co-precipitation with lead sulphate, purified using anion and cation exchange techniques, and electrodeposited onto a stainless-steel disc. The chemical yield is monitored by addition of a {sup 229}Th/{sup 225}Ra/{sup 225}Ac tracer before sample dissolution. {sup 225}Ac recovery is determined from an initial count by measurement of its {alpha}-emitting daughter, {sup 217}At. The disc is then stored for 2-3 months and recounted. The {sup 227}Ac activity is obtained by measurement of the ingrown {sup 227}Th and {sup 223}Ra activities in the 5.38-6.10 MeV region. Co-precipitation with lead sulphate enables the convenient determination of actinium, thorium and radium on the same sample digest. (author).

  16. Determination of substraces of alpha emitter elements in water

    International Nuclear Information System (INIS)

    Gascon, J.L.

    1990-01-01

    To determine alpha emitter elements in water by alpha spectrometry, it is necessary to use large volumes of samples, concentration techniq-ues and to separate the elements of interest. In this report a study is presented about two concentration techniques and the process of analysis. Firstly, the stages of concentration method by iron hydroxide coprecipitation were studied in order to improve the results. The combination of liquid-liquid extraction and ion exchange techniques was the best way. Secondly, the technique by adsorption on manganese dioxide was studied. To apply this technique it was necessary to develop analysis methods to separate uranium, thorium, plutonium, americium and radium. These methods were designed combining several techniques of separation: liquid-liquid extraction, liquid-solid extraction, ionic exchange and coprecipitation. After the analysis methods were developped the adsorption on manganese dioxide with artificial samples was studied in the laboratory. Finally, the method of adsorption on manganese dioxide was studied to determine uranium, thorium and radium in the drinking water of Madrid. (Author)

  17. Determination of alpha_s using jet cross section parameterizations at hadron colliders

    CERN Document Server

    Stenzel, H

    2001-01-01

    Precise measurements of the single inclusive jet cross section have been performed by the TEVATRON experiments and will be provided by the LHC experiments extending to larger values of transverse energy. Theoretical predictions of this observable at NLO in perturbative QCD depend both on the PDF parameterization set and on the value of the strong coupling constant alpha_s. In this paper the dependence of the jet cross section on alpha_s is investigated. A method is presented to extract alpha_s(E_T) from a cross section measurement based on a parameterization of the alpha_s dependence. Systematic uncertainties and the E_T-range of applicability are discussed. A comparative study is performed between the case of ppbar at sqrt{s}=1.8 TeV (TEVATRON) and pp scattering at sqrt{s}=14 TeV (LHC).

  18. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    The spectrometric analysis of a mixture of two chemically and spectroscopically similar compounds is illustrated for the simultaneous spectrometric determination of caffeine and theobromine, the primary stimulants in coffee and tea, based on their ultraviolet absorbances. Their analysis indicates that such measurements ...

  19. Jet Production in ep Collisions at High $Q^2$ and Determination of $\\alpha_s$

    CERN Document Server

    Aaron, F.D.; Alimujiang, K.; Andreev, V.; Antunovic, B.; Asmone, A.; Backovic, S.; Baghdasaryan, A.; Barrelet, E.; Bartel, W.; Begzsuren, K.; Belousov, A.; Bizot, J.C.; Boudry, V.; Bozovic-Jelisavcic, I.; Bracinik, J.; Brandt, G.; Brinkmann, M.; Brisson, V.; Bruncko, D.; Bunyatyan, A.; Buschhorn, G.; Bystritskaya, L.; Campbell, A.J.; Cantun Avila, K.B.; Cassol-Brunner, F.; Cerny, K.; Cerny, V.; Chekelian, V.; Cholewa, A.; Contreras, J.G.; Coughlan, J.A.; Cozzika, G.; Cvach, J.; Dainton, J.B.; Daum, K.; Deak, M.; de Boer, Y.; Delcourt, B.; Del Degan, M.; Delvax, J.; De Roeck, A.; De Wolf, E.A.; Diaconu, C.; Dodonov, V.; Dossanov, A.; Dubak, A.; Eckerlin, G.; Efremenko, V.; Egli, S.; Eliseev, A.; Elsen, E.; Falkiewicz, A.; Faulkner, P.J.W.; Favart, L.; Fedotov, A.; Felst, R.; Feltesse, J.; Ferencei, J.; Fischer, D.-J.; Fleischer, M.; Fomenko, A.; Gabathuler, E.; Gayler, J.; Ghazaryan, Samvel; Glazov, A.; Glushkov, I.; Goerlich, L.; Gogitidze, N.; Gouzevitch, M.; Grab, C.; Greenshaw, T.; Grell, B.R.; Grindhammer, G.; Habib, S.; Haidt, D.; Helebrant, C.; Henderson, R.C.W.; Hennekemper, E.; Henschel, H.; Herbst, M.; Herrera, G.; Hildebrandt, M.; Hiller, K.H.; Hoffmann, D.; Horisberger, R.; Hreus, T.; Jacquet, M.; Janssen, M.E.; Janssen, X.; Jemanov, V.; Jonsson, L.; Jung, Andreas Werner; Jung, H.; Kapichine, M.; Katzy, J.; Kenyon, I.R.; Kiesling, C.; Klein, M.; Kleinwort, C.; Kluge, T.; Knutsson, A.; Kogler, R.; Korbel, V.; Kostka, P.; Kraemer, M.; Krastev, K.; Kretzschmar, J.; Kropivnitskaya, A.; Kruger, K.; Kutak, K.; Landon, M.P.J.; Lange, W.; Lastovicka-Medin, G.; Laycock, P.; Lebedev, A.; Leibenguth, G.; Lendermann, V.; Levonian, S.; Li, G.; Lipka, K.; Liptaj, A.; List, B.; List, J.; Loktionova, N.; Lopez-Fernandez, R.; Lubimov, V.; Lytkin, L.; Makankine, A.; Malinovski, E.; Marage, P.; Marti, Ll.; Martyn, H.-U.; Maxfield, S.J.; Mehta, A.; Meyer, A.B.; Meyer, H.; Meyer, H.; Meyer, J.; Michels, V.; Mikocki, S.; Milcewicz-Mika, I.; Moreau, F.; Morozov, A.; Morris, J.V.; Mozer, Matthias Ulrich; Mudrinic, M.; Muller, K.; Murin, P.; Naroska, B.; Naumann, Th.; Newman, P.R.; Niebuhr, C.; Nikiforov, A.; Nowak, G.; Nowak, K.; Nozicka, M.; Olivier, B.; Olsson, J.E.; Osman, S.; Ozerov, D.; Palichik, V.; Panagoulias, I.; Pandurovic, M.; Papadopoulou, Th.; Pascaud, C.; Patel, G.D.; Pejchal, O.; Perez, E.; Petrukhin, A.; Picuric, I.; Piec, S.; Pitzl, D.; Placakyte, R.; Pokorny, B.; Polifka, R.; Povh, B.; Preda, T.; Radescu, V.; Rahmat, A.J.; Raicevic, N.; Raspiareza, A.; Ravdandorj, T.; Reimer, P.; Rizvi, E.; Robmann, P.; Roland, B.; Roosen, R.; Rostovtsev, A.; Rotaru, M.; Ruiz Tabasco, J.E.; Rurikova, Z.; Rusakov, S.; Salek, D.; Sankey, D.P.C.; Sauter, M.; Sauvan, E.; Schmitt, S.; Schmitz, C.; Schoeffel, L.; Schoning, A.; Schultz-Coulon, H.-C.; Sefkow, F.; Shaw-West, R.N.; Sheviakov, I.; Shtarkov, L.N.; Shushkevich, S.; Sloan, T.; Smiljanic, Ivan; Soloviev, Y.; Sopicki, P.; South, D.; Spaskov, V.; Specka, Arnd E.; Staykova, Z.; Steder, M.; Stella, B.; Stoicea, G.; Straumann, U.; Sunar, D.; Sykora, T.; Tchoulakov, V.; Thompson, G.; Thompson, P.D.; Toll, T.; Tomasz, F.; Tran, T.H.; Traynor, D.; Trinh, T.N.; Truol, P.; Tsakov, I.; Tseepeldorj, B.; Turnau, J.; Urban, K.; Valkarova, A.; Vallee, C.; Van Mechelen, P.; Vargas Trevino, A.; Vazdik, Y.; Vinokurova, S.; Volchinski, V.; von den Driesch, M.; Wegener, D.; Wissing, Ch.; Wunsch, E.; Zacek, J.; Zalesak, J.; Zhang, Z.; Zhokin, A.; Zimmermann, T.; Zohrabyan, H.; Zomer, F.; Zus, R.

    2010-01-01

    The production of jets is studied in deep-inelastic ep scattering at large negative four momentum transfer squared 150determined from these measurements is alpha_s(M_Z) = 0.1168 +/-0.0007 (exp.) +0.0046/-0.0030 (th.) +/-0.0016(pdf).

  20. Development and application of mass spectrometric techniques for ultra-trace determination of236U in environmental samples-A review.

    Science.gov (United States)

    Bu, Wenting; Zheng, Jian; Ketterer, Michael E; Hu, Sheng; Uchida, Shigeo; Wang, Xiaolin

    2017-12-01

    Measurements of the long-lived radionuclide 236 U are an important endeavor, not only in nuclear safeguards work, but also in terms of using this emerging nuclide as a tracer in chemical oceanography, hydrology, and actinide sourcing. Depending on the properties of a sample and its neutron irradiation history, 236 U/ 238 U ratios from different sources vary significantly. Therefore, this ratio can be treated as an important fingerprint for radioactive source identification, and in particular, affords a definitive means of discriminating between naturally occurring U and specific types of anthropogenic U. The development of mass spectrometric techniques makes it possible to determine ultra-trace levels of 236 U in environmental samples. In this paper, we review the current status of mass spectrometric approaches for determination of 236 U in environmental samples. Various sample preparation methods are summarized and compared. The mass spectrometric techniques emphasized herein are thermal ionization mass spectrometry (TIMS), inductively coupled plasma mass spectrometry (ICP-MS) and accelerator mass spectrometry (AMS). The strategies or principles used by each technique for the analysis of 236 U are described. The performances of these techniques in terms of abundance sensitivity and detection limit are discussed in detail. To date, AMS exhibits the best capability for ultra-trace determinations of 236 U. The levels and behaviors of 236 U in various environmental media are summarized and discussed as well. Results suggest that 236 U has an important, emerging role as a tracer for geochemical studies. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Determination of natural alpha-emitting isotopes of uranium and thorium in environmental and geological samples

    International Nuclear Information System (INIS)

    Crespo, M.T.

    1996-01-01

    It is described the complete radiochemical procedure used for the determination of uranium and thorium isotopes in environmental and geological samples by alpha spectrometry. Source preparation methods, alpha-counting and spectral analysis are also included

  2. Bulk is a determinant of oxymetazoline affinity for the alpha1A-adrenergic receptor.

    Science.gov (United States)

    McCune, Dan; Gaivin, Robert; Rorabaugh, Boyd; Perez, Dianne

    2004-01-01

    The alpha1A-adrenergic receptor (AR) has a higher affinity for several agonists and antagonists compared to alpha1B or alpha1D ARs. Mutagenesis studies were used to determine residues potentially responsible for this subtype selectivity. Oxymetazoline has a 50-fold lower affinity for alpha1D ARs compared to alpha1A ARs and also displayed a significant loss of affinity for an alpha1A Leu-290 to Phe mutant. It was concluded that steric interactions between the alpha1D ARs Phe-360 and the bulkytert-butyl group of oxymetazoline partially accounts for this lower affinity. Thus, the alpha1A AR binding pocket may more easily accommodate bulk at the paraposition of the phenyl ring than the alpha1D AR.

  3. Development and method of use of a mass spectrometric isotope dilution analysis within the use of negative thermoionisation for determination of boron traces

    International Nuclear Information System (INIS)

    Zeininger, H.

    1984-01-01

    A mass spectrometric trace boron determination using negative thermionisation was developed. It is based on the determination of the ratio of BO 2 - isotopes ( 10 B and 11 B). A high stability and a constant intensity at a given temperature of the BO 2 - ion currents allow for a computer controlled measurement with a programmed heating. The reproducibility lies at around 0,004-0,08%. The boron determination using Mels potentiometry with a BF 4 - -ion selective electrode was used as an analytical comparison method. The MS-IDA was first used on metal samples, such as Al, Zr, and steel. Later on the boron in reagents, biological material (milk powder, spinach, water plants) and water were determined. For this material-dependent hydrolysation and separation procedures were worked out. The MS-IDA in comparison to all other analytical methods used by other collaborators offers the greatest accuracy. (RB) [de

  4. A liquid chromatography-mass spectrometric method for the determination of oak moss allergens atranol and chloroatranol in perfumes

    DEFF Research Database (Denmark)

    Bossi, Rossana; Rastogi, Suresh Chandra; Bernard, Guillaume

    2004-01-01

    This paper describes a validated liquid chromatographic-tandem mass spectrometric method for quantitative analysis of the potential oak moss allergens atranol and chloroatranol in perfumes and similar products. The method employs LC-MS-MS with electrospray ionization (ESI) in negative mode...... of detection, 5.0 ng/mL and 2.4 ng/mL, respectively, for atranol and chloroatranol, achieved by this method allowed identification of these compounds at concentrations below those causing allergic skin reactions in oak-moss-sensitive patients. The recovery of chloratranol from spiked perfumes was 96+/-4%. Low...... recoveries (49+/-5%) were observed for atranol in spiked perfumes, indicating ion suppression caused by matrix components. The method has been applied to the analysis of 10 randomly selected perfumes and similar products....

  5. Determination of radium-226 by high-resolution alpha spectrometry

    International Nuclear Information System (INIS)

    Sill, C.W.

    1983-01-01

    Condition were determined under which high resolution and accurate and reliable results can be obtained. Refractory solids are dissolved completely by fusion with KF and Ba-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion. Radium is precipitated with barium by addition of lead perchlorate to a dilute HCl solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of DTPA and the Ra and Ba sulfates are reprecipitated with acetic acid to produce very small crystals. The precipitate is mounted on 0.1-μm membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution, almost as good as with actinides electrodeposited on polished steel plates, is about 60 keV full-width-half-maximum with 100 μg of barium on a 1-inch filter with a 450 mm 2 detector at 20% counting efficiency. Recovery is about 97%. One solid sample can be prepared for counting in less than 2 hours. Methods are discussed for ensuring reliability of the results. Severe contamination of the surface-barrier detector by polonium-210 and recoil products is discussed

  6. Simultaneous determinations of uranium, thorium, and plutonium in soft tissues by solvent extraction and alpha-spectrometry

    International Nuclear Information System (INIS)

    Singh, N.P.; Zimmerman, C.J.; Lewis, L.L.; Wrenn, M.E.

    1984-01-01

    A radiochemical procedure for the simultaneous determination of uranium, thorium, and plutonium, in soft tissues has been developed. The weighed amounts of tissues, spiked with 232 U, 242 Pu, and 229 th tracers, are wet ashed. Uranium, thorium, and plutonium are coprecipitated with iron as hydroxides, dissolved in concentrated HCl and the acidity adjusted to 10 M. Uranium and plutonium are extracted into 20% TLA solution in xylene, leaving thorium in the aqueous phase. Plutonium is back-extracted by reducing to the trivalent state with 0.05 M NH 4 I solution in 8 M HCl, and uranium is back-extracted with 0.1 M HCl. Thorium is extracted into 20% TLA solution from 4 M HNO 3 and back-extracted with 10 M HCl. Uranium, thorium and plutonium are electrodeposited separately onto platinum discs and counted alpha-spectrometrically using surface barrier silicon diodes and a multichannel analyzer. The method was developed using bovine liver and applied to dog and human tissues. The mean radiochemical recoveries of these actinides in different organs were better than 70%. 6 references, 2 tables

  7. The Use of Isotope Dilution Alpha Spectrometry and Liquid Scintillation Counting to Determine Radionuclides in Environmental Samples (abstract)

    Science.gov (United States)

    Bylyku, Elida

    2009-04-01

    In Albania in recent years it has been of increasing interest to determine various pollutants in the environment and their possible effects on human health. The radiochemical procedure used to identify Pu, Am, U, Th, and Sr radioisotopes in soil, sediment, water, coal, and milk samples is described. The analysis is carried out in the presence of respective tracer solutions and combines the procedure for Pu analysis based on anion exchange, the selective method for Sr isolation based on extraction chromatography using Sr-Spec resin, and the application of the TRU-Spec column for separation of Am fraction. An acid digestion method has been applied for the decomposition of samples. The radiochemical procedure involves the separation of Pu from Th, Am, and Sr by anion exchange, followed by the preconcentration of Am and Sr by coprecipitation with calcium oxalate. Am is separated from Sr by extraction chromatography. Uranium is separated from the bulk elements by liquid-liquid extraction using UTEVA® resin. Thin sources for alpha spectrometric measurements are prepared by microprecipitation with NdF3. Two International Atomic Energy Agency reference materials were analyzed in parallel with the samples.

  8. Measurement of event shape distributions and moments in $e^{+}e^{-} \\to$ hadrons at 91-209 GeV and a determination of $\\alpha_{s}$

    CERN Document Server

    Abbiendi, G.; Akesson, P.F.; Alexander, G.; Allison, John; Amaral, P.; Anagnostou, G.; Anderson, K.J.; Asai, S.; Axen, D.; Bailey, I.; Barberio, E.; Barillari, T.; Barlow, R.J.; Batley, R.J.; Bechtle, P.; Behnke, T.; Bell, Kenneth Watson; Bell, P.J.; Bella, G.; Bellerive, A.; Benelli, G.; Bethke, S.; Biebel, O.; Boeriu, O.; Bock, P.; Boutemeur, M.; Braibant, S.; Brown, Robert M.; Burckhart, H.J.; Campana, S.; Carnegie, R.K.; Carter, A.A.; Carter, J.R.; Chang, C.Y.; Charlton, D.G.; Ciocca, C.; Csilling, A.; Cuffiani, M.; Dado, S.; Roeck, A.De; Wolf, E.A.De; Desch, K.; Dienes, B.; Donkers, M.; Dubbert, J.; Duchovni, E.; Duckeck, G.; Duerdoth, I.P.; Etzion, E.; Fabbri, F.; Fanfani, A.; Ferrari, P.; Fiedler, F.; Fleck, I.; Ford, M.; Frey, A.; Gagnon, P.; Gary, John William; Geich-Gimbel, C.; Giacomelli, G.; Giacomelli, P.; Giunta, Marina; Goldberg, J.; Gross, E.; Grunhaus, J.; Gruwe, M.; Gunther, P.O.; Gupta, A.; Hajdu, C.; Hamann, M.; Hanson, G.G.; Harel, A.; Hauschild, M.; Hawkes, C.M.; Hawkings, R.; Hemingway, R.J.; Herten, G.; Heuer, R.D.; Hill, J.C.; Hoffman, Kara Dion; Horvath, D.; Igo-Kemenes, P.; Ishii, K.; Jeremie, H.; Jovanovic, P.; Junk, T.R.; Kanzaki, J.; Karlen, D.; Kawagoe, K.; Kawamoto, T.; Keeler, R.K.; Kellogg, R.G.; Kennedy, B.W.; Kluth, S.; Kobayashi, T.; Kobel, M.; Komamiya, S.; Kramer, T.; Krieger, P.; Krogh, J.von; Kuhl, T.; Kupper, M.; Lafferty, G.D.; Landsman, H.; Lanske, D.; Lellouch, D.; Lettso, J.; Levinson, L.; Lillich, J.; Lloyd, S.L.; Loebinger, F.K.; Lu, J.; Ludwig, A.; Ludwig, J.; Mader, W.; Marcellini, S.; Martin, A.J.; Masetti, G.; Mashimo, T.; Mattig, Peter; McKenna, J.; McPherson, R.A.; Meijers, F.; Menges, W.; Merritt, F.S.; Mes, H.; Meyer, Niels T.; Michelini, A.; Mihara, S.; Mikenberg, G.; Miller, D.J.; Mohr, W.; Montanari, A.; Mori, T.; Mutter, A.; Nagai, K.; Nakamura, I.; Nanjo, H.; Neal, H.A.; Nisius, R.; O'Neale, S.W.; Oh, A.; Oreglia, M.J.; Orito, S.; Pahl, C.; Pasztor, G.; Pater, J.R.; Pilcher, J.E.; Pinfold, J.; Plane, David E.; Pooth, O.; Przybycien, M.; Quadt, A.; Rabbertz, K.; Rembser, C.; Renkel, P.; Roney, J.M.; Rozen, Y.; Runge, K.; Sachs, K.; Saeki, T.; Sarkisyan, E.K.G.; Schaile, A.D.; Schaile, O.; Scharff-Hansen, P.; Schieck, J.; Schorner-Sadenius, T.; Schroder, Matthias; Schumacher, M.; Seuster, R.; Shears, T.G.; Shen, B.C.; Sherwood, P.; Skuja, A.; Smith, A.M.; Sobie, R.; Soldner-Rembold, S.; Spano, F.; Stahl, A.; Strom, David M.; Strohmer, R.; Tarem, S.; Tasevsky, M.; Teuscher, R.; Thomson, M.A.; Torrence, E.; Toya, D.; Tran, P.; Trigger, I.; Trocsanyi, Z.; Tsur, E.; Turner-Watson, M.F.; Ueda, I.; Ujvari, B.; Vollmer, C.F.; Vannerem, P.; Vertesi, R.; Verzocchi, M.; Voss, H.; Vossebeld, J.; Ward, C.P.; Ward, D.R.; Watkins, P.M.; Watson, A.T.; Watson, N.K.; Wells, P.S.; Wengler, T.; Wermes, N.; Wilson, G.W.; Wilson, J.A.; Wolf, G.; Wyatt, T.R.; Yamashita, S.; Zer-Zion, D.; Zivkovic, Lidija; CERN. Geneva

    2005-01-01

    We have studied hadronic events from e+e- annihilation data at centre-of-mass energies from 91 to 209 GeV. We present distributions of event shape observables and their moments at each energy and compare with QCD Monte Carlo models. From the event shape distributions we extract the strong coupling alpha_s and test its evolution with energy scale. The results are consistent with the running of alpha_s expected from QCD. Combining all data, the value of alpha_s (M_z) is determined to be alpha_s(Mz)=0.1191+-0.0005(stat.)+-0.0010 (expt.)+-0.0011(hadr.)+-0.0044(theo.) The energy evolution of the moments is also used to determine a value of alpha_ with slightly larger errors: alpha_s(Mz)=0.1223+-0.0005(stat.) +-0.0014(expt.) +-0.0016(hadr.) +0.0054 -0.0036 (theo).

  9. Vis-NIR spectrometric determination of Brix and sucrose in sugar production samples using kernel partial least squares with interval selection based on the successive projections algorithm.

    Science.gov (United States)

    de Almeida, Valber Elias; de Araújo Gomes, Adriano; de Sousa Fernandes, David Douglas; Goicoechea, Héctor Casimiro; Galvão, Roberto Kawakami Harrop; Araújo, Mario Cesar Ugulino

    2018-05-01

    This paper proposes a new variable selection method for nonlinear multivariate calibration, combining the Successive Projections Algorithm for interval selection (iSPA) with the Kernel Partial Least Squares (Kernel-PLS) modelling technique. The proposed iSPA-Kernel-PLS algorithm is employed in a case study involving a Vis-NIR spectrometric dataset with complex nonlinear features. The analytical problem consists of determining Brix and sucrose content in samples from a sugar production system, on the basis of transflectance spectra. As compared to full-spectrum Kernel-PLS, the iSPA-Kernel-PLS models involve a smaller number of variables and display statistically significant superiority in terms of accuracy and/or bias in the predictions. Published by Elsevier B.V.

  10. Gas chromatographic determination of pesticides in vegetable samples by sequential positive and negative chemical ionization and tandem mass spectrometric fragmentation using an ion trap analyser.

    Science.gov (United States)

    Hernando, M D; Agüera, A; Fernández-Alba, A R; Piedra, L; Contreras, M

    2001-01-01

    A selective and sensitive chromatographic method is described for the determination of nine organochlorine and organophosphorus pesticides in vegetable samples by gas chromatography-mass spectrometry. The proposed method combines the use of positive and negative chemical ionisation and tandem mass spectrometric fragmentation, resulting in a significant increase in selectivity and allowing the simultaneous confirmation and quantification of trace levels of pesticides in complex vegetable matrices. Parameters relative to ionisation and fragmentation processes were optimised to obtain maximum sensitivity. Repeatability and reproducibility studies yielded relative standard deviations lower than 25% in all cases. Identification criteria, such as retention time and relative abundance of characteristic product ions, were also evaluated in order to guarantee the correct identification of the target compounds. The method was applied to real vegetable samples to demonstrate its use in routine analysis.

  11. Experimental determination of alpha particle threshold detection in cellulose nitrate

    International Nuclear Information System (INIS)

    Knoefell, T.M.J.

    1978-01-01

    LR 115, type II, Kodak-Pathe cellulose nitrate pellicles were irradiated perpendicularly with monoenergetic alpha bemas in the energy range 2,5-5,5 Mev. The alpha particle beams were produced by an intense Am 241 source using Argon as energy attenuating. After irradiations, samples were etched with NaOH solutions without agitation at 60 0 C, by different time periods varying from 15 minutes to 3,5 hours. Measurements of density and track diameter were done using optical microscopy. The sample compositions were done by CHN method of combustion gas analysis showing good agreement with the composition of cellulose trinitrate. From detection threshold and from obtained results, the development of latent tracks only occur for alpha particles with stopping power superior to 0,87 +- 0,06 MeV.cm -2 .mg -1 , was verified. (M.C.K.) [pt

  12. Determination of the strong coupling constant $\\alpha_s$ in multijet production with the ATLAS detector at the LHC.

    CERN Document Server

    Llorente Merino, Javier; The ATLAS collaboration

    2018-01-01

    A measurement of transverse energy--energy correlations and its asymmetry in $pp$ collisions recorded by the ATLAS detector at the LHC at $\\sqrt{s} = 8$ TeV is presented. The results are intepreted as a precision test of Quantum Chromodynamics, used to determine the strong coupling constant $\\alpha_s(m_Z)$ and to test asymptotic freedom up to scales close to 1 TeV. A global fit to the transverse energy--energy correlation distributions yields $\\alpha_{\\mathrm{s}}(m_Z) = 0.1162 \\pm 0.0011 \\mbox{ (exp.)}^{+0.0084}_{-0.0070} \\mbox{ (theo.)}$, while a global fit to the asymmetry distributions yields a value of $\\alpha_{\\mathrm{s}}(m_Z) = 0.1196 \\pm 0.0013 \\mbox{ (exp.)}^{+0.0075}_{-0.0045} \\mbox{ (theo.)}$.

  13. A liquid chromatography-mass spectrometric method for the determination of oak moss allergens atranol and chloroatranol in perfumes.

    Science.gov (United States)

    Bossi, Rossana; Rastogi, Suresh C; Bernard, Guillaume; Gimenez-Arnau, Elena; Johansen, Jeanne D; Lepoittevin, Jean-Pierre; Menné, Torkil

    2004-05-01

    This paper describes a validated liquid chromatographic-tandem mass spectrometric method for quantitative analysis of the potential oak moss allergens atranol and chloroatranol in perfumes and similar products. The method employs LC-MS-MS with electrospray ionization (ESI) in negative mode. The compounds are analysed by selective reaction monitoring (SRM) of 2 or 3 ions for each compound in order to obtain high selectivity and sensitivity. The method has been validated for the following parameters: linearity; repeatability; recovery; limit of detection; and limit of quantification. The limits of detection, 5.0 ng/mL and 2.4 ng/mL, respectively, for atranol and chloroatranol, achieved by this method allowed identification of these compounds at concentrations below those causing allergic skin reactions in oak-moss-sensitive patients. The recovery of chloratranol from spiked perfumes was 96+/-4%. Low recoveries (49+/-5%) were observed for atranol in spiked perfumes, indicating ion suppression caused by matrix components. The method has been applied to the analysis of 10 randomly selected perfumes and similar products.

  14. Jet Production in ep Collisions at Low Q^2 and Determination of $\\alpha_{s}$

    CERN Document Server

    Aaron, F.D.; Alexa, C.; Andreev, V.; Antunovic, B.; Backovic, S.; Baghdasaryan, A.; Barrelet, E.; Bartel, W.; Begzsuren, K.; Belousov, A.; Bizot, J.C.; Boudry, V.; Bozovic-Jelisavcic, I.; Bracinik, J.; Brandt, G.; Brinkmann, M.; Brisson, V.; Bruncko, D.; Bunyatyan, A.; Buschhorn, G.; Bystritskaya, L.; Campbell, A.J.; Cantun Avila, K.B.; Cerny, K.; Cerny, V.; Chekelian, V.; Cholewa, A.; Contreras, J.G.; Coughlan, J.A.; Cozzika, G.; Cvach, J.; Dainton, J.B.; Daum, K.; Deak, M.; Delcourt, B.; Delvax, J.; De Wolf, E.A.; Diaconu, C.; Dodonov, V.; Dossanov, A.; Dubak, A.; Eckerlin, G.; Efremenko, V.; Egli, S.; Eliseev, A.; Elsen, E.; Falkiewicz, A.; Favart, L.; Fedotov, A.; Felst, R.; Feltesse, J.; Ferencei, J.; Fischer, D.J.; Fleischer, M.; Fomenko, A.; Gabathuler, E.; Gayler, J.; Ghazaryan, Samvel; Glazov, A.; Glushkov, I.; Goerlich, L.; Gogitidze, N.; Gouzevitch, M.; Grab, C.; Greenshaw, T.; Grell, B.R.; Grindhammer, G.; Habib, S.; Haidt, D.; Helebrant, C.; Henderson, R.C.W.; Hennekemper, E.; Henschel, H.; Herbst, M.; Herrera, G.; Hildebrandt, M.; Hiller, K.H.; Hoffmann, D.; Horisberger, R.; Hreus, T.; Jacquet, M.; Janssen, X.; Jonsson, L.; Jung, A.W.; Jung, H.; Kapichine, M.; Katzy, J.; Kenyon, I.R.; Kiesling, C.; Klein, M.; Kleinwort, C.; Kluge, T.; Knutsson, A.; Kogler, R.; Kosior, E.; Kostka, P.; Kraemer, M.; Krastev, K.; Kretzschmar, J.; Kropivnitskaya, A.; Kruger, K.; Kutak, K.; Landon, M.P.J.; Lange, W.; Lastovicka-Medin, G.; Laycock, P.; Lebedev, A.; Lendermann, V.; Levonian, S.; Li, G.; Lipka, K.; Liptaj, A.; List, B.; List, J.; Loktionova, N.; Lopez-Fernandez, R.; Lubimov, V.; Makankine, A.; Malinovski, E.; Marage, P.; Marti, Ll.; Martyn, H.U.; Maxfield, S.J.; Mehta, A.; Meyer, A.B.; Meyer, H.; Meyer, H.; Meyer, J.; Mikocki, S.; Milcewicz-Mika, I.; Moreau, F.; Morozov, A.; Morris, J.V.; Mozer, M.U.; Mudrinic, M.; Muller, K.; Murin, P.; Naumann, Th.; Newman, P.R.; Niebuhr, C.; Nikiforov, A.; Nikitin, D.; Nowak, G.; Nowak, K.; Olsson, J.E.; Osman, S.; Ozerov, D.; Palichik, V.; Panagoulias, I.; Pandurovic, M.; Papadopoulou, Th.; Pascaud, C.; Patel, G.D.; Pejchal, O.; Perez, E.; Petrukhin, A.; Picuric, I.; Piec, S.; Pitzl, D.; Placakyte, R.; Pokorny, B.; Polifka, R.; Povh, B.; Radescu, V.; Rahmat, A.J.; Raicevic, N.; Raspiareza, A.; Ravdandorj, T.; Reimer, P.; Rizvi, E.; Robmann, P.; Roland, B.; Roosen, R.; Rostovtsev, A.; Rotaru, M.; Tabasco, J.E.Ruiz; Rusakov, S.; Salek, D.; Sankey, D.P.C.; Sauter, M.; Sauvan, E.; Schmitt, S.; Schoeffel, L.; Schoning, A.; Schultz-Coulon, H.C.; Sefkow, F.; Shaw-West, R.N.; Shtarkov, L.N.; Shushkevich, S.; Sloan, T.; Smiljanic, Ivan; Soloviev, Y.; Sopicki, P.; South, D.; Spaskov, V.; Specka, A.; Staykova, Z.; Steder, M.; Stella, B.; Stoicea, G.; Straumann, U.; Sunar, D.; Sykora, T.; Tchoulakov, V.; Thompson, G.; Thompson, P.D.; Toll, T.; Tomasz, F.; Tran, T.H.; Traynor, D.; Trinh, T.N.; Truol, P.; Tsakov, I.; Tseepeldorj, B.; Turnau, J.; Urban, K.; Valkarova, A.; Vallee, C.; Van Mechelen, P.; Trevino, A.Vargas; Vazdik, Y.; Vinokurova, S.; Volchinski, V.; von den Driesch, M.; Wegener, D.; Wissing, Ch.; Wunsch, E.; Zacek, J.; Zalesak, J.; Zhang, Z.; Zhokin, A.; Zimmermann, T.; Zohrabyan, H.; Zomer, F.

    2010-01-01

    The production of jets is studied in deep-inelastic e+p scattering at low negative four momentum transfer squared 5alpha_s.

  15. Volatility of 210Po in the gross alpha determination

    Czech Academy of Sciences Publication Activity Database

    Světlík, Ivo; Belanová, A.; Vršková, M.; Hanslík, E.; Ivanovova, D.; Marešová, J.; Tomášková, Lenka; Nováková, Tereza

    2010-01-01

    Roč. 286, č. 2 (2010), s. 547-551 ISSN 0236-5731 R&D Projects: GA AV ČR IAAX00130801 Institutional research plan: CEZ:AV0Z10480505 Keywords : gross alpha * 210Po * polonium recovery Subject RIV: DL - Nuclear Waste, Radioactive Pollution ; Quality Impact factor: 0.777, year: 2010

  16. A mass spectrometric method for diagnosis of gastrointestinal infections by 13 C determination from respiratory CO2

    International Nuclear Information System (INIS)

    Cuna, Stela; Ursu, D.; Cuna, C.; Berdea, P.; Sparchez, Z.

    2000-01-01

    The use of stable carbon isotopes in metabolic research on humans and large animals is expanding rapidly due to the increasing variety of labelled compounds, greater availability of analytical facilities, and absence of health risk from radiation.This study is focused on a new mass spectrometric technique to diagnose Helicobacter pylori (HP) infection of the gastric mucosa which results in ulcers and some forms of gastric cancer. The method is based on measuring 13 C-enrichment in exhaled air by isotope ratios mass spectrometry. In this breath test, 13 C-labelled urea is given orally to the patient. If HP is present, the 13 C-urea is decomposed rapidly by these bacteria to 13 CO 2 which circulates to the lungs and is expelled in the breath where it can be detected. The protocol of the method is described and one example of the use of 13 C-urea is presented. The 13 C-enrichment in CO 2 exhaled is measured by mass spectrometry with double collector and the results are expressed in relative delta (δ) per mil ( o / oo ) units. The instrumental precision was ± 0.12 o / oo . The δ 13 C was measured in both pre and post - dose breath samples collected from infected patient at 20, 40 and 60 min post-dose. The results showed 13 C increases of > 25 o / oo at 40 min, in good agreement with the data of literature. We concluded that these breath tests are ideally suited to diagnose HP infection as a nonradioactive, noninvasive and applicable to subjects of any population method. (authors)

  17. Procedure for determination of alpha emitters in urine and dregs samples

    International Nuclear Information System (INIS)

    Serdeiro, Nelida H.

    2005-01-01

    The purpose of this work is to establish the procedure for the identification and quantification of emitting alpha radionuclides in urine and dregs samples. This procedure are applied to all laboratories of the countries of the Project ARCAL LXXVII that determinate alpha emitting radionuclides in biological samples for biological assessment [es

  18. Determination of the thermal neutron induced O-17(n,alpha) C-14 reaction cross section

    NARCIS (Netherlands)

    Wagemans, J; Wagemans, C; Bieber, R; Geltenbort, P

    1998-01-01

    The. O-17(n(th),alpha)C-14 reaction cross section was determined at the high flux reactor of the ILL in Grenoble relative to the known N-14(n(th),p)C-14 cross section. For the flux calibration measurements, N-14(2) from the air was used. The O-17(n,alpha) measurements were performed with several

  19. Spectrometric techniques 4

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  20. Spectrometric characteristics of polystyrene scintillation films

    CERN Document Server

    Astvatsaturov, A R; Gavalyan, V B; Gavalyan, V G

    1999-01-01

    The spectrometric characteristics of five types of polystyrene scintillation films with thicknesses of 10, 30, 50 and 80 mu m and of analogous 250 mu m thick plates irradiated with sup 2 sup 3 sup 9 Pu, sup 2 sup 3 sup 8 Pu and sup 2 sup 2 sup 6 Ra sources of alpha-particles have been studied. The prospects of utilization of scintillation films as radiators for detection of heavy charged particles and measurement of their energy was experimentally shown.

  1. Ionic liquid-linked dual magnetic microextraction of lead(II) from environmental samples prior to its micro-sampling flame atomic absorption spectrometric determination.

    Science.gov (United States)

    Yilmaz, Erkan; Soylak, Mustafa

    2013-11-15

    A novel and rapid microextraction approach termed as ionic liquid-linked dual magnetic microextraction (IL-DMME), was developed for the atomic absorption spectrometric determination of lead. The developed method based on a combination of dispersive liquid-liquid microextraction (DLLME) and dispersive micro solid-phase extraction (D-μ-SPE). In the first DLLME step, 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6], was selected to extract the lead-pyrrolidine-dithiocarbamate (Pb-PDC) complex from sample solution by the assistance of vortex agitator. After the first step, fifty milligrams of Fe3O4 magnetic nanoparticles (MNPs) were added to extraction of the ionic liquid and Pb-PDC complex in aqueous solution. The effective factors in proposed IL-DMME procedure, including volume of 1-butyl-3-methylimidazolium hexafluorophosphate, amount of Fe3O4 magnetic nanoparticles, vortex time, amount of ammonium pyrrolidinedithiocarbamate, sample volume and matrix effect were optimized in details. Under the optimal conditions, the method present has low detection limit (0.57 μg L(-1)), high preconcentration factor (160) and good repeatability (analysis of the certified reference materials and addition-recovery tests. The method was successfully applied to the determination of lead in water, plant and hair samples. © 2013 Elsevier B.V. All rights reserved.

  2. The determination of αs by the ALPHA collaboration

    International Nuclear Information System (INIS)

    Bruno, Mattia; Brookhaven National Laboratory, Upton, NY; Dalla Brida, Mattia; Schaefer, Stefan; Simma, Hubert; Fritzsch, Patrick; CERN, Geneva; Korzec, Tomasz; Bergische Univ. Wuppertal; Ramos, Alberto; Sint, Stefan; Sommer, Rainer; Humboldt Univ. Berlin

    2016-11-01

    We review the ALPHA collaboration strategy for obtaining the QCD coupling at high scale. In the three-flavor effective theory it avoids the use of perturbation theory at α>or similar 0.2 and at the same time has the physical scales small compared to the cutoff 1/a in all stages of the computation. The result Λ (3) MS =332(14) MeV is translated to α MS (m Z )=0.1179(10)(2) by use of (high order) perturbative relations between the effective theory couplings at the charm and beauty quark ''thresholds''. The error of this perturbative step is discussed and estimated as 0.0002.

  3. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Roos, Per

    2008-01-01

    spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for radiation protection, decommissioning of nuclear facilities, repository of nuclear waste, tracer...

  4. Direct injection liquid chromatography/electrospray ionization mass spectrometric horse urine analysis for the quantification and confirmation of threshold substances for doping control. II. Determination of theobromine.

    Science.gov (United States)

    Vonaparti, A; Lyris, E; Panderi, I; Koupparis, M; Georgakopoulos, C

    2009-04-01

    In equine sport, theobromine is prohibited with a threshold level of 2 microg mL(-1) in urine, hence doping control laboratories have to establish quantitative and qualitative methods for its determination. Two simple liquid chromatography/mass spectrometry (LC/MS) methods for the identification and quantification of theobromine were developed and validated using the same sample preparation procedure but different mass spectrometric systems: ion trap mass spectrometry (ITMS) and time-of-flight mass spectrometry (TOFMS). Particle-free diluted urine samples were directly injected into the LC/MS systems, avoiding the time-consuming extraction step. 3-Propylxanthine was used as the internal standard. The tested linear range was 0.75-15 microg mL(-1). Matrix effects were evaluated analyzing calibration curves in water and different fortified horse urine samples. A great variation in the signal of theobromine and the internal standard was observed in different matrices. To overcome matrix effects, a standard additions calibration method was applied. The relative standard deviations of intra- and inter-day analysis were lower than 8.6 and 7.2%, respectively, for the LC/ITMS method and lower than 5.7 and 5.8%, respectively, for the LC/TOFMS method. The bias was less than 8.7% for both methods. The methods were applied to two case samples, demonstrating simplicity, accuracy and selectivity. Copyright (c) 2009 John Wiley & Sons, Ltd.

  5. Optimisation of spectrometric gamma-gamma probe configuration using very low radioactivity sources for lead and zinc grade determination in borehole logging

    CERN Document Server

    Asfahani, J

    1999-01-01

    The suitability of spectrometric backscattered gamma-gamma well logging measurements to predict lead and zinc metal equivalent content is demonstrated. A centralised tool employing a gamma-ray source of very low radioactivity (1.8 MBq) is used. The logging tool is tested using sup 1 sup 3 sup 3 Ba and sup 1 sup 3 sup 7 Cs sources with a 37 mm (diameter)x75 mm NaI (TI) scintillation detector. Five source-to-detector configurations were analysed for 18 geophysical models, 13 of which had a borehole diameter of 130 mm and the other 5 had a borehole diameter of 160 mm. Regression analysis on the laboratory logging data for each configuration in order to establish the calibration equation for a lead (Pb) and zinc metal equivalent (ZME) prediction is carried out. The optimum configuration for the logging probe using a sup 1 sup 3 sup 3 Ba source was determined to be 52 mm source-to-detector spacing. This configuration gives the best results for both Pb and ZME grade. The rms deviations for Pb and ZME were 0.33 and ...

  6. A critical review of methodologies used in determination of relative bio-availability ratio of RRR-alpha-tocopheryl acetate and all-rac-alpha-tocopheryl acetate.

    Science.gov (United States)

    Dersjant-Li, Yueming; Peisker, Manfred

    2010-08-15

    Bio-availability of different alpha-tocopherol forms in livestock animals is measured by the increase in plasma or tissue concentrations of alpha-tocopherol after oral administration. It is generally accepted that RRR-alpha-tocopheryl acetate (natural source vitamin E derived from vegetable oil) has a higher bio-availability compared to all-rac-alpha-tocopheryl acetate (synthetic vitamin E, i.e. alpha-tocopherol produced by chemical synthesis). However, different bio-availability ratios have been reported in the literature. The major reason for conflicting results in literature studies was the inability to separate the proportion of alpha-tocopherol originating from test materials, from the proportion of alpha-tocopherol originating from basal dietary ingredients and pre-feeding. This causes significant variability. For bio-availability determination, a baseline or control treatment is essential. The estimation of bio-availability without correction for basal vitamin E status will lead to incorrect interpretation of the results. When using proper methodologies, it is possible to correct for the impact of alpha-tocopherol intake from basal ingredients and alpha-tocopherol originating from pre-feeding, therefore yielding results reflecting the true relative bio-availability of different alpha-tocopherol substances. When reviewing literature data a critical evaluation of the method used in determination of relative bio-availability is recommended. Copyright (c) 2010 Society of Chemical Industry.

  7. Liquid chromatographic determination of alpha-zearalenol and zearalenone in corn: collaborative study.

    Science.gov (United States)

    Bennett, G A; Shotwell, O L; Kwolek, W F

    1985-01-01

    The liquid chromatographic determination of alpha-zearalenol and zearalenone in corn was collaboratively studied. Each of 13 collaborators received 7 corn samples; 2 were blanks and 5 were spiked to contain 50, 100, and 200 ng alpha-zearalenol/g and 50, 100, 500, 1000, and 4000 ng zearalenone/g. Four sets (including blanks) of blind duplicates were included in the study. Five naturally contaminated corn samples (one in duplicate) were also provided. All collaborators detected both mycotoxins at 50 ng/g. Average recoveries reported by all collaborators ranged from 81.9% at 200 ng/g to 100.3% at 50 ng/g for alpha-zearalenol and from 77.8% at 1000 ng/g to 123% at 50 ng/g for zearalenone. Three collaborators reported false positives for both alpha-zearalenol and zearalenone. The within-laboratory CV values based on blind duplicates were 22.6% for alpha-zearalenol and 31.4% for zearalenone. The CV values based on laboratory-sample interaction were 25.6 and 33.8% for alpha-zearalenol and zearalenone, respectively. The CV values for naturally contaminated samples (including duplicates) were 47.0% for alpha-zearalenol and 37.7% for zearalenone. The method has been adopted official first action.

  8. Spectrometric techniques 3

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume III presents the applications of spectrometric techniques to atmospheric and space studies. This book reviews the spectral data processing and analysis techniques that are of broad applicability.Organized into five chapters, this volume begins with an overview of the instrumentation used for obtaining field data. This text then reviews the contribution that space-borne spectroscopy in the thermal IR has made to the understanding of the planets. Other chapters consider the instruments that have recorded the planetary emission spectra. This book discusses as well

  9. 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

    The method of indolo-.alpha.-pyrone fluorescence-determination of IAA was investigated to study possible interference from 4-chloro-indoleacetic acid and 5-hydroxyindoleacetic acid, which occur naturally. Both compounds show about 40% of the fluorescence of IAA after conversion into their .alpha.......-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...

  10. Screening Natural Content of Water-Soluble B Vitamins in Fish: Enzymatic Extraction, HILIC Separation, and Tandem Mass Spectrometric Determination.

    Science.gov (United States)

    Chatterjee, Niladri Sekhar; Kumar, K Ashok; Ajeeshkumar, K K; Kumari, K R Remya; Vishnu, K V; Anandan, Rangasamy; Mathew, Suseela; Ravishankar, C N

    2017-05-01

    Despite the potential of LC with tandem MS (MS/MS) in improving sensitivity and selectivity, analytical methods are scarce for the determination of protein-bound and phosphorylated forms of B vitamins in food. This prompted us to develop a method for LC-MS/MS determination of naturally occurring nicotinamide, nicotinic acid, thiamine, pyridoxine, riboflavin, pantothenic acid, biotin, folic acid, and cyanocobalamin in fish. Baseline separation of the vitamins was achieved in a hydrophilic interaction LC condition. An ultrasonication-assisted enzymatic extraction protocol for sample preparation was optimized and validated. The time required for extraction was significantly reduced (to 4 h), while maintaining good extraction efficiency. Acetonitrile content (80%, v/v) in the prepared sample was found to be optimum for excellent peak shape and sensitivity. The dynamic linear range of the vitamins ranged from 2.5 to 500 ng/g, and the regression coefficient values were greater than 0.99. LOQ values ranged from 0.4 to 50 ng/g for the different vitamins. The spike recovery values at 50 and 100 ng/g ranged from 87.5 to 97.5%. The intra- and interday precision values were satisfactory. Accuracy of the developed method was determined by analysis of a Certified Reference Material. The method could also be used for unambiguous determination of the natural content of the target vitamins in fish.

  11. A global determination of. alpha. sub s (M sub(Z sup 0 )) at LEP

    Energy Technology Data Exchange (ETDEWEB)

    Acton, P.D.; Alexander, G.; Allison, J.; Allport, P.P.; Anderson, K.J.; Arcelli, S.; Ashton, P.; Astbury, A.; Axen, D.; Azuelos, G.; Bahan, G.A.; Baines, J.T.M.; Ball, A.H.; Banks, J.; Barker, G.J.; Barlow, R.J.; Batley, J.R.; Beaudoin, G.; Beck, A.; Becker, J.; Behnke, T.; Bell, K.W.; Bella, G.; Berlich, P.; Bethke, S.; Biebel, O.; Binder, U.; Bloodworth, I.J.; Bock, P.; Boden, B.; Bosch, H.M.; Bougerolle, S.; Brabson, B.B.; Breuker, H.; Brown, R.M.; Brun, R.; Buijs, A.; Burckhart, H.J.; Capiluppi, P.; Carnegie, R.K.; Carter, A.A.; Carter, J.R.; Chang, C.Y.; Charlton, D.G.; Clarke, P.E.L.; Cohen, I.; Collins, W.J.; Conboy, J.E.; Cooper, M.; Couch, M.; Coupland, M.; Cuffiani, M.; Dado, S.; Dallavalle, G.M.; De Jong, S.; Debu, P.; Del Pozo, L.A.; Deninno, M.M.; Dieckmann, A.; Dittmar, M.; Dixit, M.S.; Couto e Silva, E. do; Duchovni, E.; Duckeck, G.; Duerdoth, I.P.; Dumas, D.J.P.; Elcombe, P.A.; Estabrooks, P.G.; Etzion, E.; Evans, H.G.; Fabbri, F.; Fincke-Keeler, M.; Fischer, H.M.; Fong; OPAL Collaboration

    1992-07-01

    The value of the strong coupling constant, {alpha}{sub s}(M{sub (Z{sup 0})}), is determined from a study of 15 different observables in hadronic Z{sup 0} and {tau} decays. The study includes global event shape variables, jet production rates, energy correlations, the Z{sup 0} line shape and decay asymmetries and the hadronic branching fraction of {tau}-leptons. Differences between the {alpha}{sub s} values from the different observables can be consistently attributed to unknown higher order contributions to the {Omicron}({alpha}{sub s}{sup 2}) calculations. These uncertainties may be parametrized by variations of the renormalization scale and of the parton virtuality to which the data are corrected, separately for each observable, resulting in a consistent description of the event shapes, jet rates and energy correlations with the value {alpha}{sub s}(M{sub (Z{sup 0})})=0.122{sup +0.006}{sub 0}-{sub .005} in {Omicron}({alpha}{sub s}{sup 2}). The error is dominated by the theoretical uncertainties. Application of recent calculations which include the resummation of leading and next-to-leading logarithms to all orders for some observables confirm this result with a reduced sensitivity to renormalization scale variations. The Z{sup 0} line shapes and {tau}-lepton branching ratios yield {alpha}{sub s}(M{sub (Z{sup 0})})=0.148{+-}0.021 and {alpha}{sub s}(M{sub (Z{sup 0})})=0.123{sup +0.006}{sub 0}-{sub .005}, respectively in {Omicron}({alpha}{sub s}{sup 3}). These measurements and their uncertainties are entirely independent of each other and from event shape and jet observables; the good agreement of the resulting {alpha}{sub s} values thus constitutes an important consistency check of the reliability of perturbative QCD. (orig.).

  12. A study of ultraviolet renormalon ambiguities in the determination of $\\alpha_{s}$ from $\\tau$ decay

    CERN Document Server

    Altarelli, Guido; Ridolfi, G; Nason, P; Ridolfi, G

    1995-01-01

    The divergent large-order behaviour of the perturbative series relevant for the determination of \\as from \\tau decay is controlled by the leading ultraviolet (UV) renormalon. Even in the absence of the first infrared (IR) renormalon, an ambiguity of order \\Lambda^2/m_\\tau^2 is introduced. We make a quantitative study of the practical implications of this ambiguity. We discuss the magnitude of UV renormalon corrections obtained in the large-N_f limit, which, although unrealistic, is nevertheless interesting to some extent. We then study a number of improved approximants for the perturbative series, based on a change of variable in the Borel representation, such as to displace the leading UV renormalon singularity at a larger distance from the origin than the first IR renormalon. The spread of the resulting values of \\as(m^2_\\tau) obtained by different approximants, at different renormalization scales, is exhibited as a measure of the underlying ambiguities. Finally, on the basis of mathematical models, we disc...

  13. Equilibria determination in uranium ores by alpha spectrometry

    International Nuclear Information System (INIS)

    Tormo Ferrero, M.J.

    1976-01-01

    A method for the measurement of the U-234/U-238 activities is described. The separation of the uranium from the interferring elements is carried out by ionic change with anionic resine, in chlorhydric-metanol-ascorbic acid medium. The method has been applied to different spanish ores in which the equilibrium state has been determined (author)

  14. Determination of 210Pb in marine sediment core- A comparison between alpha and gamma techniques

    International Nuclear Information System (INIS)

    Zal Uyun Wan Mahmood; Yii Mei Wo; Zaharudin Ahmad

    2010-01-01

    The most commonly used techniques of alpha and gamma spectrometry were performed to measure 210 Pb activity in marine sediment core as a comparison. Alpha analytical technique measured the activity of 210 Pb from its in-grow grand-daughter 210 Po after a chemical separation, assuming radioactive equilibrium between the two radionuclides. Meanwhile, gamma analysis technique allows direct measurement, non-destructive and no preliminary chemical separation. Through the comparison, it is found that both alpha and gamma analysis techniques were slightly difference. Overall, the results from alpha analytical technique were basically higher than those from the gamma analytical techniques. Some logical argument had been discussed to explain this situation. In routine analysis, the analytical technique used should be chosen carefully based on advantages and disadvantages of the each technique and analysis requirements. Therefore, it is recommended to determine exactly the needs and purpose of analysis and to know the sample history before decide the appropriate analytical technique. (author)

  15. Determination of the concentration of {alpha} emitting radioactive aerosols; Mesure de la concentration des aerosols radioactifs emetteurs {alpha}

    Energy Technology Data Exchange (ETDEWEB)

    Labeyrie, J. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1953-06-15

    In the first part of this work the techniques used for the quantitative measurement of the concentrations of aerosols carrying short lived (radon or thoron daughters) or long lived (uranium) {alpha} radioactive emitters are described. In the second part the author investigates the problem of the determination of radon concentration in air by means of activity determinations on airborne dusts. Special reference is made to the measurement of the radon active deposit on two types of dusts (iron oxide (yellow) and uranium oxide) in small chambers (6 liters). In the third part are given data resulting from determinations of radon and thoron concentrations in atmospheric air in the south of Paris area using this method. (author) [French] Dans la premiere partie de ce travail on expose les techniques utilisees pour la mesure quantitative des concentrations d'aerosols contenant des emetteurs radioactifs {alpha}, tant pour ceux a vie courte (derives du radon ou du thoron) que pour ceux a vie longue (uranium). Dans la seconde partie on traite le probleme de la determination de la concentration de l'air en radon par la mesure de l'activite des poussieres ayant sejourne dans cet air. En particulier, on indique pour de petits volumes (6 litres) la proportion de depot actif du radon qui est fixee sur deux types de poussieres (limonite et oxyde d'uranium) en fonction de la concentration de celles-ci. Dans la troisieme partie on donne quelques exemples de mesure par cette methode de la concentration en radon et en thoron de l'atmosphere de la region parisienne. (auteur)

  16. Determination of Pu-238 Abundance in a Plutonium Standard by an Advanced Thermal Ionization Mass Spectrometric Technique

    Science.gov (United States)

    Mason, P.; Thomas, R.

    2006-12-01

    New developments in thermal ionization mass spectrometers allow for the determination of very small minor isotope ratios. The new hardware and software capabilities require attention to detail and accounting for additional sources of measurement uncertainty. The Pu-238 isotopic composition in New Brunswick Laboratory plutonium metal standard CRM 126-A was determined by thermal ionization mass spectrometry using combined Faraday cup and ion counting detection. A dynamic acquisition scheme was employed which provided for near real-time mass fractionation correction and ion counter/Faraday detector inter-calibration. Steps taken to minimize or eliminate isobaric U-238 interferences will be described, and an evaluation detailing contributions to the uncertainty, including SEM non-linearity, will be presented.

  17. Energy dispersive x-ray fluorescence spectrometric determination of phosphorus, calcium, iron, zinc, and strontium in human bones

    International Nuclear Information System (INIS)

    Ohta, Akishige; Matsubayashi, Takashi; Itoman, Moritoshi

    1981-01-01

    Phosphorus, calcium, iron, zinc and strontium in a human bone extracted by surgery were determined by energy dispersive X-ray fluorescence spectrometry. The bone was decomposed with nitric acid, then diluted with water. A specific quantity of the solution was naturally dried on polyethylene film, and subjected to X-ray analysis. For determining the calibration curves in a mixture of phosphorus, calcium, iron, zinc and strontium, for the analysis of phosphorus and calcium, germanium was used as the secondary target and aluminum as the filter; and for the analysis of iron, zinc and strontium, molybdenum and molybdenum-aluminum were used, respectively. Consequently, the calibration curves were able to be obtained with high precision in the ranges from 5 to 500 μg of phosphorus, from 1 to 50 μg of calcium and from 0.1 to 1.0 μg of iron, zinc and strontium. In this way, in 1 mg of the human bone by wet weight, phosphorus, calcium, iron, zinc and strontium were able to be determined. (J.P.N.)

  18. Determination of total alpha index in samples of see water by coprecipitation method

    International Nuclear Information System (INIS)

    Suarez-Navarro, J.A.; Pujol, L.; Pozuelo, M.; Pablo, A. de

    1998-01-01

    An environmental radiological monitoring network in the Spanish sea waters was set up by CEDEX in 1993. Water radioactivity is determined quarterly in eleven sampling points along the Spanish coast. The gross alpha activity is one of the parameters to be determined. The usual method for monitoring the gross alpha activity includes sample evaporation to dryness on a disk and counting using ZnS(Ag) scintillation detector. Nevertheless, the gross alpha activity determination in saline waters, such as sea waters, is troublesome, because mass attenuation is high and a very small of water is needed (0.2 ml). The coprecipitation method allows to analyze 500 ml water samples, so the detection limit is reduced and sensitivity is improved. In this work, the coprecipitation method was used to determine the gross alpha activity in the radiological network of the Spanish coast sea waters during 1996 and 1997. Gross alpha activity was very homogenous. It averaged 0.0844±0.0086 Bq.1''1 and ranged from 0.062 to 0.102 Bq.1''1. In collaboration with CIEMAT a set of samples was analyzed, they averaged 0.0689±0.0074 Bq.1''1 and ranged from 0.056 to 0.082 Bq.1''1. (Author) 5 refs

  19. Does extracellular calcium determine what pool of GABA is the target for alpha-latrotoxin?

    Science.gov (United States)

    Storchak, L G; Linetska, M V; Himmelreich, N H

    2002-04-01

    -latrotoxin-released neurotransmitter has the vesicular nature. We assume that the type of the toxin membrane receptor does not determine the mechanisms of [(3)H]GABA release evoked by alpha-latrotoxin.

  20. Gas chromatographic-mass spectrometric determination of aromatic hydrocarbon metabolites from livers of fish exposed to fuel oil.

    Science.gov (United States)

    Krahn, M M; Malins, D C

    1982-10-15

    Metabolites of several two- and three-ring aromatic hydrocarbons (AHs) have been found in livers of English sole exposed to No. 2 fuel oil. Four metabolites of the C2H5-naphthalenes, six of the C3H7-naphthalenes and one each of fluorene, phenanthrene and anthracene have been partially characterized and their concentrations, which ranged from 50 to 1100 ng/g, were determined. Metabolites were separated from the liver matrix using an automated extractor/concentrator. The resulting extract was then purified by high-performance liquid chromatography, and the metabolites were characterized and quantitated by gas chromatography-mass spectrometry.

  1. Simultaneous determination of major type A and B trichothecenes, zearalenone and certain modified metabolites in Finnish cereal grains with a novel liquid chromatography-tandem mass spectrometric method.

    Science.gov (United States)

    Nathanail, Alexis V; Syvähuoko, Jenna; Malachová, Alexandra; Jestoi, Marika; Varga, Elisabeth; Michlmayr, Herbert; Adam, Gerhard; Sieviläinen, Elina; Berthiller, Franz; Peltonen, Kimmo

    2015-06-01

    A reliable and sensitive liquid chromatography-tandem mass spectrometric method was developed for the simultaneous quantitative determination in cereals of the Fusarium mycotoxins HT-2 toxin, T-2 toxin, deoxynivalenol, nivalenol and zearalenone, as well as the modified metabolites 3-acetyl-deoxynivalenol, α-zearalenol, β-zearalenol, deoxynivalenol-3-glucoside, HT-2-3-glucoside, nivalenol-3-glucoside, zearalenone-14-glucoside, zearalenone-14-sulphate, zearalenone-16-glucoside, α-zearalenol-14-glucoside and β-zearalenol-14-glucoside. The 'dilute and shoot' approach was used for sample preparation after extraction with acetonitrile:water:acetic acid (79:20:1, v/v/v). Separation was carried out using reversed-phase liquid chromatography, and detection was performed using tandem mass spectrometry in the selected reaction monitoring mode. The method was in-house validated according to performance characteristics, established in Commission Regulation EC No 401/2006 and Commission Decision EC No 657/2002, prior to its application in a nationwide survey for the analysis of barley, oat and wheat samples (n = 95) harvested in Finland during 2013. Deoxynivalenol and its glucosylated form were the most abundant of the analytes, being detected in 93 and 81 % of the samples, respectively. Concentrations of deoxynivalenol were unusually high in 2013, especially in oats, with some cases exceeding the maximum legislative limits for unprocessed oats placed on the market for first-stage processing. All modified mycotoxins analysed were detected, and the natural occurrence of some of these compounds (e.g. zearalenone-16-glucoside and nivalenol-3-glucoside) in barley, oats and/or wheat was documented for the first time.

  2. A liquid chromatography-tandem mass spectrometric method for quantitative determination of native 5-methyltetrahydrofolate and its polyglutamyl derivatives in raw vegetables.

    Science.gov (United States)

    Wang, Chao; Riedl, Ken M; Schwartz, Steven J

    2010-11-01

    Folate deficiency is a prevalent phenomenon worldwide especially in underprivileged countries. Polyglutamyl 5-methyltetrahydrofolate (5MTHF) species are the naturally occurring principle folate in store-bought vegetables. Here we report a simple and complete extraction method for the determination of native polyglutamyl 5-methyltetrahydrofolate in vegetables using high performance liquid chromatography with tandem mass spectrometric detection (HPLC-MS/MS). Coarsely chopped samples (18 different vegetables) were steamed to inactivate glutamylase enzymes and liberate folate from binding proteins and extracted in a reducing buffer with (13)C(5) 5MTHF stable isotope added as internal standard. The polyglutamyl 5-methyltetrahydrofolate species were separated in 9 min on a C(18) column using a reversed phase system. HPLC eluate was interfaced with a triple quadrupole mass spectrometer operated in electrospray positive mode. The respective pseudomolecular cation of each polyglutamyl 5-methyltetrahydrofolate species was selected for fragmentation to a common daughter ion for detection. We quantitated polyglutamyl 5-methyltetrahydrofolate in store-bought vegetables from families Brassicaceae, Asteraceae and Amaranthaceae (including mustard greens, romaine lettuce and Swiss chard) of which most have not been quantitated previously. Most vegetables from Asteraceae and those from Amaranthaceae contained similar amounts of monoglutamyl 5MTHF and polyglutamyl 5MTHF while Brassicaceae were dominated by polyglutamyls and endive species (Asteraceae) contained mainly monoglutamyl 5MTHF. The precision of the method for the various polyglutamyl 5-methyltetrahydrofolate forms was 1-9% RSD, recovery 84-91%, limit of detection 64-658 fmol and limit of quantitation 193-1994 fmol. Herein we describe a rapid, sensitive and selective HPLC-MS/MS technique to quantitate polyglutamyl 5-methyltetrahydrofolate species. This method may be suitable for analyzing the polyglutamyl 5

  3. A liquid chromatography–tandem mass spectrometric method for quantitative determination of native 5-methyltetrahydrofolate and its polyglutamyl derivatives in raw vegetables

    Science.gov (United States)

    Wang, Chao; Riedl, Ken M.; Schwartz, Steven J.

    2013-01-01

    Folate deficiency is a prevalent phenomenon worldwide especially in underprivileged countries. Polyglutamyl 5-methyltetrahydrofolate (5MTHF) species are the naturally occurring principle folate in store-bought vegetables. Here we report a simple and complete extraction method for the determination of native polyglutamyl 5-methyltetrahydrofolate in vegetables using high performance liquid chromatography with tandem mass spectrometric detection (HPLC–MS/MS). Coarsely chopped samples (18 different vegetables) were steamed to inactivate glutamylase enzymes and liberate folate from binding proteins and extracted in a reducing buffer with 13C5 5MTHF stable isotope added as internal standard. The polyglutamyl 5-methyltetrahydrofolate species were separated in 9 min on a C18 column using a reversed phase system. HPLC eluate was interfaced with a triple quadrupole mass spectrometer operated in electrospray positive mode. The respective pseudomolecular cation of each polyglutamyl 5-methyltetrahydrofolate species was selected for fragmentation to a common daughter ion for detection. We quantitated polyglutamyl 5-methyltetrahydrofolate in store-bought vegetables from families Brassicaceae, Asteraceae and Amaranthaceae (including mustard greens, romaine lettuce and Swiss chard) of which most have not been quantitated previously. Most vegetables from Asteraceae and those from Amaranthaceae contained similar amounts of monoglutamyl 5MTHF and polyglutamyl 5MTHF while Brassicaceae were dominated by polyglutamyls and endive species (Asteraceae) contained mainly monoglutamyl 5MTHF. The precision of the method for the various polyglutamyl 5-methyltetrahydrofolate forms was 1–9% RSD, recovery 84–91%, limit of detection 64–658 fmol and limit of quantitation 193–1994 fmol. Herein we describe a rapid, sensitive and selective HPLC–MS/MS technique to quantitate polyglutamyl 5-methyltetrahydrofolate species. This method may be suitable for analyzing the polyglutamyl 5

  4. A novel, donor-active solvent-assisted liquid-phase microextraction procedure for spectrometric determination of zinc

    Energy Technology Data Exchange (ETDEWEB)

    Kocurova, Livia; Fatlova, Martina; Bazel, Yaroslav; Serbin, Rastislav; Andruch, Vasil, E-mail: liviamonika.kocurova@gmail.com [Department of Analytical Chemistry, University of P. J. Safarik, Kosice (Slovakia); Balogh, Ioseph S. [Department of Chemistry, College of Nyiregyhaza (Hungary); Simon, Andras [Department of General and Analytical Chemistry, Budapest University of Technology and Economics, Budapest (Hungary); Badida, Miroslav; Rusnak, Radoslav [Department of Environmentalistics, Faculty of Mechanical Engineering, Technical University of Kosice (Slovakia)

    2014-02-15

    Based on the reaction of Zn(II), thiocyanate and 2-[2-(5-dimethylamino-thiophen-2-yl)-vinyl]- 1,3,3-trimethyl-3H-indolium bromide (DTVTI), a donor-active solvent-assisted liquid-phase microextraction procedure followed by spectrophotometric determination of zinc at 570 nm was developed. The optimum experimental conditions were investigated and found to be as follows: concentration of NH{sub 4}SCN 0.02 mol L{sup -1} concentration of DTVTI 4 x 10{sup -5} mol L{sup -1}. Various extraction solvents were studied alone as well as in mixtures with different improvers, and a mixture of toluene as the extraction solvent and tributylphosphate as the donor-active solvent in a 4:1 v/v ratio was selected. The calibration plot was linear up to 2.62 mg L{sup 1} of zinc with limit of detection 0.09 mg L{sup -1}. The developed procedure was applied for zinc determination in dietary supplements. (author)

  5. Standard test method for graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2000-01-01

    1.1 This test method covers procedures for using graphite furnace atomic absorption spectroscopy (GFAAS) to quantitatively determine lead and cadmium extracted by acetic acid at room temperature from the food-contact surface of foodware. The method is applicable to food-contact surfaces composed of silicate-based materials (earthenware, glazed ceramicware, decorated ceramicware, decorated glass, and lead crystal glass) and is capable of determining lead concentrations greater than 0.005 to 0.020 g/mL and cadmium concentrations greater than 0.0005 to 0.002 g/mL, depending on instrument design. 1.2 This test method also describes quality control procedures to check for contamination and matrix interference during GFAAS analyses and a specific sequence of analytical measurements that demonstrates proper instrument operation during the time period in which sample solutions are analyzed. 1.3 Cleaning and other contamination control procedures are described in this test method. Users may modify contamination cont...

  6. A Procedure for the Sequential Determination of Radionuclides in Environmental Samples. Liquid Scintillation Counting and Alpha Spectrometry for 90Sr, 241Am and Pu Radioisotopes

    International Nuclear Information System (INIS)

    2014-01-01

    Since 2004, IAEA activities related to the terrestrial environment have aimed at the development of a set of procedures to determine radionuclides in environmental samples. Reliable, comparable and ‘fit for purpose’ results are an essential requirement for any decision based on analytical measurements. For the analyst, tested and validated analytical procedures are extremely important tools for the production of analytical data. For maximum utility, such procedures should be comprehensive, clearly formulated and readily available for reference to both the analyst and the customer. This publication describes a combined procedure for the sequential determination of 90 Sr, 241 Am and Pu radioisotopes in environmental samples. The method is based on the chemical separation of strontium, americium and plutonium using ion exchange chromatography, extraction chromatography and precipitation followed by alpha spectrometric and liquid scintillation counting detection. The method was tested and validated in terms of repeatability and trueness in accordance with International Organization for Standardization (ISO) guidelines using reference materials and proficiency test samples. Reproducibility tests were performed later at the IAEA Terrestrial Environment Laboratory. The calculations of the massic activity, uncertainty budget, decision threshold and detection limit are also described in this publication. The procedure is introduced for the determination of 90 Sr, 241 Am and Pu radioisotopes in environmental samples such as soil, sediment, air filter and vegetation samples. It is expected to be of general use to a wide range of laboratories, including the Analytical Laboratories for the Measurement of Environmental Radioactivity (ALMERA) network for routine environmental monitoring purposes

  7. Marine gamma spectrometric survey

    International Nuclear Information System (INIS)

    Kostoglodov, V.V.

    1979-01-01

    Presented are theoretical problems physical and geochemical prerequisites and possibilities of practical application of the method of continuous submarine gamma-spectrometric survey and radiometric survey destined for rapid study of the surface layer of marine sediments. Shown is high efficiency and advantages of this method in comparison with traditional and widely spread in marine geology methods of bottom sediments investigation

  8. Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    Senturk, Hasan Basri; Gundogdu, Ali; Bulut, Volkan Numan; Duran, Celal; Soylak, Mustafa; Elci, Latif; Tufekci, Mehmet

    2007-01-01

    A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L -1 HNO 3 in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 μg L -1 , respectively. The preconcentration factor was 200. The relative standard deviation of the method was -1 . The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples

  9. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization

    Science.gov (United States)

    Loge, G.

    1994-09-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U3O8. Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF4 were found to be a kinetic bottleneck to the formation of UF6. This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid.

  10. Adaptation of atomic spectrometric methods for the determination of trace elements in whole blood and blood fractions

    International Nuclear Information System (INIS)

    Prohaska, C.

    2002-05-01

    Analytical methods were developed and optimized for the determination of the elements Ca, Cr, Cu, Fe, Mg, Mn, Se, V and Zn in whole blood and in the blood fractions plasma, erythrocytes and lymphocytes of a group of people suffering from diabetes and of a control group of healthy individuals. Cr, Mn, Se and V were analyzed by ETAAS. Ca, Cu, Fe, Mg and Zn were analyzed by ICP-OES. The status of trace elements in lymphocytes of people suffering from diabetes is changed. Physiologically interesting correlations were observed between the clinical parameters cholesterol, HDL, LDL, blood glucose, HbA1c, age and BMI and the trace element concentrations, e.g. a correlation of blood glucose and HbA1c with selenium in whole blood. An ETAAS - method for the determination of Co and Mo was developed and optimized. The samples were digested applying a mixture of HNO3 and HF, different types of graphite furnaces were tested and a multiple injection technique was applied, thereby enabling a contribution to the normal values of these elements in human whole blood. An on-line coupling of a LC, controlled by FIA, with an ICP-OES was developed to investigate the concentrations of the iron species Fe(II) and Fe(III) and the copper species Cu(I) and Cu(II) in human blood plasma. The ICP-OES instrument was adapted, batch experiments were carried out, oxidizing and reducing agents were added and the acidity of the eluens, the flow rate and the integration time were optimized. Choosing alanine for complexation of the species of interest enables their separation under physiological conditions. In the real plasma samples measured most of the copper and iron was found in their oxidized forms. (author)

  11. Selective cloud point extraction and graphite furnace atomic absorption spectrometric determination of molybdenum (VI) ion in seawater samples

    Energy Technology Data Exchange (ETDEWEB)

    Filik, Hayati, E-mail: filik@istanbul.edu.tr [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey); Cengel, Tayfun; Apak, Resat [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey)

    2009-09-30

    A cloud point extraction process using the nonionic surfactant Triton X-114 to extract molybdenum from aqueous solutions was investigated. The method is based on the complexation reaction of Mo(VI) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarine: QA) and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by graphite furnace atomic absorption spectrometry (GFAAS). The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature, incubation and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the limit of detection (LOD) for Mo(VI) was 7.0 ng L{sup -1} with an preconcentration factor of {approx}25 when 10 mL of sample solution was preconcentrated to 0.4 mL. The proposed method (with extraction) showed linear calibration within the range 0.03-0.6 {mu}g L{sup -1}. The relative standard deviation (RSD) was found to be 3.7% (C{sub Mo(VI)} = 0.05 {mu}g L{sup -1}, n = 5) for pure standard solutions, whereas RSD for the recoveries from real samples ranged between 2 and 8% (mean RSD = 3.9%). The method was applied to the determination of Mo(VI) in seawater and tap water samples with a recovery for the spiked samples in the range of 98-103%. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. In order to verify the accuracy of the method, a certified reference water sample was analysed and the results obtained were in good agreement with the certified values.

  12. Determination of total alpha activity index in samples of radioactive wastes

    International Nuclear Information System (INIS)

    Galicia C, F. J.

    2015-01-01

    This study aimed to develop a methodology of preparation and quantification of samples containing radionuclides beta and/or alpha emitters, to determine the rates of alpha and beta total activity of radioactive waste samples. For this, a device of planchettes preparer was designed, to assist the planchettes preparation in a controlled environment and free of corrosive vapors. Planchettes were prepared in three means: nitrate, carbonate and sulfate, to different mass thickness, natural uranium (alpha and beta emitter) and in case of Sr-90 (beta emitter pure) only in half nitrate; and these planchettes were quantified in an alpha/beta counter, in order to construct the self-absorption curves for alpha and beta particles. These curves are necessary to determine the rate of alpha-beta activity of any sample because they provide the self-absorption correction factor to be applied in calculating the index. Samples with U were prepared with the help of the device of planchettes preparer and subsequently were analyzed in the proportional counter Mpc-100 Pic brand. Samples with Sr-90 were prepared without the device to see if there was a different behavior with respect to obtaining mass thickness. Similarly they were calcined and carried out count in the Mpc-100. To perform the count, first the parameters of counter operating were determined: operating voltages for alpha and beta particles 630 and 1500 V respectively, a count routine was generated where the time and count type were adjusted, and counting efficiencies for alpha and beta particles, with the aid of calibration sources of 210 Po for alphas and 90 Sr for betas. According to the results, the counts per minute will decrease as increasing the mass thickness of the sample (self-absorption curve), adjusting this behavior to an exponential function in all cases studied. The minor self-absorption of alpha and beta particles in the case of U was obtained in sulfate medium. The self-absorption curves of Sr-90 follow the

  13. Determination of Uranium, Thorium and Radium 226 in Zircon containig sands by alpha spectrometry

    International Nuclear Information System (INIS)

    Spezzano, P.

    1985-01-01

    The industrial utilization of Zircon sands for the production of refractories presents radiological problems owing to the risk of inhalation of Uranium, Thorium and their decay products, present in high concentrations in such materials. A method of analysis was realized for the determination of Uranium, Thorium and Radium-226 in Zircon sands, including the total dissolution of the sample, radiochemical separation and final measurement by alpha spectrometry with surface barrier detector. The concentrations of the main alpha-emitting radionuclides presents in two samples of Zircon sands have been determined and the possibility of disequilibrium along the decay series has been pointed out

  14. Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection.

    Science.gov (United States)

    Zygler, Agata; Wasik, Andrzej; Kot-Wasik, Agata; Namieśnik, Jacek

    2011-06-01

    An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame (ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC) and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer composed of formic acid and N,N-diisopropylethylamine at pH 4.5 in ultrasonic bath, extracts were cleaned up using Strata-X 33 μm Polymeric SPE column. The analytes were separated in gradient elution mode on C(18) column and detected by mass spectrometer working with an electrospray source in negative ion mode. To confirm that analytical method is suitable for its intended use, several validation parameters, such as linearity, limits of detection and quantification, trueness and repeatibilty were evaluated. Calibration curves were linear within a studied range of concentrations (r(2) ≥ 0.999) for six investigated sweeteners (CYC, ASP, ALI, DUL, NHDC, NEO). Three compounds (ACS-K, SAC, SCL) gave non-linear response in the investigated concentration range. The method detection limits (corresponding to signal-to-noise (S/N) ratio of 3) were below 0.25 μg mL(-1) (μg g(-1)), whereas the method quantitation limits (corresponding to S/N ratio of 10) were below 2.5 μg mL(-1) (μg g(-1)). The recoveries at the tested concentrations (50%, 100% and 125% of maximum usable dose) for all sweeteners were in the range of 84.2 ÷ 106.7%, with relative standard deviations beverage, yoghurt, fish product) and the spiking level. The proposed method has been successfully applied to the determination of the nine sweeteners in drinks, yoghurts and fish products. The procedure described here is simple, accurate and precise and is suitable for routine quality control analysis of

  15. Ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of strychnine and brucine in mice plasma.

    Science.gov (United States)

    Liu, Yanwen; Zhu, Ronghua; Li, Huande; Yan, Miao; Lei, Yanqing

    2011-09-15

    A selective, simple and efficient method-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for determination of two toxic alkaloids, namely strychnine and brucine in mice plasma. The UPLC separation was carried out using a 1.7 μm BEH C(18) column (50 mm × 2.1 mm) with a mobile phase consisting of methanol:0.1% formic acid (25:75, v/v), hence providing high efficiency, high resolution and excellent peak shape for the analytes and internal standard. The method was validated over the range of 2.48-496.4 ng/ml for strychnine and 2.64-528 ng/ml for brucine, respectively. Intra- and inter-day accuracy ranged from 95.0% to 107.9% for strychnine, 93.4% to 103.3% for brucine, and the precisions were within 13.8%. The extraction recoveries of both the two alkaloids exceed 81.9%. With a simple and minor sample preparation procedure and short run-time (strychnine and brucine in vivo. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Senturk, Hasan Basri; Gundogdu, Ali [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 28049 Giresun (Turkey); Duran, Celal [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Arts and Sciences, Pamukkale University, 20020 Denizli (Turkey); Tufekci, Mehmet [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)

    2007-10-22

    A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L{sup -1} HNO{sub 3} in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 {mu}g L{sup -1}, respectively. The preconcentration factor was 200. The relative standard deviation of the method was <6%. The adsorption capacity of the resin was 12.3 mg g{sup -1}. The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples.

  17. Mass spectrometric determination of enthalpies of dissociation of gaseous complex fluorides into neutral and charged particles. Pt. 3

    International Nuclear Information System (INIS)

    Sidorov, L.N.; Skokan, E.V.; Nikitin, M.I.; Sorokin, I.D.

    1980-01-01

    Mass spectrometry is used to study ion-molecule equilibria in the saturated vapours of the two-component systems MF-UF 4 (where M is Na or K), containing the negative ions F - , UF - 5 and UF - 6 . The electron affinities of UF 5 and UF 6 are determined as 3.3 +- 0.16 eV and 4.89 +- 0.25 eV and the heats of the following reactions are: F - + UF 4 → UF - 5 ΔH 0 1100 = -98,0 +- 0.3 kcal mol -1 (-410.0 +- 1.3 kJ mol -1 ), AlF 3 + UF - 5 → AlF - 4 + UF 4 ΔH 0 1100 = -22.3 +- 0.3 kcal mol -1 (-93.3 +- 1.3 kJ mol -1 ), UF 5 + UF - 5 → UF 4 + UF - 6 ΔH 0 1087 = -3.4 +- 0.2 kcal mol -1 (-14.2 +- 0.8 kJ mol -1 ). These data and literature values are used to calculate the heat of formation of the UF - 5 ion and the heats of dissociation of the alkali metal fluorouranates into neutral and charged particles. (orig.)

  18. Determination of Uranium plus Plutonium by Alpha spectrometry in different matrix

    International Nuclear Information System (INIS)

    Equillor, Hugo E.; Campos, Juan M.

    2011-01-01

    Usually, the determination of alpha emitters by alpha spectrometry is performed with a prior purification of each of the elements to be quantified. In this work, a methodology for the determination of uranium and plutonium isotopes as jointly described, in order to improve analytical processing times and measurement. The method includes purifying uranium and plutonium, and the subsequent electrodeposition for alpha spectrometry measurement. The technique is based on the use of TBP (tributyl phosphate) as extractant and easy to obtain reactants. It is applicable to various matrices, including water, filters and soils. In the conditions described, is applied to small aliquots of approximately 0.5 g of solid. The technique produces high quality electrodeposits. (authors) [es

  19. Innovative procedure for the determination of gross-alpha/gross-beta activities in drinking water

    International Nuclear Information System (INIS)

    Wisser, S.; Frenzel, E.; Dittmer, M.

    2006-01-01

    An alternative sample preparation method for the determination of gross-alpha/beta activity concentrations in drinking water is introduced in this paper. After the freeze-drying of tap water samples, determination by liquid scintillation counting can be applied utilizing alpha/beta separation. It has been shown that there is no adsorption or loss of solid radionuclides during the freeze-drying procedure. However, the samples have to be measured quickly after the preparation since the ingrowth of daughter isotopes negatively effects the measurement. The limits of detection for gross-alpha and gross-beta activity are in the range 25-210 mBq/l, respectively, for a measurement time of only 8-9 h

  20. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    spectrometric (LC-MS/MS) method for the quantitative determination of two dermatological drugs,. Lamisil® (terbinafine) and Proscar® (finasteride), in split tablet dosage form. Methods: Thirty tablets each of the 2 studied medications were randomly selected. Tablets were weighed and divided into 3 groups. Ten tablets of ...

  1. Preparation of 237Np samples by electrodeposition and its determination by alpha spectrometry

    International Nuclear Information System (INIS)

    Mertzig, W.; Matsuda, H.T.; Araujo, B.F. de; Araujo, J.A. de

    1980-01-01

    An analytical method followed by alpha spectrometry was developed for the determination of trace amounts of actinides. A technique for quantitative electrodeposition of 237 Np, under optimal conditions, using a carrier, is presented. This method will be applied for the control of trace amounts of 237 Np in the solutions from the reprocessing (Purex process) of irradiated uranium. (C.L.B.) [pt

  2. Determination of ''226Ra by Alpha Spectrometry by Using ''225Ra as Yield Tracer

    International Nuclear Information System (INIS)

    Crespo, M. T.; Oller, O.

    1999-01-01

    A method for the determination of low-level ''226 Ra in environmental and geological samples by alpha spectrometry is described. The method is based on the use of ''225 Ra from ''229 Th as yield tracer and has been developed to analyze U, Th and Ra in the same sample. (Author) 12 refs

  3. Requirement of radiochemical recovery determination for gross alpha and gross beta estimation in drinking water

    International Nuclear Information System (INIS)

    Raveendran, Nanda; Rao, D.D.; Hegde, A.G.

    2010-01-01

    Presence of radionuclides in drinking water which emits Alpha and Beta particles are the potential sources of internal exposure in drinking water. Gross alpha and gross beta determination in drinking water and packaged drinking water (PDW) as per BIS (Bureau of Indian standards) standards is discussed here. The methods have been tested to account for losses in the radiochemical procedures using radionuclides such as 137 Cs, 90 Sr, 226 Ra, 239 Pu, 243 Am, 232 U. The methods have also been validated in an IAEA proficiency test conducted during 2009. Monitoring of gross alpha and gross beta activity observed in drinking water/packaged drinking water from various states of India were within the limits set by BIS. Average radiochemical recoveries of 84% and 63% were obtained for gross α and gross β respectively. (author)

  4. The determination of plutonium alpha activity in urine, faeces and biological materials

    International Nuclear Information System (INIS)

    Bains, M.E.D.

    1963-07-01

    Methods have been developed for the determination of plutonium alpha activity in urine, faeces and biological materials. The chemical stages involved give practically complete separation of all extraneous material from the plutonium, which is electrodeposited on to a 0.5 inch stainless steel disc to produce a thin high resolution source. The limit of detection is 0.025 μμc/sample (sixteen-hour count) when the sources are counted in a small scintillator counter, but is lowest when counted in a counter which counts particles of energy 5.05-5.25 MeV only, and which therefore discriminates against small quantities of α-active materials introduced with the reagents in the final electrodeposition stage of the process. (Any such alpha activity may readily be identified by alpha pulse height analysis). (author)

  5. Determination of alpha particle detection efficiency of an imaging plate (IP) detector

    International Nuclear Information System (INIS)

    Rahman, N.M; Iida, Takao; Yamazawa, Hiromi; Moriizumi, Jun

    2006-01-01

    In order to determine the detection efficiency of the imaging plate (IP) detector, the true radioactivity of the alpha particles, which sampled in the collection media, should be known. The true radioactivity could be accurately predicted with the help of the reference alpha spectrometer measurement. The detection efficiency calculated for the IP was estimated with the theoretical curve and the experimental data. It is assumed that the air sample contained the decay products of both 222 Rn and 220 Rn series, the most significant sources of alpha particles. The present study estimated the detection efficiency of the IP as 39.3% with an uncertainty of 2.9 that is well enough to confirm the future use of the IP as a radiation detector. Experimental materials and methods are described. (S.Y.)

  6. Liquid chromatographic mass spectrometric (LC/MS/MS) determination of plasma hydroxocobalamin and cyanocobalamin concentrations after hydroxocobalamin antidote treatment for cyanide poisoning.

    Science.gov (United States)

    Schwertner, Harvey A; Valtier, Sandra; Bebarta, Vikhyat S

    2012-09-15

    Cyanide poisoning occurs in individuals after fire smoke inhalation and after oral ingestion of cyanide. Hydroxocobalamin (HOCbl), a hydroxylated form of vitamin B(12), is often used as an antidote to treat cyanide toxicity. It has a high affinity for cyanide and rapidly removes cyanide from tissue by forming cyanocobalamin (CNCbl). Little information is available on the pharmacokinetics of HOCbl and CNCbl largely because of the lack of analytical methods for analyzing HOCbl and CNCbl. In this study, we developed a new liquid chromatographic mass spectrometric (LC/MS/MS) method for the quantitative analysis of plasma HOCbl and CNCbl in the porcine (Sus scrofa) model. The method uses on-column extraction, reversed phase gradient chromatography, and multiple reaction monitoring (MRM) for quantitation. MRM transitions monitored were 664.7→147.3 and 664.7→359.2 for HOCbl and 678.8→147.3, 678.8→359.1 678.8→457.1 for CNCbl. The limit of detection (LOD) and the lower limit of quantitation (LLOQ) were 1.0 and 1.0 μmole/L, respectively, for plasma HOCbl and 0.1 and 0.5 μmole/L for plasma CNCbl. The within-day and between-day CVs were 4.3 and 6.4% for plasma HOCbl at 500.0 μmole/L and 5.5 and 5.7% for CNCbl at 100.0 μmole/L (n=6). The plasma HOCbl and CNCbl calibrations curves were linear from 100.0 to 2000.0 and 50.0 to 500.0 μmole/L, respectively. Based on 6 separate calibration curves the average linear regression coefficient (R(2)) for both HOCbl and CNCbl was 0.992. The LC/M/MS method was found to be accurate and precise and has been validated by determining the plasma HOCbl and CNCbl concentrations in 11 pigs that were treated with HOCbl for cyanide poisoning. Published by Elsevier B.V.

  7. arXiv $\\alpha_s$ determination at NNLO$^\\star$+NNLL accuracy from the energy evolution of jet fragmentation functions at low $z$

    CERN Document Server

    d'Enterria, David

    2015-01-01

    The QCD coupling $\\alpha_s$ is extracted from the energy evolution of the first two moments (multiplicity and mean) of the parton-to-hadron fragmentation functions at low fractional hadron momentum $z$. Comparisons of the experimental $e^+e^-$ and deep-inelastic $e^\\pm$p jet data to our NNLO$^*$+NNLL predictions, allow us to obtain $\\alpha_s(m_{_{\\rm Z}})$ = 0.1205$\\pm$0.0010$^{+0.0022}_{-0.0000}$, in excellent agreement with the current world average determined using other methods at the same level of accuracy.

  8. Gross alpha and gross beta determination in surface and groundwater water by liquid scintillation counting (LSC)

    Energy Technology Data Exchange (ETDEWEB)

    Faria, Ligia S.; Moreira, Rubens M., E-mail: ligsfaria@gmail.com, E-mail: rubens@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2013-07-01

    The present study has used 40 samples of groundwater and surface water collected at four different sites along the period of one year in Brumadinho and Nova Lima, two municipalities in the State of Minas Gerais, Brazil, as part of a more extensive study aiming at determination of the natural radioactivity in the water used for domestic use. These two sites are inside an Environmental Protection Area is located in a region of very intensive iron ore exploration. In addition of mineral resources, the region has a geological characteristic that includes quartzitic conglomerates associated with uranium. Radioactivity levels were determined via liquid scintillation counting (LSC), a fast and high counting efficiency method that can be advantageously employed to determine gross alpha and gross beta activity in liquid samples. Previously to gross alpha and gross beta counting the samples were acidified with concentrated HNO{sub 3} in the field. The technique involved a pre-concentration of the sample to obtain a low detection limit. Specific details of the employed methodology are commented. The results showed that concentrations of gross alpha natural activity and gross beta values ranged from less than the detection limit of the equipment (0.03 Bq.L{sup -1}) to 0.275 ± 0.05 Bq.L{sup -1} for gross alpha. As regards gross beta, all samples were below the limit of detection. (author)

  9. Determination of $\\alpha_s$ from Hadronic Event Shapes in $e^+ e^-$ Annihilation at $192 \\le \\sqrt{s} \\le 208$ GeV

    CERN Document Server

    Achard, P.; Aguilar-Benitez, M.; Alcaraz, J.; Alemanni, G.; Allaby, J.; Aloisio, A.; Alviggi, M.G.; Anderhub, H.; Andreev, Valery P.; Anselmo, F.; Arefev, A.; Azemoon, T.; Aziz, T.; Bagnaia, P.; Bajo, A.; Baksay, G.; Baksay, L.; Baldew, S.V.; Banerjee, S.; Banerjee, Sw.; Barczyk, A.; Barillere, R.; Bartalini, P.; Basile, M.; Batalova, N.; Battiston, R.; Bay, A.; Becattini, F.; Becker, U.; Behner, F.; Bellucci, L.; Berbeco, R.; Berdugo, J.; Berges, P.; Bertucci, B.; Betev, B.L.; Biasini, M.; Biglietti, M.; Biland, A.; Blaising, J.J.; Blyth, S.C.; Bobbink, G.J.; Bohm, A.; Boldizsar, L.; Borgia, B.; Bottai, S.; Bourilkov, D.; Bourquin, M.; Braccini, S.; Branson, J.G.; Brochu, F.; Burger, J.D.; Burger, W.J.; Cai, X.D.; Capell, M.; Cara Romeo, G.; Carlino, G.; Cartacci, A.; Casaus, J.; Cavallari, F.; Cavallo, N.; Cecchi, C.; Cerrada, M.; Chamizo, M.; Chang, Y.H.; Chemarin, M.; Chen, A.; Chen, G.; Chen, G.M.; Chen, H.F.; Chen, H.S.; Chiefari, G.; Cifarelli, L.; Cindolo, F.; Clare, I.; Clare, R.; Coignet, G.; Colino, N.; Costantini, S.; de la Cruz, B.; Cucciarelli, S.; van Dalen, J.A.; de Asmundis, R.; Deglon, P.; Debreczeni, J.; Degre, A.; Deiters, K.; Della Volpe, D.; Delmeire, E.; Denes, P.; De Notaristefani, F.; De Salvo, A.; Diemoz, M.; Dierckxsens, M.; Dionisi, C.; Dittmar, M.; Doria, A.; Dova, M.T.; Duchesneau, D.; Echenard, B.; Eline, A.; El Mamouni, H.; Engler, A.; Eppling, F.J.; Ewers, A.; Extermann, P.; Falagan, M.A.; Falciano, S.; Favara, A.; Fay, J.; Fedin, O.; Felcini, M.; Ferguson, T.; Fesefeldt, H.; Fiandrini, E.; Field, J.H.; Filthaut, F.; Fisher, P.H.; Fisher, W.; Fisk, I.; Forconi, G.; Freudenreich, K.; Furetta, C.; Galaktionov, Iouri; Ganguli, S.N.; Garcia-Abia, Pablo; Gataullin, M.; Gentile, S.; Giagu, S.; Gong, Z.F.; Grenier, Gerald Jean; Grimm, O.; Gruenewald, M.W.; Guida, M.; van Gulik, R.; Gupta, V.K.; Gurtu, A.; Gutay, L.J.; Haas, D.; Hakobian, R.Sh.; Hatzifotiadou, D.; Hebbeker, T.; Herve, Alain; Hirschfelder, J.; Hofer, H.; Hohlmann, M.; Holzner, G.; Hou, S.R.; Hu, Y.; Jin, B.N.; Jones, Lawrence W.; de Jong, P.; Josa-Mutuberria, I.; Kafer, D.; Kaur, M.; Kienzle-Focacci, M.N.; Kim, J.K.; Kirkby, Jasper; Kittel, W.; Klimentov, A.; Konig, A.C.; Kopal, M.; Koutsenko, V.; Kraber, M.; Kraemer, R.W.; Krenz, W.; Kruger, A.; Kunin, A.; Ladron de Guevara, P.; Laktineh, I.; Landi, G.; Lebeau, M.; Lebedev, A.; Lebrun, P.; Lecomte, P.; Lecoq, P.; Le Coultre, P.; Le Goff, J.M.; Leiste, R.; Levtchenko, M.; Levchenko, P.; Li, C.; Likhoded, S.; Lin, C.H.; Lin, W.T.; Linde, F.L.; Lista, L.; Liu, Z.A.; Lohmann, W.; Longo, E.; Lu, Y.S.; Lubelsmeyer, K.; Luci, C.; Luminari, L.; Lustermann, W.; Ma, W.G.; Malgeri, L.; Malinin, A.; Mana, C.; Mangeol, D.; Mans, J.; Martin, J.P.; Marzano, F.; Mazumdar, K.; McNeil, R.R.; Mele, S.; Merola, L.; Meschini, M.; Metzger, W.J.; Mihul, A.; Milcent, H.; Mirabelli, G.; Mnich, J.; Mohanty, G.B.; Muanza, G.S.; Muijs, A.J.M.; Musicar, B.; Musy, M.; Nagy, S.; Natale, S.; Napolitano, M.; Nessi-Tedaldi, F.; Newman, H.; Niessen, T.; Nisati, A.; Kluge, Hannelies; Ofierzynski, R.; Organtini, G.; Palomares, C.; Pandoulas, D.; Paolucci, P.; Paramatti, R.; Passaleva, G.; Patricelli, S.; Paul, Thomas Cantzon; Pauluzzi, M.; Paus, C.; Pauss, F.; Pedace, M.; Pensotti, S.; Perret-Gallix, D.; Petersen, B.; Piccolo, D.; Pierella, F.; Pioppi, M.; Piroue, P.A.; Pistolesi, E.; Plyaskin, V.; Pohl, M.; Pozhidaev, V.; Pothier, J.; Prokofev, D.O.; Prokofev, D.; Quartieri, J.; Rahal-Callot, G.; Rahaman, M.A.; Raics, P.; Raja, N.; Ramelli, R.; Rancoita, P.G.; Ranieri, R.; Raspereza, A.; Razis, P.; Ren, D.; Rescigno, M.; Reucroft, S.; Riemann, S.; Riles, Keith; Roe, B.P.; Romero, L.; Rosca, A.; Rosier-Lees, S.; Roth, Stefan; Rosenbleck, C.; Roux, B.; Rubio, J.A.; Ruggiero, G.; Rykaczewski, H.; Sakharov, A.; Saremi, S.; Sarkar, S.; Salicio, J.; Sanchez, E.; Sanders, M.P.; Schafer, C.; Shchegelsky, V.; Schmidt-Kaerst, S.; Schmitz, D.; Schopper, H.; Schotanus, D.J.; Schwering, G.; Sciacca, C.; Servoli, L.; Shevchenko, S.; Shivarov, N.; Shoutko, V.; Shumilov, E.; Shvorob, A.; Siedenburg, T.; Son, D.; Spillantini, P.; Steuer, M.; Stickland, D.P.; Stoyanov, B.; Straessner, A.; Sudhakar, K.; Sultanov, G.; Sun, L.Z.; Sushkov, S.; Suter, H.; Swain, J.D.; Szillasi, Z.; Tang, X.W.; Tarjan, P.; Tauscher, L.; Taylor, L.; Tellili, B.; Teyssier, D.; Timmermans, Charles; Ting, S.C.C.; Ting, S.M.; Tonwar, S.C.; Toth, J.; Tully, C.; Tung, K.L.; Ulbricht, J.; Valente, E.; Van de Walle, R.T.; Veszpremi, V.; Vesztergombi, G.; Vetlitsky, I.; Vicinanza, D.; Viertel, G.; Villa, S.; Vivargent, M.; Vlachos, S.; Vodopyanov, I.; Vogel, H.; Vogt, H.; Vorobev, I.; Vorobov, A.A.; Wadhwa, M.; Wallraff, W.; Wang, X.L.; Wang, Z.M.; Weber, M.; Wienemann, P.; Wilkens, H.; Wynhoff, S.; Xia, L.; Xu, Z.Z.; Yamamoto, J.; Yang, B.Z.; Yang, C.G.; Yang, H.J.; Yang, M.; Yeh, S.C.; Zalite, A.; Zalite, Yu.; Zhang, Z.P.; Zhao, J.; Zhu, G.Y.; Zhu, R.Y.; Zhuang, H.L.; Zichichi, A.; Zilizi, G.; Zimmermann, B.; Zoller, M.

    2002-01-01

    Results are presented from a study of the structure of high energy hadronic events recorded by the L3 detector at sqrt(s)>192 GeV. The distributions of several event shape variables are compared to resummed O(alphaS^2) QCD calculations. We determine the strong coupling constant at three average centre-of-mass energies: 194.4, 200.2 and 206.2 GeV. These measurements, combined with previous L3 measurements at lower energies demonstrate the running of alphaS as expected in QCD and yield alphaS(mZ) = 0.1227 +- 0.0012 +- 0.0058, where the first uncertainty is experimental and the second is theoretical.

  10. Rapid determination of radium-224/226 in seawater sample by alpha spectrometry.

    Science.gov (United States)

    Song, Lijuan; Yang, Yonggang; Luo, Maoyi; Ma, Yan; Dai, Xiongxin

    2017-05-01

    A new radiochemical separation method has been developed for rapid determination of alpha-emitting radium isotopes in seawater samples. This method can be applied for the measurement of 226 Ra in seawater samples when 224 Ra is used as tracer for chemical recovery correction. Likewise, 226 Ra can also be added as tracer for the determination of 224 Ra in seawater sample. In the method, radium is first pre-concentrated with hydrous titanium oxide (HTiO) and is purified by combined anion/cation exchange column chromatographic separation. The radium in the eluate is then co-precipitated with HTiO, dissolved in 9 M H 2 SO 4 , and followed through a BaSO 4 micro-precipitation step to prepare a thin-layer counting source to determine the activities of 224 Ra/ 226 Ra by alpha spectrometry. Replicate spike and blank samples were measured to evaluate the performance of the procedure. The minimum detectable activity concentration was determined to be 0.5 mBq·L -1 for 226 Ra and 0.4 mBq·L -1 for 224 Ra in 1 L of seawater sample with a counting time of 48 h. The method is a promising candidate for rapid measurement for alpha-emitting Ra isotopes in a large population of environment water samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Method validation to determine total alpha beta emitters in water samples using LSC

    International Nuclear Information System (INIS)

    Al-Masri, M. S.; Nashawati, A.; Al-akel, B.; Saaid, S.

    2006-06-01

    In this work a method was validated to determine gross alpha and beta emitters in water samples using liquid scintillation counter. 200 ml of water from each sample were evaporated to 20 ml and 8 ml of them were mixed with 12 ml of the suitable cocktail to be measured by liquid scintillation counter Wallac Winspectral 1414. The lower detection limit by this method (LDL) was 0.33 DPM for total alpha emitters and 1.3 DPM for total beta emitters. and the reproducibility limit was (± 2.32 DPM) and (±1.41 DPM) for total alpha and beta emitters respectively, and the repeatability limit was (±2.19 DPM) and (±1.11 DPM) for total alpha and beta emitters respectively. The method is easy and fast because of the simple preparation steps and the large number of samples that can be measured at the same time. In addition, many real samples and standard samples were analyzed by the method and showed accurate results so it was concluded that the method can be used with various water samples. (author)

  12. Liquid chromatography/tandem mass spectrometric confirmatory method for determining aflatoxin M1 in cow milk: comparison between electrospray and atmospheric pressure photoionization sources.

    Science.gov (United States)

    Cavaliere, Chiara; Foglia, Patrizia; Pastorini, Elisabetta; Samperi, Roberto; Laganà, Aldo

    2006-01-06

    A liquid chromatography/electrospray (ESI)-tandem mass spectrometric method for the measurement of aflatoxin M1 (AFM1) in milk is described. Milk sample after protein precipitation with acetone was cleaned-up with a Carbograph-4 cartridge. Performances of the ESI source were compared with those of the atmospheric pressure photoionization source (APPI). Although a method quantification limit (MQL) of 6 ng/kg could be achieved operating with APPI source with respect to an MQL of 12 ng/kg with ESI, all the other performances being similar, then ESI was preferred as being more robust and widespread at present.

  13. Spreadsheet design and validation for characteristic limits determination in gross alpha and beta measurement

    International Nuclear Information System (INIS)

    Prado, Rodrigo G.P. do; Dalmazio, Ilza

    2013-01-01

    The identification and detection of ionizing radiation are essential requisites of radiation protection. Gross alpha and beta measurements are widely applied as a screening method in radiological characterization, environmental monitoring and industrial applications. As in any other analytical technique, test performance depends on the quality of instrumental measurements and reliability of calculations. Characteristic limits refer to three specific statistics, namely, decision threshold, detection limit and confidence interval, which are fundamental to ensuring the quality of determinations. This work describes a way to calculate characteristic limits for measurements of gross alpha and beta activity applying spreadsheets. The approach used for determination of decision threshold, detection limit and limits of the confidence interval, the mathematical expressions of measurands and uncertainty followed standards guidelines. A succinct overview of this approach and examples are presented and spreadsheets were validated using specific software. Furthermore, these spreadsheets could be used as tool to instruct beginner users of methods for ionizing radiation measurements. (author)

  14. Determination of {alpha}{sub s} and m{sub c} in deep-inelastic scattering

    Energy Technology Data Exchange (ETDEWEB)

    Alekhin, Sergey; Bluemlein, Johannes [Deutsches Elektronen-Synchrotron (DESY), Zeuthen (Germany); Moch, Sven-Olaf [Hamburg Univ. (Germany). 2. Inst. fuer Theoretische Physik

    2013-07-15

    We describe the determination of the strong coupling constant {alpha}{sub s}(M{sub Z}{sup 2}) and of the charm-quark mass m{sub c}(m{sub c}) in the MS-scheme, based on the QCD analysis of the unpolarized World deep-inelastic scattering data. At NNLO the values of {alpha}{sub s}(M{sub Z}{sup 2})=0.1134{+-}0.001(exp) and m{sub c}(m{sub c})=1.24{+-}0.03(exp){sup +0.03}{sub -0.02}(scale){sup +0.00}{sub -0.07}(th) are obtained and are compared with other determinations, also clarifying discrepancies.

  15. Quantitative determination of alpha-quartz in airborne dust samples by x-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz In airborne respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube Is employed. NiO is used as Internal standard In order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (Author) 17 refs

  16. Quantitative determination of alpha-quartz in airbone dust samples by X-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz in airbone respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube is employec. NiO is used as internal standard in order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (auth.) [es

  17. Spectrometric techniques 2

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume II provides information pertinent to vacuum ultraviolet techniques to complete the demonstration of the diversity of methods available to the spectroscopist interested in the ultraviolet visible and infrared spectral regions. This book discusses the specific aspects of the technique of Fourier transform spectroscopy.Organized into five chapters, this volume begins with an overview of the large number of systematic effects in the recording of an interferogram. This text then examines the design approach for a Fourier transform spectrometer with focus on optics.

  18. Improved sample preparation method for environmental plutonium analysis by ICP-SFMS and alpha-spectrometry

    International Nuclear Information System (INIS)

    Varga, Z.; Stefanka, Z.; Suranyi, G.; Vajda, N.

    2007-01-01

    A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective CaF 2 co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb alpha-spectrometric measurement. For 239 Pu, 240 Pu and 241 Pu limits of detection of 9.0 fg x g -1 (0.021 mBq), 1.7 fg x g -1 (0.014 mBq) and 3.1 fg x g -1 (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials agreed well with the recommended values. (author)

  19. Elastic scattering of alpha particles from 208Pb to determine the properties of the alpha cluster states of 212Po

    International Nuclear Information System (INIS)

    Basu, C.; Adhikari, S.; Mitra, A.K.; Bhattacharya, S.; Bhattacharya, C.; Ghosh, T.K.; Banerjee, K.; Rana, T.K.; Pandey, R.; Prajapati, G.; Dey, A.; Meena, J.K.; Ray, S.

    2011-01-01

    In this work the study of α + 208 Pb elastic scattering have been undertaken to study the alpha spectroscopic properties of the cluster states of 212 Po and also obtain a α + 208 Pb potential to describe both elastic scattering and to predict the alpha cluster states and their properties in 212 Po. This two body cluster core picture is appropriate as both the components are closed shell nuclei. The measurements are performed at higher energy and analyzed in terms of the microscopic folding model for elastic scattering

  20. The EEG microstate topography is predominantly determined by intracortical sources in the alpha band.

    Science.gov (United States)

    Milz, P; Pascual-Marqui, R D; Achermann, P; Kochi, K; Faber, P L

    2017-11-15

    Human brain electric activity can be measured at high temporal and fairly good spatial resolution via electroencephalography (EEG). The EEG microstate analysis is an increasingly popular method used to investigate this activity at a millisecond resolution by segmenting it into quasi-stable states of approximately 100 ms duration. These so-called EEG microstates were postulated to represent atoms of thoughts and emotions and can be classified into four classes of topographies A through D, which explain up to 90% of the variance of continuous EEG. The present study investigated whether these topographies are primarily driven by alpha activity originating from the posterior cingulate cortex (all topographies), left and right posterior cortices, and the anterior cingulate cortex (topographies A, B, and C, respectively). We analyzed two 64-channel resting state EEG datasets (N = 61 and N = 78) of healthy participants. Sources of head-surface signals were determined via exact low resolution electromagnetic tomography (eLORETA). The Hilbert transformation was applied to identify instantaneous source strength of four EEG frequency bands (delta through beta). These source strength values were averaged for each participant across time periods belonging to a particular microstate. For each dataset, these averages of the different microstate classes were compared for each voxel. Consistent differences across datasets were identified via a conjunction analysis. The intracortical strength and spatial distribution of alpha band activity mainly determined whether a head-surface topography of EEG microstate class A, B, C, or D was induced. EEG microstate class C was characterized by stronger alpha activity compared to all other classes in large portions of the cortex. Class A was associated with stronger left posterior alpha activity than classes B and D, and class B was associated with stronger right posterior alpha activity than A and D. Previous results indicated that EEG

  1. Sources of variability in the determination by evaporation method of gross alpha activity in water samples

    International Nuclear Information System (INIS)

    Baeza, A.; Corbacho, J.A.

    2013-01-01

    Determining the gross alpha activity concentration of water samples is one way to screen for waters whose radionuclide content is so high that its consumption could imply surpassing the Total Indicative Dose as defined in European Directive 98/83/EC. One of the most commonly used methods to prepare the sources to measure gross alpha activity in water samples is desiccation. Its main advantages are the simplicity of the procedure, the low cost of source preparation, and the possibility of simultaneously determining the gross beta activity. The preparation of the source, the construction of the calibration curves, and the measurement procedure itself involve, however, various factors that may introduce sufficient variability into the results to significantly affect the screening process. We here identify the main sources of this variability, and propose specific procedures to follow in the desiccation process that will reduce the uncertainties, and ensure that the result is indeed representative of the sum of the activities of the alpha emitters present in the sample. (orig.)

  2. Determination by transfer reaction of alpha widths in fluorine for astrophysical interest; Determination par reaction de transfert de largeurs alpha dans le fluor 19. Applications a l'astrophysique

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira Santos, F. de

    1995-04-15

    The nucleosynthesis of fluorine is not known. Several astrophysical models predict the alpha radiative capture onto N{sup 15} as the main fluorine production reaction. In the expression of the reaction rate, one parameter is missing: the alpha width of the resonance on the E = 4.377 MeV level in fluorine. A direct measurement is excluded due to the very low cross-section expected. We have determined this alpha width using a transfer reaction followed by analyses with FR-DWBA (Finite Range Distorted Wave Born Approximation) in a simple cluster alpha model. This experiment was carried out with a Li{sup 7} beam with E = 28 MeV onto a N{sup 15} gas target. The 16 first levels were studied. Spectroscopic factors were extracted for most of them. Alpha widths for unbound levels were determined. Many alpha width were compared with known values from direct reaction and the differences lie within the uncertainty range (factor 2). The alpha width for the E = 4.377 MeV level was determined ({gamma}{sub {alpha}} = 1.5*10{sup -15} MeV), its value is about 60 times weaker than the used value. The influence of our new rate was studied in AGB (Asymptotic Giant Branch) stars during thermal pulses. In this model the alteration is sensitive. (author)

  3. Sensitivity of ICP-MS, PERALS and alpha spectrometry for the determination of actinides

    International Nuclear Information System (INIS)

    Ayranov, M.; Krahenbiihl, U.; Rollin, S.; Burger, M.

    2004-01-01

    The purpose of this study was to compare the sensitivity of the three most popular techniques for the determination of minor actinides at environmental levels: ICP-MS, PERALS and solid state alpha spectrometry. For each method the limit of detection and the resolution were estimated in order to study the content and isotopic composition of the actinides. The sensitivities of the three determination techniques were compared. Two international reference materials, IAEA-135 (Irish Sea sediment) and IAEA-300 (Baltic Sea sediment) were analyzed for activity concentrations of 238 Pu, 239 Pu, 240 Pu, 241 Pu and 241 Am. (authors)

  4. Log-Determinant Divergences Revisited: Alpha-Beta and Gamma Log-Det Divergences

    Directory of Open Access Journals (Sweden)

    Andrzej Cichocki

    2015-05-01

    Full Text Available This work reviews and extends a family of log-determinant (log-det divergences for symmetric positive definite (SPD matrices and discusses their fundamental properties. We show how to use parameterized Alpha-Beta (AB and Gamma log-det divergences to generate many well-known divergences; in particular, we consider the Stein’s loss, the S-divergence, also called Jensen-Bregman LogDet (JBLD divergence, Logdet Zero (Bhattacharyya divergence, Affine Invariant Riemannian Metric (AIRM, and other divergences. Moreover, we establish links and correspondences between log-det divergences and visualise them on an alpha-beta plane for various sets of parameters. We use this unifying framework to interpret and extend existing similarity measures for semidefinite covariance matrices in finite-dimensional Reproducing Kernel Hilbert Spaces (RKHS. This paper also shows how the Alpha-Beta family of log-det divergences relates to the divergences of multivariate and multilinear normal distributions. Closed form formulas are derived for Gamma divergences of two multivariate Gaussian densities; the special cases of the Kullback-Leibler, Bhattacharyya, Rényi, and Cauchy-Schwartz divergences are discussed. Symmetrized versions of log-det divergences are also considered and briefly reviewed. Finally, a class of divergences is extended to multiway divergences for separable covariance (or precision matrices.

  5. Selection of the appropriate radionuclide source for the efficiency calibration in methods of determining gross alpha activity in water

    International Nuclear Information System (INIS)

    Corbacho, J.A.; Zapata-García, D.; Montaña, M.; Fons, J.; Camacho, A.; Guillén, J.; Serrano, I.; Baeza, A.; Llauradó, M.; Vallés, I.

    2016-01-01

    Measuring the gross alpha activity in water samples is a rapid, straightforward way of determining whether the water might contain a radionuclide concentration whose consumption would imply a total indicative dose (TID) greater than some reference limit – currently set at 0.1 mSv/y in Europe. There are several methods used for such measurements. Two of them are desiccation with the salts being deposited on a planchet, and coprecipitation. The main advantage of these two methods is their ease of implementation and low cost of preparing the source to measure. However, there is considerable variability in the selection of the most suitable radioactive reference standard against which to calculate the water's gross alpha activity. The goal of this paper is to propose the most appropriate reference radionuclides to use as standards in determining gross alpha activities with these two methods, taking into account the natural radioactive characteristics of a wide range of waters collected at different points in Spain. Thus, the results will be consistent with each other and representative of the sum of alpha activities of all the alpha-emitters contained in a sample. - Highlights: • Gross alpha activity in a water sample is a rapid way of determining if its consumption imply a TID greater than reference limit. • There is considerable variability in the selection of the most suitable radioactive reference standard. • A reference radionuclide to use as standards in determining gross alpha activities in natural waters is proposed.

  6. The determination of radium-226 in uranium ores and mill products by alpha energy spectrometry

    International Nuclear Information System (INIS)

    Zimmerman, J.B.; Armstrong, V.C.

    1975-12-01

    A reliable routine procedure for determining 226 Ra by alpha energy spectrometry is described. Radium is isolated as sulphate from the sample matrix by co-precipitation with a small mass of barium and analysed using a ruggedized silicon surface barrier detector. The method is capable of providing high accuracy over a large 226 Ra concentration range and is applicable to materials such as uranium ores, uranium mill products and effluent streams. Samples resulting from nitric acid leach experiments with Elliot Lake ores were examined using the procedure. The distribution of 223 Ra, 224 Ra and 226 Ra between the leach products, (residue and leach liquor), is discussed. (author)

  7. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2015-07-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  8. Standard test method for the radiochemical determination of americium-241 in soil by alpha spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2007-01-01

    1.1 This method covers the determination of americium–241 in soil by means of chemical separations and alpha spectrometry. It is designed to analyze up to ten grams of soil or other sample matrices that contain up to 30 mg of combined rare earths. This method allows the determination of americium–241 concentrations from ambient levels to applicable standards. The values stated in SI units are to be regarded as standard. 1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precaution statements, see Section 10.

  9. Determination of uranium and thorium isotopes by solid phase extraction and alpha spectrometry

    International Nuclear Information System (INIS)

    Kuruc, J.; Kovacova, M.; Strisovska, J.; Galanda, D.

    2013-01-01

    The aim of this work was to test the modified method suitable for the separation of isotopes of uranium and thorium samples of rocks, including gold ore and gold concentrate using of extraction chromatography method, after digestion of the sample, concentrating, separate the isotopes of uranium and thorium isotopes to prepare sources for the measurement of alpha spectra. Samples of rocks, gold ore and gold concentrate were digered in microwave decomposition in the environment of hydrogen peroxide and concentrated nitric acid. For the separation of uranium and thorium the vacuum box with cartridges DGA Resin and Resin(R) UTEVA (Triskem International, France) was used. Both sorbents allow separation of uranium from thorium. The results confirmed that the both sorbents give the same results within expanded uncertainty. The mass activity of monitored uranium and thorium radioisotopes was determined by alpha spectrometry method. The yields of separation were determined using uranium-232 as a tracer radionuclide; the activity of 232 U was 0.1438 Bq. Alpha spectra were measured on the Alpha spectrometer EG and G ORTEC 576A with the software MAESTRO, MCA Emulator and Gamma Vision-32 for Windows, USA. Mass activities of radionuclides were converted to mass concentration of isotopes 238 U, 234 U, 232 Th, 230 Th and 228 Th. The highest concentration of 238 U was sampled in granodiorite (Tunnel S-XIV-2, southwards, mining of Cu ore, not working there since 1990), where m( 238 U) = (0.81 ± 0.09) mg kg -1 (DGA Resin) and m( 238 U) = (0.90 ± 0.09) mg kg -1 (UTEVA(R) Resin), as well as m( 232 Th) = (18.8 ± 1.7) mg kg -1 (DGA Resin) and m( 232 Th) = (17.8 ± 1.5) mg kg -1 (UTEVA(R) Resin). In other samples of rocks, gold ore and gold concentrates have specific masses of isotopes of uranium and thorium two-to ten-folds lower. It can be concluded that the rocks, gold ores and concentrates of gold from the 'Rozalia' mine contain lower concentrations of uranium several times against

  10. Realisation of a {beta} spectrometer solenoidal and a double {beta} spectrometer at coincidence; Realisation d'un spectrometre {beta} solenoidal et d'un double spectrometre {beta} a coincidence

    Energy Technology Data Exchange (ETDEWEB)

    Moreau, J. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-06-15

    The two spectrometers have been achieved to tackle numerous problems of nuclear spectrometry. They possess different fields of application that complete themselves. The solenoidal spectrometer permits the determination of the energy limits of {beta} spectra and of their shape; it also permits the determination of the coefficients of internal conversion and reports {alpha}{sub K} / {alpha}{sub L} and it is especially efficient for the accurate energy levels of the {gamma} rays by photoelectric effect. The double coincidence spectrometer has been conceived to get a good efficiency in coincidence: indeed, the sum of the solid angles used for the {beta} and {gamma} emission is rather little lower to 4{pi} steradians. To get this efficiency, one should have sacrificed a little the resolution that is lower to the one obtained with the solenoidal spectrometer for a same brightness. Each of the elements of the double spectrometer can also be adapted to the study of angular correlations {beta}{gamma} and e{sup -}{gamma}. In this use, it is superior to the thin magnetic lens used up to here. The double spectrometer also permits the survey of the coincidences e{sup -}e{sup -}, e{sup -}{beta} of a equivalent way to a double lens; it can also be consider some adaptation for the survey of the angular correlations e{sup -}e{sup -}, e{sup -}{beta}. Finally, we applied the methods by simple spectrometry and by coincidence spectrometry, to the study of the radiances of the following radioelements: {sup 76}As (26 h), {sup 122}Sb (2,8 j), {sup 124}Sb (60 j), {sup 125}Sb (2,7 years). (M.B.) [French] Les deux spectrometres qui ont ete realises permettent d'aborder un grand nombre de problemes de spectrometrie nucleaire. Ils possedent des champs d'application tres differents qui se completent. Le spectrometre solenoidal permet la determination des energies limites des spectres {beta} et de leur forme; il permet aussi la determination des coefficients de conversion interne et

  11. Quantitative determination of plant phenolics in Urtica dioica extracts by high-performance liquid chromatography coupled with tandem mass spectrometric detection.

    Science.gov (United States)

    Orčić, Dejan; Francišković, Marina; Bekvalac, Kristina; Svirčev, Emilija; Beara, Ivana; Lesjak, Marija; Mimica-Dukić, Neda

    2014-01-15

    A method for quantification of 45 plant phenolics (including benzoic acids, cinnamic acids, flavonoid aglycones, C- and O-glycosides, coumarins, and lignans) in plant extracts was developed, based on reversed phase HPLC separation of extract components, followed by tandem mass spectrometric detection. The phenolic profile of 80% MeOH extracts of the stinging nettle (Urtica dioica L.) herb, root, stem, leaf and inflorescence was obtained by using this method. Twenty-one of the investigated compounds were present at levels above the reliable quantification limit, with 5-O-caffeoylquinic acid, rutin and isoquercitrin as the most abundant. The inflorescence extracts were by far the richest in phenolics, with the investigated compounds amounting 2.5-5.1% by weight. As opposed to this, the root extracts were poor in phenolics, with only several acids and derivatives being present in significant amounts. The results obtained by the developed method represent the most detailed U. dioica chemical profile so far. Copyright © 2013 Elsevier Ltd. All rights reserved.

  12. Determination of plutonium isotopes in bilberry using liquid scintillation spectrometry and alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Seferinoğlu, Meryem; Aslan, Nazife; Kurt, Aylin; Erden, Pınar Esra; Mert, Hülya

    2014-01-01

    This paper presents α-particle spectrometry and liquid scintillation spectrometry methods to determine plutonium isotopes in bilberry. The analytical procedure involves sample preparation steps for ashing, digestion of bilberry samples, radiochemical separation of plutonium radioisotopes and their measurement. The validity of the method was checked for coherence using the ζ test, z-test, relative bias and relative uncertainty outlier tests. The results indicated that the recommended procedures for both measurement systems could be successfully applied for the accurate determination of plutonium activities in bilberry samples. - Highlights: • Sample preparation methods for Pu using LSS and alpha spectrometry developed. • Complete separation of plutonium from interfering radionuclides. • Commercial bilberry was spiked with NPL 2011 (AH-B11144) proficiency test sample. • Results were checked using ζ test, z-test, rel. bias and rel. uncert. outlier tests. • Recommended procedures successfully applied to bilberry samples

  13. Determination of 239Pu/240Pu isotopic ratio by high resolution alpha-particle spectrometry

    International Nuclear Information System (INIS)

    Amoudry, F.; Burger, P.

    1983-05-01

    The development of passivated ion-implanted silicon detectors and of very thin alpha-particle sources improves the resolution of alpha-particle spectra and allows to separate energy pics up to now unseparate. The 239 Pu/ 240 Pu isotopic ratio of a mixture has been measured using the alpha spectrometry deconvolution code DEMO [fr

  14. Inclusive-jet photoproduction at HERA and determination of {alpha}{sub s}

    Energy Technology Data Exchange (ETDEWEB)

    Abramowicz, H. [Tel Aviv Univ. (Israel). School of Physics; Max Planck Institute for Physics, Munich (Germany); Abt, I. [Max Planck Institute for Physics, Munich (Germany); Adamczyk, L. [AGH-Univ. of Science and Technology, Krakow (PL). Faculty of Physics and Applied Computer Science] (and others)

    2012-03-15

    Inclusive-jet cross sections have been measured in the reaction ep{yields}e+jet+X for photon virtuality Q{sup 2}<1 GeV{sup 2} and {gamma}p centre-of-mass energies in the region 14217 GeV and -1<{eta}{sup jet}<2.5. In addition, measurements of double-differential inclusive-jet cross sections are presented as functions of E{sub T}{sup jet} in different regions of {eta}{sup jet}. Next-to-leading-order QCD calculations give a good description of the measurements, except for jets with low E{sub T}{sup jet} and high {eta}{sup jet}. The influence of non-perturbative effects not related to hadronisation was studied. Measurements of the ratios of cross sections using different jet algorithms are also presented; the measured ratios are well described by calculations including up to O({alpha}{sub s}{sup 2}) terms. Values of {alpha}{sub s}(MZ) were extracted from the measurements and the energy-scale dependence of the coupling was determined. The value of {alpha}{sub s}(MZ) extracted from the measurements based on the k{sub T} jet algorithm is {alpha}{sub s}(MZ) = 0.1206{sub -0.0022}{sup +0.0023}(exp.){sub -0.0035}{sup +0.0042}(th.); the results from the anti-k{sub T} and SIScone algorithms are compatible with this value and have a similar precision.

  15. The Determination of Gross Alpha And Beta Activity of Drinking Water in Turkey

    International Nuclear Information System (INIS)

    Dilaver, A.T.; Cifter, C.; Altay, T.

    2002-01-01

    Man and his environment must be protected from the adverse effects of pesticides, radiation, noise and other forms of pollutions. Radioactive materials occur naturally in the environment (for example uranium, thorium and potassium). Same radioactive compounds arise from human activities (for example from medical or industrial uses of radioactivity). Drinking water should be safe to use and aesthetically pleasing. World Health Organisation (WHO) and Turkish Standards (TSE) have established maximum contaminant levels for gross alpha and gross beta. The purpose of these study is to determine the level of gross alpha and gross beta activities of samples collected from the different Regional Directories of The State Hydraulic Works (DSI)). After that compare the results versus permissible values of World Health Organisation and Turkish Standards. Collected samples from 14 Regional Directories of The State Hydraulic Works (DSI), have completed. All the analyses results suitable for WHO and TSE. We will give all the research our final report after completed the other Regional Directories' s analyses

  16. An improved method for determination of uranium isotopic composition in urine by alpha spectrometry

    International Nuclear Information System (INIS)

    Duarte, C.L.; Szeles, M.S.M.F.

    1994-01-01

    A comparative study of source preparation techniques to determine uranium isotopic composition by alpha spectrometry, namely electrodeposition and chemical stripping with polymeric membrane containing trioctylphosphine oxide (TOPO), is presented. The mean yield obtained for electrodeposition and TOPO deposition were 85% and 74%, respectively. The mean activity ratio 235 U/ 238 U were 0.044 and 0.042 and the ratio 234 U/ 238 U were 0.994 and 1.009, using electrodeposition and TOPO deposition techniques, respectively. The method of uranium separation from urine using an ion-exchange resin Dowex 1 x 8, chloride form and citrate form, was also studied. The obtained global yields of these methods were 50% and 41%, respectively. (author)

  17. Determination of uranium and polonium in Spa rus aura ta by alpha spectrometry

    International Nuclear Information System (INIS)

    Luna P, M.; Renteria, M.; Montero C, M. E.; Manjon C, G.; Diaz, I.

    2012-01-01

    The aim of this study was optimizing conditions for the specific activities determination of some uranium-series radionuclides present in Spa rus aura ta by alpha spectrometry. Determinations of specific activities were conducted varying the type of digestion: acid attack on hot plate, controlled microwave digestion and acid attack after calcination of the sample. The latter procedure was applied only to the case of uranium isotopes determination. The variation in the isotope extraction method consisted of applying the techniques of liquid-liquid extracting using Tributyl phosphate or chromatographic UTEVA resin. Results depending on the type of treatment given to the samples were compared based on obtained chemical yields. The results reveal a higher bioaccumulation of polonium in the liver sample, with activities of 0.809, 2.495 and 2.439 Bq kg -1 fresh wt compared with the fillet. The best chemical yields of polonium were close to 60% for samples that were digested by microwave. In the case of uranium the best chemical yields, close to 80% for fillet, were obtained with a previous calcination of the sample and using the UTEVA resin. (Author)

  18. Determination of uranium and polonium in Spa rus aura ta by alpha spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Luna P, M.; Renteria, M.; Montero C, M. E. [Centro de Investigacion en Materiales Avanzados, S. C., Miguel de Cervantes No. 120, Complejo Industrial Chihuahua, 31109 Chihuahua (Mexico); Manjon C, G.; Diaz, I., E-mail: elena.montero@cimav.edu.mx [Universidad de Sevilla, Escuela Tecnica Superior de Arquitectura, Departamento de Fisica Aplicada II, San Fernando No. 4, 41004 Sevilla (Spain)

    2012-06-15

    The aim of this study was optimizing conditions for the specific activities determination of some uranium-series radionuclides present in Spa rus aura ta by alpha spectrometry. Determinations of specific activities were conducted varying the type of digestion: acid attack on hot plate, controlled microwave digestion and acid attack after calcination of the sample. The latter procedure was applied only to the case of uranium isotopes determination. The variation in the isotope extraction method consisted of applying the techniques of liquid-liquid extracting using Tributyl phosphate or chromatographic UTEVA resin. Results depending on the type of treatment given to the samples were compared based on obtained chemical yields. The results reveal a higher bioaccumulation of polonium in the liver sample, with activities of 0.809, 2.495 and 2.439 Bq kg{sup -1} fresh wt compared with the fillet. The best chemical yields of polonium were close to 60% for samples that were digested by microwave. In the case of uranium the best chemical yields, close to 80% for fillet, were obtained with a previous calcination of the sample and using the UTEVA resin. (Author)

  19. Design quality control of the activity determination total alpha liquid effluents; Diseno de control de calidad de la determinacion de actividad alfa total en efluentes liquidos

    Energy Technology Data Exchange (ETDEWEB)

    Yague, L.; Alvarez, A.; Navarro, N.; Noguerales, C.

    2011-07-01

    The total alpha activity index is the joint action of all alpha emissions in a sample. This is a very useful in designing the analytical control of liquid effluent into the environment. Presents the design of quality control applied to the determination of total alpha activity.

  20. A sequential extraction procedure to determine Ra and U isotopes by alpha-particle spectrometry in selective leachates

    International Nuclear Information System (INIS)

    Aguado, J.L.; Bolivar, J.P.; San-Miguel, E.G.; Garcia-Tenorio, R.

    2003-01-01

    A radiochemical sequential extraction procedure has been developed in our laboratory to determine 226 Ra and 234,238 U by alpha spectrometry in environmental samples. This method has been validated for both radionuclides by comparing in selected samples the values obtained through its application with the results obtained by applying alternative procedures. Recoveries obtained, counting periods applied and background levels found in the alpha spectra give suitable detection limits to allow the Ra and U determination in operational forms defined in riverbed contaminated sediments. Results obtained in these speciation studies show that 226 Ra and 234,238 U contamination tend to be associated to precipitated forms of the sediments. (author)

  1. Sensitive determination of zearalenone and alpha-zearalenol in barley and Job's-tears by liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Tanaka, T; Teshima, R; Ikebuchi, H; Sawada, J; Terao, T; Ichinoe, M

    1993-01-01

    A sensitive and reliable method for liquid chromatographic (LC) determination of zearalenone and alpha-zearalenol in barley and Job's-tears was investigated. The method by which these toxins were determined involves addition of an internal standard (zearalenone 6'-oxime) to barley and Job's-tears samples. Extracts from grain samples were cleaned up by passage through chromatography on piperidinohydroxypropyl Sephadex LH-20 as a lipophilic gel. Individual toxins were resolved by LC on a reversed-phase (ODS) column with fluorescence detection. The detection limit is estimated to be 0.2 ng for zearalenone and alpha-zearalenol standards. Known amounts of zearalenone and alpha-zearalenol (25-1250 ng) were added to a barley sample (5 g). Average recoveries for alpha-zearalenol and zearalenone, respectively, ranged from 96 to 102% (mean CV, 3.6%) and from 96 to 103% (mean CV, 3.3%). This method is applicable to determination of alpha-zearalenol and zearalenone in barley and Job's tears with satisfactory sensitivity and accuracy.

  2. Standard test method for radiochemical determination of uranium isotopes in soil by alpha spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the determination of alpha-emitting uranium isotopes in soil. This test method describes one acceptable approach to the determination of uranium isotopes in soil. 1.2 The test method is designed to analyze 10 g of soil; however, the sample size may be varied to 50 g depending on the activity level. This test method may not be able to completely dissolve all forms of uranium in the soil matrix. Studies have indicated that the use of hydrofluoric acid to dissolve soil has resulted in lower values than results using total dissolution by fusion. 1.3 The lower limit of detection is dependent on count time, sample size, detector, background, and tracer yield. The chemical yield averaged 78 % in a single laboratory evaluation, and 66 % in an interlaboratory collaborative study. 1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only. 1.5 This standard does not purport to address all of the safety concerns, if any, ass...

  3. Conductometry, spectrophotometry and mass spectrometric ...

    African Journals Online (AJOL)

    ... versus the mole ratio of [AZT]/[M2+], Job's method of continuous variation and mole ratio method showed the stoichiometry to be 1:1 (M2+:AZT) for both the cations. The metal ion-AZT complexes formed through the nitrogen of the azide group were further ascertained by liquid chromatography-mass spectrometric analysis.

  4. NZG 201 portable spectrometric unit

    International Nuclear Information System (INIS)

    Jursa, P.; Novakova, O.; Slezak, V.

    The NZG 201 spectrometric unit is a portable single-channel processing unit supplied from the mains or a battery which allows the qualitative and quantitative measurement of different types of ionizing radiation when connected to a suitable detection unit. The circuit layout and the choice of control elements makes the spectrometric unit suitable for use with scintillation detector units. The spectrometric unit consists of a pulse amplifier, an amplitude pulse analyzer, a pulse counter, a pulse rate counter with an output for a recorder, a high voltage source and a low voltage source. The block diagram is given. All circuits are modular and are mounted on PCB's. The apparatus is built in a steel cabinet with a raised edge which protects the control elements. The linear pulse amplifier has a maximum gain of 1024, the pulse counter has a maximum capacity of 10 6 -1 imp and time resolution better than 0.5 μs. The temperature interval at which the apparatus is operational is 0 to 45 degC, its weight is 12.5 kg and dimensions 36x280x310 mm, energy range O.025 to 2.5 MeV, for 137 Cs the energy resolution is 8 to 10%. The spectrometric unit NZG 2O1 may, with regard to its parameters, number and range of control elements, be used as a universal measuring unit. (J.P.)

  5. Determination of aminopolycarboxylic acids in river water by solid-phase extraction on activated charcoal cartridges and gas chromatography with mass spectrometric detection. Method performance characteristics and estimation of the uncertainty.

    Science.gov (United States)

    Jiménez, Juan J

    2013-04-03

    A new sample preparation procedure to determine aminopolycarboxylic acids (ethylenediaminetetraacetic acid, EDTA, nitrilotriacetic acid, NTA, diethylenetriaminepentaacetic acid, DTPA, and cyclohexanediaminetetraacetic acid, CDTA) in river water is described. The procedure consists of the solid-phase extraction of the aminopolycaroxyllic acids on activated charcoal cartridges after increasing the ionic strength and acidifying the sample. The extract was eluted with methanol and the analytes were methylated in presence of BF3/methanol to determine them by GC with mass spectrometric detection. Recoveries were higher than 90% with good repeatabilities and inter-day precision for concentrations close to quantification limits (about 10 μg L(-1)) and higher. It has been verified that the proposed method is robust according to the Youden and Steiner test and free of matrix effects arisen from the presence of organic matter and iron(III) as deduced from statistical tests. A bottom-up approach was followed to estimate the uncertainty of the measured concentration. At concentrations close to 10 μg L(-1) the most relevant step of the method is the calculus of the interpolated concentration which has a high value of relative standard uncertainty. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Determination of environmental actinide nuclides and 210Pb (210Po) by low-energy photon spectrometry with alpha-spectrometry

    International Nuclear Information System (INIS)

    Sakanoue, Masanobu; Yamamoto, M.; Komura, Kazuhisa

    1987-01-01

    Low-energy photon spectrometry with alpha spectrometry was used to determine the environmental concentrations of low-level actinides and other nuclides, especially 210 Pb and 210 Po. The isotopic ratio of 2 40 Pu/ 239 Pu was successfully determined by measuring L x -ray/α-ray counting ratio. A reliable method was developed for the determination of extremely low-level 237 Np global fallout in environmental samples. The non-destructive determination by Ge-LEPS for natural 210 Pb in various samples (tobacco leaves, commercially available tobacco, etc.) was also carried out with the determination of 210 Po by alpha spectrometry using 209 Po as a yield tracer. (author) 6 refs.; 5 tabs

  7. Determination of specific alpha-radioactivity of flora samples from semipalatinsk test site (STS)

    International Nuclear Information System (INIS)

    Blekhman, A.M.; Dujsenbaev, A.; Orazova, A.O.

    1999-01-01

    For further rehabilitation of soil earlier contaminated with radioactive fallout, the method of radionuclide absorption by plants is vital. The last updating of electronic system of the facility meant to analyze impulse shape /2/ helped to enlarge dynamical range of registration and reduction of identification threshold for alpha particles up to 50 keV. We have developed methods for STS flora samples preparation and performed first measurements of their specific alpha activity. Measurement results are in table 1. Measurement results analysis shows that STS flora samples can accumulate considerable concentrations of alpha active nuclides

  8. Polar angle as a determinant of amphipathic alpha-helix-lipid interactions: a model peptide study.

    Science.gov (United States)

    Uematsu, N; Matsuzaki, K

    2000-10-01

    Various physicochemical properties play important roles in the membrane activities of amphipathic antimicrobial peptides. To examine the effects of the polar angle, two model peptides, thetap100 and thetap180, with polar angles of 100 degrees and 180 degrees, respectively, were designed, and their interactions with membranes were investigated in detail. These peptides have almost identical physicochemical properties except for polar angle. Like naturally occurring peptides, these peptides selectively bind to acidic membranes, assuming amphipathic alpha-helices, and formed peptide-lipid supramolecular complex pores accompanied by lipid flip-flop and peptide translocation. Despite its somewhat lower membrane affinity, thetap100 exhibited higher membrane permeabilization activity, a greater flip-flop rate, as well as more antimicrobial activity due to a higher pore formation rate compared with thetap180. Consistent with these results, the peptide translocation rate of thetap100 was higher. Furthermore, the number of peptides constituting thetap100 pores was less than that of thetap180, and thetap100 pores involved more lipid molecules, as reflected by its cation selectivity. The polar angle was found to be an important parameter determining peptide-lipid interactions.

  9. Determination of alpha-Tocopherol (vitamin E) in irradiated garlic by high performance liquid chromatography (HPLC); Determinacao de alpha-tocoferol em alho irradiado utilizando cromatografia liquida de alta frequencia (CLAE)

    Energy Technology Data Exchange (ETDEWEB)

    Rios, Magda Dias Goncalves; Penteado, Marilene de Vuono Camargo [Sao Paulo Univ., SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Alimentos e Nutricao Experimental]. E-mail: riosmagda@hotmail.com

    2003-02-01

    The effects of {sup 60}Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the {alpha}-tocopherol concentration were studied. The {alpha}-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The {alpha}-tocopherol was determined through normal phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic {alpha}-tocopherol content. (author)

  10. Determining the level of gross alpha and beta radioactivity of water from Marilao river using liquid scintillation counter

    International Nuclear Information System (INIS)

    Cruz, J.; Magtaka, J.; Balisi, R.; Castaneda, Soledad; De Vero, J.

    2009-01-01

    This study aims to determine the level of gross alpha- and beta- radioactivity present in the Marilao River. Liquid Scintillation Counter was used to detect samples radioactivity. Water samples were taken along the different spots of Marilao River. The results showed that the radioactivity are below the Philippine National Standard for Drinking Water (PNSDW) which is 0.1 Bq/L for gross alpha activity and 1.0 Bq/L for gross beta activity set by the Dept. of Health. Hence water samples from Marilao River, is safe in terms of the level of radioactivity levels.(author)

  11. Alpha- and beta-adrenoceptors in hypertension. II. Platelet alpha 2- and lymphocyte beta 2-adrenoceptors in children of parents with essential hypertension. A model for the pathogenesis of the genetically determined hypertension

    NARCIS (Netherlands)

    Michel, M. C.; Galal, O.; Stoermer, J.; Bock, K. D.; Brodde, O. E.

    1989-01-01

    To study whether changes in alpha- and beta-adrenoceptors in human essential hypertension (EHT) might be genetically determined, we assessed platelet alpha 2- and lymphocyte beta 2-adrenoceptor density in 48 normotensive children of normotensive parents (NT) and in 41 normotensive children with one

  12. Quantitative determination of α-ionone, β-ionone, and β-damascenone and enantiodifferentiation of α-ionone in wine for authenticity control using multidimensional gas chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Langen, Johannes; Wegmann-Herr, Pascal; Schmarr, Hans-Georg

    2016-09-01

    Native concentrations of α-ionone, β-ionone, and β-damascenone were studied in various authentic and commercial wines. In addition, the enantiomeric distribution of α-ionone was determined and its merits as a potential marker for aroma adulteration in wine were discussed. For extraction of volatiles, headspace solid-phase microextraction (HS-SPME) was applied, followed by heart-cut multidimensional gas chromatography coupled to tandem mass spectrometric detection for trace-level analysis. The enantioselective analysis of α-ionone was achieved with octakis(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin as the chiral selector in the separation column for gas chromatography (GC). In all the authentic wines studied, α-ionone showed a high enantiomeric ratio in favor of the (R)-enantiomer. Since an illegal addition of α-ionone in a racemic form changes the enantiomeric ratio, this ratio may serve as an adulteration marker. Concentrations varied between authenticity markers in wine.

  13. Extraction and preconcentration of trace Al and Cr from vegetable samples by vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction prior to atomic absorption spectrometric determination.

    Science.gov (United States)

    Altunay, Nail; Yıldırım, Emre; Gürkan, Ramazan

    2018-04-15

    In the study, a simple, and efficient microextraction approach, which is termed as vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction (VA-IL-DLLME), was developed for flame atomic absorption spectrometric analysis of aluminum (Al) and chromium (Cr) in vegetables. The method is based on the formation of anionic chelate complexes of Al(III) and Cr(VI) with o-hydroxy azo dye, at pH 6.5, and then extraction of the hydrophobic ternary complexes formed in presence of cetyltrimethylammonium bromide (CTAB) into a 125 μL volume of 1-butyl-3-methylimidazolium bis(trifluorosulfonyl)imide [C 4 mim][Tf 2 N]) as extraction solvent. Under optimum conditions, the detection limits were 0.02 µg L -1 in linear working range of 0.07-100 µg L -1 for Al(III), and 0.05 µg L -1 in linear working range of 0.2-80 µg L -1 for Cr(VI). After the validation by analysis of a certified reference material (CRM), the method was successfully applied to the determination of Al and Cr in vegetables using standard addition method. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Determination of alpha activity produced by Indian tea samples using solid state nuclear track detection technique

    International Nuclear Information System (INIS)

    Azam, Ameer; Naqvi, A.H.; Srivastava, D.S.

    2001-01-01

    India has first place in the world in the production, consumption and export of tea. The average production of tea in India is about 780 million kg annually. Indian population uses tea as a favourite beverage specially with the breakfast. Tea leaves are perennial plants and they have extension root system spread over deeper layers in the soil. Soil contains uranium as trace element. Hence, uranium is transferred to the leaves as a result of uptake from the soil over the years. Since many of the decay products of uranium are alpha emitters hence tea is a source of alpha radioactivity and can cause damaging effects. Therefore, data on alpha activity of tea samples will be useful in estimating these harmful effects at least qualitatively. In the present study the alpha activity produced by thirteen samples of tea available in the local market was measured

  15. Field preconcentration of cadmium from seawater by using a minicolumn packed with Amberlite XAD-4/4-(2-pyridylazo) resorcinol and its flow-injection-flame atomic absorption spectrometric determination at the ng L{sup -1} Level

    Energy Technology Data Exchange (ETDEWEB)

    Yebra, M.C.; Salgado, J.; Puig, L.; Moreno-Cid, A. [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, 15782-Santiago de Compostela (Spain)

    2002-10-01

    A flow injection analysis-flame atomic absorption spectrometric method for the determination of cadmium in seawater was developed with the aim of yielding a sensitive assay with a low detection limit. The method employs a field flow preconcentration technique involving a minicolumn containing Amberlite XAD-4 impregnated with the complexing agent 4-(2-pyridylazo) resorcinol. A Plackett-Burman 2{sup 7} x 3/32 design for seven factors (sample pH, sample flow rate, eluent volume, eluent concentration, eluent flow rate, ethanol percentage in the eluent and minicolumn diameter) was carried out in order to find the significant variables affecting the field continuous preconcentration system (FCPS) and the flow injection elution manifold for cadmium determination in seawater samples by flame atomic absorption spectrometry. Cadmium can be preconcentrated with an enrichment factor of 1053 for a sample volume of 200 mL and a preconcentration time of 57 min. In these experimental conditions, the method provides a linear relationship between absorbance and cadmium concentration in the range from 22-1900 ng L{sup -1}, with a detection limit (3SD) of 6 ng L{sup -1}. The precision (expressed as relative standard deviation) for eleven independent determinations reached values of 8.9-0.8% in cadmium solutions of 50-700 ng L{sup -1}. Analysis of certified reference materials (SLEW-3 and NASS-5) showed good agreement with the certified value. This procedure was applied to the determination of cadmium in seawater from Galicia (Spain). (orig.)

  16. Determination of the cross-reactivities for alpha-zearalenol, beta-zearalenol, zearalanone, alpha-zearalanol, and beta-zearalanol on three commercial immunoaffinity columns targeting zearalenone.

    Science.gov (United States)

    Erbs, Marianne; Hartmann, Niccolo; Bucheli, Thomas D

    2007-01-01

    Immunoaffinity extraction has become increasingly important as a sample preparation and cleanup method in mycotoxin analysis. In this study, the antibody specificities of 3 commercial immunoaffinity columns (IACs) targeting zearalenone (ZON) were compared for alpha-zearalenol, beta-zearalenol, zearalanone, alpha-zearalanol, and beta-zearalanol. The recoveries of ZON and its 5 analogs were determined in triplicate when extracted from 10 mL circumneutral river water samples spiked with 20 ng analyte individually or in a mixture. The analytes were analyzed by means of electrospray ionization liquid chromatography/tandem mass spectrometry using deuterated internal standards for quantitation. Recoveries ranged from 69 to 115% for all analytes with relative standard deviations of 1-39%. Cross-reactivities for the analogs were > 80% when applied both individually and in a mixture. No significant competition effects were observed when the compounds were applied as a multianalyte mixture well below the stated IAC capacities. The results obtained here demonstrate that all IACs tested are highly cross-reactive towards the 5 ZON derivatives and may be applied for their simultaneous extraction or cleanup.

  17. Improved gas chromatography-negative ion chemical ionization tandem mass spectrometric method for determination of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in hair using mechanical pulverization and bead-assisted liquid-liquid extraction.

    Science.gov (United States)

    Kim, Jin Young; Cheong, Jae Chul; Lee, Jae Il; In, Moon Kyo

    2011-03-20

    A gas chromatography-negative ion chemical ionization tandem mass spectrometric (GC-NCI-MS/MS) method was developed and validated for the determination of 11-nor-Δ(9)-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in human hair. After decontamination, hair samples were weighed (25mg), mechanically pulverized with a bead mill, and incubated in 0.7 mL of 1.0M sodium hydroxide at 95 °C for 30 min. Bead-assisted liquid-liquid extraction was performed with n-hexane:ethyl acetate (9:1, v/v), a method developed in our laboratory. The extract was evaporated to dryness, derivatized with pentafluoropropanol and pentafluoropropionic anhydride, and analyzed by GC-MS/MS in the negative ion chemical ionization mode using methane as the reagent gas. The linear ranges were 0.05-10.0 pg/mg for THC-COOH with the coefficient of determination (r(2) = 0.9976). The intra-day and inter-day precisions were within 1.7 and 13.8%, respectively. The intra-day and inter-day accuracies were -4.8 to 10.0% and -3.9 to 3.8%, respectively. The limit of detection and quantification were 0.015 and 0.05 pg/mg, respectively. The recoveries were in the range of 79.4-87.1%. The results indicate that the proposed method is simple, rapid, accurate, and precise for determination of THC-COOH in hair. The method identified THC-COOH in hair specimens from suspected marijuana abusers. Copyright © 2011. Published by Elsevier Ireland Ltd.

  18. [Determination of alpha-arbutin, beta-arbutin and niacinamide in cosmetics by high performance liquid chromatography].

    Science.gov (United States)

    Cheng, Peng; Chen, Meilan; Zhu, Yan

    2010-01-01

    A high performance liquid chromatography (HPLC) method for the determination of two optical isomers of arbutin (alpha-arbutin and beta-arbutin) and niacinamide in cosmetics was developed. The samples were extracted by the mixture of salt water and chloroform (2:1, v/v). The separation was performed on an ODS-BP column (200 mm x 4.6 mm, 5 microm, Elite) with methanol-water (10:90, v/v) as the mobile phase at a flow rate of 0.5 mL/min and 25 degrees C. The detection wavelength was set at 220 nm and the sample injection volume was 20 microL. There were good linear relationships between the mass concentration and the peak areas of alpha-arbutin, beta-arbutin and niacinamide in the ranges of 0.07-50, 0.06-50 and 0.05-50 mg/L, respectively. The relative standard deviations (RSDs, n = 7) of alpha-arbutin, beta-arbutin and niacinamide were 1.65%, 1.73% and 1.33%, respectively. The proposed method has been applied for the determination of alpha-arbutin, beta-arbutin and niacinamide in cosmetics with recoveries of 91.7%-109.6%. This method is rapid, simple and suitable for the detection of whitening ingredients in cosmetic.

  19. On-line preconcentration of cobalt in drinking water using a minicolumn packed with activated carbon coupled to electrothermal atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Cerutti, Soledad; Moyano, Susana; Gasquez, Jose A.; Stripeikis, Jorge; Olsina, Roberto A.; Martinez, Luis D. E-mail: ldm@unsl.edu.ar

    2003-11-21

    An on-line flow injection preconcentration-electrothermal atomic absorption spectrometry method is developed for trace determination of cobalt in drinking water samples by sorption on a conical minicolumn packed with activated carbon at pH 9.5. The cobalt was eluted from the minicolumn with 10% (v/v) nitric acid. An enrichment factor of 190-fold for a sample volume of 10 ml was obtained. The detection limit (DL) value for the preconcentration method proposed was 5 ng l{sup -1}. The precision for 10 replicate determinations at the 50 ng l{sup -1} Co level was 4.7% relative standard deviation. The calibration graph using the preconcentration system for cobalt was linear with a correlation coefficient of 0.9993 at levels near the DLs up to at least 0.35 {mu}g l{sup -1}. The method was successfully applied to the determination of cobalt in drinking water samples.

  20. [Butanol extraction combined with dilute hydrochloric acid dissolution-atomic fluorescence spectrometric method for indirect determination of molybdenum in Chinese herbal medicine].

    Science.gov (United States)

    Lu, Jian-Ping; Geng, Guo-Xing; Tang, Yan-Kui; Lu, Zhi-Yong

    2012-12-01

    A method for indirectly determining the molybdenum in Chinese herbal medicine by butanol extraction and dilute hydrochloric acid dissolution was established for atomic fluorescence spectrometry. The molybdoarsenate heteropoly acid, formed in the presence of As(V) and ammonium molybdate in 0.3 mol x L(-1) sulphuric acid medium, was separated and enriched in the organic solvent, then the evaporation of organic reagent was implemented and the left residue was dissolved in dilute hydrochloric acid in which the arsenic content was determined on behalf of molybdenum. In the optimum experimental conditions, molybdenum content in 0-15 microg x L(-1) range depicts a good linear relationship, the detection limit and relative standard deviation of 0.44 microg x L(-1) and 1.1% were obtained, respectively. Spiked Chinese herbal medicine samples were determined with the proposed method, and recoveries of 95.6%-101.3% were achieved.

  1. Preconcentration and atomic absorption spectrometric determination of cadmium, cobalt, copper, iron, lead, manganese, nickel and zinc in water samples using 6-methyl-2-pyridinecarboxaldehyde-4-phenyl-3-thiosemicarbazone

    International Nuclear Information System (INIS)

    Khuhawar, M.Y.; Das, P.; Dewani, V.K.

    2005-01-01

    The reagent 6-methyl-2-pyridinecarboxaldehyde-4-phenyl-3-thiosemicarbazone (MPAPT) has been examined for the pre-concentration of metal ions and determination using air acetylene flame atomic absorption spectrometer. The method is based on the complexation and extraction of cadmium (II), cobalt(III), copper(II), lead(II), nickel(II), iron(II), iron(II), manganese(II) and zinc(II) in chloroform. The metal iron are back extracted in nitric acid (1:1) or after evaporation of solvent the residue is digested in nitric acid. After necessary adjustment of volume the metal ions were determined in aqueous solution. Pre-concentration is obtained 10-25 times. Metal ions recovery was 95.4-100.8% with coefficient of variation 0.2-7.5%. The method used for the determination of metals in canal and sewerage waters, within 2-6433 mu g/L with C. V 0.-5.2%. (author)

  2. Design and construction of a system for determining Radon-222 through Alpha spectroscopy

    International Nuclear Information System (INIS)

    Bonifacio, J.; Iturbe, J.L.

    1992-02-01

    The study of the present work consists on designing a system to measure gas 222 Rn, using a surface barrier detector, in order to obtaining a more accuracy measure of this isotope by means of an alpha particle spectra and thus to try to avoid the influence of the radioactivity of the isotope descendants of short half life, which are also emitting of alpha particles, since by other methods its should make a series of corrections to obtain the real value of the radon activity. (Author)

  3. Determination of the anthraquinones aloe-emodin and aloin-A by liquid chromatography with mass spectrometric and diode array detection.

    Science.gov (United States)

    Elsohly, Mahmoud A; Gul, Waseem; Avula, Bharathi; Khan, Ikhlas A

    2007-01-01

    Methods using liquid chromatography/mass spectrometry (LC/MS) and LC with diode array detection (DAD) in the UV range (LC/UV) were developed for the determination of low levels of the anthraquinones aloe-emodin and aloin-A (barbaloin) in aloe-based products. The methods were used to analyze several commercial products (liquids, semisolids, and solids) for the 2 anthraquinones. The wavelengths used for quantification of aloin-A, aloe-emodin, and emodin (internal standard) by DAD were 357, 257, and 289 nm, respectively. The on-column sensitivities were 0.25 and 0.05 ng by LC/UV and 0.01 and 0.025 ng by LC/MS for aloin-A and aloe-emodin, respectively. The methods are simple and sensitive and provide reproducible results; therefore, they are suitable for the determination of these anthraquinones in various aloe-based products.

  4. Rapid, sensitive liquid chromatographic method for determination of zearalenone and alpha- and beta-zearalenol in wheat.

    Science.gov (United States)

    Trenholm, H L; Warner, R M; Fitzpatrick, D W

    1984-01-01

    A rapid, sensitive liquid chromatographic (LC) method is described for quantitative determination of zearalenone and alpha- and beta-zearalenol in wheat. The procedure incorporates an internal standard, zearalenone oxime, to facilitate quantitation and automated analysis. A sample, buffered with pH 7.8 phosphate, is extracted with water-ethanol-chloroform (2 + 50 + 75) and cleaned up. The final residue is dissolved in LC mobile phase and injected onto a reverse phase RP-18 column under the following conditions: water-methanol-acetonitrile (5 + 3 + 2) mobile phase; fluorescence (excitation wavelength 236 nm, 418 nm cut-off emission filter) and UV (254 nm, range 0.0025 AU) detectors. The limit of detectability (twice background) is 0.5 ng for zearalenone and alpha-zearalenol standards on the fluorescence detector and 4 ng for beta-zearalenol on the UV detector, which is equivalent to 20 micrograms zearalenone and 20 micrograms alpha-zearalenol/kg, and 160 micrograms beta-zearalenol/kg feed. Standard curves are linear over the range 0-35 ng zearalenone and alpha-zearalenol on the fluorescence detector and 0-50 ng beta-zearalenol on the UV detector. Recoveries of all compounds are 87.5-101% in the range 0.1-3.0 mg/kg (ppm).

  5. Determination the total neutron yields of several semiconductor compounds using various alpha emitters

    Science.gov (United States)

    Abdullah, Ramadhan Hayder; Sabr, Barzan Nehmat

    2016-03-01

    In the present work, the cross-sections of (α,n) reactions available in the literature as a function of α-particle energies for light and medium elements have been rearranged for α-particle energies from near threshold up to 10 MeV in steps of (0.050MeV) using the (Excel and Matlab) computer programs. The obtained data were used to calculate the neutron yields (n/106α) using the quick basic-computer program (Simpson Rules). The stopping powers of alpha particle energies from near threshold to 10 MeV for light and medium elements such as (nat.Be,10B,11B,13C,14N,nat.O,nat.F,nat.Mg,nat.Al,29Si,30Si, nat.P and 46.48Ti) have been calculated using the Zeigler formula. The kinetic energies (Tα) and the branching ratios of each α-emitters such as (211Bi, 210Po, 211Po, 215Po, 217At, 218Rn, 219Rn, 222Rn, 224Ra, 226Ra, 215Th, 228Th, 232U, 234U, 236U, 238U, 238Pu, 239Pu, 241Am, 245Es, 252Fm, 254Fm, 256Fm, 257Fm and 257Md) are taken into consideration to calculate the mean kinetic energy . The polynomial expressions were used to fitting the calculated weighted average of neutron yields (n/106α) for natural light and medium elements such as (Be, B, C, N, O, F, Mg, Al, Si, P and Ti) to determine the adopted neutron yields from the best fitting equation with minimum (CHISQ) at mean kinetic energies of various α-emitters. The total neutron yields (n/s/gx/ppmi) of the mentioned natural light and medium elements have been calculated using the adopted neutron yields (n/106α) from the fitting equations at mean kinetic energies of various α-emitters. The total neutron yields (n/s/gα-emitters/gcompounds) of semiconductor compounds such as (AlN, AlP, BN, BP, SiC, TiO2, BeSiN2, MgCN2, MgSiN2 and MgSiP2) have been calculated by mixing (1gram) of compounds with (1gram) of pure α-emitters using the quick basic computer program. The aim of the present work is to constructed and fabricate the neutron sources theoretically

  6. Flame atomic absorption spectrometric determination of heavy metals in aqueous solution and surface water preceded by co-precipitation procedure with copper(II) 8-hydroxyquinoline

    Science.gov (United States)

    Ipeaiyeda, Ayodele Rotimi; Ayoade, Abisayo Ruth

    2017-12-01

    Co-precipitation procedure has widely been employed for preconcentration and separation of metal ions from the matrices of environmental samples. This is simply due to its simplicity, low consumption of separating solvent and short duration for analysis. Various organic ligands have been used for this purpose. However, there is dearth of information on the application of 8-hydroxyquinoline (8-HQ) as ligand and Cu(II) as carrier element. The use of Cu(II) is desirable because there is no contamination and background adsorption interference. Therefore, the objective of this study was to use 8-HQ in the presence of Cu(II) for coprecipitation of Cd(II), Co(II), Cr(III), Ni(II) and Pb(II) from standard solutions and surface water prior to their determinations by flame atomic absorption spectrometry (FAAS). The effects of pH, sample volume, amount of 8-HQ and Cu(II) and interfering ions on the recoveries of metal ions from standard solutions were monitored using FAAS. The water samples were treated with 8-HQ under the optimum experimental conditions and metal concentrations were determined by FAAS. The metal concentrations in water samples not treated with 8-HQ were also determined. The optimum recovery values for metal ions were higher than 85.0%. The concentrations (mg/L) of Co(II), Ni(II), Cr(III), and Pb(II) in water samples treated with 8-HQ were 0.014 ± 0.002, 0.03 ± 0.01, 0.04 ± 0.02 and 0.05 ± 0.02, respectively. These concentrations and those obtained without coprecipitation technique were significantly different. Coprecipitation procedure using 8-HQ as ligand and Cu(II) as carrier element enhanced the preconcentration and separation of metal ions from the matrix of water sample.

  7. Monoisotopic mass determination algorithm for selenocysteine-containing polypeptides from mass spectrometric data based on theoretical modeling of isotopic peak intensity ratios.

    Science.gov (United States)

    Kim, Jin Wook; Lee, Sunho; Park, Kunsoo; Na, Seungjin; Paek, Eunok; Park, Hyung Seo; Park, Heejin; Lee, Kong-Joo; Jeong, Jaeho; Kim, Hwa-Young

    2012-09-07

    Selenoproteins, containing selenocysteine (Sec, U) as the 21st amino acid in the genetic code, are well conserved from bacteria to human, except yeast and higher plants that miss the Sec insertion machinery. Determination of Sec association is important to find substrates and to understand redox action of selenoproteins. While mass spectrometry (MS) has become a common and powerful tool to determine an amino acid sequence of a protein, identification of a protein sequence containing Sec was not easy using MS because of the limited stability of Sec in selenoproteins. Se has six naturally occurring isotopes, ⁷⁴Se, ⁷⁶Se, ⁷⁷Se, ⁷⁸Se, ⁸⁰Se, and ⁸²Se, and ⁸⁰Se is the most abundant isotope. These characteristics provide a good indicator for selenopeptides but make it difficult to detect selenopeptides using software analysis tools developed for common peptides. Thus, previous reports verified MS scans of selenopeptides by manual inspection. None of the fully automated algorithms have taken into account the isotopes of Se, leading to the wrong interpretation for selenopeptides. In this paper, we present an algorithm to determine monoisotopic masses of selenocysteine-containing polypeptides. Our algorithm is based on a theoretical model for an isotopic distribution of a selenopeptide, which regards peak intensities in an isotopic distribution as the natural abundances of C, H, N, O, S, and Se. Our algorithm uses two kinds of isotopic peak intensity ratios: one for two adjacent peaks and another for two distant peaks. It is shown that our algorithm for selenopeptides performs accurately, which was demonstrated with two LC-MS/MS data sets. Using this algorithm, we have successfully identified the Sec-Cys and Sec-Sec cross-linking of glutaredoxin 1 (GRX1) from mass spectra obtained by UPLC-ESI-q-TOF instrument.

  8. [An ultrafast liquid chromatography-tandem mass spectrometric method for simultaneous determination of common artificial synthetic pigments in cooked meat products].

    Science.gov (United States)

    Chen, Xiaohong; Li, Xiaoping; Zhao, Yonggang; Pan, Shengdong; Jin, Micong

    2015-07-01

    A method based on ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) has been developed for the simultaneous determination of seven synthetic pigments in cooked meat product. After the cooked meat products were extracted by mixed extraction agent, purified by WAX column, the UFLC separation was performed on a Shim-pack XR-ODS II column (75 mm x 2.0 mm, 2.2 µm) with a linear gradient elution program of acetonitrile and ammonium acetate (AmAc, 5 mmol/L) as the mobile phase. Electrospray ionization was applied and operated in the negative ion mode. The limits of quantitation (LOQs) for the seven synthetic pigments were in the range of 0.7-5.0 µg/kg. The calibration curves showed good linearities for the seven analytes in their detection ranges, and the correlative coefficients (r) were more than 0.999. The recoveries were between 88.2%-106.5% with the RSDs in the range of 1.2%-5.0%. The method is sensitive, reproducible, quick and adapts to the simultaneous determination of the seven synthetic pigments in cooked meat product.

  9. Tween 80 coated alumina: An alternative support for solid phase extraction of copper, nickel, cobalt and cadmium prior to flame atomic absorption spectrometric determination

    Directory of Open Access Journals (Sweden)

    S.Z. Mohammadi

    2016-11-01

    Full Text Available The potential of coated alumina as a sorbent for the simultaneous separation and preconcentration of copper, nickel, cobalt and cadmium ions has been investigated. Copper, nickel, cobalt and cadmium were adsorbed quantitatively on coated alumina in the pH of 6. The main factors such as pH, amount sorbent, sample and eluent flow rate, type and volume of elution solution and interfering ions on the sorption of metal ions have been investigated in detail. Under the optimum experimental conditions, the detection limits (3Sb of this method for Cu(II, Ni(II, Co(II and Cd(II ions were 0.4, 1.0, 1.2 and 0.2 ng mL−1 in the original solution, respectively. Seven replicate determinations of a mixture of 5.0 μg of Cu(II, Ni(II, Co(II and 1.0 μg of Cd(II ions in the original solution gave a mean absorbance of 0.093, 0.071, 0.066 and 0.049 with relative standard deviations 1.9%, 2.3%, 2.6% and 2.1%, respectively. The method has been applied for the determination of trace amounts of Cu(II, Ni(II, Co(II and Cd(II ions in tobacco, brewed tea and water samples with satisfactory results.

  10. A liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (LC-APPI-MS/MS) method for the determination of triterpenoids in medicinal plant extracts.

    Science.gov (United States)

    Gobo, Luciana Assis; Viana, Carine; Lameira, Osmar Alves; de Carvalho, Leandro Machado

    2016-08-01

    An analytical method using liquid chromatography-atmospheric pressure photoionization tandem mass spectrometry with toluene as a dopant was developed for the determination of triterpenes in medicinal plant extracts. The 12 compounds determined have been shown to exhibit biological activity, such as gastroprotective, hepatoprotective, anti-inflammatory, antiviral and anti-tumor effects. The parameters of the atmospheric pressure photoionization interface were optimized to obtain the highest possible sensitivity for all of the compounds. The limits of detection and quantification ranged from 0.4 to 157.9 µg l -1 and 1.3 to 526.4 µg l -1 , respectively. The method was validated and applied to extracts of five medicinal plants species (Mansoa alliacea (Lam.) A.H.Gentry, Bauhinia variegata var variegata, Bauhinia variegata var alboflava, Cecropia obtuse Trécul and Cecropia palmate Willd) from the Amazonian region. The concentrations of the six triterpenes quantified in the samples ranged from 0.424 mg kg -1 for ursolic acid to 371.96 mg kg -1 for β-amyrin, which were quantified by using the standard addition method (n = 3). Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  11. Determination of calcium, magnesium, sodium, and potassium in foodstuffs by using a microsampling flame atomic absorption spectrometric method after closed-vessel microwave digestion: method validation.

    Science.gov (United States)

    Chekri, Rachida; Noël, Laurent; Vastel, Christelle; Millour, Sandrine; Kadar, Ali; Guérin, Thierry

    2010-01-01

    This paper describes a validation process in compliance with the NFIEN ISO/IEC 17025 standard for the determination of the macrominerals calcium, magnesium, sodium, and potassium in foodstuffs by microsampling with flame atomic absorption spectrometry after closed-vessel microwave digestion. The French Standards Commission (Agence Francaise de Normalisation) standards NF V03-110, NF EN V03-115, and XP T-90-210 were used to evaluate this method. The method was validated in the context of an analysis of the 1322 food samples of the second French Total Diet Study (TDS). Several performance criteria (linearity, LOQ, specificity, trueness, precision under repeatability conditions, and intermediate precision reproducibility) were evaluated. Furthermore, the method was monitored by several internal quality controls. The LOQ values obtained (25, 5, 8.3, and 8.3 mg/kg for Ca, Mg, Na, and K, respectively) were in compliance with the needs of the TDS. The method provided accurate results as demonstrated by a repeatability CV (CVr) of < 7% and a reproducibility CV (CVR) of < 12% for all the elements. Therefore, the results indicated that this method could be used in the laboratory for the routine determination of these four elements in foodstuffs with acceptable analytical performance.

  12. Multiresidue analysis of pesticides in olive oil by gel permeation chromatography followed by gas chromatography-tandem mass-spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez, Andres Garcia [Department of Physical and Analytical Chemistry, E.P.S. of Linares, University of Jaen, E-23700 Linares, Jaen (Spain); Martos, Natividad Ramos [Department of Physical and Analytical Chemistry, Faculty of Sciences, University of Jaen, E-23071 Jaen (Spain); Ballesteros, Evaristo [Department of Physical and Analytical Chemistry, E.P.S. of Linares, University of Jaen, E-23700 Linares, Jaen (Spain)]. E-mail: eballes@ujaen.es

    2006-02-03

    A method for the multiresidue analysis of olive oil samples for 26 pesticides is proposed. Residual pesticides are extracted from oil using an n-hexane/acetonitrile mixture, extracts being cleaned-up by gel permeation chromatography (GPC) for analysis by gas chromatography-tandem mass spectrometry (GC-MS/MS). Electron ionization and chemical ionization are employed in a single analysis for the determination of pesticides. Pesticide recoveries from virgin and refined olive oil spiked with 10, 100 and 250 {mu}g/kg concentrations of the pesticides ranged from 83.8 to 110.3%. The proposed method features good sensitivity: its limits of quantification are low enough to allow pesticide residues to be determined at concentrations below the maximum residue levels legally accepted. The precision, expressed as relative standard deviation, ranges from 4.93 to 8.11%. Applicability was tested on 40 olive oil samples. Several pesticides were detected in most of the virgin olive oil samples. By contrast, refined olive samples contained few pesticides, and only endosulfan sulphate was detected in all.

  13. Determination of primary bond scissions by mass spectrometric analysis of ultrasonic degradation products of poly(ethylene oxide-block-propylene oxide) copolymers.

    Science.gov (United States)

    Watanabe, Takehiro; Okabayashi, Masanori; Kurokawa, Daisuke; Nishimoto, Yukari; Ozawa, Tomoyuki; Kawasaki, Hideya; Arakawa, Ryuichi

    2010-07-01

    Ultrasonic degradation of poly(ethylene oxide-block-propylene oxide) copolymers consisting of a hydrophilic and a hydrophobic portion was studied with the aim to determine the location of bonds involved in the initial scission of the copolymers. LC-APCI-IT-MS and LC-APCI-orbitrap-MS were used for the detailed structural analysis of degradation products. The results indicated that initial bond scissions occurred principally at the boundary regions between backbones of polyethylene oxide (PEO) and polypropylene oxide (PPO) chains. Further structural analysis revealed the presence of oxygen adducts in the degradation products. Comparison with a thermal degradation carried out in helium atmosphere, one can conclude that the oxygen adducts are formed by radical reaction with water or dissolving oxygen molecules. The study demonstrated that chemical reactions as well as physical bond stress scissions are involved in the ultrasonic degradation of the copolymers. 2010 John Wiley & Sons, Ltd.

  14. Determination of evaporation coefficients of melt components of B2O3-GeO2 system by mass-spectrometric method

    International Nuclear Information System (INIS)

    Stolyarova, V.L.; Ambrok, A.G.; Nikolaev, E.N.; Semenov, G.A.

    1977-01-01

    Determined are the evaporation coefficients of the components of a glass-like system constituting boron oxide and germanium dioxide. Measurements were performed from the platinum channel and platinum effusion chamber of a low-temperature evaporator. Evaporation from the platinum channel was assumed to take place from an open surface in accord with Lengmuir, and that from the platinum chamber in accord with Knudsen. The evaporation coefficient was calculated on the basis of the Motzfeldt equation. In boron germanate glasses, the evaporation coefficient of germanium dioxide was shown to differ from the evaporation coefficient of pure germanium dioxide. Within the margin of error involved in the calculations, the evaporation coefficient of boron oxide coincides with the evaporation coefficient of pure boron oxide

  15. Novel solid phase extraction procedure for gold(III) on Dowex M 4195 prior to its flame atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    Tuzen, Mustafa; Saygi, Kadriye O.; Soylak, Mustafa

    2008-01-01

    A method for solid phase extraction (SPE) of gold(III) using Dowex M 4195 chelating resin has been developed. The optimum experimental conditions for the quantitative sorption of gold(III), pH, effect of flow rates, eluent types, sorption capacity and the effect of diverse ions on the sorption of gold(III) have been investigated. The chelating resin can be reused for more than 100 cycles of sorption-desorption without any significant change in sorption of gold(III) ions. The recovery values for gold(III) and detection limit (LOD) of gold were greater than 95% and 1.61 μg L -1 , respectively. The preconcentration factor was 31. The relative standard deviation of the method was -1 . The proposed method has been applied for the determination of gold(III) in some real samples including water, soil and sediment samples

  16. Diaion HP-2MG modified with 2-(2,6-dichlorobenzylideneamino) benzenethiol as new adsorbent for solid phase extraction and flame atomic absorption spectrometric determination of metal ions.

    Science.gov (United States)

    Ghaedi, M; Montazerozohori, M; Haghdoust, S; Zaare, F; Soylak, M

    2013-04-01

    A solid phase extraction method for enrichment-separation and the determination of cobalt (Co(2+)), copper (Cu(2+)), nickel (Ni(2+)), zinc (Zn(2+)) and lead (Pb(2+)) ions in real samples has been proposed. The influences of some analytical parameters like pH, flow rate, eluent type and interference of matrix ions on recoveries of analytes were optimized. The limits of detection were found in the range of 1.6-3.9 µg L(-1), while preconcentration factor for all understudy metal ions were found to be 166 with loading half time (t 1/2) less than 10 min. The procedure was applied for the enrichment-separation of analyte ions in environmental samples with recoveries higher than 94.8% and relative SD <4.9% (N = 5).

  17. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization. Final report

    International Nuclear Information System (INIS)

    Loge, G.

    1994-01-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U 3 O 8 . Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF 4 were found to be a kinetic bottleneck to the formation of UF 6 . This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid

  18. Hydride generation atomic fluorescence spectrometric determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter using multivariate optimization

    Energy Technology Data Exchange (ETDEWEB)

    Moscoso-Perez, Carmen [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Moreda-Pineiro, Jorge [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain)]. E-mail: jmoreda@udc.es; Lopez-Mahia, Purificacion [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Muniategui-Lorenzo, Soledad [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Fernandez-Fernandez, Esther [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Prada-Rodriguez, Dario [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain)

    2004-11-22

    A highly sensitive and simple method, based on hydride generation and atomic fluorescence detection, has been developed for the determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter samples. Atmospheric particulates matter was collected on glass fiber filters using a medium volume sampler (PM1 particulate matter). Two-level factorial designs have been used to optimise the hydride generation atomic fluorescence spectrometry (HG-AFS) procedure. The effects of several parameters affecting the hydride generation efficiency (hydrochloric acid, sodium tetrahydroborate and potassium iodide concentrations and flow rates) have been evaluated using a Plackett-Burman experimental design. In addition, parameters affecting the hydride measurement (delay, analysis and memory times) have been also investigated. The significant parameters obtained (sodium tetrahydroborate concentration, sodium tetrahydroborate flow rate and analysis time for As; hydrochloric acid concentration and sodium tetrahydroborate flow rate for Se(IV); and sodium tetrahydroborate concentration and sodium tetrahydroborate flow rate for Te(IV)) have been optimized by using 2{sup n} + star central composite design. Hydrochloric acid concentration and sodium tetrahydroborate flow rate were the significant parameters obtained for Sb and Bi determination, respectively. Using a univariate approach these parameters were optimized. The accuracy of methods have been verified by using several certified reference materials: SRM 1648 (urban particulate matter) and SRM 1649a (urban dust). Detection limits in the range of 6 x 10{sup -3} to 0.2 ng m{sup -3} have been achieved. The developed methods were applied to several atmospheric particulate matter samples corresponding to A Coruna city (NW Spain)

  19. Development of new efficient method for isolation of phenolics from sea algae prior to their rapid resolution liquid chromatographic-tandem mass spectrometric determination.

    Science.gov (United States)

    Klejdus, Bořivoj; Plaza, Merichel; Šnóblová, Marie; Lojková, Lea

    2017-02-20

    The extraction of phenolic compounds from 4 different sea algae samples, three brown algae (Cystoseira abies-marina, C. abies-marina grinded under cryogenic conditions with liquid nitrogen, Undaria pinnatifida and Sargassum muticum) and one red algae (Chondrus crispus) via solid phase extraction using micro-elution solid-phase extraction (μ-SPE) plate method was studied. Prior to μ-SPE, 50mg of algae with 80% methanol mixture was extracted in hyphenated series by various extraction techniques, such as pressurized liquid extraction and Ika Ultra-Turrax ® Tube Drive, in combination with ultrasound assisted extraction. The μ-SPE plate technique reduced the time of sample pre-treatment thanks to higher sensitivity and pre-concentration effect. Selected groups of benzoic acid derivatives (p-hydroxybenzoic, protocatechuic, gallic, vanillic, and syringic acids), hydroxybenzaldehydes (4-hydroxybenzaldehyde, and 3,4-dihydroxybenzaldehyde), and cinnamic acid derivatives (p-coumaric, caffeic, ferulic, sinapic, and chlorogenic acids) were determined using rapid resolution liquid chromatography coupled to mass spectrometry detection with negative ion electrospray ionization (RRLC-ESI-MS) using multiple reactions monitoring. LOQs of measured samples varied in the range 0.23-1.68ng/mL and LODs in the range 0.07-0.52ng/mL. The applied method allowed a simultaneous determination of phenolics (i.e. free, esters soluble in methanol, glycosides, and esters insoluble in methanol) in less than 5min (including alkaline or acidic hydrolysis of raw extracts) from sea algae extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Hydride generation atomic fluorescence spectrometric determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter using multivariate optimization

    International Nuclear Information System (INIS)

    Moscoso-Perez, Carmen; Moreda-Pineiro, Jorge; Lopez-Mahia, Purificacion; Muniategui-Lorenzo, Soledad; Fernandez-Fernandez, Esther; Prada-Rodriguez, Dario

    2004-01-01

    A highly sensitive and simple method, based on hydride generation and atomic fluorescence detection, has been developed for the determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter samples. Atmospheric particulates matter was collected on glass fiber filters using a medium volume sampler (PM1 particulate matter). Two-level factorial designs have been used to optimise the hydride generation atomic fluorescence spectrometry (HG-AFS) procedure. The effects of several parameters affecting the hydride generation efficiency (hydrochloric acid, sodium tetrahydroborate and potassium iodide concentrations and flow rates) have been evaluated using a Plackett-Burman experimental design. In addition, parameters affecting the hydride measurement (delay, analysis and memory times) have been also investigated. The significant parameters obtained (sodium tetrahydroborate concentration, sodium tetrahydroborate flow rate and analysis time for As; hydrochloric acid concentration and sodium tetrahydroborate flow rate for Se(IV); and sodium tetrahydroborate concentration and sodium tetrahydroborate flow rate for Te(IV)) have been optimized by using 2 n + star central composite design. Hydrochloric acid concentration and sodium tetrahydroborate flow rate were the significant parameters obtained for Sb and Bi determination, respectively. Using a univariate approach these parameters were optimized. The accuracy of methods have been verified by using several certified reference materials: SRM 1648 (urban particulate matter) and SRM 1649a (urban dust). Detection limits in the range of 6 x 10 -3 to 0.2 ng m -3 have been achieved. The developed methods were applied to several atmospheric particulate matter samples corresponding to A Coruna city (NW Spain)

  1. An Ultra-High Performance Liquid Chromatographic-Tandem Mass Spectrometric Method for the Determination of Sinomenine in Human Plasma after Transdermal Delivery of the Zhengqing Fengtongning Injection

    Directory of Open Access Journals (Sweden)

    Tingbo Chen

    2015-04-01

    Full Text Available A sensitive, precise and selective ultra-high performance liquid chromatography method coupled with triple-quadrupole mass spectrometry was developed and validated for the determination of trace amounts of sinomenine (ng/mL in minute volumes of human plasma. Fifty microliter plasma samples were precipitated using methanol to extract sinomenine. Separation was carried out on a C18 column with a water and acetonitrile mobile phase gradient with formic acid as an additive. The mass spectrometry data were obtained in the positive ion mode, and the transition of multiple reactions was monitored at m/z 330.2→181.0 for sinomenine quantification. The working assay range for sinomenine was linear from 0.1173 to 15.02 ng/mL with the lower limit of quantification of 0.1173 ng/mL. The precision and accuracy of the method was less than 15% in intra-day and inter-day experiments with a matrix effect of less than 6.5%. After validation, the quantitative method was applied to analyze sinomenine levels in human plasma after transdermal delivery of the Zhengqing Fengtongning Injection. The results showed that some samples contained sinomenine within the concentration range 0.4131–4.407 ng/mL.

  2. Development of on-line single-drop micro-extraction sequential injection system for electrothermal atomic absorption spectrometric determination of trace metals

    International Nuclear Information System (INIS)

    Anthemidis, Aristidis N.; Adam, Ibrahim S.I.

    2009-01-01

    A novel automatic sequential injection (SI) single-drop micro-extraction (SDME) system is proposed as versatile approach for on-line metal preconcentration and/or separation. Coupled to electrothermal atomic absorption spectrometry (ETAAS) the potentials of this SI scheme are demonstrated for trace cadmium determination in water samples. A non-charged complex of cadmium with ammonium diethyldithiophosphate (DDPA) was produced and extracted on-line into a 60 μL micro-drop of di-isobutyl ketone (DIBK). The extraction procedure was performed into a newly designed flow-through extraction cell coupled on a sequential injection manifold. As the complex Cd(II)-DDPA flowed continuously around the micro-droplet, the analyte was extracting into the solvent micro-drop. All the critical parameters were optimized and offered good performance characteristics and high preconcentration ratios. For 600 s micro-extraction time, the enhancement factor was 10 and the sampling frequency was 6 h -1 . The detection limit was 0.01 μg L -1 and the precision (RSD at 0.1 μg L -1 of cadmium) was 3.9%. The proposed method was evaluated by analyzing certified reference material

  3. Validation of a liquid chromatography-electrospray ionization tandem mass spectrometric method to determine six polyether ionophores in raw, UHT, pasteurized and powdered milk.

    Science.gov (United States)

    Pereira, Mararlene Ulberg; Spisso, Bernardete Ferraz; Jacob, Silvana do Couto; Monteiro, Mychelle Alves; Ferreira, Rosana Gomes; Carlos, Betânia de Souza; da Nóbrega, Armi Wanderley

    2016-04-01

    This study aimed to validate a method developed for the determination of six antibiotics from the polyether ionophore class (lasalocid, maduramicin, monensin, narasin, salinomycin and semduramicin) at residue levels in raw, UHT, pasteurized and powdered milk using QuEChERS extraction and high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The validation was conducted under an in-house laboratory protocol that is primarily based on 2002/657/EC Decision, but takes in account the variability of matrix sources. Overall recoveries between 93% and 113% with relative standard deviations up to 16% were obtained under intermediate precision conditions. CCα calculated values did not exceed 20% the Maximum Residue Limit for monensin and 25% the Maximum Levels for all other substances. The method showed to be simple, fast and suitable for verifying the compliance of raw and processed milk samples regarding the limits recommended by Codex Alimentarius and those adopted in European Community for polyether ionophores. Copyright © 2015 Elsevier Ltd. All rights reserved.

  4. Novel solid phase extraction procedure for gold(III) on Dowex M 4195 prior to its flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey)], E-mail: mtuzen@gop.edu.tr; Saygi, Kadriye O. [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Chemistry Department, 38039 Kayseri (Turkey)

    2008-08-15

    A method for solid phase extraction (SPE) of gold(III) using Dowex M 4195 chelating resin has been developed. The optimum experimental conditions for the quantitative sorption of gold(III), pH, effect of flow rates, eluent types, sorption capacity and the effect of diverse ions on the sorption of gold(III) have been investigated. The chelating resin can be reused for more than 100 cycles of sorption-desorption without any significant change in sorption of gold(III) ions. The recovery values for gold(III) and detection limit (LOD) of gold were greater than 95% and 1.61 {mu}g L{sup -1}, respectively. The preconcentration factor was 31. The relative standard deviation of the method was <5%. The adsorption capacity of the resin was 8.1 mg g{sup -1}. The proposed method has been applied for the determination of gold(III) in some real samples including water, soil and sediment samples.

  5. Quantitative determination of organochlorine pesticides in sewage sludges using soxtec, soxhlet and pressurized liquid extractions and ion trap mass-mass spectrometric detection.

    Science.gov (United States)

    Helaleh, M I H; Al-Omair, A; Ahmed, N; Gevao, B

    2005-06-01

    A new analytical method is described for the determination of organochlorine pesticides (OCPs) in sewage sludges using GC-ion trap-MS-MS. In this work, 16 organo-chlorine pesticides (OCPs) listed by the US Environmental Protection Agency (US EPA) as priority pollutants were separated and quantified. Sludge samples from three of Kuwait's wastewater treatment plants (WWTPs) were analyzed for organochlorine pesticides (OCPs). Spiked sludge samples were extracted with a mixture of (1:1 v/v) dichloromethane (DCM)/hexane. The extracts were cleaned on a silica/aluminum oxide column, then transferred to a gel permeation chromatography (GPC) column, before undergoing further silica/aluminum oxide clean-up; the presence of OCPs was then confirmed by GC-ion trap-MS-MS. Three extraction techniques, soxtec, soxhlet, and pressurized liquid extractions were utilized, compared and validated using the spiked sludge samples. The methods were validated in term of accuracy (recovery) and precision (RSD). The method recovery values varied from 76.1 to 92.9% for the three extraction techniques.

  6. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples

    International Nuclear Information System (INIS)

    Ghaedi, Mehrorang; Shokrollahi, Ardeshir; Niknam, Khodabakhsh; Niknam, Ebrahim; Najibi, Asma; Soylak, Mustafa

    2009-01-01

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1 mol L -1 HNO 3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL -1 for Cd 2+ , Pb 2+ , Pd 2+ and Ag + along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd 2+ , Pb 2+ , Pd 2+ and Ag + , respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.

  7. Rapid determination of acid herbicides in soil by liquid chromatography with tandem mass spectrometric detection based on dispersive solid phase extraction.

    Science.gov (United States)

    Kaczyński, Piotr; Łozowicka, Bożena; Jankowska, Magdalena; Hrynko, Izabela

    2016-05-15

    This study determined twenty six the highly sensitive phenoxy, pyridines, aliphatic and aromatic acid compounds in soil with a liquid chromatography tandem mass spectrometry. The samples were prepared by modified quick, easy, cheap, effective, rugged and safe (QuEChERS) analytical procedure in solid samples. Herbicides extraction effectiveness was evaluated at three different spiking levels (0.01, 0.1 and 1.0 mg kg(-1)). Fourteen different dispersive solid-phase extraction (d-SPE) sorbents in clean-up step were tested. The QuEChERS protocol with acidic alumina provided the highest number of pesticides with recoveries in the 70-120% range. The soil matrix effect was evaluated and for the majority of compounds were not significant, showing suppression or enhancement (±81-123%). The precision calculated as relative standard deviation (RSD) was below 22%. The linear relation was observed in the range 0.01-2.0 mg kg(-1) and the correlation coefficient R>0.999. The expanded measurement uncertainty was estimated as being on average, and was between 9% and 33%. The validated method was employed in the analysis of 309 real soil samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    Hernández, C; Sierra, I

    2016-09-01

    Two essential technical requirements of ISO 17025 guide for accreditation of testing and calibration laboratories are the validation of methods and the estimation of all sources of uncertainty that may affect the analytical result. Bioelimination Laboratory from Radiation Dosimetry Service of CIEMAT (Spain) uses alpha spectrometry to quantify alpha emitters (Pu, Am, Th, U and Cm isotopes) in urine and faecal samples from workers exposed to internal radiation. Therefore and as a step previous to achieving the ISO 17025 accreditation, the laboratory has performed retrospective studies based on the obtained results in the past few years to validate the analytical method. Uncertainty estimation was done identifying and quantifying all the contributions, and finally the overall combined standard uncertainty was calculated. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Mass spectrometric characterization of low-molecular-mass color pI markers and their use for direct determination of pI value of proteins.

    Science.gov (United States)

    Mazanec, Karel; Slais, Karel; Chmelík, Josef

    2006-12-01

    The use of low-molecular-mass color pI markers for the determination of pI values of proteins in gel isoelectric focusing (IEF) in combination with mass spectrometry is described. Different types of substituted phenols of known pI values within the mass range 250-400 were used here as pI markers. The pure, synthesized pI markers were studied by MALDI-TOF/TOF MS. Fragmentation studies of the pI markers were also performed. Only stable and well-characterized pI markers were used in this work. The selected pI markers were mixed with proteins, deposited on a gel and separated in a pH gradient. Color pI markers enable supervision of progress of the focusing process and also estimation of the position of the invisible focused bands. The separated bands of the pI markers (containing separated proteins) were excised, and the pI markers were eluted from each gel piece by water/ethanol and identified by MALDI-TOF/TOF MS. From the washed gel pieces the remaining carrier ampholytes were then washed out and proteins were in-gel digested with trypsin. The obtained peptides were measured by MALDI-TOF/TOF MS and the proteins identified via a protein database search. This procedure allows avoiding time-consuming protein staining and destaining procedures, which shortens the analysis time roughly by half. For comparison, IEF gels were stained with Coomassie Brilliant Blue R 250 and proteins in the gel bands were identified according to the standard proteomic protocol. This work has confirmed that our approach can give information about the correct pI values of particular proteins and shorten significantly the time of analysis.

  10. Chemometric analytical approach for the cloud point extraction and inductively coupled plasma mass spectrometric determination of zinc oxide nanoparticles in water samples.

    Science.gov (United States)

    Majedi, Seyed Mohammad; Lee, Hian Kee; Kelly, Barry C

    2012-08-07

    Cloud point extraction (CPE) with inductively coupled plasma mass spectrometry (ICPMS) was applied to the analysis of zinc oxide nanoparticles (ZnO NPs, mean diameter ~40 nm) in water and wastewater samples. Five CPE factors, surfactant (Triton X-114 (TX-114)) concentration, pH, ionic strength, incubation temperature, and incubation time, were investigated and optimized by orthogonal array design (OAD). A three-level OAD, OA(27) (3(13)) matrix was employed in which the effects of the factors and their contributions to the extraction efficiency were quantitatively assessed by the analysis of variance (ANOVA). Based on the analysis, the best extraction efficiency (87.3%) was obtained at 0.25% (w/v) of TX-114, pH = 10, salt content of 15 mM NaCl, incubation temperature of 45 °C, and incubation time of 30 min. The results showed that surfactant concentration, pH, incubation time, and ionic strength exert significant effects on the extraction efficiency. Preconcentration factors of 62 and 220 were obtained with 0.25 and 0.05% (w/v) TX-114, respectively. The relative recoveries of ZnO NPs from different environmental waters were in the range 64-123% at 0.5-100 μg/L spiked levels. The ZnO NPs extracted into the TX-114-rich phase were characterized by transmission electron microscopy (TEM) combined with energy-dispersive X-ray spectroscopy (EDS) and UV-visible spectrometry. Based on the results, no significant changes in size and shape of NPs were observed compared to those in the water before extraction. The extracted ZnO NPs were determined after microwave digestion by ICPMS. A detection limit of 0.05 μg/L was achieved for ZnO NPs. The optimized conditions were successfully applied to the analysis of ZnO NPs in water samples.

  11. Development and validation of a supercritical fluid chromatography method for the direct determination of enantiomeric purity of provitamin B5 in cosmetic formulations with mass spectrometric detection.

    Science.gov (United States)

    Khater, Syame; West, Caroline

    2015-01-01

    A rapid and efficient chiral supercritical fluid chromatography (SFC) method has been developed for the quantitative determination of panthenol enantiomers in cosmetic formulations (cream, lotion, wipe, and exfoliant). Indeed, the pharmacological effect only depends on the D form (Dexpanthenol) thus accurate measurement of its enantiomeric purity in formulated cosmetic products is of interest. The samples were prepared with liquid-liquid extraction followed by solid-phase extraction on Adsorbex amino cartridges. After testing several enantioselective columns in an attempt at reversing the elution order to have the minor enantiomer eluted first, the best separation of enantiomers and internal standard (N-acetyl-L-alanine) was achieved on a 3 μm-amylose-type immobilized polysaccharide chiral stationary phase (Chiralpak IA) in less than 6 min with a simple mobile phase comprising carbon dioxide and 11% methanol pumped at 2.3 mL/min, 25°C and 150 bar backpressure. Supercritical fluid chromatography coupled to both an optical diode-array detector and a user-friendly single-quadrupole mass spectrometer (Waters QDa) equipped with electrospray ionization source has been used. The on-line coupling ensures the technique to be more informative and improves detection sensitivity, as underivatized panthenol has a poor UV absorption. The limit of quantification (LOQ) achieved with single-ion recording was 0.5 μg/mL. The method was validated in terms of linearity, precision and accuracy and satisfactory results were obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Method development for the concentration determination of a protein in human plasma utilizing 96-well solid-phase extraction and liquid chromatography/tandem mass spectrometric detection.

    Science.gov (United States)

    Ji, Qin C; Gage, Eric M; Rodila, Ramona; Chang, Min S; El-Shourbagy, Tawakol A

    2003-01-01

    Although liquid chromatography/tandem mass spectrometry (LC/MS/MS) technology has been widely used for quantitative analysis of small organic molecules, it has been a challenging task to quantitatively analyze protein samples utilizing this technology in biological matrices for pre-clinical and clinical studies. Here we present our initial results in method development for the quantitative determination of rK5 protein concentrations in human plasma samples utilizing LC/MS/MS technology. A protein similar in structure to rK5, but with a slightly reduced molecular weight, was used as internal standard. A 96-well solid-phase extraction procedure was developed to effectively extract protein analytes from plasma samples. Quantitative analysis was obtained by a novel approach of protein monitoring that employed selective reaction monitoring (SRM). Even though mass spectrometry of the internal standard protein gave no fragment ions, SRM monitoring greatly reduced background interference. Using samples prepared in human plasma with sodium EDTA as anticoagulant, a correlation coefficient (r(2)) of 0.9940 was obtained by producing a single standard curve with the injection of six rows of standards with a concentration range from 100 ng/mL to 10 microg/mL. The mean analytical recovery for these standards ranged from 91.5 to 103.6%. The CVs for individual standard levels ranged from 3.7 to 20.9%. The experiment was also repeated using samples prepared in human plasma with sodium heparin as anticoagulant, which produced a correlation coefficient (r(2)) of 0.9952 obtained from a single standard curve with the injection of four rows of standards with a concentration range from 50 ng/mL to 10 microg/mL. The mean analytical recovery for the standards ranged from 96.2 to 104.6%. The CVs for individual standard levels ranged from 2.6 to 15.6%. Copyright 2003 John Wiley & Sons, Ltd.

  13. On-line sequential injection dispersive liquid-liquid microextraction system for flame atomic absorption spectrometric determination of copper and lead in water samples.

    Science.gov (United States)

    Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

    2009-06-30

    A simple, sensitive and powerful on-line sequential injection (SI) dispersive liquid-liquid microextraction (DLLME) system was developed as an alternative approach for on-line metal preconcentration and separation, using extraction solvent at microlitre volume. The potentials of this novel schema, coupled to flame atomic absorption spectrometry (FAAS), were demonstrated for trace copper and lead determination in water samples. The stream of methanol (disperser solvent) containing 2.0% (v/v) xylene (extraction solvent) and 0.3% (m/v) ammonium diethyldithiophosphate (chelating agent) was merged on-line with the stream of sample (aqueous phase), resulting a cloudy mixture, which was consisted of fine droplets of the extraction solvent dispersed entirely into the aqueous phase. By this continuous process, metal chelating complexes were formed and extracted into the fine droplets of the extraction solvent. The hydrophobic droplets of organic phase were retained into a microcolumn packed with PTFE-turnings. A portion of 300 microL isobutylmethylketone was used for quantitative elution of the analytes, which transported directly to the nebulizer of FAAS. All the critical parameters of the system such as type of extraction solvent, flow-rate of disperser and sample, extraction time as well as the chemical parameters were studied. Under the optimum conditions the enhancement factor for copper and lead was 560 and 265, respectively. For copper, the detection limit and the precision (R.S.D.) were 0.04 microg L(-1) and 2.1% at 2.0 microg L(-1) Cu(II), respectively, while for lead were 0.54 microg L(-1) and 1.9% at 30.0 microg L(-1) Pb(II), respectively. The developed method was evaluated by analyzing certified reference material and applied successfully to the analysis of environmental water samples.

  14. Quantitative determination of the enantiomers of methadone in human plasma and saliva by chiral column chromatography coupled with mass spectrometric detection.

    Science.gov (United States)

    George, Rani; Lobb, Michael; Haywood, Alison; Khan, Sohil; Hardy, Janet; Good, Phillip; Hennig, Stefanie; Norris, Ross

    2016-01-01

    Methadone is a potent lipophilic synthetic opioid that is effective in the treatment of cancer pain and perceived benefit in difficult pain control scenarios (especially in cases of neuropathic pain). The use of methadone in clinical practice is challenging however, due to the narrow therapeutic window and large inter- and intra-individual variability in therapeutic response. Quantitation of the enantiomers d- and l-methadone (d- and l-MTD) in plasma and saliva provides a basis for studying its pharmacokinetics in patients with cancer and for monitoring efficacy, toxicity and side-effects. This assay involves quantitation of the enantiomers of methadone using their respective deuterated internal standards, in plasma and saliva matrices with no impact of ion suppression in either matrix. The analytical recoveries of d- and l-MTD from the saliva collection devices (Salivette®) are optimised in this novel method with an accurate and simple extraction method employing dichloromethane. Optimal enantioselective separations were achieved using an α1-acid glycoprotein chiral stationary phase and triple quadrupole tandem mass spectrometer. Linearity was demonstrated over 0.05-1000µg/L for both enantiomers in plasma and in saliva with correlation coefficients greater than 0.998. The lower limit of quantitation (LLOQ) was determined to be 0.1µg/L in plasma and saliva for d- and l-MTD. Accuracy of the method ranges from 100% to 106% even at the LLOQ and total precision, expressed as the coefficient of variation, was between 0.2% and 4.4% for both analytes in both matrices. A simple one step extraction procedure resulted in recoveries greater than 95% for both analytes, at concentrations as low as 0.5µg/L, from the Salivette®. The validated method was applied successfully in 14 paired plasma and saliva samples obtained from adult patients with cancer pain receiving methadone. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Development of destructive methods of burn-up determination and their application on WWER type nuclear fuels

    International Nuclear Information System (INIS)

    Hermann, A.; Stephan, H.; Nebel, D.

    1984-03-01

    Results are described of a cooperation between the Central Institute of Nuclear Research Rossendorf and the Radium Institute 'V.G. Chlopin' Leningrad in the field of destructive burn-up determination. Laboratory methods of burn-up determination using the classical monitors 137 Cs, 106 Ru, 148 Nd and isotopes of heavy metals (U, Pu) as well as the usefulness of 90 Sr, stable isotopes of Ru and Mo as monitors are dealt with. The analysis of the fuel components uranium (spectrophotometry, potentiometric titration, mass-spectrometric isotope dilution) and plutonium (spectrophotometry, coulometric titration, mass- and alpha-spectrometric isotope dilution) is fully described. Possibilities of increasing the reproducibility (automatic adjusting of measurement conditions) and the sensibility (ion impuls counting) of mass-spectrometric measurements are proposed and applied to a precise determination of Am and Cm isotopic composition. The methods have been used for burn-up analysis of spent WWER (especially WWER-440) fuel. (author)

  16. The implications of particle energy and acidic media on gross alpha and gross beta determination using liquid scintillation

    Energy Technology Data Exchange (ETDEWEB)

    Zapata-Garcia, D. [Laboratori de Radiologia Ambiental (LRA), Departament de Quimica Analitica, Universitat de Barcelona, Marti i Franques, 1-11 Planta 3, E-08028 Barcelona (Spain); Llaurado, M., E-mail: montse.llaurado@ub.edu [Laboratori de Radiologia Ambiental (LRA), Departament de Quimica Analitica, Universitat de Barcelona, Marti i Franques, 1-11 Planta 3, E-08028 Barcelona (Spain); Rauret, G. [Laboratori de Radiologia Ambiental (LRA), Departament de Quimica Analitica, Universitat de Barcelona, Marti i Franques, 1-11 Planta 3, E-08028 Barcelona (Spain)

    2012-04-15

    The interaction of humans with radioactivity present in the environment from natural and artificial sources necessitates an evaluation of its risk on human health. Gross alpha and gross beta activities can provide a rapid evaluation of the radioactive content of a sample and can be simultaneously determined by using liquid scintillation counters. However, calibration of the liquid scintillation counter is required and is affected by many factors, such as particle energy and the acidity of the media. This study investigates what effect the particle energy used for calibration has on misclassification and how to account for this misclassification in routine measurements. The variability in measurement produced by the final pH, as well as any acids used in sample treatment, was also studied. These results showed that the most commonly used acid for these types of analyses, HNO{sub 3}, produced a high amount of misclassifications at very low pH. The results improved when HCl was used to adjust the sample to low pH. - Highlights: Black-Right-Pointing-Pointer We study the effect of alpha and beta energies on PSA optimisation. Black-Right-Pointing-Pointer The optimum PSA shifts to higher values as the alpha energy increases. Beta energies do not affect it. Black-Right-Pointing-Pointer We study the effect of pH on the simultaneous determination of gross alpha/beta activities. Black-Right-Pointing-Pointer HNO{sub 3} produces a high amount of misclassification at very low pH. Black-Right-Pointing-Pointer The results improve when HCl is used to adjust the sample to low pH.

  17. Spectrometric assembly for portable installations

    International Nuclear Information System (INIS)

    Kluger, A.; Popescu, C.

    1997-01-01

    The components of the portable spectrometric assembly are: - the detecting probe with Na I(Tl) crystal and air-tight case of industrial type; - a microcomputer; - a unit of analogical processing of the signal from the detecting probe; - a single-channel analyzer with adjustable threshold; - commands and display module; - a source of high voltage; - an electrical supply battery. The device uses the method of gamma photons detection in energetic windows. Through theoretical and experimental studies carried out during the prototype development phase, the superiority of this method has been proved as compared with the installations which make use of the classical principle of photon integral detection. The achieved prototype has a basic program enabling the setting of all working parameters (measuring time, discriminating thresholds, discriminators operating conditions, etc.). Through the included interface RS232 it is possible to transmit the data to a more powerful computer in order to continually process the results. The spectrometric assembly, realized on the basis of micro-computers, can be used in a wide range of applications: measurement of thickness and erosion of walls and tubes, measurement of level in closed containers, of soil density, etc. The adjustment for specific application is performed only through a program modification. (authors)

  18. Determination of the gross alpha and beta radioactivity levels in Emendere Village (Sindirgi-Balikesir) drinking water

    International Nuclear Information System (INIS)

    Dogru, M.; Canbazoglu, C.; Baykara, O.; Kuelahci, F.; Boz, A.

    2001-01-01

    Over 40 years old 600-700 years old people in good condition live in about 300 houses in Emendere village. Most of drinking and usage water, and 70% of Sindirgi's (Balikesir) drinking water are supplied by two main natural sources from Emendere. Apart of those sources, restorative water source near the village settlement place is commonly used for bathing. The gross alpha and beta radioactivity levels in Sindirgi's drinking water are firstly determined by CNAEM (Cekmece Nuclear Research and Training Centre) in 1999. Determined levels were both higher than the limits accepted by WHO (World Health Organisation) and TSE (Turkish Standards Institute) in drinking water. In this study, the gross alpha and beta radioactivity levels in usage and drinking water in the same place are determined by using more sample collected over the village and obtained results are conclude according to the standards determined by WHO and TSE. Ca and Mg concentrations, temperatures and pH are also determined and conclude. A health team from Balikesir State Hospital is also searched through the most of the village population. None of the radiation caused sickness was found during this search

  19. A new technique for thick source alpha counting determination of U and Th

    CERN Document Server

    Michael, C T

    2000-01-01

    A new technique for the calculation of U and Th concentration is presented based on the alpha particle spectrum taken from a thick sample by using a silicon detector. Four approaches to the analysis of the experimental data are presented, one being an improvement on the known pairs technique. By the proposed technique it is possible to calculate the concentrations of certain daughter nuclides in the two series, or the sum of the activity concentrations of others. This allows the detection of secular disequilibrium in our samples. This technique also has the advantage of being more accurate and provides the opportunity to cross-check the results derived from the different approaches.

  20. Determination of total alpha and beta activity in water for human consumption by LSC(Liquid Scintillation Counter)

    International Nuclear Information System (INIS)

    2013-01-01

    The Ordinance Brazilian of Ministry of Health (MS 2914/2011) establishes the standards for quality of water intended for human consumption, being limits values of 5.0 Bq/L for gross alpha, and 1.0 Bq/L for gross beta radioactivity. The liquid scintillation spectrometry (LSC) technique has been presented as an alternative to conventional procedure using gas flow proportional counter. The present work shows a review of the methods for determination of gross alpha and gross beta in water by using LSC. Between the factors that influence the accuracy and repeatability of the analytical results we can highlight: thermal preconcentration, type of the acid and calibration standard. A procedure was established and carried out to samples of the National Program of Intercomparison of Radionuclides in Environmental Samples for evaluation of its performance. The gross alpha and gross beta analysis in samples of the public water supplies in the Metropolitan Region of Goiania, state of Goias was carried out. The results are consistent with the guideline values form the Ministry of Health concerning radioactivity. (author)

  1. Determination of gross alpha and gross beta in soil around repository facility at Bukit Kledang, Perak, Malaysia

    Science.gov (United States)

    Adziz, Mohd Izwan Abdul; Siong, Khoo Kok

    2018-04-01

    Recently, the Long Term Storage Facility (LTSF) in Bukit Kledang, Perak, Malaysia, has been upgraded to repository facility upon the completion of decontamination and decommissioning (D&D) process. Thorium waste and contaminated material that may contain some minor amounts of thorium hydroxide were disposed in this facility. This study is conducted to determine the concentrations of gross alpha and gross beta radioactivities in soil samples collected around the repository facility. A total of 12 soil samples were collected consisting 10 samples from around the facility and 2 samples from selected residential area near the facility. In addition, the respective dose rates were measured 5 cm and 1 m above the ground by using survey meter with Geiger Muller (GM) detector and Sodium Iodide (NaI) detector. Soil samples were collected using hand auger and then were taken back to the laboratory for further analysis. Samples were cleaned, dried, pulverized and sieved prior to analysis. Gross alpha and gross beta activity measurements were carried out using gas flow proportional counter, Canberra Series 5 XLB - Automatic Low Background Alpha and Beta Counting System. The obtained results show that, the gross alpha and gross beta activity concentration ranged from 1.55 to 5.34 Bq/g with a mean value of 3.47 ± 0.09 Bq/g and 1.64 to 5.78 Bq/g with a mean value of 3.49 ± 0.09 Bq/g, respectively. These results can be used as an additional data to represent terrestrial radioactivity baseline data for Malaysia environment. This estimation will also serve as baseline for detection of any future related activities of contamination especially around the repository facility area.

  2. X-ray structure determination of fully hydrated L alpha phase dipalmitoylphosphatidylcholine bilayers.

    Science.gov (United States)

    Nagle, J F; Zhang, R; Tristram-Nagle, S; Sun, W; Petrache, H I; Suter, R M

    1996-03-01

    Bilayer form factors obtained from x-ray scattering data taken with high instrumental resolution are reported for multilamellar vesicles of L alpha phase lipid bilayers of dipalmitoylphosphatidylcholine at 50 degrees C under varying osmotic pressure. Artifacts in the magnitudes of the form factors due to liquid crystalline fluctuations have been eliminated by using modified Caillé theory. The Caillé fluctuation parameter eta 1 increases systematically with increasing lamellar D spacing and this explains why some higher order peaks are unobservable for the larger D spacings. The corrected form factors fall on one smooth continuous transform F(q); this shows that the bilayer does not change shape as D decreases from 67.2 A (fully hydrated) to 60.9 A. The distance between headgroup peaks is obtained from Fourier reconstruction of samples with four orders of diffraction and from electron density models that use 38 independent form factors. By combining these results with previous gel phase results, area AF per lipid molecule and other structural quantities are obtained for the fluid L alpha phase. Comparison with results that we derived from previous neutron diffraction data is excellent, and we conclude from diffraction studies that AF = 62.9 +/- 1.3 A2, which is in excellent agreement with a previous estimate from NMR data.

  3. Determination of the fine-structure constant {alpha} by measuring the quotient of the Planck constant and the neutron mass

    Energy Technology Data Exchange (ETDEWEB)

    Krueger, E.; Nistler, W.; Weirauch, W. [Physikalisch-Technische Bundesanstalt, Braunschweig (Germany)

    1997-04-01

    Using a special high-precision apparatus at ILL the quotient h/m{sub n} (h Planck constant, m{sub n} neutron mass) has been measured. The value measured for h/m{sub n} leads to {alpha}{sup -1} = 137.03601082(524) (relative uncertainty: 3.9{center_dot}10{sup -8}) It was the first time that this fundamental constant has been determined by means of neutrons. The experiment, which had been running since 1981 in a preliminary version and since 1987 in the final version, which was finished in December 1996, is described. (author).

  4. A Method Validation for Determination of Gross Alpha and Gross Beta in Water Sample Using Low Background Gross Alpha/ Beta Counting System

    International Nuclear Information System (INIS)

    Zal Uyun Wan Mahmood; Norfaizal Mohamed; Nita Salina Abu Bakar

    2016-01-01

    Method validation (MV) for the measurement of gross alpha and gross beta activity in water (drinking, mineral and environmental) samples using Low Background Gross Alpha/ Beta Counting System was performed to characterize precision, accuracy and reliable results. The main objective of this assignment is to ensure that both the instrument and method always good performed and resulting accuracy and reliable results. Generally, almost the results of estimated RSD, z-score and U score were reliable which are recorded as ≤30 %, less than 2 and less than 1.5, respectively. Minimum Detected Activity (MDA) was estimated based on the counting time of 100 minutes and present background counting value of gross alpha (0.01 - 0.35 cpm) and gross beta (0.50 - 2.18 cpm). Estimated Detection Limit (DL) was 0.1 Bq/ L for gross alpha and 0.2 Bq/ L for gross beta and expended uncertainty was relatively small of 9.77 % for gross alpha and 10.57 % for gross beta. Align with that, background counting for gross alpha and gross beta was ranged of 0.01 - 0.35 cpm and 0.50 - 2.18 cpm, respectively. While, sample volume was set at minimum of 500 mL and maximum of 2000 mL. These proven the accuracy and precision result that are generated from developed method/ technique is satisfactory and method is recommended to be used. Therefore, it can be concluded that the MV found no doubtful on the ability of the developed method. The test result showed the method is suitable for all types of water samples which are contained several radionuclides and elements as well as any impurities that interfere the measurement analysis of gross alpha and gross beta. (author)

  5. The determination of α{sub s} by the ALPHA collaboration

    Energy Technology Data Exchange (ETDEWEB)

    Bruno, Mattia [Deutsches Elektronen-Synchrotron (DESY), Zeuthen (Germany). John von Neumann-Inst. fuer Computing NIC; Brookhaven National Laboratory, Upton, NY (United States). Physics Dept.; Dalla Brida, Mattia; Schaefer, Stefan; Simma, Hubert [Deutsches Elektronen-Synchrotron (DESY), Zeuthen (Germany). John von Neumann-Inst. fuer Computing NIC; Fritzsch, Patrick [Madrid Univ. Autonoma (Spain). Inst. de Fisica Teorica; CERN, Geneva (Switzerland). Theory Division; Korzec, Tomasz [Humboldt Univ. Berlin (Germany). Inst. fuer Physik; Bergische Univ. Wuppertal (Germany). Dept. of Physics; Ramos, Alberto [CERN, Geneva (Switzerland). Theory Division; Sint, Stefan [Trinity College, Dublin (Ireland). School of Mathematics; Sommer, Rainer [Deutsches Elektronen-Synchrotron (DESY), Zeuthen (Germany). John von Neumann-Inst. fuer Computing NIC; Humboldt Univ. Berlin (Germany). Inst. fuer Physik; Collaboration: ALPHA Collaboration

    2016-11-15

    We review the ALPHA collaboration strategy for obtaining the QCD coupling at high scale. In the three-flavor effective theory it avoids the use of perturbation theory at α>or similar 0.2 and at the same time has the physical scales small compared to the cutoff 1/a in all stages of the computation. The result Λ{sup (3)}{sub MS}=332(14) MeV is translated to α{sub MS}(m{sub Z})=0.1179(10)(2) by use of (high order) perturbative relations between the effective theory couplings at the charm and beauty quark ''thresholds''. The error of this perturbative step is discussed and estimated as 0.0002.

  6. A rapid method for determination of the isotopic composition of uranium samples by alpha spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martin Sanchez, A.; Tome, F.V.; Diaz Bejarano, J.; Jurado Vargas, M. (Dept. de Fisica, Univ. Extremadura, Badajoz (Spain))

    1992-03-01

    A simple method of analyzing alpha spectra from natural and enriched or depleted uranium samples is developed. The procedure is non-iterative, and takes into consideration low-energy tail and branching-ratio corrections to accurately calculate the area corresponding to each uranium isotope ({sup 234}U, {sup 235}U, {sup 236}U, {sup 238}U) in the spectrum, and then the isotopic composition of the sample. A BASIC computer program, called ENURA, has been developed to perform all the necessary calculations to give the results together with their uncertainties. Several samples were prepared with different uranium concentrations made from standard solutions with known compositions, and the method was checked against the experimental measurements from these samples. Other series of uranium spectra were theoretically constructed using a given line shape in order to cover the required range of enriched or depleted uranium. (orig.).

  7. A rapid method for determination of the isotopic composition of uranium samples by alpha spectrometry

    Science.gov (United States)

    Sánchez, A. Martín; Tomé, F. Vera; Bejarano, J. Díaz; Vargas, M. Jurado

    1992-03-01

    A simple method of analyzing alpha spectra from natural and enriched or depleted uranium samples is developed. The procedure is non-iterative, and takes into consideration low-energy tail and branching-ratio corrections to accurately calculate the area corresponding to each uranium isotope (234U, 235U, 236U, 238U) in the spectrum, and then the isotopic composition of the sample. A BASIC computer program, called ENURA, has been developed to perform all the necessary calculations to give the results together with their uncertainties. Several samples were prepared with different uranium concentrations made from standard solutions with known compositions, and the method was checked against the experimental measurements from these samples. Other series of uranium spectra were theoretically constructed using a given line shape in order to cover the required range of enriched or depleted uranium.

  8. Design and construction of a system to determine Radon-222 through alpha spectroscopy

    International Nuclear Information System (INIS)

    Bonifacio M, J.

    1991-01-01

    The purpose of this work consists in the design a radon-222 gas measurement system utilizing a surface barrier detector with the objective to obtain a more accurate measurement for this isotope through an alpha particle spectrum and so to address as to avoid the activity influence of the descendants of short half-life, which are too beta particles emitters, already other methods it must be correction series to obtain the real value of radon activity. Here are presented the general properties properties of radon, the experimental part description indicating the design to measure the radon-222 gas and its parts, as well as too the standard separation of radium-226 starting from carnotite mineral. Finally, it is presented the results obtained with a discussion about it. (Author) results obtained with a discussion about it. (Author)

  9. Relative workload determines exercise-induced increases in PGC-1alpha mRNA

    DEFF Research Database (Denmark)

    Nordsborg, Nikolai Baastrup; Lundby, Carsten; Leick, Lotte

    2010-01-01

    INTRODUCTION:: The hypothesis that brief intermittent exercise induced increases in human skeletal muscle metabolic mRNA is dependent on relative workload was investigated. METHODS:: Trained (n=10) and untrained (n=8) subjects performed exhaustive intermittent cycling exercise (4x4 min @ 85% of VO2...... peak, interspersed by 3 min). Trained subjects also performed the intermittent exercise at the same absolute workload as untrained, corresponding to 70% of VO2 peak (n=6). RESULTS:: Exercise at 85% of VO2 peak elevated (Ptrained...... after exercise at 85% of VO2 peak. Likewise, PDK4 and HKII mRNA expression were only increased (Ptrained subjects. HIF2alpha mRNA only increased (Ptrained, with no difference between the 70% and 85% of VO2 peak...

  10. Alpha spectroscopy with ionization chamber to determine uranium and thorium in environmental samples

    International Nuclear Information System (INIS)

    Carvalho Conti, L.F. de.

    1983-01-01

    A high-resolution, parallel Frisch ionization chamber with an efficient area of 320 cm 2 was developed and applied as an alpha spectrometer. The resolution of the spectrum is approximatelly 40 KeV fwhm (full width half maximum) for 233 U point source. The spectrum is recorded by a 1024 channels pulse-height analyser. The counting gas is commercial available mixture of argon and methane. The counting efficiency for 233 U energy-window selected is in order of 42% for a calibration source placed on the cathode axis. No radial dependence of this efficiency was observed. The chamber was used for counting the activity of uranium and thorium isotopes on large area stainless steel planchets. The large area thin sources were prepared extracting the uranium and thorium isotopes from 1M HNO 3 - aqueous solution with polymeric membranes containing tri-n-octyl-phosphine oxide adhered on the surface of the 314 cm 2 planchet. The integral back-ground is typically 7 counts/min between 4 and 6 MeV. The sensitivity of the procedure used ofr 238 U is about 30 Bq/1 based on 3S of back-ground, 1 liter sample volume and 30 min counting time. (Author) [pt

  11. Reply to: ''Improved Determination of the CKM Angle alpha from B -> pipi decays''

    CERN Document Server

    Charles, J.; Lacker, H.; Le Diberder, F.; T'Jampens, S.

    2007-01-01

    In reply to hep-ph/0701204 we demonstrate why the arguments made therein do not address the criticism exposed in hep-ph/0607246 on the fundamental shortcomings of the Bayesian approach when it comes to the extraction of parameters of Nature from experimental data. As for the isospin analysis and the CKM angle alpha it is shown that the use of uniform priors for the observed quantities in the Explicit Solution parametrization is equivalent to a frequentist construction resulting from a change of variables, and thus relies neither on prior PDFs nor on Bayes' theorem. This procedure provides in this particular case results that are similar to the Confidence Level approach, but the treatment of mirror solutions remains incorrect and it is far from being general. In a second part it is shown that important differences subsist between the Bayesian and frequentist approaches, when following the proposal of hep-ph/0701204 and inserting additional information on the hadronic amplitudes beyond isospin invariance. In pa...

  12. Circulating alpha1-antitrypsin in the general population: Determinants and association with lung function

    Directory of Open Access Journals (Sweden)

    Berger Wolfgang

    2008-04-01

    Full Text Available Abstract Background Severe alpha1-antitrypsin (AAT deficiency associated with low AAT blood concentrations is an established genetic COPD risk factor. Less is known about the respiratory health impact of variation in AAT serum concentrations in the general population. We cross-sectionally investigated correlates of circulating AAT concentrations and its association with FEV1. Methods In 5187 adults (2669 females with high-sensitive c-reactive protein (CRP levels ≤ 10 mg/l from the population-based Swiss SAPALDIA cohort, blood was collected at the time of follow-up examination for measuring serum AAT and CRP. Results Female gender, hormone intake, systolic blood pressure, age in men and in postmenopausal women, as well as active and passive smoking were positively, whereas alcohol intake and BMI inversely correlated with serum AAT levels, independent of CRP adjustment. We observed an inverse association of AAT with FEV1 in the total study population (p Conclusion The results of this population-based study reflect a complex interrelationship between tobacco exposure, gender related factors, circulating AAT, systemic inflammatory status and lung function.

  13. Numerical analysis of alpha spectra using two different codes

    International Nuclear Information System (INIS)

    Hurtado, S.; Jimenez-Ramos, M.C.; Villa, M.; Vioque, I.; Manjon, G.; Garcia-Tenorio, R.

    2008-01-01

    This work presents an intercomparison between commercial software for alpha-particle spectrometry, Genie 2000, and the new free available software, Winalpha, developed by International Atomic Energy Agency (IAEA). In order to compare both codes, different environmental spectra containing plutonium, uranium, thorium and polonium have been analyzed, together with IAEA test alpha spectra. A statistical study was performed in order to evaluate the precision and accuracy in the analyses, and to enhance the confidence in using the software on alpha spectrometric studies

  14. High-precision (p,t) reaction measurement to determine Ne-18(alpha,p)Na-21 reaction rates

    NARCIS (Netherlands)

    Matic, A.; van den Berg, A. M.; Harakeh, M. N.; Wörtche, H. J.; Berg, G. P. A.; Couder, M.; Fisker, J. L.; Goerres, J.; LeBlanc, P.; O'Brien, S.; Wiescher, M.; Fujita, K.; Hatanaka, K.; Sakemi, Y.; Shimizu, Y.; Tameshige, Y.; Tamii, A.; Yosoi, M.; Adachi, T.; Fujita, Y.; Shimbara, Y.; Fujita, H.; Wakasa, T.; Hess, P. O.; Brown, B. A.; Schatz, H.

    2009-01-01

    x-ray bursts are identified as thermonuclear explosions in the outer atmosphere of accreting neutron stars. The thermonuclear runaway is fueled by the alpha p process that describes a sequence of (alpha,p) reactions triggered by the Ne-18(alpha,p)Na-21 breakout reaction from the hot CNO cycles. We

  15. 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...

  16. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal to determine compliance with specifications.

  17. Determination of alpha_s at NLO*+NNLL from a global fit of the low-z parton-to-hadron fragmentation functions in e+e- and DIS collisions

    CERN Document Server

    Pérez-Ramos, Redamy

    2015-01-01

    The QCD coupling alpha_s is determined from a combined analysis of experimental e+e- and e-p jet data confronted to theoretical predictions of the energy evolution of the parton-to-hadron fragmentation functions (FFs) moments --multiplicity, peak, width, skewness-- at low fractional hadron momentum z. The impact of approximate next-to-leading order (NLO*) corrections plus next-to-next-to-leading log (NNLL) resummations, compared to previous LO+NLL calculations, is discussed. A global fit of the full set of existing data, amounting to 360 FF moments at collision energies sqrt(s)~1--200 GeV, results in alpha_s(m_Z^2)=0.1189^{+0.0025}_{-0.0014} at the Z mass.

  18. Free energy determinants of secondary structure formation: I. alpha-Helices.

    Science.gov (United States)

    Yang, A S; Honig, B

    1995-09-22

    by the high free energy cost associated with burying unsatisfied hydrogen bonding groups. alpha-Helix formation may thus be viewed as a form of hydrophobic collapse constrained by the requirement that polar groups be either exposed to solvent or form hydrogen bonds. More generally it appears from this study that for a folding model to be a realistic, it must properly account for the chemical nature of the polypeptide chain, particularly the solvation energetics of amide groups.

  19. Distinguishing Pu Metal from Pu Oxide and Determining alpha-ratio using Fast Neutron Counting

    Energy Technology Data Exchange (ETDEWEB)

    Verbeke, J. M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Chapline, G. F. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Nakae, L. F. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Prasad, M. K. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Sheets, S. A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Snyderman, N. J. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2015-01-07

    We describe a new method for determining the ratio of the rate of (α, n) source neutrons to the rate of spontaneous fission neutrons, the so called α-ratio. This method is made possible by fast neutron counting with liquid scintillator detectors, which can determine the shape of the fast neutron spectrum. The method utilizes the spectral difference between fission spectrum neutrons from Pu metal and the spectrum of (α, n) neutrons from PuO2. Our method is a generalization of the Cifarelli-Hage method for determining keff for fissile assemblies, and also simultaneously determines keff along with the α-ratio.

  20. Determination of event shape distributions and [alpha][sub s][sup b] from Z[sup 0][yields] b anti b events at LEP

    Energy Technology Data Exchange (ETDEWEB)

    Akers, R. (Manchester Univ. (United Kingdom). Dept. of Physics); Alexander, G.; Allison, J.; Anderson, K.J.; Arcelli, S.; Asai, S.; Astbury, A.; Axen, D.; Azuelos, G.; Ball, A.H.; Barberio, E.; Barlow, R.J.; Bartoldus, R.; Batley, J.R.; Beaudoin, G.; Beck, A.; Beck, G.A.; Becker, J.; Beeston, C.; Behnke, T.; Bell, K.W.; Bella, G.; Bentkowski, P.; Bentvelsen, S.; Berlich, P.; Bethke, S.; Biebel, O.; Bloodworth, I.J.; Bock, P.; Bosch, H.M.; Boutemeur, M.; Braibant, S.; Bright-Thomas, P.; Brown, R.M.; Buijs, A.; Burckhart, H.J.; Burgard, C.; Capiluppi, P.; Carnegie, R.K.; Carter, A.A.; Carter, J.R.; Chang, C.Y.; Charlesworth, C.; Charlton, D.G.; Chu, S.L.; Clarke, P.E.L.; Clayton, J.C.; Clowes, S.G.; Cohen, I.; Conboy, J.E.; Coupland, M.; Cuffiani, M.; Dado, S.; Dallapiccola, C.; Darling, C.; Dallavalle, G.M.; Jong, S. de; Deng, H.; Dittmar, M.; Dixit, M.S.; Couto e Silva, E. do; Duchovni, E.; Duboscq, J.E.; Duckeck, G.; Duerdoth, I.P.; Dunwoody, U.C.; Elcombe, P.A.; Estabrooks, P.G.; Et; OPAL Collaboration

    1995-01-01

    In hadronic Z[sup 0] decays collected by the OPAL experiment at LEP, event shape variables such as jet rates, jet masses, thrust and the energy-energy correlation for Z[sup 0] [yields] b anti b events are compared to those for all flavours using secondary vertex information to tag the b quarks. The measured distributions are found to be well described by an O([alpha][sub s]) calculation for heavy quarks as well as by parton shower simulations. We also determine the ratio of the strong coupling constant for b quarks and all quarks, [alpha][sup b][sub s]/[alpha][sup incl][sub s], from these distributions. We find [alpha][sup b][sub s]/[alpha][sup incl][sub s] = 0.994 [+-] 0.005 [sup +0.010][sub -0.012], where the errors are the statistical and systematic errors. The result can be converted into the ratio for b quarks relative to the complementary flavours udsc [alpha][sup b][sub s]/[alpha][sup udsc][sub s] = 0.992 [+-] 0.007 [sup +0.013][sub -0.015]. (orig.)

  1. Application of TIMS in isotope correlations for determining the isotope ratios of plutonium

    International Nuclear Information System (INIS)

    Alamelu, D.; Aggarwal, S.K.

    2003-01-01

    Thermal ionisation mass spectrometry (TIMS) is a well-recognized technique for determining the isotopic composition of Pu in irradiated nuclear fuel samples. Other mass spectrometric methods such as ICPMS, SIMS can also be employed for the isotopic analysis of Pu. In the event of non-availability of a mass spectrometer, other techniques such as gamma spectrometry and alpha spectrometry can also be used. They have a limited applicability since data on all the Pu isotopes cannot be obtained

  2. Jet production in ep collisions at high Q{sup 2} and determination of {alpha}{sub s}

    Energy Technology Data Exchange (ETDEWEB)

    Aaron, F.D. [National Institute for Physics and Nuclear Engineering (NIPNE), Bucharest (Romania); Bucharest Univ. (Romania). Faculty of Physics; Alexa, C. [National Institute for Physics and Nuclear Engineering (NIPNE), Bucharest (Romania); Alimujiang, K. [DESY Hamburg (DE)] (and others)

    2009-03-15

    The production of jets is studied in deep-inelastic e{sup {+-}}p scattering at large negative four momentum transfer squared 150 < Q{sup 2} < 15000 GeV{sup 2} using HERA data taken in 1999-2007, corresponding to an integrated luminosity of 395 pb{sup -1}. Inclusive jet, 2-jet and 3-jet cross sections, normalised to the neutral current deep-inelastic scattering cross sections, are measured as functions of Q{sup 2}, jet transverse momentum and proton momentum fraction. The measurements are well described by perturbative QCD calculations at next-to-leading order corrected for hadronisation effects. The strong coupling as determined from these measurements is {alpha}{sub s}(M{sub Z}) = 0.1168 {+-} 0.0007 (exp.) {sup +0.0046}{sub -0.0030}(th.) {+-} 0.0016 (PDF). (orig.)

  3. Comparative determination of uranium in rock phosphates and columbite by ICP-OES, alpha and gamma spectrometry

    International Nuclear Information System (INIS)

    Singhal, R.K.; Sharma, P.K.; Bassan, M.K.T.; Basu, H.; Reddy, A.V.R.

    2011-01-01

    During this work selective separation of uranium from rock phosphate and columbite mineral was done before its quantitative estimation by using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). Uranium from the rock phosphate and columbite was extracted by sodium peroxide fusion followed by leaching in 2 M HNO 3 . To avoid spectral interference in the estimation of uranium by ICP-OES, the selective separation of uranium from the leachate was carried out by using two different extractants, 30% Tributyl Phosphates (TBP) in CCl 4 and a equi-volume mixture of Di(2-ethylhexyl) phosphoric acid (D2EHPA) and TBP in petrofin. Uranium was stripped from the organic phase by using 1 M ammonium carbonate solution. Determination of uranium by ICP-OES was done after dissolving the residue left after evaporation of ammonium carbonate solution in 4% HNO 3 . The concentration of the uranium observed in the rock phosphates samples was 40-200 μg g -1 whereas in columbite samples the concentration range was 100-600 μg g -1 . Uranium concentration evaluated by ICP-OES was complimented by gamma and alpha spectrometry. Concentration of uranium evaluated by gamma spectrometry in case of rock phosphate and columbite was in close agreement with the uranium content obtained by ICP-OES. Uranium determination by alpha spectrometry showed only minor deviation (1-2%) from the results obtained by ICP-OES in case of rock phosphates whereas in case of columbites results are off by 20-30%. (author)

  4. Determination of the isotopic composition of natural and slightly enriched uranium by alpha-spectrometry

    DEFF Research Database (Denmark)

    Kunzendorf, Helmar

    1968-01-01

    Determinations of the isotope contents of 238U, 235U and 234U in five uranium samples containing 0–5 at% 235U were carried out on the basis of a least-squares fit of the α-spectra from the samples, measured with a semiconductor detector, to the theoretically expected α-spectra. With a simple source...

  5. Standard test method for 238Pu isotopic abundance by alpha spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2001-01-01

    1.1 This test method covers the use of alpha spectrometry for determining the 238Pu isotopic abundance in plutonium samples. It is particularly useful for samples in which the 238Pu content is less than 1 % of the total plutonium content. For such samples, mass spectrometric results are less reliable than those from alpha spectrometry because of interference from any 238U isobar remaining after ion exchange. 1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  6. Standard test method for radiochemical determination of uranium isotopes in urine by alpha spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method is applicable to the determination of uranium in urine at levels of detection dependent on sample size, count time, detector background, and tracer yield. It is designed as a screening tool for detection of possible exposure of occupational workers. 1.2 This test method is designed for 50 mL of urine. This test method does not address the sampling protocol or sample preservation methods associated with its use. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  7. Standard test method for radiochemical determination of plutonium in Soil by alpha spectroscopy

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the determination of plutonium in soils at levels of detection dependent on count time, sample size, detector, background, and tracer yield. This test method describes one acceptable approach to the determination of plutonium in soil. 1.2 This test method is designed for 10 g of soil, previously collected and treated as described in Practices C998 and C999, but sample sizes up to 50 g may be analyzed by this test method. This test method may not be able to completely dissolve all forms of plutonium in the soil matrix. 1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 9.

  8. Maternal seric alpha-fetoprotein: determination of the medium values in Costa Rican pregnant women

    International Nuclear Information System (INIS)

    Salas Chaves, P.; Villalobos Castro, A.

    1999-01-01

    The present study focuses on the normal mean values of AFP in 124 Costa rican pregnant women. In the women 554 determinations were done between the fifteenth and twentieth week of gestation. For this purpose, and Irma test and normal values were established. The concentration values of AFP were expressed as multiples of the median, considering a value of 2.5 Mm as the normal superior limit and of 0.25 as the inferior limit. The confidence limits of the median were 24-57 Ku/I and the 2.5MM value located between 60-143 Ku/I. (author)

  9. Determination of alpha-Tocopherol (vitamin E) in irradiated garlic by high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rios, Magda Dias Goncalves; Penteado, Marilene de Vuono Camargo

    2003-01-01

    The effects of 60 Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the α-tocopherol concentration were studied. The α-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The α-tocopherol was determined through normal phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic α-tocopherol content. (author)

  10. PPARgamma-PGC-1alpha activity is determinant of alcohol related breast cancer

    DEFF Research Database (Denmark)

    Koefoed Petersen, Rasmus; Benzon Larsen, Signe; Jensen, Ditte Marie

    2012-01-01

    Alcohol is a risk factor for postmenopausal breast cancer. One of several proposed mechanisms is that alcohol-related breast cancer is caused by increased sex hormone levels. PPARγ inhibits aromatase transcription in breast adipocytes. We reproduced previously found allele-specific effects...... of the wildtype Pro-allele of PPARG Pro12Ala in alcohol related breast cancer. In transiently transfected cells, transcriptional activation by PPARγ and the PPARγ-PGC-1α complex was inhibited by ethanol. PPARγ 12Ala-mediated transcription activation was not enhanced by PGC-1α, resulting in allele......-specific transcription activation by the PPARγ 12Pro-PGC-1α complex. Our results suggest that PPARγ and PGC-1α activity is an important determinant of alcohol related breast cancer....

  11. Determination of primary yields in the alpha radiolysis of alkaline water

    International Nuclear Information System (INIS)

    Auclair, Guy

    2001-01-01

    This work presents a fundamental study of the radiolysis of water within the framework of the management of nuclear waste. During their storage, the packages of cemented radioactive waste are likely to release molecular hydrogen. Indeed, interstitial water undergoes decomposition under irradiation. This phenomenon is called radiolysis. In order to envisage the impact of H 2 de-gasification on the security of the installations, it is necessary to determine the primary radiolytic yields in the cementing medium (characterised by a pH ranging between 12 and 14), which provides a basic simulations thus allowing us to obtain both the quantities of gas and the pressure in the pore. Such data is currently not available in the literature. Studies were undertaken with a beam of accelerated helium ions in order to reproduce the conditions of irradiation on solutions at pH = 13 in order to determine a first complete series of radiolytic yields.A more complete study was undertaken on the effects of LET and pH on the yield of molecular hydrogen. The results seem to show that the yield of this primary product is little influenced by pH. Such results were in good agreement with those obtained by Monte-Carlo simulations. These studies have shown that, contrary to γ irradiations, the irradiations with α-particles do not lead to the same characteristic times. The extrapolation of this data with respect to the problem of the packaging of nuclear waste is delicate due to the limited amount of results in the literature and also the chemical and physical complexity of the concretes. (author) [fr

  12. Determination of total alpha activity index in samples of radioactive wastes; Determinacion del indice de actividad alfa total en muestras de desechos radiactivos

    Energy Technology Data Exchange (ETDEWEB)

    Galicia C, F. J.

    2015-07-01

    This study aimed to develop a methodology of preparation and quantification of samples containing radionuclides beta and/or alpha emitters, to determine the rates of alpha and beta total activity of radioactive waste samples. For this, a device of planchettes preparer was designed, to assist the planchettes preparation in a controlled environment and free of corrosive vapors. Planchettes were prepared in three means: nitrate, carbonate and sulfate, to different mass thickness, natural uranium (alpha and beta emitter) and in case of Sr-90 (beta emitter pure) only in half nitrate; and these planchettes were quantified in an alpha/beta counter, in order to construct the self-absorption curves for alpha and beta particles. These curves are necessary to determine the rate of alpha-beta activity of any sample because they provide the self-absorption correction factor to be applied in calculating the index. Samples with U were prepared with the help of the device of planchettes preparer and subsequently were analyzed in the proportional counter Mpc-100 Pic brand. Samples with Sr-90 were prepared without the device to see if there was a different behavior with respect to obtaining mass thickness. Similarly they were calcined and carried out count in the Mpc-100. To perform the count, first the parameters of counter operating were determined: operating voltages for alpha and beta particles 630 and 1500 V respectively, a count routine was generated where the time and count type were adjusted, and counting efficiencies for alpha and beta particles, with the aid of calibration sources of {sup 210}Po for alphas and {sup 90}Sr for betas. According to the results, the counts per minute will decrease as increasing the mass thickness of the sample (self-absorption curve), adjusting this behavior to an exponential function in all cases studied. The minor self-absorption of alpha and beta particles in the case of U was obtained in sulfate medium. The self-absorption curves of Sr-90

  13. A sequential method for the determination of 210Pb, 226Ra, and uranium and thorium radioisotopes by LSC and alpha-spectrometry.

    Science.gov (United States)

    Lozano, J C; Tomé, F Vera; Rodríguez, P Blanco; Prieto, C

    2010-01-01

    A procedure for the determination of (210)Pb, and alpha-emitting radioisotopes of uranium, thorium, and radium from the same aliquot of a sample has been proposed. The key step consisted in the recovery of Pb(II) and Ra by precipitation of insoluble Pb(NO(3))(2), the uranium and thorium radioisotopes remaining in solution. Afterwards, the fractions were handled by specific, well consolidated procedures. Lead-210 was determined by the LSC technique while the uranium, thorium, and radium radioisotopes were measured with silicon alpha-spectrometers. The procedure was applied to a reference sample and several environmental samples obtaining satisfactory results. Copyright 2009 Elsevier Ltd. All rights reserved.

  14. A procedure for the determination of Po-210 in water samples by alpha spectrometry

    International Nuclear Information System (INIS)

    2009-01-01

    Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is a extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004 the Environment programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. In the case of 210 Po, this started with the collection and review of about 130 papers from the scientific literature. Based on this review, two candidate methods for the chemical separation of 210 Po from water samples were selected for testing, refinement and validation in accordance with ISO guidelines. A comprehensive methodology for calculation of results including quantification of measurement uncertainty was also developed. This report presents the final procedure which was developed based on that work

  15. Engineering of factors determining alpha-amylase and cyclodextrin glycosyltransferase specificity in the cyclodextrin glycosyltransferase from Thermoanaerobacterium thermosulfurigenes EM1

    NARCIS (Netherlands)

    Wind, RD; Buitelaar, RM; Dijkhuizen, L

    1998-01-01

    The starch-degrading enzymes alpha-amylase and cyclodextrin glycosyltransferase (CGTase) are functionally and structurally closely related, with CGTases containing two additional domains (called D and E) compared to the three domains of alpha-amylases (A, B and C). Amino acid residue 196

  16. Gamma spectrometric analyses of environmental samples at PINSTECH

    International Nuclear Information System (INIS)

    Faruq, M.U.; Parveen, N.; Ahmed, B.; Aziz, A.

    1979-01-01

    Gamma spectrometric analyses of air and other environmental samples from PINSTECH were carried out. Air particulate samples were analyzed by a Ge(Li) detector on a computer-based multichannel analyzer. Other environmental samples were analyzed by a Na(T1) scintillation detector spectrometer and a multichannel analyzer with manual analysis. Concentration of radionuclides in the media was determined and the sources of their production were identified. Age of the fall out was estimated from the ratios of the fission products. (authors)

  17. Comparison of analytical methods used to determine 235U, 238U and 210Pb from sediment samples by alpha, beta and gamma spectrometry

    International Nuclear Information System (INIS)

    Vesterbacka, P.; Klemola, S.; Salahel-Din, K.

    2009-01-01

    An intercomparison of the methodology (alpha, beta and gamma spectrometry) used for 238 U, 235 U and 210 Pb determination was carried out based on 38 sediment samples. The activity range of the samples varied from 10-700 Bq/kg for 210 Pb, 1-35 Bq/kg for 235 U and 10-800 Bq/ kg for 238 U. Results obtained using the three methods were not statistically different at high activity levels, but agreement between the results decreased at lower sample activity levels. For 210 Pb, the smallest difference was found between alpha and gamma spectrometry. A good correlation between results from alpha and gamma spectrometry was observed over the whole activity range. In beta spectrometry, the results were slightly higher than those obtained by alpha or gamma spectrometry due to the impurity of 228 Ra. In 238 U analysis, good correspondence was observed between 238 U determined by gamma and alpha spectrometry, particularly at higher 238 U activity concentrations over 100 Bq/kg. In 235 U analysis, attention needs to be paid to interference from 226 Ra and its reduction. (author)

  18. Measurement of the spectral functions of axial-vector hadronic $\\tau$ decays and determination of $\\alpha_{s}(M^2_\\tau)$

    CERN Document Server

    Barate, R; Décamp, D; Ghez, P; Goy, C; Lees, J P; Lucotte, A; Merle, E; Minard, M N; Nief, J Y; Pietrzyk, B; Alemany, R; Boix, G; Casado, M P; Chmeissani, M; Crespo, J M; Delfino, M C; Fernández, E; Fernández-Bosman, M; Garrido, L; Graugès-Pous, E; Juste, A; Martínez, M; Merino, G; Miquel, R; Mir, L M; Park, I C; Pascual, A; Perlas, J A; Riu, I; Sánchez, F; Colaleo, A; Creanza, D; De Palma, M; Gelao, G; Iaselli, Giuseppe; Maggi, G; Maggi, M; Nuzzo, S; Ranieri, A; Raso, G; Ruggieri, F; Selvaggi, G; Silvestris, L; Tempesta, P; Tricomi, A; Zito, G; Huang, X; Lin, J; Ouyang, Q; Wang, T; Xie, Y; Xu, R; Xue, S; Zhang, J; Zhang, L; Zhao, W; Abbaneo, D; Becker, U; Bright-Thomas, P G; Casper, David William; Cattaneo, M; Ciulli, V; Dissertori, G; Drevermann, H; Forty, Roger W; Frank, M; Hagelberg, R; Hansen, J B; Harvey, J; Janot, P; Jost, B; Lehraus, Ivan; Mato, P; Minten, Adolf G; Moneta, L; Pacheco, A; Pusztaszeri, J F; Ranjard, F; Rolandi, Luigi; Rousseau, D; Schlatter, W D; Schmitt, M; Schneider, O; Tejessy, W; Teubert, F; Tomalin, I R; Wachsmuth, H W; Wagner, A; Ajaltouni, Ziad J; Badaud, F; Chazelle, G; Deschamps, O; Falvard, A; Ferdi, C; Gay, P; Guicheney, C; Henrard, P; Jousset, J; Michel, B; Monteil, S; Montret, J C; Pallin, D; Perret, P; Podlyski, F; Proriol, J; Rosnet, P; Hansen, J D; Hansen, J R; Hansen, P H; Nilsson, B S; Rensch, B; Wäänänen, A; Daskalakis, G; Kyriakis, A; Markou, C; Simopoulou, Errietta; Siotis, I; Vayaki, Anna; Blondel, A; Bonneaud, G R; Brient, J C; Bourdon, P; Rougé, A; Rumpf, M; Valassi, Andrea; Verderi, M; Videau, H L; Focardi, E; Parrini, G; Zachariadou, K; Corden, M; Georgiopoulos, C H; Jaffe, D E; Antonelli, A; Bencivenni, G; Bologna, G; Bossi, F; Campana, P; Capon, G; Cerutti, F; Chiarella, V; Felici, G; Laurelli, P; Mannocchi, G; Murtas, F; Murtas, G P; Passalacqua, L; Pepé-Altarelli, M; Curtis, L; Halley, A W; Lynch, J G; Negus, P; O'Shea, V; Raine, C; Scarr, J M; Smith, K; Teixeira-Dias, P; Thompson, A S; Thomson, E; Buchmüller, O L; Dhamotharan, S; Geweniger, C; Graefe, G; Hanke, P; Hansper, G; Hepp, V; Kluge, E E; Putzer, A; Sommer, J; Tittel, K; Werner, S; Wunsch, M; Beuselinck, R; Binnie, David M; Cameron, W; Dornan, Peter J; Girone, M; Goodsir, S M; Martin, E B; Marinelli, N; Moutoussi, A; Nash, J; Sedgbeer, J K; Spagnolo, P; Williams, M D; Ghete, V M; Girtler, P; Kneringer, E; Kuhn, D; Rudolph, G; Betteridge, A P; Bowdery, C K; Buck, P G; Colrain, P; Crawford, G; Finch, A J; Foster, F; Hughes, G; Jones, R W L; Williams, M I; Giehl, I; Greene, A M; Hoffmann, C; Jakobs, K; Kleinknecht, K; Quast, G; Renk, B; Rohne, E; Sander, H G; Van Gemmeren, P; Zeitnitz, C; Aubert, Jean-Jacques; Benchouk, C; Bonissent, A; Bujosa, G; Carr, J; Coyle, P; Etienne, F; Leroy, O; Motsch, F; Payre, P; Talby, M; Sadouki, A; Thulasidas, M; Trabelsi, K; Aleppo, M; Antonelli, M; Ragusa, F; Berlich, R; Blum, Walter; Büscher, V; Dietl, H; Ganis, G; Kroha, H; Lütjens, G; Mannert, C; Männer, W; Moser, H G; Schael, S; Settles, Ronald; Seywerd, H C J; Stenzel, H; Wiedenmann, W; Wolf, G; Boucrot, J; Callot, O; Chen, S; Cordier, A; Davier, M; Duflot, L; Grivaz, J F; Heusse, P; Höcker, A; Jacholkowska, A; Kim, D W; Le Diberder, F R; Lefrançois, J; Lutz, A M; Schune, M H; Tournefier, E; Veillet, J J; Videau, I; Zerwas, D; Azzurri, P; Bagliesi, G; Batignani, G; Bettarini, S; Boccali, T; Bozzi, C; Calderini, G; Carpinelli, M; Ciocci, M A; Dell'Orso, R; Fantechi, R; Ferrante, I; Foà, L; Forti, F; Giassi, A; Giorgi, M A; Gregorio, A; Ligabue, F; Lusiani, A; Marrocchesi, P S; Messineo, A; Palla, Fabrizio; Rizzo, G; Sanguinetti, G; Sciabà, A; Tenchini, Roberto; Tonelli, G; Vannini, C; Venturi, A; Verdini, P G; Blair, G A; Bryant, L M; Chambers, J T; Green, M G; Medcalf, T; Perrodo, P; Strong, J A; Von Wimmersperg-Töller, J H; Botterill, David R; Clifft, R W; Edgecock, T R; Haywood, S; Norton, P R; Thompson, J C; Wright, A E; Bloch-Devaux, B; Colas, P; Emery, S; Kozanecki, Witold; Lançon, E; Lemaire, M C; Locci, E; Pérez, P; Rander, J; Renardy, J F; Roussarie, A; Schuller, J P; Schwindling, J; Trabelsi, A; Vallage, B; Black, S N; Dann, J H; Johnson, R P; Kim, H Y; Konstantinidis, N P; Litke, A M; McNeil, M A; Taylor, G; Booth, C N; Brew, C A J; Cartwright, S L; Combley, F; Kelly, M S; Lehto, M H; Reeve, J; Thompson, L F; Affholderbach, K; Böhrer, A; Brandt, S; Cowan, G D; Grupen, Claus; Saraiva, P; Smolik, L; Stephan, F; Apollonio, M; Bosisio, L; Della Marina, R; Giannini, G; Gobbo, B; Musolino, G; Rothberg, J E; Wasserbaech, S R; Armstrong, S R; Charles, E; Elmer, P; Ferguson, D P S; Gao, Y; González, S; Greening, T C; Hayes, O J; Hu, H; Jin, S; McNamara, P A; Nachtman, J M; Nielsen, J; Orejudos, W; Pan, Y B; Saadi, Y; Scott, I J; Walsh, J; Wu Sau Lan; Wu, X; Zobernig, G

    1998-01-01

    An analysis based on 124000 selected tau pairs recorded by the ALEPH detector at LEP provides the vector (V) and axial-vector (A) spectral functions of hadronic tau decays together with their total widths. This allows the evaluation of finite energy chiral sum rules that are weighted integrals over the (V-A) spectral functions. In addition, a precise measurement of alpha_s along with a determination of nonperturbative contributions at the tau mass scale is performed. The experimentally and theoretically most robust determination of alpha_s(M_tau^2) is obtained from the (V+A) fit that yields alpha_s(M_tau^2) = 0.334 +/- 0.022 giving alpha_s(M_Z^2) = 0.1202 +/- 0.0027 after the extrapolation to the mass of the Z boson. The approach of the Operator Product Expansion (OPE) is tested experimentally studying the evolution of the tau hadronic widths to masses smaller than the tau mass.

  19. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    Administrator

    Dedicated to the memory of the late Professor S K Rangarajan. Spectrometric mixture analysis: An unexpected wrinkle. †. ROBERT DE LEVIE. Chemistry Department ..... For a quick visual check of the mixture spectra, we plotted the absorbances of those solutions that have a constant value of c + t, such as (0, 180), (90,.

  20. Molecular determinants of desensitization and assembly of the chimeric GABA(A) receptor subunits (alpha1/gamma2) and (gamma2/alpha1) in combinations with beta2 and gamma2

    DEFF Research Database (Denmark)

    Elster, L; Kristiansen, U; Pickering, D S

    2001-01-01

    , as opposed to the staining of the (gamma2/alpha1)-containing receptors, which was only slightly higher than background. To explain this, the (alpha1/gamma2) and (gamma2/alpha1) chimeras may act like alpha1 and gamma2 subunits, respectively, indicating that the extracellular N-terminal segment is important...... in combination with beta2 or beta2gamma2. Surprisingly, the (alpha1/gamma2)(gamma2/alpha1)beta2 subunit combination did desensitize, indicating that the C-terminal segment of the alpha1 subunit may be important for desensitization. Moreover, desensitization was observed for the (alpha1/gamma2)beta2gamma2...

  1. Determination of the Crystal Structure of Human Zn-Alpha 2-Gylcoprotein, A Protein Implicated in Breast Cancer

    National Research Council Canada - National Science Library

    Bjorkman, Pamela

    2000-01-01

    Zn-alpha 2-glycoprotein (ZAG) is a 41 kDa soluble protein whose sequence and domain organization are surprisingly similar to those of the membrane glycoproteins of the major histocompatibility complex (MHC...

  2. Effect of polarized radiative transfer on the Hanle magnetic field determination in prominences: Analysis of hydrogen H alpha line observations at Pic-du-Midi

    Science.gov (United States)

    Bommier, V.; Deglinnocenti, E. L.; Leroy, J. L.; Sahal-Brechot, S.

    1985-01-01

    The linear polarization of the Hydrogen H alpha line of prominences has been computed, taking into account the effect of a magnetic field (Hanle effect), of the radiative transfer in the prominence, and of the depolarization due to collisions with the surrounding electrons and protons. The corresponding formalisms are developed in a forthcoming series of papers. In this paper, the main features of the computation method are summarized. The results of computation have been used for interpretation in terms of magnetic field vector measurements from H alpha polarimetric observations in prominences performed at Pic-du-Midi coronagraph-polarimeter. Simultaneous observations in one optically thin line (He I D(3)) and one optically thick line (H alpha) give an opportunity for solving the ambiguity on the field vector determination.

  3. Determination of Non-Transferrin Bound Iron, Transferrin Bound Iron, Drug Bound Iron and Total Iron in Serum in a Rats after IV Administration of Sodium Ferric Gluconate Complex by Simple Ultrafiltration Inductively Coupled Plasma Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Murali K. Matta

    2018-02-01

    Full Text Available A rapid, sensitive and specific ultrafiltration inductively-coupled plasma mass spectrometry method was developed and validated for the quantification of non-transferrin bound iron (NTBI, transferrin bound iron (TBI, drug bound iron (DI and total iron (TI in the same rat serum sample after intravenous (IV administration of iron gluconate nanoparticles in sucrose solution (Ferrlecit®. Ultrafiltration with a 30 kDa molecular cut-off filter was used for sample cleanup. Different elution solvents were used to separate each form of iron from sample serum. Isolated fractions were subjected to inductively-coupled mass spectrometric analysis after microwave digestion in 4% nitric acid. The reproducibility of the method was evaluated by precision and accuracy. The calibration curve demonstrated linearity from 5–500 ng/mL with a regression (r2 of more than 0.998. This method was effectively implemented to quantify rat pharmacokinetic study samples after intravenous administration of Ferrlecit®. The method was successfully applied to a pharmacokinetic (PK study of Ferrlecit in rats. The colloidal iron followed first order kinetics with half-life of 2.2 h and reached background or pre-dose levels after 12 h post-dosing. The drug shown a clearance of 0.31 mL/min/kg and volume of distribution of 0.05 L/kg. 19.4 ± 2.4 mL/h/kg.

  4. Quantitative MALDI tandem mass spectrometric imaging of cocaine from brain tissue with a deuterated internal standard.

    NARCIS (Netherlands)

    Pirman, D.A.; Reich, R.F.; Kiss, A.; Heeren, R.M.A.; Yost, R.A.

    2013-01-01

    Mass spectrometric imaging (MSI) is an analytical technique used to determine the distribution of individual analytes within a given sample. A wide array of analytes and samples can be investigated by MSI, including drug distribution in rats, lipid analysis from brain tissue, protein differentiation

  5. Studies of the acidic components of the Colorado Green River formation oil shale-Mass spectrometric identification of the methyl esters of extractable acids.

    Science.gov (United States)

    Haug, P.; Schnoes, H. K.; Burlingame, A. L.

    1971-01-01

    Study of solvent extractable acidic constituents of oil shale from the Colorado Green River Formation. Identification of individual components is based on gas chromatographic and mass spectrometric data obtained for their respective methyl esters. Normal acids, isoprenoidal acids, alpha, omega-dicarboxylic acids, mono-alpha-methyl dicarboxylic acids and methyl ketoacids were identified. In addition, the presence of monocyclic, benzoic, phenylalkanoic and naphthyl-carboxylic acids, as well as cycloaromatic acids, is demonstrated by partial identification.

  6. Trace uranium analysis in geological sample by isotope dilution-alpha spectrometry and comparison with other techniques

    International Nuclear Information System (INIS)

    Shihomatsu, H.M.; Iyer, S.S.

    1988-12-01

    Establishment of uranium determination in geological samples by alpha spectrometric isotope dilution technique using 233 U tracer is described in the present work. The various steps involved in the method namely, preparation of the sample, electrodeposition, alpha spectrometry, isotope dilution, calculation of the concentration and error statistics are discussed in detail. The experimental parameters for the electrodeposition of uranium, like current density, pH concentration of the electrolyte solution, deposition time, electrode distance were all optimised based on the efficiency of the deposition. The total accuracy and precision of the IDAS using 233 U tracer in the determination of uranium in mineral and granite samples were of the order of 1 to 2% for the concentration range of 50-1500 ppm of U. Our results are compared with those obtained by others workers using similar and different techniques. (author) [pt

  7. Determination of Neptunium, Americium and Curium in Spent Nuclear Fuel Samples by Alpha Spectrometry Using 239Np and 243Am as a Spike and a Tracer

    International Nuclear Information System (INIS)

    Jeo, Kih-Soo; Song, Byung-Chul; Kim, Young-Bok; Han, Sun-Ho; Jeon, Young-Shin; Jung, Euo-Chang; Jee, Kwang-Yong

    2007-01-01

    Determination of actinide elements and fission products in spent nuclear fuels is of importance for a burnup determination and source term evaluation. Especially, the amounts of uranium and plutonium isotopes are used for the evaluation of a burnup credit in spent nuclear fuels. Additionally, other actinides such as Np, Am and Cm in spent nuclear fuel samples is also required for the purposes mentioned above. In this study, 237 Np, 241 Am and 244 Cm were determined by an alpha spectrometry for the source term data for high burnup spent nuclear fuels ranging from 37 to 62.9 GWD/MtU as a burnup. Generally, mass spectrometry has been known as the most powerful method for isotope determinations such as high concentrations of uranium and plutonium. However, in the case of minor actinides such as Np, Am and Cm, alpha spectrometry would be recommended instead. Determination of the transuranic elements in spent nuclear fuel samples is different from that for environmental samples because the amount of each nuclide in the spent fuel samples is higher and the relative ratios between each nuclide are also different from those for environmental samples. So, it is important to select an appropriate tracer and an optimum sample size depending on the nuclides and analytical method. In this study 237 Np was determined by an isotope dilution alpha(gamma) spectrometry using 239 Np as a spike, and 241 Am and curium isotopes were determined by alpha spectrometry using 243 Am as a tracer. The content of each nuclide was compared with that by the Origen-2 code

  8. Novel atomic absorption spectrometric and rapid spectrophotometric methods for the quantitation of paracetamol in saliva: application to pharmacokinetic studies.

    Science.gov (United States)

    Issa, M M; Nejem, R M; El-Abadla, N S; Al-Kholy, M; Saleh, Akila A

    2008-01-01

    A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III) (method I); oxidation of p-aminophenol after the hydrolysis of paracetamol (method II). Iron (II) then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III) in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II) at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 mug/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 mug/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 mug/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%.

  9. Structure elucidation of metabolite x17299 by interpretation of mass spectrometric data.

    Science.gov (United States)

    Zhang, Qibo; Ford, Lisa A; Evans, Anne M; Toal, Douglas R

    2017-01-01

    A major bottleneck in metabolomic studies is metabolite identification from accurate mass spectrometric data. Metabolite x17299 was identified in plasma as an unknown in a metabolomic study using a compound-centric approach where the associated ion features of the compound were used to determine the true molecular mass. The aim of this work is to elucidate the chemical structure of x17299, a new compound by de novo interpretation of mass spectrometric data. An Orbitrap Elite mass spectrometer was used for acquisition of mass spectra up to MS 4 at high resolution. Synthetic standards of N,N,N -trimethyl-l-alanyl-l-proline betaine (l,l-TMAP), a diastereomer, and an enantiomer were chemically prepared. The planar structure of x17299 was successfully proposed by de novo mechanistic interpretation of mass spectrometric data without any laborious purification and nuclear magnetic resonance spectroscopic analysis. The proposed structure was verified by deuterium exchanged mass spectrometric analysis and confirmed by comparison to a synthetic standard. Relative configuration of x17299 was determined by direct chromatographic comparison to a pair of synthetic diastereomers. Absolute configuration was assigned after derivatization of x17299 with a chiral auxiliary group followed by its chromatographic comparison to a pair of synthetic standards. The chemical structure of metabolite x17299 was determined to be l,l-TMAP.

  10. Processing of gamma-ray spectrometric logs

    International Nuclear Information System (INIS)

    Umiastowski, K.; Dumesnil, P.

    1984-10-01

    CEA (Commissariat a l'Energie Atomique) has developped a gamma-ray spectrometric tool, containing an analog-to-digital converter. This new tool permits to perform very precise uranium logs (natural gamma-ray spectrometry), neutron activation logs and litho-density logs (gamma-gamma spectrometric logs). Specific processing methods were developped to treate the particular problems of down-hole gamma-ray spectrometry. Extraction of the characteristic gamma-ray peak, even if they are superposed on the background radiation of very high intensity, is possible. This processing methode enables also to obtain geological informations contained in the continuous background of the spectrum. Computer programs are written in high level language for SIRIUS (VICTOR) and APOLLO computers. Exemples of uranium and neutron activation logs treatment are presented [fr

  11. Integration of metal-resistant determinants from the plasmid of an Acidocella strain into the chromosome of Escherichia coli DH5alpha.

    Science.gov (United States)

    Ghosh, Sajalendu; Mahapatra, Nitish R; Nandi, Suvobroto; Banerjee, Pataki C

    2005-01-01

    Acidophilic bacteria of mine origin are ideal systems for studying microbial metal resistance because of their ability to grow in the presence of high concentrations of metal salts. We have previously shown that the metal-resistant transformants obtained after transformation of Escherichia coli DH5alpha with plasmid DNA preparation from Acidocella sp. strain GS19h did not contain any plasmid suggesting chromosomal integration of the plasmid(s) (Appl Environ Microbiol 1997; 63: 4523-4527). The present study provides evidence in support of this suggestion. The pulsed field gel electrophoresis (PFGE) pattern of genomic DNA of the plasmidless metal-resistant transformants differed markedly from that of the untransformed DH5alpha strain. Moreover, when the recombinant plasmids constructed by cloning plasmid DNA fragments of the Acidocella strain GS19h in the vector pBluescript II KS+ were used to transform E. coli DH5alpha strain, no plasmid DNA was detected in some of the zinc- and ampicillin-resistant (ZnrAmpr) clones. The PFGE pattern of genomic DNA of such a transformed clone also differed markedly from that of the parent strain, suggesting chromosomal integration of the recombinant plasmid(s) containing both ampicillin- and zinc-resistance determinants. This observation was further supported by hybridization of chromosomal DNA of the plasmidless ZnrAmpr E. coli DH5alpha clone with the probes made from the plasmid DNA of strain GS19h and the vector DNA. Thus, this study corroborates our previous finding and documents the phenomenon of integration of metal-resistant determinants from the Acidocella GS19h plasmid(s) into the chromosome of E. coli DH5alpha.

  12. DETERMINATION OF MUSHROOM TOXIN ALPHA-AMANITIN IN SERUM BY LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY AFTER SOLID-PHASE EXTRACTION

    Directory of Open Access Journals (Sweden)

    Maja Vujović

    2015-03-01

    Full Text Available Alpha-amanitin is a cyclic peptide which belongs to a large group of mushroom toxins known as amatoxins. Being responsible for the majority of fatal mushroom poisonings, they require rapid detection and excretion from the body fluids. In accordance with these requirements, a simple and an accurate method was developed for successful identification and quantification of alpha-amanitin in serum with electrospray liquid chromatography–mass spectrometry (LC-ESI-MS after collision-induced dissociation. The method conforms to the established International Conference on Harmonization Q2A/Q2B 1996 guidelines on the validation of analytical methods. Linearity, precision, extraction recovery and stability test on blank serum spiked with alpha-amanitin and stored in different conditions met the acceptance criteria. The obtained calibration curve was linear over the concentration range 5-100 ng/mL with a lower limit of quantification (LOQ of 5 ng/mL and limit of detection (LOD of 2.5 ng/mL. The mean intra- and inter-day precision and accuracy were 6.05% and less than ±15% of nominal values, respectively. The neutral solid phase extraction with copolymer hydrophilic–lipophilic balance cartridges was found optimal for sample preparation with the mean recovery of 91.94%. The proposed method demonstrated high sensitivity and selectivity which can be useful both for clinical and forensic toxicology analysis of alpha-amanitin at low concentrations.

  13. Quark mass corrections to the perturbative thrust and its effect on the determination of alpha sub s

    CERN Document Server

    Banerjee, S

    2002-01-01

    We consider the effects of quark masses to the perturbative thrust in e sup + e sup - annihilation. In particular we show that perturbative power corrections resulting from non-zero quark masses considerably alters the size of the non-perturbative power corrections and consequently, significantly changes the fitted value of alpha sub s. (author)

  14. Overexpression and purification of the primase domain of bacteriophage P4 gp alpha for structure determination by NMR

    NARCIS (Netherlands)

    de Planque, M.R.R.; Ziegelin, G.; Lanka, E.; Boelens, R.

    2003-01-01

    Bacteriophage P4 is a temperate phage of E. coli and other Gram-negative prokaryotes. Its alpha gene encodes a 777-residue multifunctional protein, gpa, that is essential and sufficient for the initiation of P4 DNA replication. The gpa protein attaches to the P4 origin of replication, unwinds the

  15. Substrate Preferences and Catalytic Parameters Determined by Structural Characteristics of Sterol 14[alpha]-Demethylase (CYP51) from Leishmania infantum

    Energy Technology Data Exchange (ETDEWEB)

    Hargrove, Tatiana Y.; Wawrzak, Zdzislaw; Liu, Jialin; Nes, W. David; Waterman, Michael R.; Lepesheva, Galina I. (Vanderbilt); (TTU); (NWU)

    2012-05-14

    Leishmaniasis is a major health problem that affects populations of {approx}90 countries worldwide, with no vaccine and only a few moderately effective drugs. Here we report the structure/function characterization of sterol 14{alpha}-demethylase (CYP51) from Leishmania infantum. The enzyme catalyzes removal of the 14{alpha}-methyl group from sterol precursors. The reaction is essential for membrane biogenesis and therefore has great potential to become a target for antileishmanial chemotherapy. Although L. infantum CYP51 prefers C4-monomethylated sterol substrates such as C4-norlanosterol and obtusifoliol (V{sub max} of {approx}10 and 8 min{sup -1}, respectively), it is also found to 14{alpha}-demethylate C4-dimethylated lanosterol (V{sub max} = 0.9 min{sup -1}) and C4-desmethylated 14{alpha}-methylzymosterol (V{sub max} = 1.9 min{sup -1}). Binding parameters with six sterols were tested, with K{sub d} values ranging from 0.25 to 1.4 {mu}m. Thus, L. infantum CYP51 is the first example of a plant-like sterol 14{alpha}-demethylase, where requirements toward the composition of the C4 atom substituents are not strict, indicative of possible branching in the postsqualene portion of sterol biosynthesis in the parasite. Comparative analysis of three CYP51 substrate binding cavities (Trypanosoma brucei, Trypanosoma cruzi, and L. infantum) suggests that substrate preferences of plant- and fungal-like protozoan CYP51s largely depend on the differences in the enzyme active site topology. These minor structural differences are also likely to underlie CYP51 catalytic rates and drug susceptibility and can be used to design potent and specific inhibitors.

  16. High-performance liquid chromatographic separation of carminic acid, alpha- and beta-bixin, and alpha- and beta-norbixin, and the determination of carminic acid in foods.

    Science.gov (United States)

    Lancaster, F E; Lawrence, J F

    1996-05-03

    During a study of natural food colours, a simple and reliable high-performance liquid chromatography system was developed for use with cochineal and annato. An isocratic mobile phase, consisting of methanol and 6% aqueous acetic acid, resolved bixin and norbixin, while a gradient system was used to separate carminic acid and the annato compounds. The carminic acid contents of cochineal extract, carmine and carmine hydrosoluble were determined using an isocratic mobile phase (40:60, v/v). The detection limit for carminic acid in the various products was approximately 100 ng/g. Carminic acid was determined quantitatively in fruit beverages, yogurt and candies. It was demonstrated that, because of decomposition, carminic acid was not suitable for use in candies when manufacturing temperatures above 100 degrees C were required. Most membrane filters are not suitable for use with cochineal solutions, but a cellulose membrane filter did not adsorb carminic acid and was used successfully to remove impurities from water-based cochineal products and food extracts containing carminic acid.

  17. Study of natural diamond detector spectrometric properties under neutron irradiation

    CERN Document Server

    Alekseyev, A B; Kaschuck, Y; Krasilnikov, A; Portnov, D; Tugarinov, S

    2002-01-01

    Natural diamond detector (NDD) performance was studied up to a neutron fluence of 10 sup 1 sup 5 neutron/cm sup 2. The variations of the NDD spectrometric response to incident alpha-particles from sup 2 sup 4 sup 1 Am source after exposure to fast neutron fluences up to 3x10 sup 1 sup 6 n/cm sup 2 were examined. No significant variations up to the level of 10 sup 1 sup 4 n/cm sup 2 were observed. Degradation of charge collection efficiency at higher fluences is reported. No remarkable increase of the NDD leakage current and count rate change had been observed up to a neutron fluence of 3x10 sup 1 sup 6 n/cm sup 2. The charge collection efficiency variations of neutron irradiated diamond spectrometer were studied ex situ under gamma-rays, beta-radiation and visible light excitation. Charge collection efficiency restoration up to 75% level and the NDD performance stabilization by extrinsic low-intensity visible light (550 nm

  18. Direct determination of the estrogenic compounds 8-prenylnaringenin, zearalenone, alpha- and beta-zearalenol in beer by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Maragou, Niki C; Rosenberg, Erwin; Thomaidis, Nikolaos S; Koupparis, Michael A

    2008-08-15

    A novel LC-ESI-MS method for the simultaneous determination of four of the most significant estrogenic compounds naturally occurring in beer, 8-prenylnaringenin (8-PN), zearalenone (ZON), alpha-zearalenol (alpha-ZOL) and beta-zearalenol (beta-ZOL) which requires minimal sample preparation was developed using a chemometric approach. Experimental design was applied to assess the effects of the LC-ESI-MS parameters (mobile phase flow rate, drying gas flow, nebuliser pressure and capillary potential) on the obtained signal and to optimize the values in order to provide maximum sensitivity and detectability. The proposed method is simple, consisting only of degassing the beer and diluting with water (1:1, v/v) before injection. Comparison between the two internal standards used, zearalanone (ZAN) and 4,2'-dihydroxychalcone (4,2'-DHC), showed that ZAN performs better as internal standard not only for the mycotoxins but for 8-PN as well, giving lower % RSDs. Under inter-day conditions mean recoveries were 107% for ZON, 87.8% for alpha-ZOL, 72.8% for beta-ZOL, and 77.5% for 8-PN. The corresponding % RSDs ranged between 5.0 and 8.0. The method limits of detection were 1.3, 1.4, 1.0 and 0.8 ng mL(-1) for ZON, alpha-ZOL, beta-ZOL and 8-PN, respectively. The method was applied to 15 beer samples obtained from local supermarkets and the concentration of the phytoestrogen 8-PN in beer ranged between <0.8 and 38.6 ng mL(-1), while neither ZON nor its metabolites, alpha-ZOL and beta-ZOL, were detected.

  19. Determination of $\\alpha_S$ using OPAL hadronic event shapes at $\\sqrt{s}$ = 91 − 209 GeV and resummed NNLO calculations

    CERN Document Server

    Abbiendi, G; Akesson, P F; Alexander, G; Anagnostou, G; Anderson, K J; Asai, S; Axen, D; Bailey, I; Barberio, E; Barillari, T; Barlow, R J; Batley, R J; Bechtle, P; Behnke, T; Bell, K W; Bell, P J; Bella, G; Bellerive, A; Benelli, G; Bethke, S; Biebel, O; Boeriu, O; Bock, P; Boutemeur, M; Braibant, S; Brown, R M; Burckhart, H J; Campana, S; Capiluppi, P; Carnegie, R K; Carter, A A; Carter, J R; Chang, C Y; Charlton, D G; Ciocca, C; Csilling, A; Cuffiani, M; Dado, S; Dallavalle, M; De Roeck, A; De Wolf, E A; Desch, K; Dienes, B; Dubbert, J; Duchovni, E; Duckeck, G; Duerdoth, I P; Etzion, E; Fabbri, F; Ferrari, P; Fiedler, F; Fleck, I; Ford, M; Frey, A; Gagnon, P; Gary, J W; Geich-Gimbel, C; Giacomelli, G; Giacomelli, P; Giunta, M; Goldberg, J; Gross, E; Grunhaus, J; Gruwe, M; Gupta, A; Hajdu, C; Hamann, M; Hanson, G G; Harel, A; Hauschild, M; Hawkes, C M; Hawkings, R; Herten, G; Heuer, R D; Hill, J C; Horvath, D; Igo-Kemenes, P; Ishii, K; Jeremie, H; Jovanovic, P; Junk, T R; Kanzaki, J; Karlen, D; Kawagoe, K; Kawamoto, T; Keeler, R K; Kellogg, R G; Kennedy, B W; Kluth, S; Kobayashi, T; Kobel, M; Komamiya, S; Kramer, T; Krasznahorkay, Jr A; Krieger, P; von Krogh, J; Kuhl, T; Kupper, M; Lafferty, G D; Landsman, H; Lanske, D; Lellouch, D; Letts, J; Levinson, L; Lillich, J; Lloyd, S L; Loebinger, F K; Lu, J; Ludwig, A; Ludwig, J; Mader, W; Marcellini, S; Martin, A J; Mashimo, T; Mattig, P; McKenna, J; McPherson, R A; Meijers, F; Menges, W; Merritt, F S; Mes, H; Meyer, N; Michelini, A; Mihara, S; Mikenberg, G; Miller, D J; Mohr, W; Mori, T; Mutter, A; Nagai, K; Nakamura, I; Nanjo, H; Neal, H A; O’Neale, S W; Oh, A; Oreglia, M J; Orito, S; Pahl, C; Pasztor, G; Pater, J R; Pilcher, J E; Pinfold, J; Plane, D E; Pooth, O; Przybycien, M; Quadt, A; Rabbertz, K; Rembser, C; Renkel, P; Roney, J M; Rossi, A M; Rozen, Y; Runge, K; Sachs, K; Saeki, T; Sarkisyan, E K G; Schaile, A D; Schaile, O; Scharff-Hansen, P; Schieck, J; Schorner-Sadenius, T; Schroder, M; Schumacher, M; Seuster, R; Shears, T G; Shen, B C; Sherwood, P; Skuja, A; Smith, A M; Sobie, R; Soldner-Rembold, S; Spano, F; Stahl, A; Strom, D; Strohmer, R; Tarem, S; Tasevsky, M; Teuscher, R; Thomson, M A; Torrence, E; Toya, D; Trigger, I; Trocsanyi, Z; Tsur, E; Turner-Watson, M F; Ueda, I; Ujvari, B; Vollmer, C F; Vannerem, P; Vertesi, R; Verzocchi, M; Voss, H; Vossebeld, J; Ward, C P; Ward, D R; Watkins, P M; Watson, A T; Watson, N K; Wells, P S; Wengler, T; Wermes, N; Wilson, G W; Wilson, J A; Wolf, G; Wyatt, T R; Yamashita, S; Zer-Zion, D; Zivkovic, L

    2011-01-01

    Hadronic event shape distributions from e+e− annihilation measured by the OPAL experiment at centre-of-mass energies between 91 GeV and 209 GeV are used to determine the strong coupling αS. The results are based on QCD predictions complete to the next-to-next-to-leading order (NNLO), and on NNLO calculations matched to the resummed next-to-leading-log-approximation terms (NNLO+NLLA). The combined NNLO result from all variables and centre-of-mass energies is αS(mZ0) = 0.1201 ± 0.0008(stat.) ± 0.0013(exp.) ± 0.0010(had.) ± 0.0024(theo.). while the combined NNLO+NLLA result is αS(mZ0) = 0.1189 ± 0.0008(stat.) ± 0.0016(exp.) ± 0.0010(had.) ± 0.0036(theo.). The completeness of the NNLO and NNLO+NLLA results with respect to missing higher order contributions, studied by varying the renormalization scale, is improved compared to previous results based on NLO or NLO+NLLA predictions only. The observed energy dependence of αS agrees with the QCD prediction of asymptotic freedom and excludes the absence o...

  20. Status of {alpha}{sub s} determinations from the non-perturbatively renormalised three-gluon vertex

    Energy Technology Data Exchange (ETDEWEB)

    Parrinello, C. [Liverpool Univ. (United Kingdom). Dept. of Math. Sci.; Richards, D.G. [Dept. of Physics and Astronomy, University of Edinburgh, Edinburgh EH9 3JZ (United Kingdom); Alles, B. [Dept. di Fisica, Sezione Teorica, Universita di Milano, Via Celoria 16, 20133-Milano (Italy); Panagopoulos, H. [Department of Natural Sciences, University of Cyprus, 1678 Nicosia (Cyprus); Pittori, C. [L.P.T.H.E., Universite de Paris Sud, Centre d`Orsay, 91405 Orsay (France)

    1998-04-01

    We demonstrate the feasibility of computing {alpha}{sub s} from the lattice three-gluon vertex in the Landau gauge. Data from 16{sup 4} and 24{sup 4} quenched lattices at {beta}=6.0 are presented. Our main result is that 2-loop asymptotic scaling is observed for momenta in the range 1.8-2.3 GeV, where lattice artifacts appear to be under control. (orig.). 6 refs.

  1. Critical review for the determination of the minimum detectable activity (MDA) of alpha-emitter radionuclides in environmental samples

    International Nuclear Information System (INIS)

    Gasco, C.; Anton, M.P.

    1996-12-01

    Different criteria for the calculation of the Minimum Detectable Activity (MDA) of an alpha emitter in environmental levels are reviewed in this report. Practical examples of its application to previously analyzed samples are shown. The authors propose a criteria based on prior calculations that applies to the radiochemical activities performed in the laboratory. The calculation procedure has been discussed with scientist from other laboratories in order to establish a general criteria to calculate the MDA

  2. RAPID DETERMINATION OF 237 NP AND PU ISOTOPES IN WATER BY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Jones, V.; Culligan, B.; Nichols, S.; Noyes, G.

    2010-06-23

    A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of {sup 237}Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry; a hybrid approach. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry so that long and short-lived Pu isotopes can be measured successfully. The method allows for simultaneous extraction of 20 samples (including QC samples) in 4 to 6 hours, and can also be used for emergency response. {sup 239}Pu, {sup 242}Pu and {sup 237}Np were measured by ICP-MS, while {sup 236}Pu, {sup 238}Pu, and {sup 239}Pu were measured by alpha spectrometry.

  3. Rapid determination of actinides in urine by inductively coupled plasma mass spectrometry and alpha spectrometry: a hybrid approach.

    Science.gov (United States)

    Maxwell, Sherrod L; Jones, Vernon D

    2009-11-15

    A new rapid separation method that allows separation and preconcentration of actinides in urine samples was developed for the measurement of longer lived actinides by inductively coupled plasma mass spectrometry (ICP-MS) and short-lived actinides by alpha spectrometry; a hybrid approach. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration, if required, is performed using a streamlined calcium phosphate precipitation. Similar technology has been applied to separate actinides prior to measurement by alpha spectrometry, but this new method has been developed with elution reagents now compatible with ICP-MS as well. Purified solutions are split between ICP-MS and alpha spectrometry so that long- and short-lived actinide isotopes can be measured successfully. The method allows for simultaneous extraction of 24 samples (including QC samples) in less than 3h. Simultaneous sample preparation can offer significant time savings over sequential sample preparation. For example, sequential sample preparation of 24 samples taking just 15 min each requires 6h to complete. The simplicity and speed of this new method makes it attractive for radiological emergency response. If preconcentration is applied, the method is applicable to larger sample aliquots for occupational exposures as well. The chemical recoveries are typically greater than 90%, in contrast to other reported methods using flow injection separation techniques for urine samples where plutonium yields were 70-80%. This method allows measurement of both long-lived and short-lived actinide isotopes. (239)Pu, (242)Pu, (237)Np, (243)Am, (234)U, (235)U and (238)U were measured by ICP-MS, while (236)Pu, (238)Pu, (239)Pu, (241)Am, (243)Am and (244)Cm were measured by alpha spectrometry. The method can also be adapted so that the separation of uranium isotopes for assay is not required, if uranium assay by direct dilution of the urine sample

  4. RAPID DETERMINATION OF ACTINIDES IN URINE BY INDUCTIVELY-COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY: A HYBRID APPROACH

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Jones, V.

    2009-05-27

    A new rapid separation method that allows separation and preconcentration of actinides in urine samples was developed for the measurement of longer lived actinides by inductively coupled plasma mass spectrometry (ICP-MS) and short-lived actinides by alpha spectrometry; a hybrid approach. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration, if required, is performed using a streamlined calcium phosphate precipitation. Similar technology has been applied to separate actinides prior to measurement by alpha spectrometry, but this new method has been developed with elution reagents now compatible with ICP-MS as well. Purified solutions are split between ICP-MS and alpha spectrometry so that long- and short-lived actinide isotopes can be measured successfully. The method allows for simultaneous extraction of 24 samples (including QC samples) in less than 3 h. Simultaneous sample preparation can offer significant time savings over sequential sample preparation. For example, sequential sample preparation of 24 samples taking just 15 min each requires 6 h to complete. The simplicity and speed of this new method makes it attractive for radiological emergency response. If preconcentration is applied, the method is applicable to larger sample aliquots for occupational exposures as well. The chemical recoveries are typically greater than 90%, in contrast to other reported methods using flow injection separation techniques for urine samples where plutonium yields were 70-80%. This method allows measurement of both long-lived and short-lived actinide isotopes. 239Pu, 242Pu, 237Np, 243Am, 234U, 235U and 238U were measured by ICP-MS, while 236Pu, 238Pu, 239Pu, 241Am, 243Am and 244Cm were measured by alpha spectrometry. The method can also be adapted so that the separation of uranium isotopes for assay is not required, if uranium assay by direct dilution of the urine sample is preferred instead

  5. CANALPH-3: a portable three-channel alpha spectrometer for measuring the daughter products of radon and thoron

    International Nuclear Information System (INIS)

    Carson, D.W.

    1979-07-01

    A portable three-channel alpha spectrometer for the measurment of radon and thoron daughters in uranium mines or homes is described. The computer programs for analysing the data to give the working levels of radon and thoron by both the alpha spectrometric and modified Kusnetz methods are included along with some typical results

  6. Mass spectrometric examinations of Hungarian triassic dolomites

    International Nuclear Information System (INIS)

    Vitalis, Gy.; Kada I-ne

    1982-01-01

    A limited number of mass spectrometric investigations (viz.:57) of representative rock types were applied both in the research work of geology and the mining for the industry of building materials of Hungary. Tabulated results covering all rock types and all stratigraphic levels of the Hungarian Triassic are given. Sr, Mn, Ti and Cr trace elements had the highest occurrence and Zn, Y or Pb, Ba, V or Cu, depending on the genetical type of the rock studied, has relatively higher concentrations as well. The results of the examinations of Hungarian Triassic dolomites were discussed according to genetical types, all represented by a small level of trace elements. (Sz.J.)

  7. Outdoor spectrometric measurement of gamma source activities

    International Nuclear Information System (INIS)

    Cespirova, I.

    2003-01-01

    Two methods for outdoor activity measurements are described. The one is the in situ measurement method which is based on a proportionality between the flux density of non-dispersed photons of the given energy at the detector site and the specific activity of the relevant radionuclide in soil. The other method, for the monitoring of large areas, uses the spectrometric IRIS system (Integrated Radiation Information System), located on a helicopter for aerial monitoring or in a car for terrestrial measurement. (P.A.)

  8. Evaluation of mass spectrometric techniques for characterization of engineered proteins

    DEFF Research Database (Denmark)

    Roepstorff, P; Schram, K H; Andersen, Jens S.

    1995-01-01

    Mass spectrometric characterization of engineered proteins has been examined using bovine recombinant Acyl-CoA-Binding Protein (rACBP), [15N]-labeled rACBP, and a number of sequence variants of ACBP produced by site-directed mutagenesis. The mass spectrometric techniques include ESIMS and MALDIMS...

  9. Mass Spectrometric Studies of Oxides

    Science.gov (United States)

    Jacobson, Nathan S.

    2012-01-01

    Current studies at NASA Glenn on oxide thermodynamics are discussed. Previous studies on the vaporization of B2O3 in reducing atmospheres led to inconsistent studies when B was used as a reductant. It is shown that liquid B2O3 does not wet B and a clear phase separation was noted in the Knudsen cell. This problem was solved by using FeB and Fe2B to supply a different and constant activity of B. The thermodynamic data thus derived are compared to quantum chemical composite calculations. A major problem in high temperature mass spectrometry is the determination of accurate ionization cross sections, particularly for molecules. The method of Deutsch and Mark shows promise and some sample calculations are discussed. Finally current studies on the thermodynamics of rare earth silicates are discussed. Here the problems are obtaining a measurable signal from SiO2 vaporization and non-equilibrium vaporization. The use of a Ta reducing agent provides a stronger signal, which is related to silica activity. The Whitman-Motzfeld relation adapted to KEMS measurements is applied to obtain equilibrium pressures.

  10. Calculus of radiolytic products generation in water due to alpha radiation. Determination of the spent nuclear fuels matrix alteration rate Determination of velocity of spent fuel matrix

    International Nuclear Information System (INIS)

    Quinones, J.; Serrano, J.; Diaz Arocas, P.; Rodriguez Almazan, J. L.; Bruno, J.; Cera, E.; Merino, J.; Esteban, J. A.; Martinez-Esparza, A.

    2000-01-01

    The generation of radiolytic products as a result of alpha radiation in the surface of the spent fuel is a key process in order to understand how the it becomes degraded in repository conditions. The present work has established a radiolytic model based on a set of reactions involving fuel oxidation-dissolution and radiolytic products recombination. It also includes the decrease of the dose rates as the main alpha emitters decay away. Four cases, with varying parameters of the system, have been assessed. The results show a decrease in both the concentration of the radiolytic products in the gap water and the degradation of the fuel matrix. It has been estimated that in the period of the evaluation (10''6 years) up to 52% of the pellet is altered in the conservative cases, whereas only 11% is altered in the realistic cases. No significant differences were observed when the carbonates reactions were included in the system. (Author)

  11. Method of determining the variation of concentration of the potential alpha energy of radon daughters with time without changing the filter

    International Nuclear Information System (INIS)

    Feddersen, C.

    1979-01-01

    Considering the drawbacks of sample measurement of radon daughter concentration or potential alpha energy concentration, a method is described allowing to determine the variation with time of the measuring quantities mentioned. For this purpose, the same filter is exposed in defined time intervals and the decay curve is evaluated using Markov's method. Residual activity of preceding measurements is estimated as a function of the density of measuring points. A practicable technique is given for taking into account residual activity together with the background. An apparatus consisting of commercial devices and special accessories of own manufacture is described. The results obtained with this apparatus are illustrated and discussed using two examples. (author)

  12. Determination of 222Rn in fresh water: development of a robust method of analysis by alpha/beta separation liquid scintillation spectrometry.

    Science.gov (United States)

    Pates, Jacqueline M; Mullinger, Neil J

    2007-01-01

    Liquid scintillation spectrometry is used widely for determining (222)Rn in natural waters; however, the benefits of alpha/beta separation have not been fully explored. The extractants toluene and Ultima Gold F were compared, and both performed well for a range of extreme waters. A robust method for calibrating extraction and counting efficiencies has been developed. Detection limits are 20 mBql(-1) (toluene) and 16 mBql(-1) (UGF) for a 60 min count and 600-ml sample, halving the required sample volume.

  13. Isolation and structure determination of two novel C(13{sup 2})-OH bacteriopheophytin {alpha} allomers from a coastal salt pond sediment

    Energy Technology Data Exchange (ETDEWEB)

    Ocampo, R. [Universite Louis Pasteur, Strasbourg (France). Faculte de Chimie; Repeta, D.J. [Woods Hole Oceanographic Institution (United States). Dept. of Marine Chemistry and Geochemistry

    2002-07-01

    We report the isolation and structure determination [RP-18 HPLC, UV-Vis, MS, {sup 1}H NMR, and two-dimensional 1H NMR (COSY and ROESY)] of two novel C(13{sup 2})-OH bacteriopheophytin a allomers from a coastal salt pond sediment (Salt Pond, MA, USA). These allomers are formed by oxidative transformation of bacteriochlorophyll a and/or bacteriopheophytin {alpha}, and may play, through fossilization, an important role as intermediates on the formation of some ETIO porphyrins isolated early from sediments. (Author)

  14. Molecular determinants of desensitization and assembly of the chimeric GABA(A) receptor subunits (alpha1/gamma2) and (gamma2/alpha1) in combinations with beta2 and gamma2

    DEFF Research Database (Denmark)

    Elster, L; Kristiansen, U; Pickering, D S

    2001-01-01

    Two gamma-aminobutyric acid(A) (GABA(A)) receptor chimeras were designed in order to elucidate the structural requirements for GABA(A) receptor desensitization and assembly. The (alpha1/gamma2) and (gamma2/alpha1) chimeric subunits representing the extracellular N-terminal domain of alpha1 or gam...... receptor with respect to the direct activation by pentobarbital. This suggests differences in the mechanism of channel activation for pentobarbital and GABA....

  15. Determination of zearalenone and its metabolites alpha- and beta-zearalenol in beer samples by high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zöllner, P; Berner, D; Jodlbauer, J; Lindner, W

    2000-02-11

    A fast, robust and sensitive LC-MS-MS method for the determination of zearalenone (ZON) and its metabolites alpha-zearalenol (alpha-ZOL) and beta-zearalenol (beta-ZOL) in beer samples is described. Sample preparation was performed by direct RP-18 solid-phase extraction of undiluted beer samples followed by selective determination of analytes by LC-MS-MS applying an atmospheric pressure chemical ionization (APCI) interface. Using the negative ion mode limits of determination of 0.03-0.06 microg l(-1) beer and limits of quantification of 0.07-0.15 microg l(-1) beer were achieved, which was distinctly more sensitive than in the positive ion mode. Twenty-three beer samples from different countries, produced from different grains and under different brewing conditions, were investigated by this method, but only in one sample could beta-ZOL and ZON be detected. Independently of the type of beer, relative standard deviations between 2.1% and 3.3%, a linear working range of 0.15 microg l(-1) to 500 microg l(-1) beer and recovery rates around 100% could be achieved when zearalanone (ZAN) was used as internal standard.

  16. A Procedure for the Sequential Determination of Radionuclides in Phosphogypsum Liquid Scintillation Counting and Alpha Spectrometry for 210Po, 210Pb, 226Ra, Th and U Radioisotopes

    International Nuclear Information System (INIS)

    2014-01-01

    Since 2004, the Environment Programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. Reliable, comparable and 'fit for purpose' results are essential requirements for any decision based on analytical measurements. For the analyst, tested and validated analytical procedures are extremely important tools for the production of such analytical data. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. In this publication, a combined procedure for the sequential determination of 210Po, 210Pb, 226Ra, Th and U radioisotopes in phosphogypsum is described. The method is based on the dissolution of small amounts of phosphogypsum by microwave digestion, followed by sequential separation of 210Po, 210Pb, Th and U radioisotopes by selective extraction chromatography using Sr, TEVA and UTEVA resins. Radium-226 is separated from interfering elements using Ba(Ra)SO4 co-precipitation. Lead-210 is determined by liquid scintillation counting. The alpha source of 210Po is prepared by autodeposition on a silver plate. The alpha sources of Th and U are prepared by electrodeposition on a stainless steel plate. A comprehensive methodology for the calculation of results, including the quantification of measurement uncertainty, was also developed. The procedure is introduced as a recommended procedure and validated in terms of trueness, repeatability and reproducibility in accordance with ISO guidelines

  17. Model for assessing alpha doses for a Reference Japanese Man

    International Nuclear Information System (INIS)

    Kawamura, Hisao

    1993-01-01

    In view of the development of the nuclear fuel cycle in this country, it is urgently important to establish dose assessment models and related human and environmental parameters for long-lived radionuclides. In the current program, intake and body content of actinides (Pu, Th, U) and related alpha-emitting nuclides (Ra and daughters) have been studied as well as physiological aspects of Reference Japanese Man as the basic model of man for dosimetry. The ultimate object is to examine applicability of the existing models particularly recommended by the ICRP for workers to members of the public. The result of an interlaboratory intercomparison of 239 Pu + 240 Pu determination including our result was published. Alpha-spectrometric determinations of 226 Ra in bone yielded repesentative bone concentration level in Tokyo and Ra-Ca O.R. (bone-diet) which appear consistent with the literature value for Sapporo and Kyoto by Ohno using a Rn emanation method. Specific effective energies for alpha radiation from 226 Ra and daughters were calculated using the ICRP dosimetric model for bone incorporating masses of source and target organs of Reference Japanese Man. Reference Japanese data including the adult, adolescent, child and infant of both sexes was extensively and intensively studied by Tanaka as part of the activities of the ICRP Task Group on Reference Man Revision. Normal data for the physical measurements, mass and dimension of internal organs and body surfaces and some of the body composition were analysed viewing the nutritional data in the Japanese population. Some of the above works are to be continued. (author)

  18. Jet production in ep collisions at low Q{sup 2} and determination of {alpha}{sub s}

    Energy Technology Data Exchange (ETDEWEB)

    Aaron, F.D. [National Institute for Physics and Nuclear Engineering (NIPNE), Bucharest (Romania); Bucharest Univ. (Romania). Faculty of Physics; Aldaya Martin, M. [DESY Hamburg (Germany); Alexa, C. [National Institute for Physics and Nuclear Engineering (NIPNE), Bucharest (RO)] (and others)

    2009-10-15

    The production of jets is studied in deep-inelastic e{sup +}p scattering at low negative four momentum transfer squared 5 < Q{sup 2} < 100 GeV{sup 2} and at inelasticity 0.2 < y < 0.7 using data recorded by the H1 detector at HERA in the years 1999 and 2000, corresponding to an integrated luminosity of 43.5 pb{sup -1}. Inclusive jet, 2-jet and 3-jet cross sections as well as the ratio of 3-jet to 2-jet cross sections are measured as a function of Q{sup 2} and jet transverse momentum. The 2-jet cross section is also measured as a function of the proton momentum fraction {xi}. The measurements are well described by perturbative quantum chromodynamics at next-to-leading order corrected for hadronisation effects and are subsequently used to extract the strong coupling {alpha}{sub s}. (orig.)

  19. Determination of C and O and other elements by alpha-induced X-ray energy spectrometry

    International Nuclear Information System (INIS)

    Henningsen, W.P.; Schaetzler, H.P.; Kuehn, W.

    1978-01-01

    X-ray energy spectrometry combined with alpha-excitation by means of radionuclides, especially Po-210, has been found as a versatile tool for multielement analysis. Down to Z = 6 (carbon) qualitative and quantitative measurements have been carried out with energy resolution good enough to separate adjacent elements. Thereby errors and lowest detectable concentrations were in the region of one percent. By utilizing M- and L-X-radiation the set of detectable elements can be opened to high atomic numbers. As an example with special regard to environmental research cadmium in organic matrix was measured down to 100 ppm without any preconcentration. Much lower detection limits might be reached by appropriate measures. (orig.) [de

  20. Jet production in ep collisions at low Q {sup 2} and determination of {alpha}{sub s}

    Energy Technology Data Exchange (ETDEWEB)

    Aaron, F.D.; Alexa, C.; Rotaru, M.; Stoicea, G. [National Inst. for Physics and Nuclear Engineering, Bucharest (Romania); Andreev, V.; Belousov, A.; Eliseev, A.; Fomenko, A.; Gogitidze, N.; Lebedev, A.; Loktionova, N.; Malinovski, E.; Rusakov, S.; Shtarkov, L.N.; Soloviev, Y.; Vazdik, Y. [Lebedev Physical Inst., Moscow (Russian Federation); Antunovic, B.; Bartel, W.; Brandt, G.; Campbell, A.J.; Cholewa, A.; Deak, M.; Eckerlin, G.; Elsen, E.; Felst, R.; Fischer, D.J.; Fleischer, M.; Gayler, J.; Ghazaryan, S.; Glazov, A.; Gouzevitch, M.; Grell, B.R.; Haidt, D.; Helebrant, C.; Jung, H.; Katzy, J.; Kleinwort, C.; Knutsson, A.; Kosior, E.; Kraemer, M.; Krastev, K.; Kutak, K.; Levonian, S.; Lipka, K.; List, J.; Marti, Ll.; Meyer, A.B.; Meyer, H.; Meyer, J.; Niebuhr, C.; Nikiforov, A.; Olsson, J.E.; Panagoulias, I.; Papadopoulou, T.; Pitzl, D.; Placakyte, R.; Radescu, V.; Schmitt, S.; Sefkow, F.; Staykova, Z.; Steder, M.; Vargas Trevino, A.; Vinokurova, S.; Driesch, M. von den; Wissing, C.; Wuensch, E. [DESY, Hamburg (Germany); Backovic, S.; Dubak, A.; Lastovicka-Medin, G.; Picuric, I.; Raicevic, N. [Univ. of Montenegro, Podgorica (ME); Baghdasaryan, A.; Volchinski, V.; Zohrabyan, H. [Yerevan Physics Inst. (Armenia); Barrelet, E. [Universites Paris VI et VII, CNRS/IN2P3, LPNHE, Paris (France); Begzsuren, K.; Ravdandorj, T.; Tseepeldorj, B. [Inst. of Physics and Technology of the Mongolian Academy of Sciences, Ulaanbaatar (Mongolia); Bizot, J.C.; Brisson, V.; Delcourt, B.; Jacquet, M.; Li, G.; Pascaud, C.; Tran, T.H.; Zhang, Z.; Zomer, F. [Univ. Paris-Sud, CNRS/IN2P3, LAL, Orsay (France); Boudry, V.; Moreau, F.; Specka, A. [Ecole Polytechnique, CNRS/IN2P3, LLR, Palaiseau (France); Bozovic-Jelisavcic, I.; Mudrinic, M.; Pandurovic, M.; Smiljanic, I. [Vinca Inst. of Nuclear Sciences, Belgrade (RS); Bracinik, J.; Kenyon, I.R.; Newman, P.R.; Shaw-West, R.N.; Thompson, P.D. [Univ. of Birmingham, School of Physics and Astronomy (United Kingdom)] [and others

    2010-05-15

    The production of jets is studied in deep-inelastic e {sup +} p scattering at low negative four momentum transfer squared 5alpha}{sub s}. (orig.)

  1. Gamma-spectrometric examination of hot particles emitted during the Chernobyl accident

    International Nuclear Information System (INIS)

    Balashazy, I.; Szabadine-Szende, G.; Loerinc, M.; Zombori, P.

    1987-05-01

    Ge(Li) gamma-spectrometric examination of hot particles prepared from air filtered dust of Budapest air after the Chernobyl accident is presented. The method of separating hot particles is described and their concentration in the air is determined. The radioactive isotope composition of hot particles is discussed and compared with that of dust samples. Finally, the inhalation probability and radiation burden of hot particles are evaluated. (author)

  2. 5alphaDH-DOC (5alpha-dihydro-deoxycorticosterone) activates androgen receptor in castration-resistant prostate cancer.

    Science.gov (United States)

    Uemura, Motohide; Honma, Seijiro; Chung, Suyoun; Takata, Ryo; Furihata, Mutsuo; Nishimura, Kazuo; Nonomura, Norio; Nasu, Yasutomo; Miki, Tsuneharu; Shuin, Taro; Fujioka, Tomoaki; Okuyama, Akihiko; Nakamura, Yusuke; Nakagawa, Hidewaki

    2010-08-01

    Prostate cancer often relapses during androgen-depletion therapy, even under the castration condition in which circulating androgens are drastically reduced. High expressions of androgen receptor (AR) and genes involved in androgen metabolism indicate a continued role for AR in castration-resistant prostate cancers (CRPCs). There is increasing evidence that some amounts of 5alpha-dihydrotestosterone (DHT) and other androgens are present sufficiently to activate AR within CRPC tissues, and enzymes involved in the androgen and steroid metabolism, such as 5alpha-steroid reductases, are activated in CRPCs. In this report, we screened eight natural 5alphaDH-steroids to search for novel products of 5alpha-steroid reductases, and identified 11-deoxycorticosterone (DOC) as a novel substrate for 5alpha-steroid reductases in CRPCs. 11-Deoxycorticosterone (DOC) and 5alpha-dihydro-deoxycorticosterone (5alphaDH-DOC) could promote prostate cancer cell proliferation through AR activation, and type 1 5alpha-steroid reductase (SRD5A1) could convert from DOC to 5alphaDH-DOC. Sensitive liquid chromatography-tandem mass spectrometric analysis detected 5alphaDH-DOC in some clinical CRPC tissues. These findings implicated that under an extremely low level of DHT, 5alphaDH-DOC and other products of 5alpha-steroid reductases within CRPC tissues might activate the AR pathway for prostate cancer cell proliferation and survival under castration.

  3. Liquid chromatography-tandem mass spectrometric assay for the nucleoside reverse transcriptase inhibitor emtricitabine in human plasma

    NARCIS (Netherlands)

    Sparidans, Rolf W.; Prins, Jan M.; Schellens, Jan H. M.; Beijnen, Jos H.

    2007-01-01

    A liquid chromatography-tandem mass spectrometric assay for the determination of the antiretroviral nucleoside emtricitabine in human plasma was developed and validated using a simple sample pre-treatment procedure. After addition of 5'-deoxy-5-fluorocytidine as the internal standard and protein

  4. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide powder and pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Total Carbon by Combustion and Gravimetry 7-17 Total Boron by Titrimetry 18-28 Isotopic Composition by Mass Spectrometry 29-38 Chloride and Fluoride Separation by Pyrohydrolysis 39-45 Chloride by Constant-Current Coulometry 46-54 Fluoride by Ion-Selective Electrode 55-63 Water by Constant-Voltage Coulometry 64-72 Impurities by Spectrochemical Analysis 73-81 Soluble Boron by Titrimetry 82-95 Soluble Carbon by a Manometric Measurement 96-105 Metallic Impurities by a Direct Reader Spectrometric Method 106-114

  5. Rapid determination of (237)Np and plutonium isotopes in urine by inductively-coupled plasma mass spectrometry and alpha spectrometry.

    Science.gov (United States)

    Maxwell, Sherrod L; Culligan, Brian K; Jones, Vernon D; Nichols, Sheldon T; Noyes, Gary W; Bernard, Maureen A

    2011-08-01

    A new rapid separation method was developed for the measurement of plutonium and neptunium in urine samples by inductively-coupled plasma mass spectrometry (ICP-MS) and/or alpha spectrometry with enhanced uranium removal. This method allows separation and preconcentration of plutonium and neptunium in urine samples using stacked extraction chromatography cartridges and vacuum box flow rates to facilitate rapid separations. There is an increasing need to develop faster analytical methods for emergency response samples. There is also enormous benefit to having rapid bioassay methods in the event that a nuclear worker has an uptake (puncture wound, etc.) to assess the magnitude of the uptake and guide efforts to mitigate dose (e.g., tissue excision and chelation therapy). This new method focuses only on the rapid separation of plutonium and neptunium with enhanced removal of uranium. For ICP-MS, purified solutions must have low salt content and low concentration of uranium due to spectral interference of (238)U(1)H(+) on m/z 239. Uranium removal using this method is enhanced by loading plutonium and neptunium initially onto TEVA resin, then moving plutonium to DGA resin where additional purification from uranium is performed with a decontamination factor of almost 1×10(5). If UTEVA resin is added to the separation scheme, a decontamination factor of ~3 × 10(6) can be achieved.

  6. Determination of human serum alpha1-acid glycoprotein and albumin binding of various marketed and preclinical kinase inhibitors.

    Science.gov (United States)

    Zsila, Ferenc; Fitos, Ilona; Bencze, Gyula; Kéri, György; Orfi, László

    2009-01-01

    There are about 380 protein kinase inhibitors in drug development as of today and 15 drugs have been marketed already for the treatment of cancer. This time 139 validated kinase targets are in the focus of drug research of pharmaceutical companies and big efforts are made for the development of new, druglike kinase inhibitors. Plasma protein binding is an important factor of the ADME profiling of a drug compound. Human serum albumin (HSA) and alpha(1)-acid glycoprotein (AAG) are the most relevant drug carriers in blood plasma. Since previous literature data indicated that AAG is the principal plasma binding component of some kinase inhibitors the present work focuses on the comprehensive evaluation of AAG binding of a series of marketed and experimental kinase inhibitors by using circular dichroism (CD) spectroscopy approach. HSA binding was also evaluated by affinity chromatography. Protein binding interactions of twenty-six kinase inhibitors are characterized. The contribution of AAG and HSA binding data to the pharmacokinetic profiles of the investigated therapeutic agents is discussed. Structural, biological and drug binding properties of AAG as well as the applicability of the CD method in studying drug-protein binding interactions are also briefly reviewed.

  7. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    DEFF Research Database (Denmark)

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed...

  8. Gas chromatographic-mass spectrometric separation, identification and determination of C6-C12 cyclic imides in thermally treated epoxy and alkyd resins to locate hot spots inside large electricity generators.

    Science.gov (United States)

    Husain, S; Alvi, S N; Rao, R N

    1999-11-05

    A simple and rapid GC-MS method for separation, identification and quantitative determination of long-chain cyclic imides in the 300 degrees C thermally treated epoxy and alkyd resins has been developed. The method provides a positive means of identifying C6-C12 cyclic imide derivatives by GC-MS and enables the specific area of overheating to be identified, thereby averting catastrophic failures of power generators in service.

  9. On-line complexation of zinc with 5-Br-PADAP and preconcentration using a knotted reactor for inductively coupled plasma atomic emission spectrometric determination in river water samples

    Energy Technology Data Exchange (ETDEWEB)

    Salonia, J.A.; Wuilloud, R.G.; Gasquez, J.A.; Olsina, R.A.; Martinez, L.D. [Area de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, 5700 San Luis (Argentina)

    2000-08-01

    An on-line zinc preconcentration and determination system implemented with inductively coupled plasma atomic emission spectrometry (ICP-AES) associated with flow injection (FI) was studied. The zinc was retained as zinc-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Zn-(5-Br-PADAP)) complex at pH 9.2. The zinc complex was removed from the knotted reactor (KR) with 30% v/v nitric acid. An enrichment factor of 42 was obtained for the KR system with respect to ICP-AES using pneumatic nebulization. The detection limit for the preconcentration of 10 mL of aqueous solution was 0.09 {mu}g/L. The precision for 10 replicate determinations at the 5 {mu}g/L Zn level was 2.3% relative standard deviation (RSD), calculated with the peak heights obtained. The calibration graph using the preconcentration system for zinc was linear with a correlation coefficient of 0.9997 at levels near the detection limits up to at least 100 {mu}g/L. The method was succesfully applied to the determination of zinc in river water samples. (orig.)

  10. Energy dispersive X-Ray fluorescence spectrometric study of ...

    African Journals Online (AJOL)

    Energy dispersive X-Ray fluorescence spectrometric study of compositional differences in trace elements in dried Moringa oleifera leaves grown in two different agro-ecological locations in Ebonyi State, Nigeria.

  11. Sex determines cortisol and alpha-amylase responses to acute physical and psychosocial stress in patients with avoidant personality disorder.

    Science.gov (United States)

    Tanaka, Yoshihiro; Ishitobi, Yoshinobu; Inoue, Ayako; Oshita, Harumi; Okamoto, Kana; Kawashima, Chiwa; Nakanishi, Mari; Aizawa, Saeko; Masuda, Koji; Maruyama, Yoshihiro; Higuma, Haruka; Kanehisa, Masayuki; Ninomiya, Taiga; Akiyoshi, Jotaro

    2016-08-01

    Avoidant personality disorder (AVPD) has excessive and pervasive anxiety and discomfort in social situations. The aims of this study were to explore the relationship between AVPD and physical and psychological stress and psychological tests. We evaluated 93 AVPD patients and 355 nonpatient controls by salivary amylase and cortisol responses during exposure to the Trier Social Stress Test (TSST) and electrical stimulation stress. Spielberger state-trait anxiety inventory (STAI), Profile of Mood State (POMS), Beck Depression Inventory (BDI), Depression and Anxiety Cognition Scale (DACS), and Childhood Trauma Questionnaire (CTQ) were administered. Following electrical stimulation, salivary cortisol levels in female AVPD decreased significantly less than that in female's controls, but salivary cortisol levels did not show a difference between male AVPD patients and controls. Salivary alpha-amylase (sAA) levels did not show a difference between females or male AVPD patients and controls. Following TSST exposure, sAA levels did not show a difference between females or male AVPD patients and controls. Salivary cortisol levels did not show a difference between females or male AVPD patients and controls. In the AVPD patients, POMS scores were significantly higher compared with the controls. STAI, BDI, DACS scores, and CTQ significantly increased in the AVPD patients compared with the controls. LF in heart rate variability in AVPD significantly increased more compared with controls. These results suggest that heightened sympathetic reactivity in female AVPD co-occurs with attenuated salivary cortisol responses to electric stimulation stress and there is a significant difference between AVPD and controls in mood, anxiety, social cognition, and automatic nerve systems.

  12. Alpha spetrometric determination of 226Ra in water samples by using ion exchanger MnO2-PAN

    International Nuclear Information System (INIS)

    Gardonova, V.; Dulanska, S.; Matel, L.; Bilohuscin, J.; Horvathova, B.; Sebesta, F.

    2014-01-01

    A method for 226 Ra preconcentration and separation from water samples using MnO 2 -PAN (polyacrylonitrile) ion absorber composite was proposed, optimized and verified. The optimization was focused on prevention of the destruction of MnO 2 -PAN composite absorber during radium elution from the column, testing of multiple use of the resin, influence of calcium concentration on radiochemical yields and application of the method for various types of water samples. Absorber was produced at Czech Technical University in Prague and now is also commercially available from Triskem International, France as MnO 2 -PAN Resin.This absorber with grain size (0.1-0.3) mm was used for 226 Ra preconcentration from various types of water samples at pH = (6.5-7.0). Radium was eluted from the ion exchanger MnO 2 -PAN with 20 mL of 6.5 mol/L HCl at flow rate of 1.5 mL/min. Samples were precipitated with Ba 2+ to form Ba(Ra)SO 4 microprecipitate for alpha spectrometry counting..The proposed method was applied to samples of natural mineral, mountain spring, drinking and natural healing waters from Slovakia, Slovenia and Czech Republic. Radium radiochemical recoveries were monitored by non-isotopic tracer 133 Ba and they were in the range of (92 - 100) %. The obtained 226 Ra activities in the analyzed samples were compared with the limit values set in Edict 528 of the Ministry of Health of the Slovak Republic in 2007 and no limit was exceeded. (authors)

  13. Structural details (kinks and non-alpha conformations) in transmembrane helices are intrahelically determined and can be predicted by sequence pattern descriptors.

    Science.gov (United States)

    Rigoutsos, Isidore; Riek, Peter; Graham, Robert M; Novotny, Jiri

    2003-08-01

    One of the promising methods of protein structure prediction involves the use of amino acid sequence-derived patterns. Here we report on the creation of non-degenerate motif descriptors derived through data mining of training sets of residues taken from the transmembrane-spanning segments of polytopic proteins. These residues correspond to short regions in which there is a deviation from the regular alpha-helical character (i.e. pi-helices, 3(10)-helices and kinks). A 'search engine' derived from these motif descriptors correctly identifies, and discriminates amongst instances of the above 'non-canonical' helical motifs contained in the SwissProt/TrEMBL database of protein primary structures. Our results suggest that deviations from alpha-helicity are encoded locally in sequence patterns only about 7-9 residues long and can be determined in silico directly from the amino acid sequence. Delineation of such variations in helical habit is critical to understanding the complex structure-function relationships of polytopic proteins and for drug discovery. The success of our current methodology foretells development of similar prediction tools capable of identifying other structural motifs from sequence alone. The method described here has been implemented and is available on the World Wide Web at http://cbcsrv.watson.ibm.com/Ttkw.html.

  14. Heteronuclear relayed E.COSY revisited: determination of 3J(H(alpha),C(gamma)) couplings in Asx and aromatic residues in proteins.

    Science.gov (United States)

    Löhr, F; Pérez, C; Köhler, R; Rüterjans, H; Schmidt, J M

    2000-09-01

    Constant-time 3D heteronuclear relayed E.COSY [Schmidt et al. (1996) J. Biomol. NMR, 7, 142-152], as based on generic 2D small-flip-angle HMQC-COSY [Schmidt et al. (1995) J. Biomol. NMR, 6, 95-105], has been modified to allow for quantitative determination of heteronuclear three-bond 3J(H(alpha),C(gamma)) couplings. The method is applicable to amino acid spin topologies with carbons in the gamma position which lack attached protons, i.e. to asparagine, aspartate, and aromatic residues in uniformly 13C-enriched proteins. The pulse sequence critically exploits heteronuclear triple-quantum coherence (HTQC) of CH2 moieties involving geminal H(beta) proton pairs, taking advantage of improved multiple-quantum relaxation properties, at the same time avoiding scalar couplings between those spins involved in multiple-quantum coherence, thus yielding E.COSY-type multiplets with a splitting structure that is simpler than with the original scheme. Numerical least-squares 2D line-shape simulation is used to extract 3J(H(alpha),C(gamma)) coupling constants which are of relevance to side-chain chi1 dihedral-angle conformations in polypeptides. Methods are demonstrated with recombinant 15N,13C-enriched ribonuclease T1 and Desulfovibrio vulgaris flavodoxin with bound oxidized FMN.

  15. The use of emulsions for the determination of methylmercury and inorganic mercury in fish-eggs oil by cold vapor generation in a flow injection system with atomic absorption spectrometric detection.

    Science.gov (United States)

    Burguera, J L; Quintana, I A; Salager, J L; Burguera, M; Rondón, C; Carrero, P; Anton de Salager, R; Petit de Peña, Y

    1999-04-01

    An on-line time based injection system used in conjunction with cold vapor generation atomic absorption spectrometry and microwave-aided oxidation with potassium persulfate has been developed for the determination of the different mercury species in fish-eggs oil samples. A three-phase surfactant-oil-water emulsion produced an advantageous flow when a peristaltic pump was used to introduce the highly viscous sample into the system. The optimum proportion of the oil-water mixture ratio was 2:3 v/v with a Tween 20 surfactant concentration in the emulsion of 0.008% v/v. Inorganic mercury was determined after reduction with sodium borohydride while total mercury was determined after an oxidation step with persulfate prior to the reduction step to elemental mercury with the same reducing agent. The difference between total and inorganic mercury determined the organomercury content in samples. A linear calibration graph was obtained in the range 0.1-20 micrograms l-1 of Hg2+ by injecting 0.7 ml of samples. The detection limits based on 3 sigma of the blank signals were 0.11 and 0.12 microgram l-1 for total and inorganic mercury, respectively. The relative standard deviation of ten independent measurements were 2.8 and 2.2% for 10 micrograms l-1 and 8.8 and 9.0% for 0.1 microgram l-1 amounts of total and inorganic mercury, respectively. The recoveries of 0.3, 0.6 and 8 micrograms l-1 of inorganic and organic mercury added to fish-eggs oil samples ranged from 93.0 to 94.8% and from 100 to 106%, respectively. Good agreement with those values obtained for total mercury content in real samples by electrothermal atomic absorption spectrometry was also obtained, differences between mean values were catfish-eggs oil samples from the northwestern coast of Venezuela were measured; while the organic mercury lay in the range 2.0 and 3.3 micrograms l-1, inorganic mercury was not detected.

  16. Solid Phase Extraction of Trace Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) Ions in Beverages on Functionalized Polymer Microspheres Prior to Flame Atomic Absorption Spectrometric Determinations.

    Science.gov (United States)

    Berber, Hale; Alpdogan, Güzin

    2017-01-01

    In this study, poly(glycidyl methacrylate-methyl methacrylate-divinylbenzene) was synthesized in the form of microspheres, and then functionalized by 2-aminobenzothiazole ligand. The sorption properties of these functionalized microspheres were investigated for separation, preconcentration and determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions using flame atomic absorption spectrometry. The optimum pH values for quantitative sorption were 2 - 4, 5 - 8, 6 - 8, 4 - 6, 2 - 6 and 2 - 3 for Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II), respectively, and also the highest sorption capacity of the functionalized microspheres was found to be for Cu(II) with the value of 1.87 mmol g -1 . The detection limits (3σ; N = 6) obtained for the studied metals in the optimal conditions were observed in the range of 0.26 - 2.20 μg L -1 . The proposed method was successfully applied to different beverage samples for the determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions, with the relative standard deviation of <3.7%.

  17. Comparison of serum copper determination by colorimetric and atomic absorption spectrometric methods in seven different laboratories. The S.F.B.C. (Société Française de Biologie Clinique) Trace Element Group.

    Science.gov (United States)

    Arnaud, J; Chappuis, P; Zawislak, R; Houot, O; Jaudon, M C; Bienvenu, F; Bureau, F

    1993-02-01

    An interlaboratory collaborative trial was conducted on the determination of serum copper using two different methods, based on colorimetry (test combination Copper, Boehringer Mannheim, Mannheim, Germany) and flame atomic absorption spectrometry (FAAS). The general performance of the colorimetric method was below that of FAAS, except for sensitivity and linear range, as assessed by detection limit (0.44 versus 1.32 mumol/L) and upper limit of linearity (150 versus 50 mumol/L). The range of the between-run CVs and the recovery of standard additions were, respectively, 2.3-11.9% and 92-127% for the colorimetric method and 1.1-6.0% and 93-101% for the FAAS method. Interferences were minimal with both methods. The two techniques correlated satisfactorily (the correlation coefficients ranged from 0.945-0.970 among laboratories) but the colorimetric assay exhibited slightly higher results than the FAAS method. Each method was transferable among laboratories.

  18. Effect of alpha-interferon alone and combined with other antineoplastic agents on renal cell carcinoma determined by the tetrazolium microculture assay.

    Science.gov (United States)

    Homma, Y; Aso, Y

    1994-01-01

    The antiproliferative effect of various alpha-interferons (alpha-IFNs), alone or combined with other agents, on a renal cell carcinoma cell line was evaluated by the tetrazolium microculture assay to examine the rationale for combination therapies. Cells incubated in 96-week microculture plates at 5 x 10(3)/well were exposed to various agents for 3 days. There were no obvious differences in the growth inhibition caused by the 5 kinds of alpha-IFN examined as single agents. The combination of alpha-IFN with the following agents was also assessed: 5-fluorouracil (5FU), methotrexate (MTX), mitomycin C, bleomycin, cis-diaminedichloroplatinum (CDDP), vinblastine, etoposide (ETOP), alpha-IFN, tumor necrosis factor-alpha (TNF), and alpha-difluoromethylornithine. Synergism was observed for the combination of alpha-IFN+TNF, while the other combinations had additive or subadditive effects. No interference or antagonism was found. Trimodal combinations of alpha-IFN+MTX with either 5FU, ETOP, or CDDP all showed subadditive effects. These results indicated that an increased antiproliferative effect, although not necessarily synergistic, was obtained by the combination of alpha-IFN with a variety of antineoplastic agents, providing a rationale to seek for combination therapies including alpha-IFN for treating renal cell carcinoma.

  19. Liquid chromatography tandem mass spectrometric determination of triterpenes in human fluids: Evaluation of markers of dietary intake of olive oil and metabolic disposition of oleanolic acid and maslinic acid in humans.

    Science.gov (United States)

    Pozo, Oscar J; Pujadas, Mitona; Gleeson, Sarah Biel; Mesa-García, Maria Dolores; Pastor, Antoni; Kotronoulas, Aristotelis; Fitó, Montserrat; Covas, Maria-Isabel; Navarro, José Ramón Fernández; Espejo, Juan Antonio; Sanchez-Rodriguez, Estefania; Marchal, Rosa; Calleja, Miguel Angel; de la Torre, Rafael

    2017-10-16

    Olive oil is rich in several minor components like maslinic (MA) and oleanolic (OA) acids which have cardioprotective, antitumor, and anti-inflammatory properties. In order to assess the health benefits in humans provided by the olive oil triterpenes (MA and OA), suitable analytical methods able to quantify the low concentrations expected in human fluids are required. In this study, the LC-MS/MS quantification of both OA and MA in plasma and urine has been evaluated. The plasmatic method is based on the direct determination of the analytes. The urinary detection requires more sensitivity which was reached by derivatization with 2-picolylamine. Additionally, the urinary species present after MA and OA ingestion were evaluated by the direct detection of several phase II metabolites previously synthesized. Our results showed that OA is metabolized as both sulfate and glucuronide conjugates whereas MA is mainly excreted as glucuronide. Based on this information, the method for the urinary detection of MA and OA involved an enzymatic hydrolysis. Both plasmatic and urinary methods were validated with suitable precision and accuracy at all tested levels. Required sensitivity was achieved in both matrices. Up to our knowledge, this is the first method able to quantify the low concentration levels of triterpenes present in urine. Samples from two healthy volunteers who received virgin olive oils with different triterpenes content were analyzed. Some preliminary clues on the metabolic disposition of OA and MA after olive oil intake are provided. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Spectrometric estimation of sample amount in aliquot for a direct solid sampling system and its application to the determination of trace impurities in silver nanoparticles by ETV-ICP-OES.

    Science.gov (United States)

    Nakata, Kenichi; Okamoto, Yasuaki; Ishizaka, Syoji; Fujiwara, Terufumi

    2016-04-01

    A method based on a tungsten boat furnace vaporiser, tungsten sample cuvettes, and an inductively coupled plasma (ICP) optical emission spectrometer has been developed for the direct determination of silicon, phosphorus, and sulphur in silver nanoparticles. The important point in the proposed method is that the entire sample in each batch is vaporised, which enables simultaneous measurement of the emission of not only the analyte but also the silver matrix. Furthermore, since the silver nanoparticles are sufficiently pure, the contribution of impurities to the sample amounts will be negligible. Therefore, this estimation is suitable for measuring the sample amount in each aliquot instead of the conventional weighing procedure using a microbalance; therefore, no tedious weighing procedures for estimating the sample amount introduced into the ETV device are needed. An additional advantage is that pretreatment and/or predigestion are unnecessary. The sample throughput is approximately 35 batches per hour. The detection limits of silicon, phosphorus, and sulphur in the silver nanoparticles (dry powder) are 15, 4.2, and 62 µg g(-1), respectively. Analytical results for various silver nanoparticles as both dry particles and in suspended solutions are described, and these values are compared to those obtained by conventional weighing with a microbalance. This methodology is useful for rapid screening and accurate analysis of silver nanoparticles, especially for industrial applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Solid phase extraction of cadmium on 2-mercaptobenzothiazole loaded on sulfur powder in the medium of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate and cold vapor generation-atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    Pourreza, N.; Ghanemi, K.

    2010-01-01

    A novel solid phase extractor for preconcentration of cadmium at ng L -1 levels has been developed. Cadmium ions were retained on a column packed with sulfur powder modified with 2-mercaptobenzothiazole (2-MBT) in the medium of 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim] + PF 6 - ) ionic liquid. The presence of ionic liquid during modification of sulfur enhanced the retention of cadmium ions on the column. The retained cadmium ions were eluted with 2 mol L -1 solution of HCl and measured by cold vapor generation-atomic absorption spectrometry (CVG-AAS). By using reaction cell-gas liquid separator (RC-GLS), gaseous cadmium vapors were produced and reached the atomic absorption spectrometer, instantaneously. The influence of different variables on both processes of solid phase extraction and CVG-AAS determination of cadmium ions was investigated. The calibration curve was linear in the range of 10-200 ng L -1 of cadmium in the initial solution with r = 0.9992 (n = 8) under optimum conditions. The limit of detection based on three times the standard deviation of the blank (3S b , n = 10) was 4.6 ng L -1 . The relative standard deviation (R.S.D.) of 25 and 150 ng L -1 of cadmium was 4.1 and 2.2% (n = 8), respectively. The procedure was validated by the analysis of a certified reference material (DORM-3), water and fish samples.

  2. Measurement of fission yields for 232-Th (n,f) at 14,7 MeV by direct gamma spectrometric method

    International Nuclear Information System (INIS)

    Chouak, K.; Berrada, M.; Embarech, K.

    1994-01-01

    Fission yields for the reaction 232-Th (n,f) were measured at 14,7 MeV using the activation technique with direct gamma spectrometric method. Neutrons were produced via the T(d,n) sup 4 He reaction. The neutron fluences were determined relative to the well-known sup 2 sup 7 Al(n,p) sup 2 sup 7 Mg or sup 2 sup 7 Al(n,alpha) sup 2 sup 4 Na cross section, according to the irradiation time. Yields of fission products were determined by measuring the induced gamma ray activities of the irradiated Th foils, using a calibrated Ge(Li) detector. All necessary corrections were taken into account: self absorption, coincidence losses and natural gamma rays. Fifty six cumulative yields were measured and only twenty one corresponding results were found in the literature (Crouch,1977). A satisfactory agreement is observed between our results and the published data with the exception of the masses:A=134 and A=140. 1 tab., 2 refs. (author)

  3. Buffett's Alpha

    DEFF Research Database (Denmark)

    Frazzini, Andrea; Kabiller, David; Heje Pedersen, Lasse

    Berkshire Hathaway has realized a Sharpe ratio of 0.76, higher than any other stock or mutual fund with a history of more than 30 years, and Berkshire has a significant alpha to traditional risk factors. However, we find that the alpha becomes insignificant when controlling for exposures to Betting-Against-Beta...... in publicly traded stocks versus wholly-owned private companies, we find that the former performs the best, suggesting that Buffett's returns are more due to stock selection than to his effect on management. These results have broad implications for market efficiency and the implementability of academic...

  4. Numerical bias estimation for mass spectrometric mass isotopomer analysis.

    Science.gov (United States)

    Yang, Tae Hoon; Bolten, Christoph J; Coppi, Maddalena V; Sun, Jun; Heinzle, Elmar

    2009-05-15

    Mass spectrometric (MS) isotopomer analysis has become a standard tool for investigating biological systems using stable isotopes. In particular, metabolic flux analysis uses mass isotopomers of metabolic products typically formed from (13)C-labeled substrates to quantitate intracellular pathway fluxes. In the current work, we describe a model-driven method of numerical bias estimation regarding MS isotopomer analysis. Correct bias estimation is crucial for measuring statistical qualities of measurements and obtaining reliable fluxes. The model we developed for bias estimation corrects a priori unknown systematic errors unique for each individual mass isotopomer peak. For validation, we carried out both computational simulations and experimental measurements. From stochastic simulations, it was observed that carbon mass isotopomer distributions and measurement noise can be determined much more precisely only if signals are corrected for possible systematic errors. By removing the estimated background signals, the residuals resulting from experimental measurement and model expectation became consistent with normality, experimental variability was reduced, and data consistency was improved. The method is useful for obtaining systematic error-free data from (13)C tracer experiments and can also be extended to other stable isotopes. As a result, the reliability of metabolic fluxes that are typically computed from mass isotopomer measurements is increased.

  5. Development of a screened cathode gas flow proportional counter for in situ field determination of alpha contamination in soil

    Energy Technology Data Exchange (ETDEWEB)

    Bush, S.P.

    1997-02-01

    This study resulted in the design, construction and testing of a gas flow proportional counter for in-situ determination of soil contamination. The uniqueness of this detector is the screened material used for the cathode. A Pu-239 source of 0.006 {micro}Ci was mounted to the outside of the cathode to simulate radioactive soil. The detector probe was placed into a laboratory mock-up and tested to determine operating voltage, efficiency and energy resolution. Two gas flow proportional counters were built and tested. The detectors are cylindrical, each with a radius of 1.905 cm, having an anode wire with a radius of 0.0038 cm. The length of the smaller detector`s anode was 2.54 cm, and the length of the larger detector`s anode was 7.64 cm. Therefore, the active volumes were 28.96 cm{sup 3} and 87.10 cm{sup 3}, respectively, for the small and large detector. An operating voltage of 1,975 volts was determined to be sufficient for both detectors. The average efficiency was 2.59 {+-} 0.12% and 76.71 {+-} 10.81% for the small volume and large volume detectors, respectively. The average energy resolution for the low-energy peak of the small detector was 4.24 {+-} 1.28% and for the large-energy peak was 1.37 {+-} 0.66%. The large detectors` energy resolution was 17.75 {+-} 3.74%. The smaller detector, with better energy resolution, exhibited a bi-modal spectrum, whereas the larger detector`s spectrum centered around a single broad peak.

  6. A procedure for the rapid determination of Pu isotopes and Am-241 in soil and sediment samples by alpha spectrometry

    International Nuclear Information System (INIS)

    2009-01-01

    Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is a extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004 the Environment Programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. In this report, a rapid procedure for the determination of Pu and Am radionuclides in soil and sediment samples is described that can be used in emergency situations. The method provides accurate and reliable results for the activity concentrations of elevated levels of 239,240 Pu, 238 Pu and 241 Am in soil and sediment samples over the course of 24 hours. The procedure has been validated in accordance with ISO guidelines

  7. Total alpha and beta determination by liquid scintillation counting in water samples from a Brazilian intercomparison exercise

    International Nuclear Information System (INIS)

    Dias, Fabiana F.; Taddei, Maria Helena T.; Pontedeiro, Elizabeth May Braga Dulley

    2009-01-01

    This paper describes CNEN/LAPOC's participation in the Brazilian Intercomparison Exercise (PNI) for simultaneous determination of total radioactivity in water samples, which took place in August and December 2008. The Proficiency Test (PT) also involved a short description of the nuclear analytical technique employed, emphasizing sources of uncertainty. A Liquid Scintillation System (Packard TRICARB 2700) was used with appropriate corrections applied to final results, expressed as Bq L -1 . Participation and PT data provide independent information on performance of a Laboratory and have an important role in method validation; especially because it allows the assessment of method performance over an entire range of concentrations and matrices. PT is also an important tool to demonstrate equivalence of measurements, if not their metrological comparability, and to promote education and improvement of Lab practices. (author)

  8. Determination of the Dalitz-plot parameter {alpha} for the decay {eta}{yields}3{pi}{sup 0} with the Crystal Ball at MAMI; Bestimmung des Dalitz-Plot-Parameters {alpha} fuer den Zerfall {eta} {yields} 3{pi}{sup 0} mit dem Crystal Ball am MAMI

    Energy Technology Data Exchange (ETDEWEB)

    Unverzagt, Marc

    2008-05-26

    In order to determine the Dalitz-plot parameter {alpha} experiments were evaluated, Which were performed with the Crystal Ball/TAPS facility at the accelerator MAMI of the Institute for Nuclear Physics at the Johannes Gutenberg University in Mainz in the years 2004 and 2005. {eta} mesons wer produced via the reaction {gamma}p{yields}{eta}p. From four different analyses the following four in this thesis determined Dalitz-plot parameters with the given statistics resulted: {eta} without proton: {alpha}=-0.0314{+-}0.0013{sub -0.0014}{sup +0.0017} (1.1.10{sup 6} events), {eta} with proton: {alpha}=-0.0338{+-}0.0020{sub -0.0022}{sup +0.0019} (4.2.10{sup 5} events), {delta}{sup +} magnetic dipole moment without proton: {alpha}=-0.0277{+-}0.0013{sub -0.0019}{sup +0.0014} (7.1.10{sup 5} events), {delta}{sup +} magnetic dipole moment with proton: {alpha}=-0.0272{+-}0.0019{sub -0.0043}{sup +0.0022} (3.1.10{sup 5} events).

  9. Determination of thorium and uranium isotopes in the mining lixiviation liquor samples

    Energy Technology Data Exchange (ETDEWEB)

    Reis Júnior, Aluísio de Souza; Monteiro, Roberto Pellacani Guedes, E-mail: reisas@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-07-01

    The alpha spectrometric analysis refers to determination of thorium and uranium isotopes in the mining lixiviation liquor samples. The analytical procedure involves sample preparation steps for rare earth elements, thorium and uranium separation using selective etching with hydrofluoric acid and further radiochemical separation of these using TRU chromatographic resins (Eichrom Industries Inc. USA) besides electroplating of the isolated radionuclides. An isotopic tracer is used to determine the overall chemical yield and to ensure traceability to a national standard. The results are compared to results obtained for the same samples by Becquerel laboratory. We improved the method looking for reproducibility and isotopes isolation as required by alpha spectrometry and the method showing effective in analysis of mining liquor. (author)

  10. Comparison of the analytical methods used to determine natural and artificial radionuclides from environmental samples by gamma, alpha and beta spectrometry

    DEFF Research Database (Denmark)

    Pöllänen, Roy; Virtanen, Sinikka; Kämäräinen, Meerit

    In CAMNAR, an extensive interlaboratory exercise on the analytical methods used to determine several radionuclides present in the environmental samples was organized. Activity concentration of different natural radionuclides, such as Rn-222, Pb-210, Po-210, K-40, Ra-226, Ra-228 and isotopes of ur...... Nordic and European countries participated in the intercomparison. Extraordinary variation between the results reported by different laboratories were revealed for some radionuclides indicating the need of future intercomparisons especially in the case of natural water samples.......In CAMNAR, an extensive interlaboratory exercise on the analytical methods used to determine several radionuclides present in the environmental samples was organized. Activity concentration of different natural radionuclides, such as Rn-222, Pb-210, Po-210, K-40, Ra-226, Ra-228 and isotopes...... of uranium, in addition to artificial Cs-137 and Am-241 were analysed from lake sediment samples and drinking water. The measurement techniques were gamma-ray spectrometry, alpha spectrometry, liquid scintillation counting and inductively coupled plasma mass spectrometry. Twenty six laboratories from nine...

  11. Use of sulfur hexafluoride airflow studies to determine the appropriate number and placement of air monitors in an alpha inhalation exposure laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Newton, G.J.; Hoover, M.D.

    1995-12-01

    Determination of the appropriate number and placement of air monitors in the workplace is quite subjective and is generally one of the more difficult tasks in radiation protection. General guidance for determining the number and placement of air sampling and monitoring instruments has been provided by technical reports such as Mishima, J. These two documents and other published guidelines suggest that some insight into sampler placement can be obtained by conducting airflow studies involving the dilution and clearance of the relatively inert tracer gas sulfur hexafluoride (SF{sub 6}) in sampler placement studies and describes the results of a study done within the ITRI alpha inhalation exposure laboratories. The objectives of the study were to document an appropriate method for conducting SF{sub 6} dispersion studies, and to confirm the appropriate number and placement of air monitors and air samplers within a typical ITRI inhalation exposure laboratory. The results of this study have become part of the technical bases for air sampling and monitoring in the test room.

  12. A highly conserved phenylalanine in the alpha, beta-T cell receptor (TCR) constant region determines the integrity of TCR/CD3 complexes

    DEFF Research Database (Denmark)

    Caspar-Bauguil, S; Arnaud, J; Huchenq, A

    1994-01-01

    In the present study, we have investigated the importance of a phenylalanine (phe195) in the Tcr-C alpha region on Tcr-alpha,beta/CD3 membrane expression. An exchange of phe195 with a tyrosine residue does not affect Tcr/CD3 membrane expression; however, exchange with aspartic acid, histidine or ...

  13. Mass Spectrometric Immunoassays in Characterization of Clinically Significant Proteoforms

    Directory of Open Access Journals (Sweden)

    Olgica Trenchevska

    2016-03-01

    Full Text Available Proteins can exist as multiple proteoforms in vivo, as a result of alternative splicing and single-nucleotide polymorphisms (SNPs, as well as posttranslational processing. To address their clinical significance in a context of diagnostic information, proteoforms require a more in-depth analysis. Mass spectrometric immunoassays (MSIA have been devised for studying structural diversity in human proteins. MSIA enables protein profiling in a simple and high-throughput manner, by combining the selectivity of targeted immunoassays, with the specificity of mass spectrometric detection. MSIA has been used for qualitative and quantitative analysis of single and multiple proteoforms, distinguishing between normal fluctuations and changes related to clinical conditions. This mini review offers an overview of the development and application of mass spectrometric immunoassays for clinical and population proteomics studies. Provided are examples of some recent developments, and also discussed are the trends and challenges in mass spectrometry-based immunoassays for the next-phase of clinical applications.

  14. Spectrometric electronic equipment for a 90-channel cherenkov mass spectrometer

    International Nuclear Information System (INIS)

    Astvatsaturov, R.G.; Basiladze, S.G.; Ivanov, V.I.

    1978-01-01

    Detecting spectrometric electronic equipment of a 90-channel cherenkov γ-spectrometer operating on-line with HP2116B type computer is described. The equipment contains linear amplifiers, analog memory blocks, a linear summator, discriminators, and a coincidence circuit. Three computer-controlled systems are used for checking the characteristics of the spectrometric electronic equipment, photomultipliers, and also for energy calibrations of the detectors. The long-term stability of the equipment has been measured with the aid of the checkup systems. It is established that the average instability of the pedestal magnitudes for all the channels is less than 10%, while the instability of the transmission coefficients is not worse than 0.5% for 5 days. The average nonlinearity over all the channels is 0.6%. The resolution time of the spectrometric equipment is 180 nsec

  15. Standard test methods for chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide (Gd2O3) powder

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 These test methods cover procedures for the chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide powders to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Carbon by Direct CombustionThermal Conductivity C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Total Chlorine and Fluorine by Pyrohydrolysis Ion Selective Electrode C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Loss of Weight on Ignition 7-13 Sulfur by CombustionIodometric Titration Impurity Elements by a Spark-Source Mass Spectrographic C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical,Nuclear, and Radiochemical Analysis of Uranium Hexafluoride C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry Gadolinium Content in Gadolinium Oxid...

  16. Rapid and sensitive lateral flow immunoassay method for determining alpha fetoprotein in serum using europium (III) chelate microparticles-based lateral flow test strips.

    Science.gov (United States)

    Liang, Rong-Liang; Xu, Xu-Ping; Liu, Tian-Cai; Zhou, Jian-Wei; Wang, Xian-Guo; Ren, Zhi-Qi; Hao, Fen; Wu, Ying-Song

    2015-09-03

    Alpha-fetoprotein (AFP), a primary marker for many diseases including various cancers, is important in clinical tumor diagnosis and antenatal screening. Most immunoassays provide high sensitivity and accuracy for determining AFP, but they are expensive, often complex, time-consuming procedures. A simple and rapid point-of-care system that integrates Eu (III) chelate microparticles with lateral flow immunoassay (LFIA) has been developed to determine AFP in serum with an assay time of 15 min. The approach is based on a sandwich immunoassay performed on lateral flow test strips. A fluorescence strip reader was used to measure the fluorescence peak heights of the test line (HT) and the control line (HC); the HT/HC ratio was used for quantitation. The Eu (III) chelate microparticles-based LFIA assay exhibited a wide linear range (1.0-1000 IU mL(-1)) for AFP with a low limit of detection (0.1 IU mL(-1)) based on 5ul of serum. Satisfactory specificity and accuracy were demonstrated and the intra- and inter-assay coefficients of variation (CV) for AFP were both <10%. Furthermore, in the analysis of human serum samples, excellent correlation (n = 284, r = 0.9860, p < 0.0001) was obtained between the proposed method and a commercially available CLIA kit. Results indicated that the Eu (III) chelate microparticles-based LFIA system provided a rapid, sensitive and reliable method for determining AFP in serum, indicating that it would be suitable for development in point-of-care testing. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Determination of the efficiency variation with the alpha and beta radiation energies for a hands and feet circulating gas proportional detector system

    International Nuclear Information System (INIS)

    Morgado, M.M.; Moraes, M.A.P.V. de

    1994-01-01

    The alpha and beta efficiency calibrations of a gas flow detector have been performed in the energy range of 3-5.5 MeV for alpha radiation and 0.1-1.5 MeV for beta radiation. This detector is being used for laboratorial monitoring in a hand and foot monitor system. The results obtained showed a strong increase in efficiency as the alpha (α) energy or beta (β) energy increase. Values of efficiency 2-4 times larger were obtained in these energy ranges. (author). 5 refs, 2 figs, 4 tabs

  18. The thiol proteinases from the latex of Carica papaya L. IV. Proteolytic specificities of chymopapain and papaya proteinase omega determined by digestion of alpha-globin chains.

    Science.gov (United States)

    Jacquet, A; Kleinschmidt, T; Dubois, T; Schnek, A G; Looze, Y; Braunitzer, G

    1989-08-01

    The proteolytic specificities of chymopapain and papaya proteinase omega were investigated by using the alpha-chains of manatee and mole haemoglobin, whose primary structures are known, as substrates. The resulting peptides from each enzymatic cleavage were isolated by gel filtration on Sephadex G-25, followed by reversed-phase HPLC of the separated peaks and, in some cases, further purified by preparative thin-layer electrophoresis. The purified peptides were then identified on the basis of their amino-acid composition. The proteolytic specificities of chymopapain and papaya proteinase omega, deduced from the experimental cleavage patterns, are compared to that of papain. As in the case of papain, the specificity-determining factor is the amino-acid residue of the substrate that will be bound in subsite S2 (the next but one from the scissible bond). Aromatic residues in this position, preferred by papain, are not important for chymopapain and papaya proteinase omega. Cleavages preferentially occur when S2 is occupied by leucine, valine or threonine. For chymopapain, proline in position S2 also causes cleavage.

  19. Colorimetric determination of alpha and beta-cyclodextrins and studies on optimization of CGTase production from B. firmus using factorial designs

    Directory of Open Access Journals (Sweden)

    Ilma Hiroko Higuti

    2004-11-01

    Full Text Available Cyclodextrin glycosyltransferase (EC 2.4.1.19, CGTase production from B. firmus, isolated from soil of Curitiba, PR, was optimized in shake flask using an experimental design approach. The CGTase was produced when the carbon source was starch and beta-CD, but when simple sugars such as glucose, galactose, lactose, sucrose, and maltose were used, there was no enzyme production. CGTase production was the same with either organic nitrogen or inorganic nitrogen source. CGTase activity decreased 2-fold when incubation temperature was increased from 28 to 37 ° C, and decreased 2.1- fold when the initial pH was lowered from 10.3 to 7.4. The colorimetric determinations of alpha - and beta -CD were analyzed as a non-linear relationship and the equilibrium constant for alpha -CD/methyl orange and beta -CD/phenolphthalein complexes were 7.69 x 10³ L / mol and 2.33 x 10³ L/ mol, respectively.A produção de ciclodextrina glicosiltransferase (EC2.4.1.19, CGTase de B. firmus isolada de solo de Curitiba, PR, foi otimizada com o uso de modelo estatístico fatorial. Foi estudado o efeito de componentes no meio básico bem como pH inicial e temperatura na produção da enzima. O modelo de fatorial 2k-1 foi usado. A atividade da CGTase foi monitorada pelo método colorimétrico com alaranjado de metila. Houve produção da CGTase quando a fonte de carbono era amido e beta-CD, mas quando galactose, lactose, sacarose e maltose foram usadas, nγo houve nenhuma produηγo de enzima. A produηão de CGTase foi a mesma com a fonte de nitrogênio orgânico ou inorgânico. A atividade da CGTase diminuiu 2 vezes quando a temperatura de incubação foi aumentada de 28 a 37 ° C, e diminuiu 2,1 vezes quando o pH inicial foi abaixado de 10,3 a 7,4. As determinações colorimetricas de alfa e beta - CD foram analisadas como regressão não linear e a constante de equilíbrio para os complexos alfa -CD/alaranjado de metila e beta -CD/fenolftaleina foram 7,69 x 10³ L/mol e 2

  20. Determination of 210Pb by direct gamma-ray spectrometry, beta counting via 210Bi and alpha-particle spectrometry via 210Po in coal, slag and ash samples from thermal power plant

    International Nuclear Information System (INIS)

    Seslak, Bojan; Vukanac, Ivana; Kandic, Aleksandar; Durasevic, Mirjana; Eric, Milic; Jevremovic, Aleksandar

    2017-01-01

    In order to compare three different techniques and estimate radiological impact, activity concentration of 210 Pb in coal, slag and ash samples from thermal power plant 'Nikola Tesla', Serbia, were measured, and results are presented in this study. Determination of 210 Pb was carried out in three ways: using HPGe gamma spectrometer and via in-growth of 210 Po and 210 Bi by alpha-particle spectrometry and proportional counting, respectively. The results obtained for three different techniques were compared. Statistical analysis and comparison of methods were carried out by combination of Z score and χ 2 statistical tests. Tests results, as well as values of measured activities concentrations obtained by alpha and gamma spectrometry, showed that gamma spectrometry is a valid alternative to time-consuming alpha spectrometry for low level activity measurements of 210 Pb. This remark is also valid even for gamma spectrometers with poor efficiency in low energy region. (author)

  1. Phosphoinositide 3-kinase alpha-dependent regulation of branching morphogenesis in murine embryonic lung: evidence for a role in determining morphogenic properties of FGF7.

    Directory of Open Access Journals (Sweden)

    Edward Carter

    Full Text Available Branching morphogenesis is a critical step in the development of many epithelial organs. The phosphoinositide-3-kinase (PI3K pathway has been identified as a central component of this process but the precise role has not been fully established. Herein we sought to determine the role of PI3K in murine lung branching using a series of pharmacological inhibitors directed at this pathway. The pan-class I PI3K inhibitor ZSTK474 greatly enhanced the branching potential of whole murine lung explants as measured by an increase in the number of terminal branches compared with controls over 48 hours. This enhancement of branching was also observed following inhibition of the downstream signalling components of PI3K, Akt and mTOR. Isoform selective inhibitors of PI3K identified that the alpha isoform of PI3K is a key driver in branching morphogenesis. To determine if the effect of PI3K inhibition on branching was specific to the lung epithelium or secondary to an effect on the mesenchyme we assessed the impact of PI3K inhibition in cultures of mesenchyme-free lung epithelium. Isolated lung epithelium cultured with FGF7 formed large cyst-like structures, whereas co-culture with FGF7 and ZSTK474 induced the formation of defined branches with an intact lumen. Together these data suggest a novel role for PI3K in the branching program of the murine embryonic lung contradictory to that reported in other branching organs. Our observations also point towards PI3K acting as a morphogenic switch for FGF7 signalling.

  2. 8-Quinolineboronic acid as a potential phosphorescent molecular switch for the determination of alpha-fetoprotein variant for the prediction of primary hepatocellular carcinoma

    International Nuclear Information System (INIS)

    Liu Jiaming; Li Feiming; Liu Zhenbo; Lin Changqing; Lin Shaoqin; Lin Liping; Wang Xinxing; Li Zhiming

    2010-01-01

    8-Quinolineboronic acid phosphorescent molecular switch (8-QBA-PMS) in the 'off' state emitted weak room temperature phosphorescence (RTP) of 8-QBA on the acetylcellulose membrane (ACM) with the perturbation of Pb 2+ . When 8-QBA-PMS was used to label concanavalin agglutinin (Con A) to form 8-QBA-PMS-Con A based on the reaction between -OH of 8-QBA-PMS and -COOH of Con A, 8-QBA-PMS turned 'on' automatically due to its structure change, and RTP of the system increased 2.7 times. Besides, -NH 2 of 8-QBA-PMS-Con A could carry out affinity adsorption (AA) reaction with the -COOH of alpha-fetoprotein variant (AFP-V) to form the product Con A-AFP-V-Con A-8-QBA-PMS containing -NH-CO- bond, causing the RTP of the system to further increase. Moreover, the amount of AFP-V was linear to the ΔI p of the system in the range of 0.012-2.40 (fg spot -1 ). Thus, a new affinity sensitive adsorption solid substrate room temperature phosphorimetry using 8-QBA-PMS as labelling reagent (8-QBA-PMS-AASSRTP) for the determination of AFP-V was proposed with the detection limit (LD) of 9 x 10 -15 g mL -1 . It had been used to determine AFP-V in human serum with the results agreeing with enzyme-link immunoassay (ELISA), showing promise for the prediction of PHC due to the intimate association between AFP-V and primary hepatocellular carcinoma (PHC). The mechanism of the promethod was also discussed.

  3. Computer-Assisted Determination of Minimum Energy Conformations. 7. A pharmacophore Model of the Active Region of the Alpha2-Adrenoceptor.

    Science.gov (United States)

    1992-09-01

    helpful discussions on the adrenergic system; Fu-Lian Hsu, Research Directorate, CRDEC, for his advice on synthesis and chemical interactions; Duane...Miller and Yoshiya Amomiya, Ohio State University, Columbus, OH, for their assistance in the synthesis of suggested alpha2- adrenergic compounds...Preferred Conformations of Ephedrine Isomers and the Nature of the Alpha Adrenergic Receptor," J. Pharmacol. Exp. Ther. Vol. 164 (1), pp 75-81 (1968). 24

  4. A rapid method of extraction of uranium and thorium from granite for alpha spectrometry

    International Nuclear Information System (INIS)

    Gascoyne, M.; Larocque, J.P.A.

    1984-01-01

    The lithium metaborate fusion technique for analysis of rock samples has been adapted for the alpha spectrometric determination of uranium and thorium isotope abundances in granite. Powdered granite is spiked with a solution of a uranium-thorium isotope tracer, mixed with LiBO 2 in a 1: 3 ratio and fused at 950 o C in a graphite crucible. The mixture is poured into 1 M HNO 3 and stirred until dissolved. Uranium and thorium are simultaneously extracted with 10% tributylphosphate(TBP) in amyl acetate using AI(NO 3 ) 3 as the salting agent, and then back-extracted into 1 M H 2 SO 4 . Uranium is separated from thorium using anion exchange resin and, after further purification, each is plated onto steel discs for alpha counting. Overall chemical yields are adequate at present (generally 20 to 60%). Preliminary tests show the TBP extraction step to be almost quantitative for both elements, in spite of the presence of silicon and high concentrations of aluminium. This procedure is much faster than the usual acid digestion technique, and uranium and thorium discs for counting can be prepared in approximately eight hours, starting from rock powder. (author)

  5. A rapid method of extraction of uranium and thorium from granite for alpha spectrometry

    International Nuclear Information System (INIS)

    Gascoyne, M.; Larocque, J.P.A.

    1984-01-01

    The lithium metaborate fusion technique for analysis of rock samples has been adapted for the alpha spectrometric determination of uranium and thorium isotope abundances in granite. Powdered granite is spiked with a solution of a uranium-thorium isotope tracer, mixed with LiBO 2 in a 1:3 ratio and fused at 950 0 C in a graphite crucible. The mixture is poured into 1 M HNO 3 and stirred until dissolved. Uranium and thorium are simultaneously extracted with 10% tributylphosphate (TBP) in amyl acetate using Al(NO 3 ) 3 as the salting agent, and then back-extracted into 1 M H 2 SO 4 . Uranium is separated from thorium using anion exchange resin and, after further purification, each is plated onto steel discs for alpha counting. Overall chemical yields are adequate at present (generally 20 to 60%). Preliminary tests show the TBP extraction step to be almost quantitative for both elements, in spite of the presence of silicon and high concentrations of aluminium. This procedure is much faster than the usual digestion technique, and uranium and thorium discs for counting can be prepared in approximately eight hours, starting from rock powder. (orig.)

  6. A rapid method of extraction of uranium and thorium from granite for alpha spectrometry

    Science.gov (United States)

    Gascoyne, M.; Larocque, J. P. A.

    1984-06-01

    The lithium metaborate fusion technique for analysis of rock samples has been adapted for the alpha spectrometric determination of uranium and thorium isotope abundances in granite. Powdered granite is spiked with a solution of a uranium-thorium isotope tracer, mixed with LiBO 2 in a 1:3 ratio and fused at 950°C in a graphite crucible. The mixture is poured into 1 M HNO 3 and stirred until dissolved. Uranium and thorium are simultaneously extracted with 10% tributylphosphate (TBP) in amyl acetate using Al(NO 3) 3 as the salting agent, and then back-extracted into 1 M H 2SO 4. Uranium is separated from thorium using anion exchange resin and, after further purification, each is plated onto steel discs for alpha counting. Overall chemical yields are adequate at present (generally 20 to 60%). Preliminary tests show the TBP extraction step to be almost quantitative for both elements, in spite of the presence of silicon and high concentrations of aluminium. This procedure is much faster than the usual acid digestion technique, and uranium and thorium discs for counting can be prepared in approximately eight hours, starting from rock powder.

  7. Preparation and spectrometric identification of amide derivatives with antimalaric

    International Nuclear Information System (INIS)

    Ferreira, E.J.

    1987-01-01

    The structures of polymeric compounds using spectrometric analysis of infrared, ultraviolet and protonic magnetic resonance and 13 C nuclear magnetic resonance are studied. Some structural models are used such as antimalaric-sulfones and pyrimidinic derivatives, and non-polymeric derivatives of active compounds. A comparative analysis on structures less complexes is shown. (M.J.C.). Spectrums 186 p [pt

  8. X-Ray Fluorescence Spectrometry. I.- Determination of thorium in ores; Espectrometria de fluorescencia de rayos X. A.- Aplicacion a la determinacion de torio en minerales

    Energy Technology Data Exchange (ETDEWEB)

    Bermudez Polonio, J.; Crus Castillo, F. de la; Fernandez Cellini, R.

    1961-07-01

    A X-ray spectrometric method has been developed for analysis of thorium in ores in the range of concentration from 0.01 to 0.5 percent ThO{sub 2}, using selenium as a internal standard. The concentration of thorium is determined in a working curve prepared by plotting the percentage of ThO{sub 2} against the ratio intensity of the Th L{alpha}{sub 1} line to Sek{sub {beta}}1 line. (Author) 17 refs.

  9. Spatio-temporal profiling and degradation of alpha-amylase isozymes during barley seed germination

    DEFF Research Database (Denmark)

    Bak-Jensen, K.S.; Laugesen, Sabrina; Østergaard, Ole

    2007-01-01

    Ten genes from two multigene families encode barley alpha-amylases. To gain insight into the occurrence and fate of individual isoforms during seed germination, the alpha-amylase repertoire was mapped by using a proteomics approach consisting of 2D gel electrophoresis, western blotting, and mass...... spectrometry. Mass spectrometric analysis confirmed that the 29 alpha-amylase positive 2D gel spots contained products of one ( GenBank accession gi| 113765) and two ( gi vertical bar 4699831 and gi vertical bar 166985) genes encoding alpha-amylase 1 and 2, respectively, but lacked products from seven other...... genes. Eleven spots were identified only by immunostaining. Mass spectrometry identified 12 full-length forms and 12 fragments from the cultivar Barke. Products of both alpha-amylase 2 entries co-migrated in five full-length and one fragment spot. The alpha-amylase abundance and the number of fragments...

  10. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 These test methods cover procedures for subsampling and for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride UF6. Most of these test methods are in routine use to determine conformance to UF6 specifications in the Enrichment and Conversion Facilities. 1.2 The analytical procedures in this document appear in the following order: Note 1—Subcommittee C26.05 will confer with C26.02 concerning the renumbered section in Test Methods C761 to determine how concerns with renumbering these sections, as analytical methods are replaced with stand-alone analytical methods, are best addressed in subsequent publications. Sections Subsampling of Uranium Hexafluoride 7 - 10 Gravimetric Determination of Uranium 11 - 19 Titrimetric Determination of Uranium 20 Preparation of High-Purity U3O 8 21 Isotopic Analysis 22 Isotopic Analysis by Double-Standard Mass-Spectrometer Method 23 - 29 Determination of Hydrocarbons, Chlorocarbons, and Partially Substitut...

  11. Kinetic Stability May Determine the Interaction Dynamics of the Bifunctional Protein DCoH1, the Dimerization Cofactor of the Transcription Factor HNF-1[alpha

    Energy Technology Data Exchange (ETDEWEB)

    Rho, H.; Jones, C.N.; Rose, R.B. (NCSU)

    2010-12-07

    The two disparate functions of DCoH1 (dimerization cofactor of HNF-1)/PCD (pterin-4a-carbinolamine dehydratase) are associated with a change in oligomeric state. DCoH dimers enhance the activity of the diabetes-associated transcription factor HNF-1{alpha} (hepatocyte nuclear factor-1{alpha}), while the PCD activity of DCoH1 homotetramers aids in aromatic amino acid metabolism. These complexes compete for the same interface of the DCoH dimer. Formation of the DCoH1/HNF-1{alpha} complex requires cofolding. The homotetramer of the DCoH1 paralogue, DCoH2, interacts with HNF-1{alpha} through simple mixing. To further investigate regulation of DCoH/HNF-1{alpha} complex formation, we measured the stability of the DCoH1 homotetramer through unfolding studies by intrinsic tryptophan fluorescence. DCoH2 unfolding is reversible. Surprisingly, the DCoH1 homotetramer is resistant to guanidine unfolding but refolds at a much lower guanidine concentration. We show that a point mutation at the DCoH1 tetramer interface, Thr 51 Ser, overcomes the dissociation barrier of the homotetramer and increases the interaction with HNF-1{alpha}. The 1.8 {angstrom} resolution crystal structure of DCoH1 T51S shows the presence of an ordered water molecule at the tetramer interface, as in DCoH2, which may destabilize the homotetramer. The equilibrium unfolding data were fit to a two-state model with no apparent intermediate. Folding intermediates were detectable by size exclusion chromatography. For wild-type DCoH1 the intermediates changed with time, suggesting a kinetic origin for the unfolding barrier of the homotetramer. We propose an unfolding pathway in which the tetramer unfolds slowly, but the dimer folds reversibly. Implications for regulation of DCoH1/HNF-1{alpha} complex formation are discussed.

  12. Rapid and sensitive lateral flow immunoassay method for determining alpha fetoprotein in serum using europium (III) chelate microparticles-based lateral flow test strips

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Rong-Liang; Xu, Xu-Ping; Liu, Tian-Cai; Zhou, Jian-Wei; Wang, Xian-Guo; Ren, Zhi-Qi [Institute of Antibody Engineering, School of Biotechnology, Southern Medical University, Guangzhou 510515, Guangdong (China); Hao, Fen [DaAn Gene Co. Ltd. of Sun Yat-sen University, 19 Xiangshan Road, Guangzhou 510515 (China); Wu, Ying-Song, E-mail: wg@smu.edu.cn [Institute of Antibody Engineering, School of Biotechnology, Southern Medical University, Guangzhou 510515, Guangdong (China)

    2015-09-03

    Alpha-fetoprotein (AFP), a primary marker for many diseases including various cancers, is important in clinical tumor diagnosis and antenatal screening. Most immunoassays provide high sensitivity and accuracy for determining AFP, but they are expensive, often complex, time-consuming procedures. A simple and rapid point-of-care system that integrates Eu (III) chelate microparticles with lateral flow immunoassay (LFIA) has been developed to determine AFP in serum with an assay time of 15 min. The approach is based on a sandwich immunoassay performed on lateral flow test strips. A fluorescence strip reader was used to measure the fluorescence peak heights of the test line (H{sub T}) and the control line (H{sub C}); the H{sub T}/H{sub C} ratio was used for quantitation. The Eu (III) chelate microparticles-based LFIA assay exhibited a wide linear range (1.0–1000 IU mL{sup −1}) for AFP with a low limit of detection (0.1 IU mL{sup −1}) based on 5ul of serum. Satisfactory specificity and accuracy were demonstrated and the intra- and inter-assay coefficients of variation (CV) for AFP were both <10%. Furthermore, in the analysis of human serum samples, excellent correlation (n = 284, r = 0.9860, p < 0.0001) was obtained between the proposed method and a commercially available CLIA kit. Results indicated that the Eu (III) chelate microparticles-based LFIA system provided a rapid, sensitive and reliable method for determining AFP in serum, indicating that it would be suitable for development in point-of-care testing. - Highlights: • Europium (III) chelate microparticles was used as a label for LIFA. • Quantitative detection by using H{sub T}/H{sub C} ratio was achieved. • LIFA for simple and rapid AFP detection in human serum. • The sensitivity and linearity was more excellent compared with QD-based ICTS. • This method could be developed for rapid point-of-care screening.

  13. Determination of the isotopic ratio 234 U/238 U and 235 U/238 U in uranium commercial reagents by alpha spectroscopy

    International Nuclear Information System (INIS)

    Iturbe G, J.L.

    1990-02-01

    In this work the determination of the isotope ratio 234 U/ 238 U and 235 U/ 238 U obtained by means of the alpha spectroscopy technique in uranium reagents of commercial marks is presented. The analyzed uranium reagents were: UO 2 (*) nuclear purity, UO 3 (*) poly-science, metallic uranium, uranyl nitrate and uranyl acetate Merck, uranyl acetate and uranyl nitrate Baker, uranyl nitrate (*) of the Refinement and Conversion Department of the ININ, uranyl acetate (*) Medi-Lab Sigma of Mexico and uranyl nitrate Em Science. The obtained results show that the reagents that are suitable with asterisk (*) are in radioactive balance among the one 234 U/ 238 U, since the obtained value went near to the unit. In the case of the isotope ratio 235 U/ 238 U the near value was also obtained the one that marks the literature that is to say 0.04347, what indicates that these reagents contain the isotope of 235 U in the percentage found in the nature of 0.71%. The other reagents are in radioactive imbalance among the 234 U/ 238 U, the found values fluctuated between 0.4187 and 0.1677, and for the quotient of activities 235 U/ 238 U its were of 0.0226, and the lowest of 0.01084. Also in these reagents it was at the 236 U as impurity. The isotope of 236 U is an isotope produced artificially, for what is supposed that the reagents that are in radioactive imbalance were synthesized starting from irradiated fuel. (Author)

  14. INTERLABORATORY STUDY OF A THERMOSPRAY-LIQUID CHROMATOGRAPHIC/MASS SPECTROMETRIC METHOD FOR SELECTED N-METHYL CARBAMATES, N-METHYL CARBAMOYLOXIMES, AND SUBSTITUTED UREA PESTICIDES

    Science.gov (United States)

    A thermospray-liquid chromatographic/mass spectrometric (TS-LC/MS) method was evaluated in an interlaboratory study for determining 3 N-methyl carbamates (bendiocarb, carbaryl, and carbofuran), 3-N-methyl carbamoyloximes (aldicarb, methomyl, and oxamyl), 2 substituted urea pestic...

  15. Mass spectrometric identification of an azobenzene derivative produced by smectite-catalyzed conversion of 3-amino-4-hydroxyphenylarsonic acid.

    Science.gov (United States)

    Wershaw, R L; Rutherford, D W; Rostad, C E; Garbarino, J R; Ferrer, Imma; Kennedy, K R; Momplaisir, Georges-Marie; Grange, Andrew

    2003-05-01

    The compound 3-amino-4-hydroxyphenylarsonic acid (3-amino-HPAA) reacts with smectite to form a soluble azobenzene arsonic acid compound. This reaction is of particular interest because it provides a possible mechanism for the formation of a new type of arsenic compound in natural water systems. 3-Amino-HPAA is a degradation product excreted by chickens that are fed rations amended with roxarsone. Roxarsone is used to control coccidial intestinal parasites in most of the broiler chickens grown in the United States. The structure of the azobenzene arsonic acid compound was first inferred from negative-ion and positive-ion low-resolution mass-spectrometric analyses of the supernatant of the smectite suspension. Elemental composition of the parent ion determined by high-resolution positive-ion mass spectrometric measurements was consistent with the proposed structure of the azobenzene arsonic acid compound.

  16. Mass spectrometric identification of an azobenzene derivative produced by smectite-catalyzed conversion of 3-amino-4-hydroxyphenylarsonic acid

    Science.gov (United States)

    Wershaw, R. L.; Rutherford, D.W.; Rostad, C.E.; Garbarino, J.R.; Ferrer, I.; Kennedy, K.R.; Momplaisir, G.-M.; Grange, A.

    2003-01-01

    The compound 3-amino-4-hydroxyphenylarsonic acid (3-amino-HPAA) reacts with smectite to form a soluble azobenzene arsonic acid compound. This reaction is of particular interest because it provides a possible mechanism for the formation of a new type of arsenic compound in natural water systems. 3-Amino-HPAA is a degradation product excreted by chickens that are fed rations amended with roxarsone. Roxarsone is used to control coccidial intestinal parasites in most of the broiler chickens grown in the United States. The structure of the azobenzene arsonic acid compound was first inferred from negative-ion and positive-ion low-resolution mass-spectrometric analyses of the supernatant of the smectite suspension. Elemental composition of the parent ion determined by high-resolution positive-ion mass spectrometric measurements was consistent with the proposed structure of the azobenzene arsonic acid compound. Published by Elsevier Science B.V.

  17. Uranium determination in zirconium

    International Nuclear Information System (INIS)

    Serdeiro, N.H.; Bianco de Salas, G.H.; Correia, R.J.

    1987-01-01

    The method used for the spectrometric uranium determination with 2-(2-thiolase)-5-diethylaminophenol was modified for its application in the zirconium samples analysis with an uranium content of the 0.1% order. The samples, previously dissolved in nitric acid, were submitted to a separative stage of liquid-liquid extraction, with a trioctylphosphine (TOPO) oxide diluted in cyclohexane. A sodium fluoride aqueous solution was necessary to be aggregated in the spectrometric determination so as to complex the zirconium vestiges, which could be present, originated by the Zr/U high relation of the initial sample. Under the established working conditions, different spectrometric assays, dyes absorption spectra and its uranium complex, complex stability, PH influence determination of the dyes-uranium relation, calculation of the complex's apparent formation constant and its molar absorption, were performed. (Author)

  18. A rapid alpha spectrometric method for estimation of 233U in bulk of thorium

    International Nuclear Information System (INIS)

    Rao, K.S.; Sankar, R.; Dhami, P.S.; Tripathi, S.C.; Gandhi, P.M.

    2015-01-01

    Analytical methods play important role in entire nuclear fuel cycle. Almost all the methods find applications in some way or the other in nuclear industry. Methods which cannot be directly used owing to selectivity, find application after chemical separation of analyte from interfering components. The analytical techniques used in PUREX process are almost well matured whereas in THOREX process the analytical techniques are constantly evolving as regards to simplicity, accuracy and time of analysis

  19. Sexually dimorphic genome-wide binding of retinoid X receptor alpha (RXRα determines male-female differences in the expression of hepatic lipid processing genes in mice.

    Directory of Open Access Journals (Sweden)

    Astrid Kosters

    Full Text Available Many hepatic functions including lipid metabolism, drug metabolism, and inflammatory responses are regulated in a sex-specific manner due to distinct patterns of hepatic gene expression between males and females. Regulation for the majority of these genes is under control of Nuclear Receptors (NRs. Retinoid X Receptor alpha (RXRα is an obligate partner for multiple NRs and considered a master regulator of hepatic gene expression, yet the full extent of RXRα chromatin binding in male and female livers is unclear. ChIP-Seq analysis of RXRα and RNA Polymerase2 (Pol2 binding was performed livers of both genders and combined with microarray analysis. Mice were gavage-fed with the RXR ligand LG268 for 5 days (30 mg/kg/day and RXRα-binding and RNA levels were determined by ChIP-qPCR and qPCR, respectively. ChIP-Seq revealed 47,845 (male and 46,877 (female RXRα binding sites (BS, associated with ∼12,700 unique genes in livers of both genders, with 91% shared between sexes. RXRα-binding showed significant enrichment for 2227 and 1498 unique genes in male and female livers, respectively. Correlating RXRα binding strength with Pol2-binding revealed 44 genes being male-dominant and 43 female-dominant, many previously unknown to be sexually-dimorphic. Surprisingly, genes fundamental to lipid metabolism, including Scd1, Fasn, Elovl6, and Pnpla3-implicated in Fatty Liver Disease pathogenesis, were predominant in females. RXRα activation using LG268 confirmed RXRα-binding was 2-3 fold increased in female livers at multiple newly identified RXRα BS including for Pnpla3 and Elovl6, with corresponding ∼10-fold and ∼2-fold increases in Pnpla3 and Elovl6 RNA respectively in LG268-treated female livers, supporting a role for RXRα regulation of sexually-dimorphic responses for these genes. RXRα appears to be one of the most widely distributed transcriptional regulators in mouse liver and is engaged in determining sexually-dimorphic expression of key

  20. Determination of the Dalitz plot parameter {alpha} for the decay {eta}{yields}3{pi}{sup 0} with the Crystal Ball at MAMI-B

    Energy Technology Data Exchange (ETDEWEB)

    Unverzagt, M.; Beck, R.; Lang, M.; Nikolaev, A.; Schumann, S. [University Mainz, Institut fuer Kernphysik, Mainz (Germany); University Bonn, Helmholtz-Institut fuer Strahlen- und Kernphysik, Bonn (Germany); Aguar-Bartolome, P.; Ahrens, J.; Arends, H.J.; Heid, E.; Jahn, O.; Krambrich, D.; Martinez-Fabregate, M.; Rost, M.; Thomas, A.; Walcher, T. [University Mainz, Institut fuer Kernphysik, Mainz (Germany); Annand, J.R.M.; Codling, R.; Livingston, K.; MacGregor, I.J.D.; McGeorge, J.C.; Owens, R.O.; Rosner, G. [University of Glasgow, Department of Physics and Astronomy, Glasgow (United Kingdom); Bekrenev, V. [Petersburg Nuclear Physics Institute, Gatchina (Russian Federation); Boillat, B.; Krusche, B.; Zehr, F. [University Basel, Institut fuer Physik, Basel (Switzerland); Braghieri, A.; Pedroni, P.; Rostomyan, T. [INFN Sezione di Pavia, Pavia (Italy); Branford, D.; Glazier, D.I.; Tarbert, C.M.; Watts, D.P. [Univ. of Edinburgh, School of Physics, Edinburgh (United Kingdom); Briscoe, W.J. [The George Washington Univ., Center for Nuclear Studies, Washington, D.C. (United States); Brudvik, J.W.; Nefkens, B.M.K.; Prakhov, S.N.; Price, J.W.; Starostin, A. [Univ. of California at Los Angeles, Los Angeles, CA (United States); Cherepnya, S.; Fil' kov, L.V.; Kashevarov, V.L. [Lebedev Physical Inst., Moscow (Russian Federation); Downie, E.J. [Univ. Mainz, Inst. fuer Kernphysik, Mainz (Germany); Univ. of Glasgow, Dept. of Physics and Astronomy, Glasgow (United Kingdom); Gregor, R.; Kotulla, M.; Lugert, S.; Metag, V.; Novotny, R. [Univ. Giessen, II. Physikalisches Inst., Giessen (Germany); Hornidge, D. [Mount Allison Univ., Sackville, NB (Canada); Kondratiev, R.; Lisin, V.; Polonski, A. [Institute for Nuclear Research, Moscow (Russian Federation); Korolija, M.; Mekterovic, D.; Supek, I. [Rudjer Boskovic Inst., Zagreb (Croatia); Manley, D.M. [Kent State Univ., Kent, OH (United States); Sober, D. [The Catholic Univ. of America, Washington, D.C. (United States)

    2009-02-15

    A precise measurement of the Dalitz plot parameter, {alpha}, for the {eta}{yields}3{pi}{sup 0} decay is presented. The experiment was performed with the Crystal Ball and TAPS large-acceptance photon detectors at the tagged photon beam facility of the MAMI-B electron accelerator in Mainz. High statistics of 1.8.10{sup 6} {eta}{yields}3{pi}{sup 0} events were obtained, giving the result {alpha}=-0.032{+-}0.002{sub stat}{+-}0.002{sub syst}. (orig.)

  1. Design and construction of a system for determining Radon-222 through Alpha spectroscopy; Diseno y construccion de un sistema para determinar Radon-222 mediante Espectroscopia alfa

    Energy Technology Data Exchange (ETDEWEB)

    Bonifacio, J.; Iturbe, J.L

    1992-02-15

    The study of the present work consists on designing a system to measure gas {sup 222} Rn, using a surface barrier detector, in order to obtaining a more accuracy measure of this isotope by means of an alpha particle spectra and thus to try to avoid the influence of the radioactivity of the isotope descendants of short half life, which are also emitting of alpha particles, since by other methods its should make a series of corrections to obtain the real value of the radon activity. (Author)

  2. Field methods for determining contents of alpha-radiating nuclides on the areas contaminated with depositions after the Chernobyl nuclear power station failure

    International Nuclear Information System (INIS)

    Pitkevich, V.A.; Duba, V.V.

    1992-01-01

    The work is aimed at creating field methods for estimating contents of alpha-radiating nuclides on the areas contaminated with depositions after the Chernobyl' station failure and for measuring the density of alpha-particles flux at various depths of soil. The methods make it possible to estimate the character of migration of isotopes Pu in depth. Instrumental and physical grounding of the methods are given. One can find the results of field measurements of α-active nuclides content in depositions. The results of measurement prove theoretical and practical feasibility of the suggested methods. 2 refs.; 4 figs.; 1 tabs

  3. PARTIAL LEAST SQUARES−NEAR INFRARED SPECTROMETRIC ...

    African Journals Online (AJOL)

    dominating absorption of ethanol, water and in some cases, sugars strongly influences the determination of ... PLS–FTIR has been employed to determine sucrose in fruit juices and glucose, total protein, cholesterol ... ionization detector and ECTm-5 capillary column (GC 1000, Dani) were used to determine ethanol and ...

  4. Coulomb correction to elastic. alpha. -. alpha. scattering

    Energy Technology Data Exchange (ETDEWEB)

    Bera, P.K.; Jana, A.K.; Haque, N.; Talukdar, B. (Department of Physics, Visva-Bharati University, Santiniketan-731235, West Bengal, India (IN))

    1991-02-01

    The elastic {alpha}-{alpha} scattering is treated within the framework of a generalized phase-function method (GPFM). This generalization consists in absorbing the effect of Coulomb interaction in the comparison functions for developing the phase equation. Based on values of scattering phase shifts computed by the present method, it is concluded that the GPFM provides an uncomplicated approach to rigorous Coulomb correction in the {alpha}-{alpha} scattering.

  5. Activator protein 2alpha mediates parathyroid TGF-alpha self-induction in secondary hyperparathyroidism.

    Science.gov (United States)

    Arcidiacono, Maria Vittoria; Cozzolino, Mario; Spiegel, Noah; Tokumoto, Masanori; Yang, Jing; Lu, Yan; Sato, Tetsuhiko; Lomonte, Carlo; Basile, Carlo; Slatopolsky, Eduardo; Dusso, Adriana S

    2008-10-01

    In secondary hyperparathyroidism, enhanced expression of TGF-alpha in the parathyroid leads to its own upregulation, generating a feed-forward loop for TGF-alpha activation of its receptor, EGFR receptor (EGFR), which promotes parathyroid hyperplasia. These studies examined the role of activator protein 2alpha (AP2), an inducer of TGF-alpha gene transcription, in the upregulation of parathyroid TGF-alpha in secondary hyperparathyroidism. In rat and human secondary hyperparathyroidism, parathyroid AP2 expression strongly correlated with TGF-alpha levels and with the rate of parathyroid growth, as expected. Furthermore, the increases in rat parathyroid content of AP2 and its binding to a consensus AP2 DNA sequence preceded the increase in TGF-alpha induced by high dietary phosphate. More significant, in A431 cells, which provide a model of enhanced TGF-alpha and TGF-alpha self-induction, mutating the core AP2 site of the human TGF-alpha promoter markedly impaired promoter activity induced by endogenous or exogenous TGF-alpha. Important for therapy, in five-sixths nephrectomized rats fed high-phosphate diets, inhibition of parathyroid TGF-alpha self-induction using erlotinib, a highly specific inhibitor of TGF-alpha/EGFR-driven signals, reduced AP2 expression dosage dependently. This suggests that the increases in parathyroid AP2 occur downstream of EGFR activation by TGF-alpha and are required for TGF-alpha self-induction. Indeed, in A431 cells, erlotinib inhibition of TGF-alpha self-induction caused parallel reductions in AP2 expression and nuclear localization, as well as TGF-alpha mRNA and protein levels. In summary, increased AP2 expression and transcriptional activity at the TGF-alpha promoter determine the severity of the hyperplasia driven by parathyroid TGF-alpha self-upregulation in secondary hyperparathyroidism.

  6. Hepatic processing determines dual activity of alpha-tocopheryl succinate: a novel paradigm for a shift in biological activity due to provitamin-to-vitamin conversion

    Czech Academy of Sciences Publication Activity Database

    Neužil, Jiří; Massa, H.

    2005-01-01

    Roč. 327, č. 4 (2005), s. 1024-1027 ISSN 0006-291X Institutional research plan: CEZ:AV0Z5052915; CEZ:AV0Z50520514 Keywords : vitamin E * alpha-tocopheryl succinate * hepatic processing Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 3.000, year: 2005

  7. High-precision Si-28(p,t)Si-26 reaction to determine Mg-22(alpha, p)Al-25 reaction rates

    NARCIS (Netherlands)

    Matic, A.; van den Berg, A. M.; Harakeh, M. N.; Wortche, H. J.; Beard, M.; Berg, G. P. A.; Goerres, J.; LeBlanc, P.; O'Brien, S.; Wiescher, M.; Fujita, K.; Hatanaka, K.; Sakemi, Y.; Shimizu, Y.; Tameshige, Y.; Tamii, A.; Yosoi, M.; Adachi, T.; Fujita, Y.; Shimbara, Y.; Fujita, H.; Wakasa, T.; Greene, J. P.; Crowter, R.; Schatz, H.

    2011-01-01

    The rise time of stellar x-ray bursts is a signature of thermonuclear runaway processes in the atmosphere of neutron stars and is highly sensitive to a series of (alpha, p) reactions via high-lying resonances in sd-shell nuclei. Lacking data for the relevant resonance levels, the stellar reaction

  8. Intrahepatic expression of interferon alpha & interferon alpha ...

    African Journals Online (AJOL)

    kemrilib

    Alpha m-RNA while 30% only expressed Interferon Alpha Receptor m-RNA. Responders and non-responders to Interferon therapy ... expression of IFN Alpha Receptor mRNA. Regardless of the response to interferon, histological .... generation reverse hybridisation, line probe assay. (Inno-LiPA HCV II; Innogenetics, Ghent,.

  9. The nitric oxide-donating pravastatin derivative, NCX 6550 [(1S-[1alpha(betaS*, deltaS*), 2alpha, 6alpha, 8beta-(R*), 8a alpha

    Science.gov (United States)

    Dever, G; Spickett, C M; Kennedy, S; Rush, C; Tennant, G; Monopoli, A; Wainwright, C L

    2007-01-01

    Statins possess anti-inflammatory effects that may contribute to their ability to slow atherogenesis, whereas nitric oxide (NO) also influences inflammatory cell adhesion. This study aimed to determine whether a novel NO-donating pravastatin derivative, NCX 6550 [(1S-[1alpha(betaS*,deltaS*),2alpha,6alpha,8beta-(R*),8a alpha

  10. Quantitative determination of alpha-quartz in airborne dust samples by x-ray diffraction; Determinacion cuantitativa de cuarzo-alfa en polvo atmosferico mediante difraccion de rayos X

    Energy Technology Data Exchange (ETDEWEB)

    Bayon, A.; Roca, M.

    1982-07-01

    The quantitative determination by X-ray diffractometry of alpha-quartz In airborne respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube Is employed. NiO is used as Internal standard In order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (Author) 17 refs.

  11. Mass spectrometric detection of radiocarbon for dating applications

    OpenAIRE

    Synal Hans-Arno

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which however can be completely eliminated in charge changing proces...

  12. Mass spectrometric analysis of nanogram levels of ruthenium

    International Nuclear Information System (INIS)

    Delmore, J.E.

    1979-01-01

    Previous investigations have demonstrated the possibility of using ruthenium originating from the spontaneous fission of 238 U for geochronological purposes. Because the abundance of ruthenium is low in geologic specimens and isotopic data are required, an indepth study of the production of steady mass spectrometer ion beams from nanogram amounts of ruthenium was undertaken. The results of this continuing mass spectrometric investigation are presented with some illustrative data

  13. System for Gamma an X rays fluorescence spectrometric

    International Nuclear Information System (INIS)

    Alonso Abad, D.; Arista Romeu, E.; Bolanos Perez, L. and others

    1997-01-01

    A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

  14. Gamma spectrometric system based on the personal computer Pravetz-83

    International Nuclear Information System (INIS)

    Yanakiev, K; Grigorov, T.; Vuchkov, M.

    1985-01-01

    A gamma spectrometric system based on a personal microcomputer Pravets-85 is described. The analog modules are NIM standard. ADC data are stored in the memory of the computer via a DMA channel and a real-time data processing is possible. The results from a series of tests indicate that the performance of the system is comparable with that of comercially avalable computerized spectrometers Ortec and Canberra

  15. Analysis of plutonium isotope ratios including238Pu/239Pu in individual U-Pu mixed oxide particles by means of a combination of alpha spectrometry and ICP-MS.

    Science.gov (United States)

    Esaka, Fumitaka; Yasuda, Kenichiro; Suzuki, Daisuke; Miyamoto, Yutaka; Magara, Masaaki

    2017-04-01

    Isotope ratio analysis of individual uranium-plutonium (U-Pu) mixed oxide particles contained within environmental samples taken from nuclear facilities is proving to be increasingly important in the field of nuclear safeguards. However, isobaric interferences, such as 238 U with 238 Pu and 241 Am with 241 Pu, make it difficult to determine plutonium isotope ratios in mass spectrometric measurements. In the present study, the isotope ratios of 238 Pu/ 239 Pu, 240 Pu/ 239 Pu, 241 Pu/ 239 Pu, and 242 Pu/ 239 Pu were measured for individual Pu and U-Pu mixed oxide particles by a combination of alpha spectrometry and inductively coupled plasma mass spectrometry (ICP-MS). As a consequence, we were able to determine the 240 Pu/ 239 Pu, 241 Pu/ 239 Pu, and 242 Pu/ 239 Pu isotope ratios with ICP-MS after particle dissolution and chemical separation of plutonium with UTEVA resins. Furthermore, 238 Pu/ 239 Pu isotope ratios were able to be calculated by using both the 238 Pu/( 239 Pu+ 240 Pu) activity ratios that had been measured through alpha spectrometry and the 240 Pu/ 239 Pu isotope ratios determined through ICP-MS. Therefore, the combined use of alpha spectrometry and ICP-MS is useful in determining plutonium isotope ratios, including 238 Pu/ 239 Pu, in individual U-Pu mixed oxide particles. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Spent nuclear fuel/water interface behavior: Alpha dose rate profile determination for model surfaces and microcracks by using Monte-Carlo methods

    Science.gov (United States)

    Tribet, M.; Mougnaud, S.; Jégou, C.

    2017-05-01

    This work aims to better understand the nature and evolution of energy deposits at the UO2/water reactional interface subjected to alpha irradiation, through an original approach based on Monte-Carlo-type simulations, using the MCNPX code. Such an approach has the advantage of describing the energy deposit profiles on both sides of the interface (UO2 and water). The calculations have been performed on simple geometries, with data from an irradiated UOX fuel (burnup of 47 GWd.tHM-1 and 15 years of alpha decay). The influence of geometric parameters such as the diameter and the calculation steps at the reactional interface are discussed, and the exponential laws to be used in practice are suggested. The case of cracks with various different apertures (from 5 to 35 μm) has also been examined and these calculations have also enabled new information on the mean range of radiolytic species in cracks, and thus on the local chemistry.

  17. Comparative analysis of dose rates in bricks determined by neutron activation analysis, alpha counting and X-ray fluorescence analysis for the thermoluminescence fine grain dating method

    Czech Academy of Sciences Publication Activity Database

    Bártová, H.; Kučera, Jan; Musílek, L.; Trojek, T.

    2014-01-01

    Roč. 104, NOV (2014), s. 393-397 ISSN 0969-806X. [1st International Conference on Dosimetry and its Applications (ICDA). Prague, 23.6.2013-28.6.2013] R&D Projects: GA MŠk(XE) LM2011019 Institutional support: RVO:61389005 Keywords : Alpha coutning * neutron activation analysis * X-ray fluorescence * thermoluminescence dating * dose rate Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 1.380, year: 2014

  18. Importance of salt in the production matrix of the efficiency curve for the determination of the total alpha activity in water samples; Importancia de la matriz salina en la fabricacion de la curva de eficiencia para la determinacion del indice de actividad alfa total en muestras de agua

    Energy Technology Data Exchange (ETDEWEB)

    Baeza, A.; Corbacho, J. A.

    2011-07-01

    The determination of total alpha activity by the evaporation method allows obtaining, from a quick and inexpensive technique, the order of magnitude of the total activity of all alpha emitters present in a sample of water. This study shows that the detection efficiency curve varies significantly depending on the sodium salt is used to manufacture calibration and/or reference radionuclide used. (Author)

  19. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    Administrator

    The resulting calculation is simple, and typically yields a determinant ratio which, at least for a small number of mixture components, .... nes, both caffeine and theobromine have acid–base equilibria that make their ultraviolet spectra poten- tially pH-dependent. For a quantitative application of Beer's law we must therefore ...

  20. Procedure for the determination of uranium on cellulose air-sampling filters by photon-electron-rejecting-alpha-liquid-scintillation spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    McDowell, W.J.; Case, G.N.

    1986-08-01

    A procedure is described for obtaining from cellulose air-sampling filters the total uranium content whether it be in the form of metal, oxide, tetrafluoride or most other salts of uranium. It is demonstrated that the uranium content can be accurately assayed by low-temperature ashing of the filter paper, dissolving the ash in a mixed nitrate-sulfate system, extracting the uranium selectively into a scintillator containing a high-molecular-weight amine sulfate, and counting the extract using a Photon-Electron-Rejecting-Alpha-Liquid-Scintillation (PERALS) spectrometer. 2 refs., 4 figs., 2 tabs.

  1. Spectrometric Analysis for Pulse Jet Mixer Testing

    International Nuclear Information System (INIS)

    ZEIGLER, KRISTINE

    2004-01-01

    The Analytical Development Section (ADS) was tasked with providing support for a Hanford River Protection Program-Waste Treatment Program (RPP-WTP) project test involving absorption analysis for non-Newtonian pulse jet mixer testing for small scale (PJM) and prototype (CRV) tanks with sparging. Tanks filled with clay were mixed with various amounts of powdered dye as a tracer. The objective of the entire project was to determine the best mixing protocol (nozzle velocity, number of spargers used, total air flow, etc.) by determining the percent mixed volume through the use of an ultraviolet-visible (UV-Vis) spectrometer. The dye concentration within the sample could be correlated to the volume fraction mixed in the tank. Samples were received in vials, a series of dilutions were generated from the clay, allowed to equilibrate, then centrifuged and siphoned for the supernate liquid to analyze by absorption spectroscopy. Equilibration of the samples and thorough mixing of the samples were a continuous issue with dilution curves being difficult to obtain. Despite these technical issues, useful data was obtained for evaluation of various mix conditions

  2. Determination of total alpha and beta activity in water for human consumption by LSC(Liquid Scintillation Counter); Determinacao de atividades alfa e beta total em agua para consumo humano por LSC (Contador de Cintilacao Liquida))

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2013-07-01

    The Ordinance Brazilian of Ministry of Health (MS 2914/2011) establishes the standards for quality of water intended for human consumption, being limits values of 5.0 Bq/L for gross alpha, and 1.0 Bq/L for gross beta radioactivity. The liquid scintillation spectrometry (LSC) technique has been presented as an alternative to conventional procedure using gas flow proportional counter. The present work shows a review of the methods for determination of gross alpha and gross beta in water by using LSC. Between the factors that influence the accuracy and repeatability of the analytical results we can highlight: thermal preconcentration, type of the acid and calibration standard. A procedure was established and carried out to samples of the National Program of Intercomparison of Radionuclides in Environmental Samples for evaluation of its performance. The gross alpha and gross beta analysis in samples of the public water supplies in the Metropolitan Region of Goiania, state of Goias was carried out. The results are consistent with the guideline values form the Ministry of Health concerning radioactivity. (author)

  3. Quantitative Mass Spectrometric Analysis and Post-Extraction Stability Assessment of the Euglenoid Toxin Euglenophycin

    Directory of Open Access Journals (Sweden)

    Paul V. Zimba

    2013-09-01

    Full Text Available Euglenophycin is a recently discovered toxin produced by at least one species of euglenoid algae. The toxin has been responsible for several fish mortality events. To facilitate the identification and monitoring of euglenophycin in freshwater ponds, we have developed a specific mass spectrometric method for the identification and quantitation of euglenophycin. The post-extraction stability of the toxin was assessed under various conditions. Euglenophycin was most stable at room temperature. At 8 °C there was a small, but statistically significant, loss in toxin after one day. These methods and knowledge of the toxin’s stability will facilitate identification of the toxin as a causative agent in fish kills and determination of the toxin’s distribution in the organs of exposed fish.

  4. Mass Spectrometric Calibration of Controlled Fluoroform Leak Rate Devices Technique and Uncertainty Analysis

    CERN Document Server

    Balsley, S D; Laduca, C A

    2003-01-01

    Controlled leak rate devices of fluoroform on the order of 10 sup - sup 8 atm centre dot cc sec sup - sup 1 at 25 C are used to calibrate QC-1 War Reserve neutron tube exhaust stations for leak detection sensitivity. Close-out calibration of these tritium-contaminated devices is provided by the Gas Dynamics and Mass Spectrometry Laboratory, Organization 14406, which is a tritium analytical facility. The mass spectrometric technique used for the measurement is discussed, as is the first principals calculation (pressure, volume, temperature and time). The uncertainty of the measurement is largely driven by contributing factors in the determination of P, V and T. The expanded uncertainty of the leak rate measurement is shown to be 4.42%, with a coverage factor of 3 (k=3).

  5. Mass spectrometric identification of proteins and characterization of their post-translational modifications in proteome analysis

    DEFF Research Database (Denmark)

    Roepstorff, P; Larsen, Martin Røssel

    2001-01-01

    for more than 425.000 protein sequences. However, the cellular functions are determined by the set of proteins expressed in the cell--the proteome. Two-dimensional gel electrophoresis, mass spectrometry and bioinformatics have become important tools in correlating the proteome with the genome. The current......High-throughput DNA sequencing has resulted in increasing input in protein sequence databases. Today more than 20 genomes have been sequenced and many more will be completed in the near future, including the largest of them all, the human genome. Presently, sequence databases contain entries...... dominant strategies for identification of proteins from gels based on peptide mass spectrometric fingerprinting and partial sequencing by mass spectrometry are described. After identification of the proteins the next challenge in proteome analysis is characterization of their post...

  6. Pharmacologic specificity of alpha-2 adrenergic receptor subtypes

    Energy Technology Data Exchange (ETDEWEB)

    Petrash, A.; Bylund, D.

    1986-03-01

    The authors have defined alpha-2 adrenergic receptor subtypes in human and rat tissues using prazosin as a subtype selective drug. Prazosin has a lower affinity (250 nM) at alpha-2A receptor and a higher affinity (5 nM) at alpha-2B receptors. In order to determine if other adrenergic drugs are selective for one or the other subtypes, the authors performed (/sup 3/H)yohimbine inhibition experiments with various adrenergic drugs in tissues containing alpha-2A, alpha-2B or both subtypes. Oxymetazoline, WB4101 and yohimbine were found to be 80-, 20- and 10-fold more potent at alpha-2A receptors than at alpha-2B receptors. Phentolamine, adazoxan, (+)- and (-)-mianserin, clonidine, (+)-butaclamol, (-)- and (+)-norepinephrine, epinephrine, dopamine and thioridazine were found to have equal affinities for the two subtypes. These results further validate the subdivision of alpha-2 adrenergic receptors into alpha-2A and alpha-2B subtypes.

  7. Challenges and recent advances in mass spectrometric imaging of neurotransmitters

    Science.gov (United States)

    Gemperline, Erin; Chen, Bingming; Li, Lingjun

    2014-01-01

    Mass spectrometric imaging (MSI) is a powerful tool that grants the ability to investigate a broad mass range of molecules, from small molecules to large proteins, by creating detailed distribution maps of selected compounds. To date, MSI has demonstrated its versatility in the study of neurotransmitters and neuropeptides of different classes toward investigation of neurobiological functions and diseases. These studies have provided significant insight in neurobiology over the years and current technical advances are facilitating further improvements in this field. neurotransmitters, focusing specifically on the challenges and recent Herein, we advances of MSI of neurotransmitters. PMID:24568355

  8. Detection of organic materials by spectrometric radiography method

    CERN Document Server

    Naydenov, S V; Onyshchenko, G.M.; Lecoq, P.; Smith, C.

    2008-01-01

    In this paper we report a spectrometric approach to dual-energy digital radiography that has been developed and applied to identify specific organic substances and discern small differences in their effective atomic number. An experimental setup has been designed, and a theoretical description proposed based on the experimental results obtained. The proposed method is based on application of special reference samples made of materials with different effective atomic number and thickness, parameters known to affect X-ray attenuation in the low-energy range. The results obtained can be used in the development of a new generation of multi-energy customs or medical X-ray scanners.

  9. Knudsen cell mass spectrometric study of the Cs2IOH(g) molecule thermodynamics

    International Nuclear Information System (INIS)

    Roki, F-Z.; Ohnet, M-N.; Fillet, S.; Chatillon, C.; Nuta, I.

    2013-01-01

    Highlights: • The pronounced ionic character leads to only dissociative ionization processes. • Ions formed are same as those coming from pure dimmers. • De-convolution of the ions origin needs accurate thermodynamic values for the pure gas phase. • Mass spectrometric interpretation has to be performed gradually and as a function of suitable condensed compositions. • Thermal functions have to be fully estimated. -- Abstract: The gas phase of the CsI + CsOH system is analyzed by high temperature Knudsen cell mass spectrometry in order to confirm the existence of the Cs 2 IOH(g) complex molecule. The mass spectrometric analysis is quite complex since such molecules undergo dissociative ionization into fragment ions that mix with the same ions from dimers of the pure compounds in the same vapor phase. Varying the chemical conditions for vaporization by using different CsI + CsOH mixture contents showed that the ionization of the Cs 2 IOH(g) molecule led to five different fragment ions, Cs 2 OH + , Cs 2 I + , Cs + , CsOH + and CsI + . This complex ionization pattern was studied in relation with previous assessed values for the vaporization of CsOH and CsI pure compounds in which monomer and dimer molecules are predominant. The equilibrium constant for the reaction CsI(g) + CsOH(g) = Cs 2 IOH(g) was determined and, after modeling the structure of the Cs 2 IOH molecule, the enthalpy of formation was determined using the third law of thermodynamics, as follows: Δ f H°(Cs 2 IOH, g, 298.15 K) = −578 ± 14.7 kJ · mole −1

  10. Gamma spectrometric discrimination of special nuclear materials

    International Nuclear Information System (INIS)

    Dowdall, M.; Mattila, A.; Ramebaeck, H.; Aage, H.K.; Palsson, S.E.

    2012-12-01

    This report presents details pertaining to an exercise conducted as part of the NKS-B programme using synthetic gamma ray spectra to simulate the type of data that may be encountered in the interception of material potentially containing special nuclear materials. A range of scenarios were developed involving sources that may or may not contain special nuclear materials. Gamma spectral data was provided to participants as well as ancillary data and participants were asked, under time constraint, to determine whether or not the data was indicative of circumstances involving special nuclear materials. The situations varied such that different approaches were required in order to obtain the correct result in each context. In the majority of cases participants were able to correctly ascertain whether or not the situations involved special nuclear material. Although fulfilling the primary goal of the exercise, some participants were not in a position to correctly identify with certainty the material involved, Situations in which the smuggled material was being masked by another source proved to be the most challenging for participants. (Author)

  11. Mass spectrometric analysis of monolayer protected nanoparticles

    Science.gov (United States)

    Zhu, Zhengjiang

    Monolayer protected nanoparticles (NPs) include an inorganic core and a monolayer of organic ligands. The wide variety of core materials and the tunable surface monolayers make NPs promising materials for numerous applications. Concerns related to unforeseen human health and environmental impacts of NPs have also been raised. In this thesis, new analytical methods based on mass spectrometry are developed to understand the fate, transport, and biodistributions of NPs in the complex biological systems. A laser desorption/ionization mass spectrometry (LDI-MS) method has been developed to characterize the monolayers on NP surface. LDI-MS allows multiple NPs taken up by cells to be measured and quantified in a multiplexed fashion. The correlations between surface properties of NPs and cellular uptake have also been explored. LDI-MS is further coupled with inductively coupled plasma mass spectrometry (ICP-MS) to quantitatively measure monolayer stability of gold NPs (AuNPs) and quantum dots (QDs), respectively, in live cells. This label-free approach allows correlating monolayer structure and particle size with NP stability in various cellular environments. Finally, uptake, distribution, accumulation, and excretion of NPs in higher order organisms, such as fish and plants, have been investigated to understand the environmental impact of nanomaterials. The results indicate that surface chemistry is a primary determinant. NPs with hydrophilic surfaces are substantially less toxic and present a lower degree of bioaccumulation, making these nanomaterials attractive for sustainable nanotechnology.

  12. Gamma spectrometric discrimination of special nuclear materials

    Energy Technology Data Exchange (ETDEWEB)

    Dowdall, M. [Norwegian Radiation Protection Authority (Norway); Mattila, A. [Radiation and Nuclear Safety Authority, Helsinki (Finland); Ramebaeck, H. [Swedish Defence Research Agency, Stockholm (Sweden); Aage, H.K. [Danish Emergency Management Agency, Birkeroed (Denmark); Palsson, S.E. [Icelandic Radiation Safety Authority, Reykjavik (Iceland)

    2012-12-15

    This report presents details pertaining to an exercise conducted as part of the NKS-B programme using synthetic gamma ray spectra to simulate the type of data that may be encountered in the interception of material potentially containing special nuclear materials. A range of scenarios were developed involving sources that may or may not contain special nuclear materials. Gamma spectral data was provided to participants as well as ancillary data and participants were asked, under time constraint, to determine whether or not the data was indicative of circumstances involving special nuclear materials. The situations varied such that different approaches were required in order to obtain the correct result in each context. In the majority of cases participants were able to correctly ascertain whether or not the situations involved special nuclear material. Although fulfilling the primary goal of the exercise, some participants were not in a position to correctly identify with certainty the material involved, Situations in which the smuggled material was being masked by another source proved to be the most challenging for participants. (Author)

  13. Alpha particle studies during JET DT experiments

    International Nuclear Information System (INIS)

    1999-01-01

    The 1997 DT experiment (DTE1) at the Joint European Torus included studies of the behaviour of alpha particles in high temperature plasmas. Clear alpha particle heating was observed in a series of otherwise similar 10MW hot-ion H-modes by scanning the DT mixture from 0%T to 93%T. Maxima in central temperature and energy content were obtained which corresponded with the maximum in fusion yield. Alfven Eigenmodes (AEs) have been detected in JET, driven by NBI or ICRH fast ions. However, in agreement with theory, no AE activity was observed in DT plasmas which could be attributed to alpha particle drive, except in the afterglow of some Optimised Shear pulses. Ion Cyclotron Emission (ICE) was detected at harmonics of the alpha particle cyclotron frequency at the outer edge of the plasma. The ICE is interpreted as being close to magnetoacoustic cyclotron instability, driven by inverted alpha distributions at the plasma edge. The high-energy neutral particle spectra showed features, which are ascribed to a mixture of alphas, neutralised by helium-like impurities, and deuterons, born from elastic collisions with alpha particles and neutralised by hydrogen-like impurities. The results of all these studies are consistent with classical alpha particle trapping and slowing-down. Future DT experiments will aim to increase alpha particle pressure, so interactions with plasma instabilities can be studied. The measurement of knock-on neutral triton spectra offers a clean way to determine confined alpha densities in these future experiments. (author)

  14. Alpha particle studies during JET DT experiments

    International Nuclear Information System (INIS)

    2001-01-01

    The 1997 DT experiment (DTE1) at the Joint European Torus included studies of the behaviour of alpha particles in high temperature plasmas. Clear alpha particle heating was observed in a series of otherwise similar 10MW hot-ion H-modes by scanning the DT mixture from 0%T to 93%T. Maxima in central temperature and energy content were obtained which corresponded with the maximum in fusion yield. Alfven Eigenmodes (AEs) have been detected in JET, driven by NBI or ICRH fast ions. However, in agreement with theory, no AE activity was observed in DT plasmas which could be attributed to alpha particle drive, except in the afterglow of some Optimised Shear pulses. Ion Cyclotron Emission (ICE) was detected at harmonics of the alpha particle cyclotron frequency at the outer edge of the plasma. The ICE is interpreted as being close to magnetoacoustic cyclotron instability, driven by inverted alpha distributions at the plasma edge. The high-energy neutral particle spectra showed features, which are ascribed to a mixture of alphas, neutralised by helium-like impurities, and deuterons, born from elastic collisions with alpha particles and neutralised by hydrogen-like impurities. The results of all these studies are consistent with classical alpha particle trapping and slowing-down. Future DT experiments will aim to increase alpha particle pressure, so interactions with plasma instabilities can be studied. The measurement of knock-on neutral triton spectra offers a clean way to determine confined alpha densities in these future experiments. (author)

  15. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Jian [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Sengupta, Mrinal K. [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Thermo Fisher Scientific, Dionex Products, 445 Lakeside Drive, Sunnyvale, CA, 94085 (United States); Yuan, Dongxing [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Dasgupta, Purnendu K., E-mail: Dasgupta@uta.edu [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States)

    2014-06-01

    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  16. Workshop on Precision Measurements of $\\alpha_s$

    Energy Technology Data Exchange (ETDEWEB)

    Bethke, Siegfried; /Munich, Max Planck Inst.; Hoang, Andre H.; /Vienna U.; Kluth, Stefan; /Munich, Max Planck Inst.; Schieck, Jochen; /Munich U.; Stewart, Iain W.; Aoki, S.; Beneke, M.; Bethke, S.; Blumlein, J.; Brambilla, N.; Brodsky, S.; /MIT, LNS

    2011-10-01

    These are the proceedings of the Workshop on Precision Measurements of {alpha}{sub s} held at the Max-Planck-Institute for Physics, Munich, February 9-11, 2011. The workshop explored in depth the determination of {alpha}{sub s}(m{sub Z}) in the {ovr MS} scheme from the key categories where high precision measurements are currently being made, including DIS and global PDF fits, {tau}-decays, electro-weak precision observables and Z-decays, event-shapes, and lattice QCD. These proceedings contain a short summary contribution from the speakers, as well as the lists of authors, conveners, participants, and talks.

  17. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solutions

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1999-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solution to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Determination of Uranium 7 Specific Gravity by Pycnometry 15-20 Free Acid by Oxalate Complexation 21-27 Determination of Thorium 28 Determination of Chromium 29 Determination of Molybdenum 30 Halogens Separation by Steam Distillation 31-35 Fluoride by Specific Ion Electrode 36-42 Halogen Distillate Analysis: Chloride, Bromide, and Iodide by Amperometric Microtitrimetry 43 Determination of Chloride and Bromide 44 Determination of Sulfur by X-Ray Fluorescence 45 Sulfate Sulfur by (Photometric) Turbidimetry 46 Phosphorus by the Molybdenum Blue (Photometric) Method 54-61 Silicon by the Molybdenum Blue (Photometric) Method 62-69 Carbon by Persulfate Oxidation-Acid Titrimetry 70 Conversion to U3O8 71-74 Boron by ...

  18. Alpha Shape Topology of the Cosmic Web

    NARCIS (Netherlands)

    Weygaert, Rien van de; Platen, Erwin; Vegter, Gert; Eldering, Bob; Kruithof, Nico

    2010-01-01

    We study the topology of the Megaparsec Cosmic Web on the basis of the Alpha Shapes of the galaxy distribution. The simplicial complexes of the alpha shapes are used to determine the set of Betti numbers (βk, k = 1, . . . , D), which represent a complete characterization of the topology of a

  19. Characterization of HPGe gamma spectrometric detectors systems for Instrumental Neutron Activation Analysis (INAA) at the Colombian Geological Survey

    Energy Technology Data Exchange (ETDEWEB)

    Sierra, O., E-mail: osierra@sgc.gov.co; Parrado, G., E-mail: gparrado@sgc.gov.co; Cañón, Y.; Porras, A.; Alonso, D.; Herrera, D. C.; Peña, M., E-mail: mlpena@sgc.gov.co; Orozco, J. [Colombian Geological Survey, Nuclear Affairs Technical Division, Neutron Activation Analysis Laboratory, Bogota D. C. (Colombia)

    2016-07-07

    This paper presents the progress made by the Neutron Activation Analysis (NAA) laboratory at the Colombian Geological Survey (SGC in its Spanish acronym), towards the characterization of its gamma spectrometric systems for Instrumental Neutron Activation Analysis (INAA), with the aim of introducing corrections to the measurements by variations in sample geometry. Characterization includes the empirical determination of the interaction point of gamma radiation inside the Germanium crystal, through the application of a linear model and the use of a fast Monte Carlo N-Particle (MCNP) software to estimate correction factors for differences in counting efficiency that arise from variations in sample density between samples and standards.

  20. Asymmetric Morita-Baylis-Hillman Reaction: Catalyst Development and Mechanistic Insights Based on Mass Spectrometric Back-Reaction Screening.

    Science.gov (United States)

    Isenegger, Patrick G; Bächle, Florian; Pfaltz, Andreas

    2016-12-05

    An efficient protocol for the evaluation of catalysts for the asymmetric Morita-Baylis-Hillman (MBH) reaction was developed. By mass spectrometric back-reaction screening of quasi-enantiomeric MBH products, an efficient bifunctional phosphine catalyst was identified that outperforms literature-known catalysts in the MBH reaction of methyl acrylate with aldehydes. The close match between the selectivities measured for the forward and back reaction and kinetic measurements provided strong evidence that the aldol step and not the subsequent proton transfer is rate- and enantioselectivity-determining. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Finite size vertex correction to the strong decay of eta sub c and chi sub c states and a determination of alpha sub s (m sub c)

    CERN Document Server

    Ping Rong Gang; Zou Bing Song

    2002-01-01

    The authors calculate the correction to the two-gluon decay width due to the finite extension of the vertex function. The authors obtain the corrected factor to the zero-range vertex gamma = 1.32, gamma = 1.45, gamma= 1.26 for eta sub c , chi sub c sub 0 , and chi sub c sub 2 , respectively. With the decay width GAMMA(eta sub c->2 g) the authors extract the value alpha sub s (m sub c) 0.28 +- 0.05 which agrees with that calculated from the same correction to the process GAMMA(J/psi -> 3 g). This correction to the process GAMMA(eta sub c -> 2 g) is not as large as that to the process GAMMA(J/psi -> 3 g)

  2. Evaluation of accuracy and uncertainty of ELISA assays for the determination of interleukin-4, interleukin-5, interferon-gamma and tumor necrosis factor-alpha

    DEFF Research Database (Denmark)

    Borg, Lone; Kristiansen, Jesper; Christensen, Jytte M

    2002-01-01

    , and robustness. Traceability was ensured by the use of World Health Organization International Standards (WHO IS). An uncertainty budget, which combined the contribution from all known uncertainty components, was established for each cytokine ELISA. The between-run relative analytical standard deviation (RSDA...... for each of the cytokines. The combined relative standard uncertainty (U(result)/C(result)) was 28%, 22-62%, 28% and 24% for the IL-4, IL-5, IFN-gamma and TNF-alpha results, respectively. The major contributions to uncertainty came from the relative analytical standard deviation and from the uncertainty...... by the ELISAs are very limited. The task of evaluating measurement uncertainty would be much easier if producers of international reference standards reported the uncertainty of the value of standards. The model for evaluating uncertainty presented in this paper is applicable to other types of assays...

  3. Design and construction of a system to determine Radon-222 through alpha spectroscopy; Diseno y construccion de un sistema para determinar Radon-222 mediante espectroscopia alfa

    Energy Technology Data Exchange (ETDEWEB)

    Bonifacio M, J. [Universidad Autonoma del Estado de Mexico. Facultad de Quimica. Toluca (Mexico)

    1991-12-31

    The purpose of this work consists in the design a radon-222 gas measurement system utilizing a surface barrier detector with the objective to obtain a more accurate measurement for this isotope through an alpha particle spectrum and so to address as to avoid the activity influence of the descendants of short half-life, which are too beta particles emitters, already other methods it must be correction series to obtain the real value of radon activity. Here are presented the general properties properties of radon, the experimental part description indicating the design to measure the radon-222 gas and its parts, as well as too the standard separation of radium-226 starting from carnotite mineral. Finally, it is presented the results obtained with a discussion about it. (Author) results obtained with a discussion about it. (Author)

  4. Tandem mass spectrometric studies of lanthanum-α-hydroxycarboxylate complexes

    International Nuclear Information System (INIS)

    Kumar, Pranaw; Telmore, V.M.; Jaison, P.G.; Sadhu, Biswajit; Sundararajan, Mahesh

    2017-01-01

    The complexation of lanthanides with hydroxycarboxylic acids is important to understand its separation behavior on liquid chromatography. Electrospray ionization mass spectrometry (ESI-MS) being the soft ionization technique is known for studying the speciation and stoichiometry of metal ligand species. The gentle ionization process of this technique is well suited for transferring the species from solution to gas phase with the retention of stoichiometry. The use of tandem mass spectrometric application has been utilized for studying the path of dissociation. The possible pathways of fragmentation and its geometry have been explained by using the density functional theory (OFT) in the gas phase. Present work describes integrated DFT and tandem mass spectrometric studies of La with α-hydroxyisobutyric acid (HIBA) along with their dissociation studies. In this study, unusual elimination of -CO with the loss of m/z 28 from the complex was observed. This fragmentation resulted the conversion of HIBA into acetone in the fragmented product. The possible fragmentation pathways with the energetic were identified

  5. Mass spectrometric detection of radiocarbon for dating applications

    Energy Technology Data Exchange (ETDEWEB)

    Synal, H.-A., E-mail: synal@phys.ethz.ch [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland); Schulze-Koenig, T.; Seiler, M.; Suter, M.; Wacker, L. [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland)

    2013-01-15

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV {sup 14}C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  6. Mass spectrometric detection of radiocarbon for dating applications

    International Nuclear Information System (INIS)

    Synal, H.-A.; Schulze-König, T.; Seiler, M.; Suter, M.; Wacker, L.

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV 14 C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  7. Mass spectrometric detection of radiocarbon for dating applications

    Science.gov (United States)

    Synal, H.-A.; Schulze-König, T.; Seiler, M.; Suter, M.; Wacker, L.

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV 14C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  8. Spectrometric properties and radiation damage of BGO crystals

    Science.gov (United States)

    Kim, Gen C.; Gasanov, Eldar M.

    1997-07-01

    Spectrometric properties, such as light output, energy resolution BGO crystals before and after (superscript 60)Co gamma-ray (dose 10(superscript 4) - 10(superscript 6) R) and neutron irradiation (fluence 10(superscript 14) cm(superscript -2)) are investigated. Condition for degradation of spectrometric properties and their recovering after irradiation are studied. The energy spectrum of the photons emitted from BGO crystals irradiated with neutron fluence contains the long living background peak which is caused by self-irradiation with radioactive isotopes produced in the crystals. The defect production was studied in crystals under the high dose gamma-irradiation with (superscript 60)Co isotope. It was found that after doses above 10(superscript 8) R the color center at 365 nm and doses higher than 10(superscript 9) R a wide absorption band in the region of 300 - 350 nm occur. Comparison of these results with those of reactor irradiation has shown that under the high dose gamma-irradiation the structure defect production takes place.

  9. Elimination of alpha-gal xenoreactive epitope: alpha-galactosidase treatment of porcine heart valves.

    Science.gov (United States)

    Choi, Sun-Young; Jeong, Hee-Jin; Lim, Hong-Gook; Park, Seong-Sik; Kim, Soo-Hwan; Kim, Yong Jin

    2012-05-01

    Porcine heart valves are among the most widely used tissue valves in clinical heart valve implantation. However, immunologic responses have been implicated as potential causes of the limited durability of xenograft heart valves. The study aim was to determine the effectiveness of alpha-galactosidase treatment used to degrade the major xenoreactive antigens found in xenograft heart valves. Fresh porcine heart valves and pericardium treated with alpha-galactosidase were studied to evaluate the xenoreactive galactose (alpha1,3) galactose (alpha-gal) antigen. Removal of the alpha-gal epitope from the porcine heart valve was monitored via 3,3'-diaminobenzidine staining intensity, while the removal of alpha-gal from N-glycans on porcine heart valves treated with recombinant alpha-galactosidase was determined either qualitatively or quantitatively by mass fingerprinting using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). The porcine pericardium was used for monitoring the change in mechanical properties after alpha-galactosidase treatment. In addition, the biomechanical modification property of collagen fiber rearrangement on tissue was assessed using transmission electron microscopy (TEM). Following a 24-h incubation at pH 7.2, 4 degrees C, employing 0.1 U/ml of Bacteroides thetaiotaomicron-derived recombinant alpha-galactosidase, the enzyme effectively removed the alpha-gal epitopes expressed on porcine heart valves. The identification type of alpha-gal N-glycan on fresh aortic valve, aortic wall, pulmonary valve, and pulmonary wall was 7.1%, 10.3%, 6% and 8%, respectively. In the presence of alpha-galactosidase treatment, alpha-gal-containing N-glycans were converted into alpha-gal-negative N-glycans. Likewise, alpha-gal-containing N-glycans were not detected when MALDI-TOF MS quantitative analysis was used. Furthermore, no significant difference was observed in the mechanical properties and findings from TEM in alpha

  10. Determination of curium-242 by α spectrometry and mass spectrometry in spent nuclear fuels

    International Nuclear Information System (INIS)

    Chartier, F.; Aubert, M.; Degros, J.P.; Duda, J.M.

    2004-01-01

    Curium-242 is a particularly important isotope in spent nuclear fuels due to its contribution to the residual power and also of its radioactive decrease chain. The determination of its content is therefore essential to improve the knowledge of the nuclear data. According to the nature and the cooling time of the spent fuel, the 242 Cm content can be lower than the detection limit of the classically used mass spectrometric techniques. To overcome this limitation, alpha spectrometry can be advantageously used for this radionuclide of short period (T = 162.9 days). From dilute solutions of MOX fuels of short time of cooling and for which the content of 242 Cm is about a few tens of pg, the development of different successive chemical separations permitted to get sufficiently pure curium fractions to perform curium isotopic analysis by thermal ionization mass spectrometry but also the determination of the 242 Cm/ 244 Cm ratio by alpha spectrometry. The agreement on the ratios determined by the two techniques has allowed to spread the measure by alpha spectrometry to a UOX fuel of content in 242 Cm even lower. The association of the 242 Cm/ 244 Cm ratio measurement with the 244 Cm/ 238 U ratio obtained by thermal ionization mass spectrometry and isotope dilution, with a 248 Cm/ 233 U spike, permits to know the content in curium-242 in relation to uranium-238 which is used as a reference in the fuel. (author)

  11. Determination of uranium in liquid samples

    International Nuclear Information System (INIS)

    Macefat, Martina R.; Grahek, Zeljko; Ivsic, Astrid G.

    2008-01-01

    Full text: Uranium is a natural occurring radionuclide and the first member of natural radioactive chains which makes its determination in natural materials interesting from geochemical and radioecological aspect. It can be quantitatively determined as element and/or its radioisotopes by different spectrometric methods (ICP-MS, spectrophotometry, alpha spectrometry). It is necessary to develop inexpensive, rapid and sensitive methods for the routine analysis. Therefore, in this paper, development of a new method for the isolation of uranium from liquid samples and subsequent determination by spectrophotometry and ICP-MS will be described. It is possible to isolate uranium from drinking and seawater using extraction chromatography or mixed solvent ion exchange. Uranium can be strongly bound on the TRU extraction chromatographic resin from nitric acid (chemical recovery is 100%) and can be separated from other interfering elements, while separation from thorium, which can be also strongly bound on this resin, is possible with hydrochloric acid. It is also possible to separate uranium from thorium on the anion exchanger Amberlite CG-400 (NO 3 - form) because uranium is much more weakly bound on this exchanger from alcoholic solutions of nitric acid. After the separation uranium is determined by ICP-MS and by spectrophotometric method with arsenazo III (λ max =652 nm). Developed method enables selection of the optimal mode of isolation for the given purposes. (author)

  12. Implantation of alpha spectrometry methodology for the determination of U and Th isotopes in igneous rocks: application to the study of radioactive desequilibrium in the Trindade Island, Brazil

    International Nuclear Information System (INIS)

    Santos, Rosana Nunes dos

    2001-01-01

    This work describes the implementation of experimental procedures for alpha spectrometry measurement of 238 U, 234 U and 230 Th activities in silicates. The best experimental conditions were defined using 233 U, 232 U and 229 Th radioactive tracers and simulating the usual conditions found in processing silicates. The chemical procedures consists of the following steps: radioactive tracer addition and sample dissolution by acid digestion, U and Th pre-concentration by co-precipitation, element separation and purification by ion exchange chromatography and electrodeposition in inox steel disks. In order to evaluate its effectiveness, the procedure was applied to the Brazilian geological standards BB-1 (basalt) and GB-1 (granite). The obtained chemical yields for uranium and thorium are of about 60% and 70%, respectively, for both matrices. The described methodology furnishes activity measurements with less than 4% relative precision and accuracies of about 1%, that are essential for petrogenetic applications. The 238 U and 232 Th series disequilibrium conditions were investigated by alpha spectrometry, together with neutron activation analysis and natural gamma-ray spectrometry. 234 U/ 238 U, 238 U/ 232 Th and 230 Th/ 232 Th activity ratios and the 234 Th, 214 Pb, 214 Bi, 235 U, 228 Ac, 212 Pb, 212 Bi and 208 Tl specific activities were obtained. These results were interpreted with the help of additional constraints given by the larger and smaller elements concentrations, measured by X-ray fluorescence. The 232 Th series is in secular radioactive equilibrium in all analysed samples. In the case of the 238 U series, the equilibrium condition was verified, as expected, in the oldest rocks from the Trindade Island (Trindade Complex and Desejado Sequence). On the other hand, the results show that, in the samples from the last three volcanic episodes in the island (Morro Vermelho Formation, Valado Formation and Vulcao do Paredao), the 230 Th and 238 U are not in

  13. Opposing actions of the progesterone metabolites, 5alpha-dihydroprogesterone (5alphaP) and 3alpha-dihydroprogesterone (3alphaHP) on mitosis, apoptosis, and expression of Bcl-2, Bax and p21 in human breast cell lines.

    Science.gov (United States)

    Wiebe, John P; Beausoleil, Michel; Zhang, Guihua; Cialacu, Valentin

    2010-01-01

    Previous studies have shown that breast tissues and breast cell lines convert progesterone (P) to 5alpha-dihydroprogesterone (5alphaP) and 3alpha-dihydroprogesterone (3alphaHP) and that 3alphaHP suppresses, whereas 5alphaP promotes, cell proliferation and detachment. The objectives of the current studies were to determine if the 5alphaP- and 3alphaHP-induced changes in cell numbers are due to altered rates of mitosis and/or apoptosis, and if 3alphaHP and 5alphaP act on tumorigenic and non-tumorigenic cells, regardless of estrogen (E) and P receptor status. The studies were conducted on tumorigenic (MCF-7, MDA-MB-231, T47D) and non-tumorigenic (MCF-10A) human breast cell lines, employing several methods to assess the effects of the hormones on cell proliferation, mitosis, apoptosis and expression of Bcl-2, Bax and p21. In all four cell lines, 5alphaP increased, whereas 3alphaHP decreased cell numbers, [(3)H]thymidine uptake and mitotic index. Apoptosis was stimulated by 3alphaHP and suppressed by 5alphaP. 5alphaP resulted in increases in Bcl-2/Bax ratio, indicating decreased apoptosis; 3alphaHP resulted in decreases in Bcl-2/Bax ratio, indicating increased apoptosis. The effects of either 3alphaHP or 5alphaP on cell numbers, [(3)H]thymidine uptake, mitosis, apoptosis, and Bcl-2/Bax ratio, were abrogated when cells were treated simultaneously with both hormones. The expression of p21 was increased by 3alphaHP, and was unaffected by 5alphaP. The results provide the first evidence that 5alphaP stimulates mitosis and suppresses apoptosis, whereas 3alphaHP inhibits mitosis and stimulates apoptosis. The opposing effects of 5alphaP and 3alphaHP were observed in all four breast cell lines examined and the data suggest that all breast cancers (estrogen-responsive and unresponsive) might be suppressed by blocking 5alphaP formation and/or increasing 3alphaHP. The findings further support the hypothesis that progesterone metabolites are key regulatory hormones and that changes

  14. Electrospun polydimethylsiloxane/polyacrylonitrile/titanium dioxide nanofibers as a new coating for determination of alpha-linolenic acid in milk by direct immersion-solid phase nanoextraction.

    Science.gov (United States)

    Sadeghi, Sahar; Mollahosseini, Afsaneh

    2018-01-15

    In this study, polydimethylsiloxane/polyacrylonitrile/titanium dioxide (PDMS/PAN/TiO 2 ) nanofibers were synthesized via electrospinning method to extract and quantify alpha-linolenic acid (ALA, C18:3), as a model analyte, in milk by direct immersion-solid phase nanoextraction (DI-SPNE) with gas chromatography-flame ionization detector (GC-FID). The affecting factors on the electrospinning process such as, PDMS concentration, amount of TiO 2 nanoparticles (NPs), voltage, and electrospinning distance were optimized using Taguchi's orthogonal design. The SPNE experimental conditions such as, extraction time, agitation rate, pH and salt concentration, were also optimized using response surface methodology (RSM) based on a central composite design (CCD). Under optimized conditions, the resulting calibration curve was linear in the range of 1-4000ngmL -1 with R 2 =0.998. The intraday, interday, and fiber-to-fiber repeatability were calculated and the corresponding relative standard deviation was less than 9% in all the cases. The limit of detection and limit of quantification were found to be 0.2 and 0.6ngmL -1 , respectively. Omega-3 enriched milk was used as a real sample and the value of relative recoveries were measured to be in the range of 92-106%. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. The measurement of $\\alpha_s$ from event shapes with the DELPHI detector at the highest LEP energies

    CERN Document Server

    Abdallah, J; Adam, W; Adzic, P; Albrecht, T; Alderweireld, T; Alemany-Fernandez, R; Allmendinger, T; Allport, P P; Amaldi, Ugo; Amapane, N; Amato, S; Anashkin, E; Andreazza, A; Andringa, S; Anjos, N; Antilogus, P; Apel, W D; Arnoud, Y; Ask, S; Åsman, B; Augustin, J E; Augustinus, A; Baillon, Paul; Ballestrero, A; Bambade, P; Barbier, R; Bardin, Dimitri Yuri; Barker, G; Baroncelli, A; Battaglia, Marco; Baubillier, M; Becks, K H; Begalli, M; Behrmann, A; Ben-Haim, E; Benekos, N C; Benvenuti, Alberto C; Bérat, C; Berggren, M; Berntzon, L; Bertrand, D; Besançon, M; Besson, N; Bloch, D; Blom, M; Bluj, M; Bonesini, M; Boonekamp, M; Booth, P S L; Borisov, G; Botner, O; Bouquet, B; Bowcock, T J V; Boyko, I; Bracko, M; Brenner, R; Brodet, E; Brückman, P; Brunet, J M; Bugge, L; Buschmann, P; Calvi, M; Camporesi, T; Canale, V; Carena, F; Castro, N; Cavallo, F R; Chapkin, M M; Charpentier, P; Checchia, P; Chierici, R; Shlyapnikov, P; Chudoba, J; Chung, S U; Cieslik, K; Collins, P; Contri, R; Cosme, G; Cossutti, F; Costa, M J; Crennell, D J; Cuevas-Maestro, J; D'Hondt, J; Dalmau, J; Da Silva, T; Da Silva, W; Della Ricca, G; De Angelis, A; de Boer, Wim; De Clercq, C; De Lotto, B; De Maria, N; De Min, A; De Paula, L S; Di Ciaccio, Lucia; Di Simone, A; Doroba, K; Drees, J; Dris, M; Eigen, G; Ekelöf, T J C; Ellert, M; Elsing, M; Espirito-Santo, M C; Fanourakis, G K; Fassouliotis, D; Feindt, M; Fernández, J; Ferrer, A; Ferro, F; Flagmeyer, U; Föth, H; Fokitis, E; Fulda-Quenzer, F; Fuster, J A; Gandelman, M; García, C; Gavillet, P; Gazis, E N; Gokieli, R; Golob, B; Gómez-Ceballos, G; Gonçalves, P; Graziani, E; Grosdidier, G; Grzelak, K; Guy, J; Haag, C; Hallgren, A; Hamacher, K; Hamilton, K; Haug, S; Hauler, F; Hedberg, V; Hennecke, M; Herr, H; Hoffman, J; Holmgren, S O; Holt, P J; Houlden, M A; Hultqvist, K; Jackson, J N; Jarlskog, G; Jarry, P; Jeans, D; Johansson, E K; Johansson, P D; Jonsson, P; Joram, C; Jungermann, L; Kapusta, F; Katsanevas, S; Katsoufis, E C; Kernel, G; Kersevan, Borut P; Kerzel, U; Kiiskinen, A P; King, B T; Kjaer, N J; Kluit, P; Kokkinias, P; Kourkoumelis, C; Kuznetsov, O; Krumshtein, Z; Kucharczyk, M; Lamsa, J; Leder, G; Ledroit, F; Leinonen, L; Leitner, R; Lemonne, J; Lepeltier, V; Lesiak, T; Liebig, W; Liko, D; Lipniacka, A; Lopes, J H; López, J M; Loukas, D; Lutz, P; Lyons, L; MacNaughton, J; Malek, A; Maltezos, S; Mandl, F; Marco, J; Marco, R; Maréchal, B; Margoni, M; Marin, J C; Mariotti, C; Markou, A; Martínez-Rivero, C; Masik, J; Mastroyiannopoulos, N; Matorras, F; Matteuzzi, C; Mazzucato, F; Mazzucato, M; McNulty, R; Meroni, C; Migliore, E; Mitaroff, W A; Mjörnmark, U; Moa, T; Moch, M; Mönig, K; Monge, R; Montenegro, J; Moraes, D; Moreno, S; Morettini, P; Müller, U; Münich, K; Mulders, M; Mundim, L M; Murray, W; Muryn, B; Myatt, Gerald; Myklebust, T; Nassiakou, M; Navarria, Francesco Luigi; Nawrocki, K; Nicolaidou, R; Nikolenko, M; Oblakowska-Mucha, A; Obraztsov, V F; Olshevskii, A G; Onofre, A; Orava, Risto; Österberg, K; Ouraou, A; Oyanguren, A; Paganoni, M; Paiano, S; Palacios, J P; Palka, H; Papadopoulou, T D; Pape, L; Parkes, C; Parodi, F; Parzefall, U; Passeri, A; Passon, O; Peralta, L; Perepelitsa, V F; Perrotta, A; Petrolini, A; Piedra, J; Pieri, L; Pierre, F; Pimenta, M; Piotto, E; Podobnik, T; Poireau, V; Pol, M E; Polok, G; Poropat, P; Pozdnyakov, V; Pukhaeva, N; Pullia, Antonio; Rames, J; Ramler, L; Read, A; Rebecchi, P; Rehn, J; Reid, D; Reinhardt, R; Renton, P B; Richard, F; Rídky, J; Rivero, M; Rodríguez, D; Romero, A; Ronchese, P; Roudeau, Patrick; Rovelli, T; Ruhlmann-Kleider, V; Ryabtchikov, D; Sadovskii, A; Salmi, L; Salt, J; Savoy-Navarro, A; Schwickerath, U; Segar, A; Sekulin, R L; Siebel, M; Sissakian, A N; Smadja, G; Smirnova, O G; Sokolov, A; Sopczak, A; Sosnowski, R; Spassoff, Tz; Stanitzki, M; Stocchi, A; Strauss, J; Stugu, B; Szczekowski, M; Szeptycka, M; Szumlak, T; Tabarelli de Fatis, T; Taffard, A C; Tegenfeldt, F; Timmermans, J; Tkatchev, L G; Tobin, M; Todorovova, S; Tomé, B; Tonazzo, A; Tortosa, P; Travnicek, P; Treille, D; Tristram, G; Trochimczuk, M; Troncon, C; Turluer, M L; Tyapkin, I A; Tyapkin, P; Tzamarias, S; Uvarov, V; Valenti, G; van Dam, P; Van Eldik, J; Van Lysebetten, A; Van Remortel, N; Van Vulpen, I B; Vegni, G; Veloso, F; Venus, W A; Verdier, P; Verzi, V; Vilanova, D; Vitale, L; Vrba, V; Wahlen, H; Washbrook, A J; Weiser, C; Wicke, D; Wickens, J H; Wilkinson, G; Winter, M; Witek, M; Yushchenko, O P; Zalewska-Bak, A; Zalewski, Piotr; Zavrtanik, D; Zhuravlov, V; Zimin, N I; Zinchenko, A I; Zupan, M

    2004-01-01

    Hadronic event shape distributions are determined from data in e+e- collisions between 183 and 207 GeV. From these the strong coupling alpha_s is extracted in O(alpha_s^2), NLLA and matched O(alpha_s^2)+NLLA theory. Hadronisation corrections evaluated with fragmentation model generators as well as an analytical power ansatz are applied. Comparing these measurements to those obtained at and around M_Z allows a combined measurement of alpha_s from all DELPHI data and a test of the energy dependence of the strong coupling.

  16. 5th colloquium on atomic spectrometric trace analysis

    International Nuclear Information System (INIS)

    Welz, B.

    1989-01-01

    This book deals with apparatus, use-oriented and theoretical aspects of trace analysis and spectroscopy. General articles are concerned with the analysis of environmentally relevant samples; a comparison of modern spectroscopic techniques, the coupling of hydride production, chromatography and spectrometry; chemical modifiers for graphite tube furnace atomic absorption spectroscopy (AAS), and possible applications of flow injection to atomic spectrometric trace analysis - one of the outstanding subjects of the colloquium. About one quarter of the 85 contributions deals with new techniques including flow injection. Other priority subjects are the theory and application of graphite tube furnace AAS, and a comparison between different dissolution methods and direct solid analysis. Medicine and toxicology, analysis of biological materials and environmentally relevant samples are in the foreground of use-oriented papers. (orig./BBR) [de

  17. Advances in Mass Spectrometric Tools for Probing Neuropeptides

    Science.gov (United States)

    Buchberger, Amanda; Yu, Qing; Li, Lingjun

    2015-07-01

    Neuropeptides are important mediators in the functionality of the brain and other neurological organs. Because neuropeptides exist in a wide range of concentrations, appropriate characterization methods are needed to provide dynamic, chemical, and spatial information. Mass spectrometry and compatible tools have been a popular choice in analyzing neuropeptides. There have been several advances and challenges, both of which are the focus of this review. Discussions range from sample collection to bioinformatic tools, although avenues such as quantitation and imaging are included. Further development of the presented methods for neuropeptidomic mass spectrometric analysis is inevitable, which will lead to a further understanding of the complex interplay of neuropeptides and other signaling molecules in the nervous system.

  18. Mass spectrometric methods for trace analysis of metals

    International Nuclear Information System (INIS)

    Bahr, U.; Schulten, H.R.

    1981-01-01

    A brief outline is given of the principles of mass spectrometry (MS) and the fundamentals of qualitative and quantitative mass spectrometric analysis emphasizing recent developments and results. Classical methods of the analysis of solids, i.e. spark-source MS and thermal ionization MS, as well as recent methods of metal analysis are described. Focal points in this survey of recently developed techniques include secondary ion MS, laser probe MS, plasma ion source MS, gas discharge MS and field desorption MS. Here, a more detailed description is given and the merits of these emerging methods are discussed more explicitly. In particular, the results of the field desorption techniques in elemental analyses are reviewed and critically evaluated

  19. Calculus of radiolytic products generation in water due to alpha radiation. Determination of the spent nuclear fuels matrix alteration rate Determination of velocity of spent fuel matrix; Calculo de la generacion de productos radioliticos en agua por radiacion {alpha}. Determinacion de la velocidad de alteracion de la matriz del combustible nuclear gastado

    Energy Technology Data Exchange (ETDEWEB)

    Quinones, J.; Serrano, J.; Diaz Arocas, P.; Rodriguez Almazan, J. L. [Ciemat. Madrid (Spain); Bruno, J.; Cera, E.; Merino, J.; Esteban, J. A.; Martinez-Esparza, A. [Enresa. Madrid (Spain)

    2000-07-01

    The generation of radiolytic products as a result of alpha radiation in the surface of the spent fuel is a key process in order to understand how the it becomes degraded in repository conditions. The present work has established a radiolytic model based on a set of reactions involving fuel oxidation-dissolution and radiolytic products recombination. It also includes the decrease of the dose rates as the main alpha emitters decay away. Four cases, with varying parameters of the system, have been assessed. The results show a decrease in both the concentration of the radiolytic products in the gap water and the degradation of the fuel matrix. It has been estimated that in the period of the evaluation (10''6 years) up to 52% of the pellet is altered in the conservative cases, whereas only 11% is altered in the realistic cases. No significant differences were observed when the carbonates reactions were included in the system. (Author)

  20. A comparative study of pulsed-laser fluorimetric and radiochemical determination of uranium in a urinalysis program

    International Nuclear Information System (INIS)

    Warner, D.A.

    1985-01-01

    A method utilizing a pulsed-laser fluorimeter for the determination of trace levels of uranium in urine is evaluated as an alternative to the radiochemical separation and alpha spectrometric measurement of the element. The pulsed-laser fluorimeter is a compact electro-optical instrument which measures the fluorescence of a uranyl complex formed by adding an analytical reagent to the sample. Fluorescence of the uranyl complex is the result of ultraviolet excitation generated by a nitrogen laser tube. Sample preparation requires the complete oxidation of all organics which could contribute to the fluorescence signal. Results from the analysis of pooled and artificial urine by both methods are compared. The accuracy of each method is comparable for those experiments. Additional work is in progress to determine the feasibility of using the pulsed-laser fluorimetric method in a urinalysis feasibility of using the pulsed-laser fluorimetric method in a urinalysis program. The advantages and disadvantages of each method are reviewed

  1. Determination of radium in water

    International Nuclear Information System (INIS)

    Hohorst, F.A.; Huntley, M.W.; Hartenstein, S.D.

    1995-10-01

    These detailed work instructions (DWIs) are tailored for the analysis of radium-226 and radium-228 in drinking water supplies from ground water and surface water sources and composites derived from them. The instructions have been adapted from several sources, including a draft EPA method. One objective was to minimize the generation of mixed wastes. Quantitative determinations of actinium-228 are made at 911 keV. The minimum detection level (MDL) for the gamma spectrometric measurements at this energy vary with matrix, volume, geometry, detector, background, and counting statistics. The range of MDL's for current detectors is 0.07 to 0.5 Bq/sample. Quantitative determinations of radium-226 are made by counting the high energy alpha particles which radium-226 progeny emit using liquid scintillation counting (LSC). The minimum detectable activity (MDA) is 3.8 E-3 Bq/sample. The maximum concentration which may be counted on available instruments without dilution is about 2 E + 5 Bq/sample. Typically, this determination of radium in a 2 L sample has a yield of 80%. If radium-228 is determined using a 16 h count after 50 h grow-in, the typical MDL is 1 E-9 to 8 E-9 μCi/mL (1 to 8 pCi/L). If radium-226 is determined using a 2.5 h count after 150 h grow-in, the typical MDA is about 1 E-10 μCi/mL (0. 1 pCi/L)

  2. Determination of radium in water

    Energy Technology Data Exchange (ETDEWEB)

    Hohorst, F.A.; Huntley, M.W.; Hartenstein, S.D.

    1995-10-01

    These detailed work instructions (DWIs) are tailored for the analysis of radium-226 and radium-228 in drinking water supplies from ground water and surface water sources and composites derived from them. The instructions have been adapted from several sources, including a draft EPA method. One objective was to minimize the generation of mixed wastes. Quantitative determinations of actinium-228 are made at 911 keV. The minimum detection level (MDL) for the gamma spectrometric measurements at this energy vary with matrix, volume, geometry, detector, background, and counting statistics. The range of MDL`s for current detectors is 0.07 to 0.5 Bq/sample. Quantitative determinations of radium-226 are made by counting the high energy alpha particles which radium-226 progeny emit using liquid scintillation counting (LSC). The minimum detectable activity (MDA) is 3.8 E-3 Bq/sample. The maximum concentration which may be counted on available instruments without dilution is about 2 E + 5 Bq/sample. Typically, this determination of radium in a 2 L sample has a yield of 80%. If radium-228 is determined using a 16 h count after 50 h grow-in, the typical MDL is 1 E-9 to 8 E-9 {mu}Ci/mL (1 to 8 pCi/L). If radium-226 is determined using a 2.5 h count after 150 h grow-in, the typical MDA is about 1 E-10 {mu}Ci/mL (0. 1 pCi/L).

  3. Lyman Alpha Control

    CERN Document Server

    Nielsen, Daniel Stefaniak

    2015-01-01

    This document gives an overview of how to operate the Lyman Alpha Control application written in LabVIEW along with things to watch out for. Overview of the LabVIEW code itself as well as the physical wiring of and connections from/to the NI PCI-6229 DAQ box is also included. The Lyman Alpha Control application is the interface between the ALPHA sequencer and the HighFinesse Wavelength Meter as well as the Lyman Alpha laser setup. The application measures the wavelength of the output light from the Lyman Alpha cavity through the Wavelength Meter. The application can use the Wavelength Meter’s PID capabilities to stabilize the Lyman Alpha laser output as well as switch between up to three frequencies.

  4. New ALPHA-2 magnet

    CERN Multimedia

    Anaïs Schaeffer

    2012-01-01

    On 21 June, members of the ALPHA collaboration celebrated the handover of the first solenoid designed for the ALPHA-2 experiment. The magnet has since been successfully installed and is working well.   Khalid Mansoor, Sumera Yamin and Jeffrey Hangst in front of the new ALPHA-2 solenoid. “This was the first of three identical solenoids that will be installed between now and September, as the rest of the ALPHA-2 device is installed and commissioned,” explains ALPHA spokesperson Jeffrey Hangst. “These magnets are designed to allow us to transfer particles - antiprotons, electrons and positrons - between various parts of the new ALPHA-2 device by controlling the transverse size of the particle bunch that is being transferred.” Sumera Yamin and Khalid Mansoor, two Pakistani scientists from the National Centre for Physics in Islamabad, came to CERN in February specifically to design and manufacture these magnets. “We had the chance to work on act...

  5. Measurements of $\\alpha_s$ in $pp$ Collisions at the LHC

    CERN Document Server

    Warburton, Andreas; The ATLAS collaboration

    2015-01-01

    The coupling of the strong force, $\\alpha_s$, is deemed to be a fundamental parameter of Nature, and, beyond the quark masses, constitutes the only free parameter in the QCD Lagrangian. Provided is an overview of CERN Large Hadron Collider (LHC) measurements of $\\alpha_s(M_Z)$ evaluated at the $Z$-boson mass and of the running of $\\alpha_s(Q)$ as a function of energy-momentum transfer $Q$. The measurements were performed by the ATLAS and CMS Collaborations using proton-proton ($pp$) collisions with centre-of-mass energies of 7 TeV and data samples with time-integrated luminosities of up to 5 fb$^{-1}$. Four different categories of observable were used in the described extractions of $\\alpha_s$: inclusive jet cross sections, 3-jet to 2-jet inclusive cross-section ratios, 3-jet mass cross sections, and top-quark pair production cross sections. These results, which include the first NNLO measurement of $\\alpha_s$ at a hadron collider and the first determinations of $\\alpha_s$ at energy scales above 1 TeV, are co...

  6. Comparison of two ultra-sensitive methods for the determination of 232Th by recovery corrected pre-concentration radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Glover, S.E.; Qu, H.; LaMont, S.P.; Grimm, C.A.; Filby, R.H.

    2001-01-01

    The determination of isotopic thorium by alpha spectrometric methods is a routine practice for bioassay and environmental measurement programs. Alpha-spectrometry has excellent detection limits (by mass) for all isotopes of thorium except 232 Th due to its extremely long half-life. Improvements in the detection limit an sensitivity over previously reported methods of pre-concentration neutron activation analysis (PCNAA) for the recovery corrected, isotopic determination of thorium in various matrices is discussed. Following irradiation, the samples were dissolved, 231 Pa added as a tracer, and Pa isolated by two different methods and compared (extraction chromatography and anion exchange chromatography) followed by alpha spectrometry for recovery correction. Ion exchange chromatography was found to be superior for this application at this time, principally for reliability. The detection limit for 232 Th of 3.5 x 10 -7 Bq is almost three orders of magnitude lower than for alpha spectrometry using the PCRNAA method and one order of magnitude below previously reported PCNAA methods. (author)

  7. Improved peak shape fitting in alpha spectra.

    Science.gov (United States)

    Pommé, S; Caro Marroyo, B

    2015-02-01

    Peak overlap is a recurrent issue in alpha-particle spectrometry, not only in routine analyses but also in the high-resolution spectra from which reference values for alpha emission probabilities are derived. In this work, improved peak shape formulae are presented for the deconvolution of alpha-particle spectra. They have been implemented as fit functions in a spreadsheet application and optimum fit parameters were searched with built-in optimisation routines. Deconvolution results are shown for a few challenging spectra with high statistical precision. The algorithm outperforms the best available routines for high-resolution spectrometry, which may facilitate a more reliable determination of alpha emission probabilities in the future. It is also applicable to alpha spectra with inferior energy resolution. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

  8. Energy dependence of event shapes and of $\\alpha_s$ at LEP 2

    CERN Document Server

    Abreu, P; Adye, T; Adzic, P; Albrecht, Z; Alderweireld, T; Alekseev, G D; Alemany, R; Allmendinger, T; Allport, P P; Almehed, S; Amaldi, Ugo; Amapane, N; Amato, S; Anassontzis, E G; Andersson, P; Andreazza, A; Andringa, S; Antilogus, P; Apel, W D; Arnoud, Y; Åsman, B; Augustin, J E; Augustinus, A; Baillon, Paul; Bambade, P; Barão, F; Barbiellini, Guido; Barbier, R; Bardin, Dimitri Yuri; Barker, G; Baroncelli, A; Battaglia, Marco; Baubillier, M; Becks, K H; Begalli, M; Behrmann, A; Beillière, P; Belokopytov, Yu A; Belous, K S; Benekos, N C; Benvenuti, Alberto C; Bérat, C; Berggren, M; Bertini, D; Bertrand, D; Besançon, M; Bianchi, F; Bigi, M; Bilenky, S M; Bizouard, M A; Bloch, D; Blom, H M; Bonesini, M; Bonivento, W; Boonekamp, M; Booth, P S L; Borgland, A W; Borisov, G; Bosio, C; Botner, O; Boudinov, E; Bouquet, B; Bourdarios, C; Bowcock, T J V; Boyko, I; Bozovic, I; Bozzo, M; Branchini, P; Brenke, T; Brenner, R A; Brückman, P; Brunet, J M; Bugge, L; Buran, T; Burgsmüller, T; Buschbeck, Brigitte; Buschmann, P; Cabrera, S; Caccia, M; Calvi, M; Camporesi, T; Canale, V; Carena, F; Carroll, L; Caso, Carlo; Castillo-Gimenez, M V; Cattai, A; Cavallo, F R; Chabaud, V; Chapkin, M M; Charpentier, P; Chaussard, L; Checchia, P; Chelkov, G A; Chierici, R; Chliapnikov, P V; Chochula, P; Chorowicz, V; Chudoba, J; Cieslik, K; Collins, P; Contri, R; Cortina, E; Cosme, G; Cossutti, F; Cowell, J H; Crawley, H B; Crennell, D J; Crépé, S; Crosetti, G; Cuevas-Maestro, J; Czellar, S; Davenport, Martyn; Da Silva, W; Deghorain, A; Della Ricca, G; Delpierre, P A; Demaria, N; De Angelis, A; de Boer, Wim; De Clercq, C; De Lotto, B; De Min, A; De Paula, L S; Dijkstra, H; Di Ciaccio, Lucia; Dolbeau, J; Doroba, K; Dracos, M; Drees, J; Dris, M; Duperrin, A; Durand, J D; Eigen, G; Ekelöf, T J C; Ekspong, Gösta; Ellert, M; Elsing, M; Engel, J P; Erzen, B; Espirito-Santo, M C; Falk, E; Fanourakis, G K; Fassouliotis, D; Fayot, J; Feindt, Michael; Fenyuk, A; Ferrari, P; Ferrer, A; Ferrer-Ribas, E; Ferro, F; Fichet, S; Firestone, A; Flagmeyer, U; Föth, H; Fokitis, E; Fontanelli, F; Franek, B J; Frodesen, A G; Frühwirth, R; Fulda-Quenzer, F; Fuster, J A; Galloni, A; Gamba, D; Gamblin, S; Gandelman, M; García, C; Gaspar, C; Gaspar, M; Gasparini, U; Gavillet, P; Gazis, E N; Gelé, D; Ghodbane, N; Gil, I; Glege, F; Gokieli, R; Golob, B; Gómez-Ceballos, G; Gonçalves, P; González-Caballero, I; Gopal, Gian P; Gorn, L; Górski, M; Guz, Yu; Gracco, Valerio; Grahl, J; Graziani, E; Green, C; Grimm, H J; Gris, P; Grosdidier, G; Grzelak, K; Günther, M; Guy, J; Hahn, F; Hahn, S; Haider, S; Hallgren, A; Hamacher, K; Hansen, J; Harris, F J; Hedberg, V; Heising, S; Hernández, J J; Herquet, P; Herr, H; Hessing, T L; Heuser, J M; Higón, E; Holmgren, S O; Holt, P J; Hoorelbeke, S; Houlden, M A; Hrubec, Josef; Huet, K; Hughes, G J; Hultqvist, K; Jackson, J N; Jacobsson, R; Jalocha, P; Janik, R; Jarlskog, C; Jarlskog, G; Jarry, P; Jean-Marie, B; Johansson, E K; Jönsson, P E; Joram, C; Juillot, P; Kapusta, F; Karafasoulis, K; Katsanevas, S; Katsoufis, E C; Keränen, R; Kersevan, Borut P; Khomenko, B A; Khovanskii, N N; Kiiskinen, A P; King, B J; Kinvig, A; Kjaer, N J; Klapp, O; Klein, H; Kluit, P M; Kokkinias, P; Koratzinos, M; Kostyukhin, V; Kourkoumelis, C; Kuznetsov, O; Krammer, Manfred; Kriznic, E; Krstic, J; Krumshtein, Z; Kubinec, P; Kurowska, J; Kurvinen, K L; Lamsa, J; Lane, D W; Langefeld, P; Lapin, V; Laugier, J P; Lauhakangas, R; Leder, Gerhard; Ledroit, F; Lefébure, V; Leinonen, L; Leisos, A; Leitner, R; Lemonne, J; Lenzen, Georg; Lepeltier, V; Lesiak, T; Lethuillier, M; Libby, J; Liko, D; Lipniacka, A; Lippi, I; Lörstad, B; Loken, J G; Lopes, J H; López, J M; López-Fernandez, R; Loukas, D; Lutz, P; Lyons, L; MacNaughton, J N; Mahon, J R; Maio, A; Malek, A; Malmgren, T G M; Maltezos, S; Malychev, V; Mandl, F; Marco, J; Marco, R P; Maréchal, B; Margoni, M; Marin, J C; Mariotti, C; Markou, A; Martínez-Rivero, C; Martínez-Vidal, F; Martí i García, S; Mastroyiannopoulos, N; Matorras, F; Matteuzzi, C; Matthiae, Giorgio; Masik, J; Mazzucato, F; Mazzucato, M; McCubbin, M L; McKay, R; McNulty, R; McPherson, G; Meroni, C; Meyer, W T; Migliore, E; Mirabito, L; Mitaroff, Winfried A; Mjörnmark, U; Moa, T; Moch, M; Møller, R; Mönig, K; Monge, M R; Moreau, X; Morettini, P; Morton, G A; Müller, U; Münich, K; Mulders, M; Mulet-Marquis, C; Muresan, R; Murray, W J; Muryn, B; Myatt, Gerald; Myklebust, T; Naraghi, F; Nassiakou, M; Navarria, Francesco Luigi; Navas, S; Nawrocki, K; Negri, P; Némécek, S; Neufeld, N; Neumeister, N; Nicolaidou, R; Nielsen, B S; Nikolenko, M; Nomokonov, V P; Normand, Ainsley; Nygren, A; Obraztsov, V F; Olshevskii, A G; Onofre, A; Orava, Risto; Orazi, G; Österberg, K; Ouraou, A; Paganoni, M; Paiano, S; Pain, R; Paiva, R; Palacios, J; Palka, H; Papadopoulou, T D; Papageorgiou, K; Pape, L; Parkes, C; Parodi, F; Parzefall, U; Passeri, A; Passon, O; Pegoraro, M; Peralta, L; Pernicka, Manfred; Perrotta, A; Petridou, C; Petrolini, A; Phillips, H T; Pierre, F; Pimenta, M; Piotto, E; Podobnik, T; Pol, M E; Polok, G; Poropat, P; Pozdnyakov, V; Privitera, P; Pukhaeva, N; Pullia, Antonio; Radojicic, D; Ragazzi, S; Rahmani, H; Ratoff, P N; Read, A L; Rebecchi, P; Redaelli, N G; Regler, Meinhard; Reid, D; Reinhardt, R; Renton, P B; Resvanis, L K; Richard, F; Rídky, J; Rinaudo, G; Røhne, O M; Romero, A; Ronchese, P; Rosenberg, E I; Rosinsky, P; Roudeau, Patrick; Rovelli, T; Royon, C; Ruhlmann-Kleider, V; Ruiz, A; Saarikko, H; Sacquin, Yu; Sadovskii, A; Sajot, G; Salt, J; Sampsonidis, D; Sannino, M; Schneider, H; Schwemling, P; Schwering, B; Schwickerath, U; Schyns, M A E; Scuri, F; Seager, P; Sedykh, Yu; Segar, A M; Sekulin, R L; Shellard, R C; Sheridan, A; Siebel, M; Simard, L C; Simonetto, F; Sissakian, A N; Smadja, G; Smirnov, N; Smirnova, O G; Smith, G R; Sopczak, André; Sosnowski, R; Spassoff, Tz; Spiriti, E; Sponholz, P; Squarcia, S; Stanescu, C; Stanic, S; Stevenson, K; Stocchi, A; Strub, R; Stugu, B; Szczekowski, M; Szeptycka, M; Tabarelli de Fatis, T; Tegenfeldt, F; Terranova, F; Thomas, J; Timmermans, J; Tinti, N; Tkatchev, L G; Todorova-Nová, S; Tomaradze, A G; Tomé, B; Tonazzo, A; Tortora, L; Tranströmer, G; Treille, D; Tristram, G; Trochimczuk, M; Troncon, C; Tsirou, A L; Turluer, M L; Tyapkin, I A; Tzamarias, S; Ullaland, O; Uvarov, V; Valenti, G; Vallazza, E; Van der Velde, C; van Apeldoorn, G W; van Dam, P; Van Doninck, W K; Van Eldik, J; Van Lysebetten, A; Van Vulpen, I B; Vassilopoulos, N; Vegni, G; Ventura, L; Venus, W A; Verbeure, F; Verlato, M; Vertogradov, L S; Verzi, V; Vilanova, D; Vitale, L; Vlasov, E; Vodopyanov, A S; Vollmer, C F; Voulgaris, G; Vrba, V; Wahlen, H; Walck, C; Weiser, C; Wicke, D; Wickens, J H; Wilkinson, G R; Winter, M; Witek, M; Wolf, G; Yi, J; Yushchenko, O P; Zaitsev, A; Zalewska-Bak, A; Zalewski, Piotr; Zavrtanik, D; Zevgolatakos, E; Zimin, N I; Zucchelli, G C; Zumerle, G

    1999-01-01

    Infrared and collinear safe event shape distributions and their mean values are determined using the data taken at ve di erent centre of mass energies above $M_Z$ with the DELPHI detector at LEP. From the event shapes, the strong coupling $\\alpha_s$ is extracted in $O(\\alpha^2_s)$, NLLA and a combined scheme using hadronisation corrections evaluated with fragmentation model generators as well as using an analytical power ansatz. Comparing these measurements to those obtained at MZ, the energy dependence (running) of $\\alpha_s$ is accessible. The logarithmic energy slope of the inverse strong coupling is measured to be $d\\alpha_{s}^{-1}/d log(E_{cm}) = 1.39 \\pm 0.34(stat) \\pm 0.17(syst)$, in good agreement with the QCD expectation of 1.27.

  9. Alpha Shapes and Proteins

    DEFF Research Database (Denmark)

    Winter, Pawel; Sterner, Henrik; Sterner, Peter

    2009-01-01

    We provide a unified description of (weighted) alpha shapes, beta shapes and the corresponding simplicialcomplexes. We discuss their applicability to various protein-related problems. We also discuss filtrations of alpha shapes and touch upon related persistence issues.We claim that the full...... potential of alpha-shapes and related geometrical constructs in protein-related problems yet remains to be realized and verified. We suggest parallel algorithms for (weighted) alpha shapes, and we argue that future use of filtrations and kinetic variants for larger proteins will need such implementation....

  10. Alpha 1-adrenoceptor subtype affinities of drugs for the treatment of prostatic hypertrophy. Evidence for heterogeneity of chloroethylclonidine-resistant rat renal alpha 1-adrenoceptor

    NARCIS (Netherlands)

    Michel, M. C.; Büscher, R.; Kerker, J.; Kraneis, H.; Erdbrügger, W.; Brodde, O. E.

    1993-01-01

    We have used radioligand binding and inositol phosphate accumulation studies to determine the affinity at mixed alpha 1A- and alpha 1B-adrenoceptors (rat cerebral cortex and kidney), alpha 1A-adrenoceptors (rat cerebral cortex and kidney following inactivation of alpha 1B-adrenoceptors by

  11. Mass spectrometric imaging of red fluorescent protein in breast tumor xenografts

    NARCIS (Netherlands)

    Chughtai, K.; Jiang, L.; Post, H.; Winnard Jr., P.T.; Greenwood, T.R.; Raman, V.; Bhujwalla, Z.V.; Heeren, R.M.A.; Glunde, K.

    2013-01-01

    Abstract. Mass spectrometric imaging (MSI) in combination with electrospray mass spectrometry (ESI-MS) is a powerful technique for visualization and identification of a variety of different biomolecules directly from thin tissue sections. As commonly used tools for molecular reporting,

  12. Enrichment/isolation of phosphorylated peptides on hafnium oxide prior to mass spectrometric analysis.

    Science.gov (United States)

    Rivera, José G; Choi, Yong Seok; Vujcic, Stefan; Wood, Troy D; Colón, Luis A

    2009-01-01

    Hafnium oxide (hafnia) exhibits unique enrichment properties towards phosphorylated peptides that are complementary to those of titanium oxide (titania) and zirconium oxide (zirconia) for use with mass spectrometric analysis in the field of proteomics.

  13. Targeted Alpha Therapy: From Alpha to Omega

    International Nuclear Information System (INIS)

    Allen, Barry J; Clarke, Raymond; Huang Chenyu

    2013-01-01

    This review covers the broad spectrum of Targeted Alpha Therapy (TAT) research in Australia; from in vitro and in vivo studies to clinical trials. The principle of tumour anti-vascular alpha therapy (TAVAT) is discussed in terms of its validation by Monte Carlo calculations of vascular models and the potential role of biological dosimetry is examined. Summmary of this review is as follows: 1. The essence of TAT 2. Therapeutic objectives 3. TAVAT and Monte Carlo microdosimetry 4. Biological dosimetry 5. Preclinical studies 6. Clinical trials 7. What next? 8. Obstacles. (author)

  14. Alpha1-antitrypsin deficiency

    DEFF Research Database (Denmark)

    Stolk, Jan; Seersholm, Niels; Kalsheker, Noor

    2006-01-01

    The Alpha One International Registry (AIR), a multinational research program focused on alpha1-antitrypsin (AAT) deficiency, was formed in response to a World Health Organization recommendation. Each of the nearly 20 participating countries maintains a national registry of patients with AAT defic...... epidemiology, inflammatory and signalling processes, therapeutic advances, and lung imaging techniques....

  15. Alpha clustering in nuclei

    International Nuclear Information System (INIS)

    Hodgson, P.E.

    1990-01-01

    The effects of nucleon clustering in nuclei are described, with reference to both nuclear structure and nuclear reactions, and the advantages of using the cluster formalism to describe a range of phenomena are discussed. It is shown that bound and scattering alpha-particle states can be described in a unified way using an energy-dependent alpha-nucleus potential. (author)

  16. In vitro evaluation and determination of responsible fraction of coffee beans and dried sugar beet leaves for alpha-glucosidase inhibition.

    OpenAIRE

    K. Singh; A. Kafka; B-H Kang; R. Goundra; Y-I Kwon; E. Apostolidis

    2013-01-01

    Summary. Recent studies have identified that hydrophobic phenolic phytochemicals and hydrophilic Amadori compounds have potential for type 2 diabetes management via inhibition of carbohydrate hydrolysis enzymes. Here, we determined the phenolic content, α-glucosidase inhibitory activity, and pancreatic α-amylase inhibitory activity of water extracts of roasted and unroasted coffee beans and dried sugar beet leaves. Sugar beet leaves appeared to have the lowest total phenolic content while unr...

  17. Determination of radium isotopes in environmental samples by gamma spectrometry, liquid scintillation counting and alpha spectrometry: a review of analytical methodology

    International Nuclear Information System (INIS)

    Jia, Guogang; Jia, Jing

    2012-01-01

    Radium (Ra) isotopes are important from the viewpoints of radiation protection and environmental protection. Their high toxicity has stimulated the continuing interest in methodology research for determination of Ra isotopes in various media. In this paper, the three most routinely used analytical techniques for Ra isotope determination in biological and environmental samples, i.e. low-background γ-spectrometry, liquid scintillation counting and α-spectrometry, were reviewed, with emphasis on new methodological developments in sample preparation, preconcentration, separation, purification, source preparation and measurement techniques. The accuracy, selectivity, traceability, applicability and minimum detectable activity (MDA) of the three techniques were discussed. It was concluded that the MDA (0.1 mBq L −1 ) of the α-spectrometry technique coupled with chemical separation is about two orders of magnitude lower than that of low-background HPGe γ-spectrometry and LSC techniques. Therefore, when maximum sensitivity is required, the α-spectrometry technique remains the first choice. - Highlights: ► A review is made for determination of Ra isotopes in environmental samples. ► Gamma spectrometry, LSC and a-spectrometry are the main concerned radiometric approach. ► Sample preparation, preconcentration, separation and source preparation are discussed. ► The methods can analyse air, water, seawater, soil, sediment and foodstuffs samples. ► Some new data obtained recently from our laboratory for Ra method study are included.

  18. Comparison of alpha decay and alpha transfer reactions in the lead region. [R matrix theory, absolute alpha widths, cross sections, 93 MeV

    Energy Technology Data Exchange (ETDEWEB)

    DeVries, R.M.

    1978-01-01

    Data were taken for five transitions in the lead region allowing a quantitative comparison with corresponding alpha-decay data via R-matrix theory using the same target + alpha nuclear potential. Good agreement between the absolute reduced widths determined from the two sets of data suggests that in transfer reactions, as in alpha decay, an alpha particle in its ground state is transferred in a one-step process. In a separate analysis, elastic and total reaction cross sections for the systems ..cap alpha.. + /sup 208/Pb, /sup 209/Bi were analyzed to obtain a limited set of potentials which, in turn, were used to calculate absolute alpha widths. Existing shell model calculations give ..gamma../sub ..cap alpha..//sup 2/ values three orders of magnitude smaller.

  19. Use of human chorionic gonadtropin and alpha-fetoprotein radioimmunoassays: specificity and apparent half-life determination after delivery and in patients with germ cell tumors

    International Nuclear Information System (INIS)

    Mann, K.; Lamerz, R.; Hellmann, Th.; Kuemper, H.J.; Staehler, G.; Karl, H.J.

    1980-01-01

    The specificity of commercially available hCG and hCG-β antibodies (anti-hCG-β from N.I.A.M.D.D. (SB6), Serono (S), Biosigma (B), Union Carbide (UC) (I.R.E.) and anti-hCG from Union Carbide) were compared. Using 125 I-hCG (CR 115), the crossreactivity with LH (LER 960) was 5.5% for SB6, 0.25% for S and 0.3% for B. In the homologous hCG system UC, crossreactivity was 0.06% with hCG-β and 1.2% with LH, in the hCG-β system UC, it was 2.2% with hCG and 0.01% with LH. Parallel standard curves for hCG, the 2nd I.R.P. hCG and hCG-β were found exclusively with the 125 I-hCG, anti-hCG-β system S. Consequently accurate estimates of the total hCG or hCG-β content in serum and standardization with the 2nd I.R.P. is possible. This system is the most useful for clinical purposes. The serum half-life of hCG was calculated in 10 pregnant women after delivery and was found to be 10 to 34h. AFP half-life time, determined by the double antibody radioimmunoassay was 4.0+-1.8 (+- SD) days in pregnant women after delivery (n=60) and 3.8+-0.9 days in neonates during the first 16 days of life (n=26). Altogether, apparent half-life determinations were carried out in 29 patients with nonseminomatous germ cell tumours. The results indicate that half-life determinations of hCG and AFP may have a predictive value with respect to the monitoring of therapy. (Auth.)

  20. Evolution of Substrate Specificity within a Diverse Family of [beta/alpha]-Barrel-fold Basic Amino Acid Decarboxylases X-ray Structure Determination of Enzymes with Specificity for L-Arginine and Carboxynorspermidine

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Xiaoyi; Lee, Jeongmi; Michael, Anthony J.; Tomchick, Diana R.; Goldsmith, Elizabeth J.; Phillips, Margaret A. (Sungkyunkwan); (UTSMC)

    2010-08-26

    Pyridoxal 5{prime}-phosphate (PLP)-dependent basic amino acid decarboxylases from the {beta}/{alpha}-barrel-fold class (group IV) exist in most organisms and catalyze the decarboxylation of diverse substrates, essential for polyamine and lysine biosynthesis. Herein we describe the first x-ray structure determination of bacterial biosynthetic arginine decarboxylase (ADC) and carboxynorspermidine decarboxylase (CANSDC) to 2.3- and 2.0-{angstrom} resolution, solved as product complexes with agmatine and norspermidine. Despite low overall sequence identity, the monomeric and dimeric structures are similar to other enzymes in the family, with the active sites formed between the {beta}/{alpha}-barrel domain of one subunit and the {beta}-barrel of the other. ADC contains both a unique interdomain insertion (4-helical bundle) and a C-terminal extension (3-helical bundle) and it packs as a tetramer in the asymmetric unit with the insertions forming part of the dimer and tetramer interfaces. Analytical ultracentrifugation studies confirmed that the ADC solution structure is a tetramer. Specificity for different basic amino acids appears to arise primarily from changes in the position of, and amino acid replacements in, a helix in the {beta}-barrel domain we refer to as the 'specificity helix.' Additionally, in CANSDC a key acidic residue that interacts with the distal amino group of other substrates is replaced by Leu{sup 314}, which interacts with the aliphatic portion of norspermidine. Neither product, agmatine in ADC nor norspermidine in CANSDC, form a Schiff base to pyridoxal 5{prime}-phosphate, suggesting that the product complexes may promote product release by slowing the back reaction. These studies provide insight into the structural basis for the evolution of novel function within a common structural-fold.

  1. Genetics Home Reference: alpha thalassemia

    Science.gov (United States)

    ... Facebook Twitter Home Health Conditions Alpha thalassemia Alpha thalassemia Printable PDF Open All Close All Enable Javascript to view the expand/collapse boxes. Description Alpha thalassemia is a blood disorder that reduces the production ...

  2. Radio spectrometric survey of un-surveyed areas in Syria

    International Nuclear Information System (INIS)

    Aissa, M.; Al-Hent, R; Jubeli, Y.

    2002-11-01

    The values and distribution of the radioelements e U, e Th, % K and Ur units in the surface geological formations of the west and south sectors of Syrian region, were estimated using carbone gamma ray spectrometric survey. The radiometric maps were prepared, as well as, many geological profiles, cross sections studied in different locations and geochemical samples were analyzed by laboratory gamma ray spectrometry and by x-ray diffractometry, the results of the all sets were compared. In general, the survey shows, low radioelement concentrations in the area, especially on basic rocks (Jabal Al-arab, Hawran) south Syria, and on ultra basic rocks (ophiolitic complex) north-west Syria, but there are some separate anomalous spots were connected with phosphate rocks, detected on cretaceous and Palaeogene age. Some times we noticed high radioelement concentrations haloes associated with fractured zones were already arise from secondary uranium mineralization, as a result of solutions movement through fissures in carbonatic and/or chalk like limestone rocks. finally, the obtained concentrations, represent a background values which has no significant importance for uranium exploration point of view. (author)

  3. Mass Spectrometric C-14 Detection Techniques: Progress Report

    Science.gov (United States)

    Synal, H.

    2013-12-01

    Accelerator Mass Spectrometry (AMS) has been established as the best-suited radiocarbon detection technique. In the past years, significant progress with AMS instrumentation has been made resulting in a boom of new AMS facilities around the World. Today, carbon only AMS systems predominantly utilize 1+ charge state and molecule destruction in multiple ion gas collisions in stripper gas cell. This has made possible a significant simplification of the instruments, a reduction of ion energies and related to this less required space of the installations. However, state-of-the-art AMS instruments have still not reached a development stage where they can be regarded as table-top systems. In this respect, more development is needed to further advance the applicability of radiocarbon not only in the traditional fields of dating but also in biomedical research and new fields in Earth and environmental sciences. In a the proof-of-principle experiment the feasibility of radiocarbon detection over the entire range of dating applications was demonstrated using a pure mass spectrometer and ion energies below 50 keV. Now an experimental platform has been completed to test performance and to explore operation and measurement conditions of pure mass spectrometric radiocarbon detection. This contribution will overview the physical principles, which make this development possible and discuss key parameters of the instrumental design and performance of such an instrument.

  4. Status of mass spectrometric radiocarbon detection at ETHZ

    Energy Technology Data Exchange (ETDEWEB)

    Seiler, Martin; Maxeiner, Sascha; Wacker, Lukas; Synal, Hans-Arno

    2015-10-15

    A prototype of a mass spectrometric radiocarbon detection instrument without accelerator stage was built for the first time and set into operation at ETH Zurich. The system is designed as an experimental platform to optimize performance of {sup 14}C detection at low ion energies and to study the most relevant processes that may limit system performance. The optimized stripper unit incorporates differential pumping to maintain a low gas outflow and a revised tube design to better match the phase space volume of the ion beam at low energies. The system is fully operational and has demonstrated true radiocarbon dating capabilities. The overall beam transmission through the stripper tube is about 40% for the 1{sup +} charge state. Radiocarbon analyses with an overall precision of 0.6% were obtained on a single sample under regular measurement conditions. By analyzing multiple targets of the same sample material an uncertainty level of 0.3% has been reached. The background level corresponds to a radiocarbon age of 40,000 years.

  5. A comparison of the alpha and gamma radiolysis of CMPO

    Energy Technology Data Exchange (ETDEWEB)

    Bruce J. Mincher; Stephen P. Mezyk; Gary Groenewold; Gracy Elias

    2011-06-01

    The radiation chemistry of CMPO has been investigated using a combination of irradiation and analytical techniques. The {alpha}-, and {gamma}-irradiation of CMPO resulted in identical degradation rates (G-value, in {mu}mol Gy{sup -1}) for both radiation types, despite the difference in their linear energy transfer (LET). Similarly, variations in {gamma}-ray dose rates did not affect the degradation rate of CMPO. The solvent extraction behavior was different for the two radiation types, however. Gamma-irradiation resulted in steadily increasing distribution ratios for both forward and stripping extractions, with respect to increasing absorbed radiation dose. This was true for samples irradiated as a neat organic solution, or irradiated in contact with the acidic aqueous phase. In contrast, {alpha}-irradiated samples showed a rapid drop in distribution ratios for forward and stripping extractions, followed by essentially constant distribution ratios at higher absorbed doses. These differences in extraction behavior are reconciled by mass spectrometric examination of CMPO decomposition products under the different irradiation sources. Irradiation by {gamma}-rays resulted in the rupture of phosphoryl-methylene bonds with the production of phosphinic acid products. These species are expected to be complexing agents for americium that would result in higher distribution ratios. Irradiation by {alpha}-sources appeared to favor rupture of carbamoyl-methylene bonds with the production of less deleterious acetamide products.

  6. Deficiency of alpha7 cholinergic receptors facilitates bacterial clearance in Escherichia coli peritonitis

    NARCIS (Netherlands)

    Giebelen, Ilona A. J.; Le Moine, Alain; van den Pangaart, Petra S.; Sadis, Claude; Goldman, Michel; Florquin, Sandrine; van der Poll, Tom

    2008-01-01

    BACKGROUND: The efferent vagus nerve can inhibit inflammation via interaction between acetylcholine and alpha7 cholinergic receptors. METHODS: To determine the role played by alpha7 receptors in antibacterial defense, peritonitis was induced in alpha7 receptor-deficient (alpha7(-/-)) and wild-type

  7. Photoelectron diffraction study and structure determination of ultrathin hafnium silicide layers on silicon(1 0 0) using Mg K{alpha} radiation and synchrotron light

    Energy Technology Data Exchange (ETDEWEB)

    Fluechter, C.R. [Experimentelle Physik 1, Universitaet Dortmund, Otto-Hahn-Str. 4, D-44221 Dortmund (Germany); DELTA, Universitaet Dortmund, Maria-Goeppert-Mayer-Str. 2, D-44227 Dortmund (Germany)], E-mail: christian.fluechter@uni-dortmund.de; Siervo, A. de [Laboratorio Nacional de Luz Sincrotron, C.P. 6192, 13084-971 Campinas, SP (Brazil); Weier, D. [Experimentelle Physik 1, Universitaet Dortmund, Otto-Hahn-Str. 4, D-44221 Dortmund (Germany); DELTA, Universitaet Dortmund, Maria-Goeppert-Mayer-Str. 2, D-44227 Dortmund (Germany); Schuermann, M. [Experimentelle Physik 1, Universitaet Dortmund, Otto-Hahn-Str. 4, D-44221 Dortmund (Germany); Berges, U. [Experimentelle Physik 1, Universitaet Dortmund, Otto-Hahn-Str. 4, D-44221 Dortmund (Germany); DELTA, Universitaet Dortmund, Maria-Goeppert-Mayer-Str. 2, D-44227 Dortmund (Germany); Dreiner, S. [Experimentelle Physik 1, Universitaet Dortmund, Otto-Hahn-Str. 4, D-44221 Dortmund (Germany); Carazzolle, M.F. [Instituto de Fisica, Universidade Estadual de Campinas, C.P. 6165, 13083-970 Campinas, SP (Brazil); Landers, R. [Laboratorio Nacional de Luz Sincrotron, C.P. 6192, 13084-971 Campinas, SP (Brazil); Instituto de Fisica, Universidade Estadual de Campinas, C.P. 6165, 13083-970 Campinas, SP (Brazil); Kleiman, G.G. [Instituto de Fisica, Universidade Estadual de Campinas, C.P. 6165, 13083-970 Campinas, SP (Brazil); Westphal, C. [Experimentelle Physik 1, Universitaet Dortmund, Otto-Hahn-Str. 4, D-44221 Dortmund (Germany); DELTA, Universitaet Dortmund, Maria-Goeppert-Mayer-Str. 2, D-44227 Dortmund (Germany)

    2007-05-15

    In order to increase the switching speed and the efficiency of modern semiconductor devices a further down scaling is desired. Thus, the SiO{sub 2} gate dielectric might be replaced by layers of a material with a much higher dielectric constant like HfO{sub 2}. A major problem of the system HfO{sub 2}/Si(1 0 0) is the silicidation of hafnium at the interface. Therefore, ultrathin films (3-30 A) of HfSi{sub 2} on Si(1 0 0) were investigated by photoelectron spectroscopy, low-energy electron diffraction and X-ray photoelectron diffraction. Synchrotron light with an energy of h{nu} = 180 eV was used for excitation. First results were obtained using a Mg X-ray tube (h{nu} = 1253.6 eV). In order to determine the structure of the films, the recorded photoelectron diffraction patterns were compared to computer simulations of model structures. The simulations for the low-energy measurements were performed using the program MSPHD. As a result a modified zirconium silicide structure is presented in order to describe the structure of ultrathin HfSi{sub 2} films on Si(1 0 0)

  8. $\\alpha_{S}$ Evolution from 35 GeV to 202 GeV and Flavour Independence

    CERN Document Server

    Biebel, O.

    2000-01-01

    Determinations of the strong coupling constant alpha_S at centre-of-mass energies of 192 through 202 GeV at LEP are presented. The energy evolution of alpha_S is in agreement with the prediction of QCD. The combined investigation of OPAL and JADE data in the energy range of 35 through 189 GeV yields alpha_S(m_Z)=0.1187^{+0.0034}_{-0.0019}. The strenght of the strong coupling is flavour independent if quark mass effects are taken into account.

  9. A spectrometrical method to measure the deuterium content in 2H-enriched water

    International Nuclear Information System (INIS)

    Dumke, I.

    1980-04-01

    A test method and spectrometer has been developed for emission-spectrometrical measurement of the deuterium content in water enriched with deuterium. The water sample is melted into a previously evacuated glas tube and a gas discharge is excited in vapour over the cooled sample to adjust to a low vapour pressure with high frequency. The intensities of the H(α) and D(α) lines appearing in the spectrum determine the D-content. Both lines were resolved by a Fabry-Perot interferometer and geometrically separated fed to two photodetectors. The remaining spectrum is filtered off. Following electronic calculation of the signals, the measured value is indicated which has to be corrected by a standard curve. The relative measuring accuracy is about +-1% for enrichments of over 1% D and less than +-5% in the region of 0.3-1% D. The detection limit is about 0.03% D (sample amount: 50 μl, average of 5 samples). (orig./HP) [de

  10. Mass spectrometric investigation of neutral and charged constituents in saturated vapor over PrI3

    International Nuclear Information System (INIS)

    Motalov, V.B.; Vorobiev, D.E.; Kudin, L.S.; Markus, T.

    2009-01-01

    The Knudsen effusion mass spectrometric technique was used to study vapor species over praseodymium triiodide. The monomer, PrI 3 , and dimer, Pr 2 I 6 , molecules and the negative ions, PrI 4 - and Pr 2 I 7 - , were observed in saturated vapor in the temperature range from 856 K to 1048 K. The partial vapor pressures of neutral constituents were determined and the enthalpies of sublimation obtained using the second and the third laws of thermodynamics (Δ s H deg. (298.15 K) = 291 ± 4 kJ mol -1 for PrI 3 , and Δ s H deg. (298.15 K) = 400 ± 30 kJ mol -1 for Pr 2 I 6 ). The equilibrium constants for various ion molecular reactions were measured and the enthalpies of reactions obtained. The enthalpies of formation, Δ f H deg. (298.15 K) kJ mol -1 , of gaseous molecules and ions were calculated and are as follows: -374 ± 6 (PrI 3 ), -929 ± 30 (Pr 2 I 6 ), -867 ± 30 (PrI 4 - ), -1432 ± 50 (Pr 2 I 7 - )

  11. Mass spectrometric characterization of the sarcoplasmic reticulum from rabbit skeletal muscle by on-membrane digestion.

    Science.gov (United States)

    Staunton, Lisa; Ohlendieck, Kay

    2012-03-01

    The sarcoplasmic reticulum from skeletal muscle constitutes an elaborate membrane system that contains a considerable number of integral and very large proteins that exist in highly complex supramolecular clusters. Conventional proteomics using two-dimensional gel electrophoresis greatly underestimates the presence of these proteins. Here, we have applied one-dimensional gradient gels and on-membrane digestion to overcome this technical problem. Mass spectrometric analysis has determined the presence of 31 distinct protein species in the sarcoplasmic reticulum, including key Ca2+-handling proteins such as the ryanodine receptor, Ca2+-ATPase, calsequestrin and sarcalumenin. Immunoblotting confirmed the relative position of these Ca2+-regulatory elements in analytical gel replicas. Interestingly, aldolase and phosphofructokinase were found to be present in the purified sarcoplasmic reticulum, supporting the idea of a close physical coupling between the glycolytic pathway and the energy-dependent sarcoplasmic reticulum. Hence, on-membrane digestion is highly suitable as the method of choice for studying integral and high-molecular-mass proteins in proteomic studies.

  12. Quantitation of dissolved gas content in emulsions and in blood using mass spectrometric detection

    Science.gov (United States)

    Grimley, Everett; Turner, Nicole; Newell, Clayton; Simpkins, Cuthbert; Rodriguez, Juan

    2011-01-01

    Quantitation of dissolved gases in blood or in other biological media is essential for understanding the dynamics of metabolic processes. Current detection techniques, while enabling rapid and convenient assessment of dissolved gases, provide only direct information on the partial pressure of gases dissolved in the aqueous fraction of the fluid. The more relevant quantity known as gas content, which refers to the total amount of the gas in all fractions of the sample, can be inferred from those partial pressures, but only indirectly through mathematical modeling. Here we describe a simple mass spectrometric technique for rapid and direct quantitation of gas content for a wide range of gases. The technique is based on a mass spectrometer detector that continuously monitors gases that are rapidly extracted from samples injected into a purge vessel. The accuracy and sample processing speed of the system is demonstrated with experiments that reproduce within minutes literature values for the solubility of various gases in water. The capability of the technique is further demonstrated through accurate determination of O2 content in a lipid emulsion and in whole blood, using as little as 20 μL of sample. The approach to gas content quantitation described here should greatly expand the range of animals and conditions that may be used in studies of metabolic gas exchange, and facilitate the development of artificial oxygen carriers and resuscitation fluids. PMID:21497566

  13. Alpha Thalassemia (For Parents)

    Science.gov (United States)

    ... the body has a problem producing alpha globin Beta thalassemia : when the body has a problem producing beta ... Transfusion Blood Test: Hemoglobin Electrophoresis Sickle Cell Disease Beta Thalassemia Blood All About Genetics Prenatal Genetic Counseling Genetic ...

  14. Fasting induces basolateral uptake transporters of the SLC family in the liver via HNF4alpha and PGC1alpha.

    Science.gov (United States)

    Dietrich, Christoph G; Martin, Ina V; Porn, Anne C; Voigt, Sebastian; Gartung, Carsten; Trautwein, Christian; Geier, Andreas

    2007-09-01

    Fasting induces numerous adaptive changes in metabolism by several central signaling pathways, the most important represented by the HNF4alpha/PGC-1alpha-pathway. Because HNF4alpha has been identified as central regulator of basolateral bile acid transporters and a previous study reports increased basolateral bile acid uptake into the liver during fasting, we hypothesized that HNF4alpha is involved in fasting-induced bile acid uptake via upregulation of basolateral bile acid transporters. In rats, mRNA of Ntcp, Oatp1, and Oatp2 were significantly increased after 48 h of fasting. Protein expression as determined by Western blot showed significant increases for all three transporters 72 h after the onset of fasting. Whereas binding activity of HNF1alpha in electrophoretic mobility shift assays remained unchanged, HNF4alpha binding activity to the Ntcp promoter was increased significantly. In line with this result, we found significantly increased mRNA expression of HNF4alpha and PGC-1alpha. Functional studies in HepG2 cells revealed an increased endogenous NTCP mRNA expression upon cotransfection with either HNF4alpha, PGC-1alpha, or a combination of both. We conclude that upregulation of the basolateral bile acid transporters Ntcp, Oatp1, and Oatp2 in fasted rats is mediated via the HNF4alpha/PGC-1alpha pathway.

  15. Synthesis and analytics of 2,2,3,4,4-d5-19-nor-5alpha-androsterone--an internal standard in doping analysis.

    Science.gov (United States)

    Gaertner, Peter; Bica, Katharina; Felzmann, Wolfgang; Forsdahl, Guro; Gmeiner, Günter

    2007-05-01

    A short and efficient synthesis of pentadeuterated 2,2,3,4,4-d5-19-nor-5alpha-androsterone 7 starting from 19-norandrost-4-ene-3,17-dione 1 by a d1-L-Selectride mediated stereo- and regioselective reduction of the 3-keto group is presented. The use of compound 7 as internal standard for the detection of anabolic steroids via mass spectrometric techniques such as gas chromatography-mass spectrometry (GC-MS) is discussed.

  16. Measurement of radium micro-precipitates using alpha spectrometry and total alpha counting methods

    International Nuclear Information System (INIS)

    Hosseini, T.; Fathivand, A.A.

    2004-01-01

    Background: This study consists of two parts. The first part deals with both qualitative and quantitative analysis of 226 Ra suing alpha spectrometry measurement method. In the second part, the percentage of radioactive equilibrium between 226 Radium and its daughter products were determined by alpha spectrometry and total alpha measurement system after elapsed time of 15 days from precipitation. Materials and methods: Twelve 226 Radium samples as Barium-Radium Sulfate in form of micro-precipitates on millipore and What man 42 filters were prepared. An alpha spectrometer with surface barrier detector and a total alpha measurement system consists of scintillation crystal assembly Zinc Silver were used for counting. Results: The minimum detection limit of alpha spectrometry and total alpha counting for 226 Radium measurements in samples for counting time equal to 10000 seconds, were found to be 3.7 mBq and 15.8 mBq respectively. Results from total alpha counting showed that radioactive equilibrium between 226 Radium and its daughter products reached to about 92%± 3.5, where as, in the case of alpha spectrometry radioactive equilibrium, it was destroyed due to vacuum during counting the sample. Also in case of alpha spectrometry, the optimum sample to detector distance, was found to be 0.5 centimeter. Conclusion: From this study it was concluded that micro-precipitation can be used as a proper method for sample preparation and alpha spectrometry due to its lower detection limit to measure low concentration of 224 Radium and 226 Radium in these precipitates, prepared from different samples. Besides it is not time consuming and sources can be measured immediately after sample preparation

  17. ALPHA-2: the sequel

    CERN Multimedia

    Katarina Anthony

    2012-01-01

    While many experiments are methodically planning for intense works over the long shutdown, there is one experiment that is already working at full steam: ALPHA-2. Its final components arrived last month and will completely replace the previous ALPHA set-up. Unlike its predecessor, this next generation experiment has been specifically designed to measure the properties of antimatter.   The ALPHA team lower the new superconducting solenoid magnet into place. The ALPHA collaboration is working at full speed to complete the ALPHA-2 set-up for mid-November – this will give them a few weeks of running before the AD shutdown on 17 December. “We really want to get some experience with this device this year so that, if we need to make any changes, we will have time during the long shutdown in which to make them,” says Jeffrey Hangst, ALPHA spokesperson. “Rather than starting the 2014 run in the commissioning stage, we will be up and running from the get go.&...

  18. High-performance liquid chromatography/mass spectrometric identification of dibenzylbutyrolactone-type lignans: insights into electrospray ionization tandem mass spectrometric fragmentation of lign-7-eno-9,9'-lactones and application to the lignans of Linum usitatissimum L. (Common Flax).

    Science.gov (United States)

    Schmidt, Thomas J; Alfermann, A Wilhelm; Fuss, Elisabeth

    2008-11-01

    In continuation of our studies into the mass spectrometric detection of natural lignans and their identification in complex mixtures such as crude plant extracts, the electrospray ionization tandem mass spectrometric (ESI-MS/MS) fragmentation of Delta(7,8)-unsaturated dibenzylbutyrolactone-type lignans (lign-7-eno-9,9'-lactones) was studied in detail. It is demonstrated that the characteristic fragmentation allows unambiguous identification including distinction between constitutional isomers. These lignans containing an alpha,beta-unsaturated lactone structure exist as equilibrium mixtures of E- and Z-isomers indistinguishable by mass spectrometry, but it is shown that chromatographic retention time can be used to distinguish between the isomeric forms. Based on these observations, re-analysis of the dichloromethane extract obtained from flowering aerial parts of Linum usitatissimum L. by high-performance liquid chromatography (HPLC)/ESI-MS/MS led to the identification of eighteen lignans of these types (five lignano- and one lignenolactone previously reported along with five further lignano- as well as seven lignenolactones hitherto unreported for this plant). The simultaneous identification of eighteen different lignans in the complex matrix of a crude plant extract by a single analysis demonstrates the potential of this method, which will certainly lead to new insights into the lignan composition and metabolism of different Linum species and many other plants.

  19. Acetylation and glycation of fibrinogen in vitro occur at specific lysine residues in a concentration dependent manner: A mass spectrometric and isotope labeling study

    Energy Technology Data Exchange (ETDEWEB)

    Svensson, Jan, E-mail: jan.svensson@ki.se [Department of Molecular Medicine and Surgery, Karolinska Institutet, Karolinska University Hospital (Solna), SE-171 76 Stockholm (Sweden); Karolinska Institutet, Department of Clinical Sciences, Danderyd Hospital, SE-182 88 Stockholm (Sweden); Bergman, Ann-Charlotte [Department of Molecular Medicine and Surgery, Karolinska Institutet, Karolinska University Hospital (Solna), SE-171 76 Stockholm (Sweden); Adamson, Ulf [Karolinska Institutet, Department of Clinical Sciences, Danderyd Hospital, SE-182 88 Stockholm (Sweden); Blombaeck, Margareta [Department of Molecular Medicine and Surgery, Karolinska Institutet, Karolinska University Hospital (Solna), SE-171 76 Stockholm (Sweden); Wallen, Hakan; Joerneskog, Gun [Karolinska Institutet, Department of Clinical Sciences, Danderyd Hospital, SE-182 88 Stockholm (Sweden)

    2012-05-04

    Highlights: Black-Right-Pointing-Pointer Fibrinogen was incubated in vitro with glucose or aspirin. Black-Right-Pointing-Pointer Acetylations and glycations were found at twelve lysine sites by mass spectrometry. Black-Right-Pointing-Pointer The labeling by aspirin and glucose occurred dose-dependently. Black-Right-Pointing-Pointer No competition between glucose and aspirin for binding to fibrinogen was found. -- Abstract: Aspirin may exert part of its antithrombotic effects through platelet-independent mechanisms. Diabetes is a condition in which the beneficial effects of aspirin are less prominent or absent - a phenomenon called 'aspirin resistance'. We investigated whether acetylation and glycation occur at specific sites in fibrinogen and if competition between glucose and aspirin in binding to fibrinogen occurs. Our hypothesis was that such competition might be one explanation to 'aspirin resistance' in diabetes. After incubation of fibrinogen in vitro with aspirin (0.8 mM, 24 h) or glucose (100 mM, 5-10 days), we found 12 modified sites with mass spectrometric techniques. Acetylations in the {alpha}-chain: {alpha}K191, {alpha}K208, {alpha}K224, {alpha}K429, {alpha}K457, {alpha}K539, {alpha}K562, in the {beta}-chain: {beta}K233, and in the {gamma}-chain: {gamma}K170 and {gamma}K273. Glycations were found at {beta}K133 and {gamma}K75, alternatively {gamma}K85. Notably, the lysine 539 is a site involved in FXIII-mediated cross-linking of fibrin. With isotope labeling in vitro, using [{sup 14}C-acetyl]salicylic acid and [{sup 14}C]glucose, a labeling of 0.013-0.084 and 0.12-0.5 mol of acetylated and glycated adduct/mol fibrinogen, respectively, was found for clinically (12.9-100 {mu}M aspirin) and physiologically (2-8 mM glucose) relevant plasma concentrations. No competition between acetylation and glycation could be demonstrated. Thus, fibrinogen is acetylated at several lysine residues, some of which are involved in the cross-linking of

  20. Alpha particles detection in nitrocellulose

    International Nuclear Information System (INIS)

    Romero C, M.

    1976-01-01

    The method for the manufacturing of the detection films follows these steps: preparation of the mass which includes nitrocellulose in the form of cotton as raw material ethyl acetate, cellosolve acetate, isopropyl and butyl alcohols as solvents and dioctyl phtalate as plasticiser; dilution of the paste; pouring of the diluted mass; and drying of the detection films. The results obtained experimentally are: The determination of the development times of the different thicknesses of the manufactured films. Response linearity of the detectors, variation of the number of tracks according to the distance of the source to the detector. Sizes of the diameter of the tracks depending of the distance detector-alpha emmission source. As a conclusion we can say the the nitrocellulose detectors are specific for alpha radiation; the more effective thicknesses in uranium prospecting works were those of 60 microns, since for the laboratory works the thicknesses of 30 to 40 microns were the ideal; the development technique of the detection films is simple and cheap and can be realized even in another place than the laboratory; this way of the manufacturing of nitrocellulose detection film sensitive to alpha nuclear radiation is open to future research. (author)