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Sample records for determine unknown trace

  1. Unknown foundation determination for scour.

    Science.gov (United States)

    2012-04-01

    Unknown foundations affect about 9,000 bridges in Texas. For bridges over rivers, this creates a problem : regarding scour decisions as the calculated scour depth cannot be compared to the foundation depth, and a : very conservative costly approach m...

  2. Determination of the origin of unknown irradiated nuclear fuel.

    Science.gov (United States)

    Nicolaou, G

    2006-01-01

    An isotopic fingerprinting method is presented to determine the origin of unknown nuclear material with forensic importance. Spent nuclear fuel of known origin has been considered as the 'unknown' nuclear material in order to demonstrate the method and verify its prediction capabilities. The method compares, using factor analysis, the measured U, Pu isotopic compositions of the 'unknown' material with U, Pu isotopic compositions simulating well known spent fuels from a range of commercial nuclear power stations. Then, the 'unknown' fuel has the same origin as the commercial fuel with which it exhibits the highest similarity in U, Pu compositions.

  3. Determination of the origin of unknown irradiated nuclear fuel

    International Nuclear Information System (INIS)

    Nicolaou, G.

    2006-01-01

    An isotopic fingerprinting method is presented to determine the origin of unknown nuclear material with forensic importance. Spent nuclear fuel of known origin has been considered as the 'unknown' nuclear material in order to demonstrate the method and verify its prediction capabilities. The method compares, using factor analysis, the measured U, Pu isotopic compositions of the 'unknown' material with U, Pu isotopic compositions simulating well known spent fuels from a range of commercial nuclear power stations. Then, the 'unknown' fuel has the same origin as the commercial fuel with which it exhibits the highest similarity in U, Pu compositions

  4. Bayesian source term determination with unknown covariance of measurements

    Science.gov (United States)

    Belal, Alkomiet; Tichý, Ondřej; Šmídl, Václav

    2017-04-01

    Determination of a source term of release of a hazardous material into the atmosphere is a very important task for emergency response. We are concerned with the problem of estimation of the source term in the conventional linear inverse problem, y = Mx, where the relationship between the vector of observations y is described using the source-receptor-sensitivity (SRS) matrix M and the unknown source term x. Since the system is typically ill-conditioned, the problem is recast as an optimization problem minR,B(y - Mx)TR-1(y - Mx) + xTB-1x. The first term minimizes the error of the measurements with covariance matrix R, and the second term is a regularization of the source term. There are different types of regularization arising for different choices of matrices R and B, for example, Tikhonov regularization assumes covariance matrix B as the identity matrix multiplied by scalar parameter. In this contribution, we adopt a Bayesian approach to make inference on the unknown source term x as well as unknown R and B. We assume prior on x to be a Gaussian with zero mean and unknown diagonal covariance matrix B. The covariance matrix of the likelihood R is also unknown. We consider two potential choices of the structure of the matrix R. First is the diagonal matrix and the second is a locally correlated structure using information on topology of the measuring network. Since the inference of the model is intractable, iterative variational Bayes algorithm is used for simultaneous estimation of all model parameters. The practical usefulness of our contribution is demonstrated on an application of the resulting algorithm to real data from the European Tracer Experiment (ETEX). This research is supported by EEA/Norwegian Financial Mechanism under project MSMT-28477/2014 Source-Term Determination of Radionuclide Releases by Inverse Atmospheric Dispersion Modelling (STRADI).

  5. A 'range test' for determining scatterers with unknown physical properties

    Science.gov (United States)

    Potthast, Roland; Sylvester, John; Kusiak, Steven

    2003-06-01

    We describe a new scheme for determining the convex scattering support of an unknown scatterer when the physical properties of the scatterers are not known. The convex scattering support is a subset of the scatterer and provides information about its location and estimates for its shape. For convex polygonal scatterers the scattering support coincides with the scatterer and we obtain full shape reconstructions. The method will be formulated for the reconstruction of the scatterers from the far field pattern for one or a few incident waves. The method is non-iterative in nature and belongs to the type of recently derived generalized sampling schemes such as the 'no response test' of Luke-Potthast. The range test operates by testing whether it is possible to analytically continue a far field to the exterior of any test domain Omegatest. By intersecting the convex hulls of various test domains we can produce a minimal convex set, the convex scattering support of which must be contained in the convex hull of the support of any scatterer which produces that far field. The convex scattering support is calculated by testing the range of special integral operators for a sampling set of test domains. The numerical results can be used as an approximation for the support of the unknown scatterer. We prove convergence and regularity of the scheme and show numerical examples for sound-soft, sound-hard and medium scatterers. We can apply the range test to non-convex scatterers as well. We can conclude that an Omegatest which passes the range test has a non-empty intersection with the infinity-support (the complement of the unbounded component of the complement of the support) of the true scatterer, but cannot find a minimal set which must be contained therein.

  6. Photometric determination of traces of metals

    International Nuclear Information System (INIS)

    Onishi, H.

    1986-01-01

    The first three editions of this widely used classic were published under the title Colorimetric Determination of Traces of Metals, with E.B. Sandell as author. Part I (General Aspects) of the fourth edition was co-authored by E.B. Sandell and H. Onishi and published in 1978. After Sandell's death in 1984, Onishi assumed the monumental task of revising Part II. This book (Part IIA) consists of 21 chapters in which the photometric determinations of the individual metals, aluminium to lithium (including the lanthanoids), are described. Each chapter is divided into three sections: Separations, Methods of Determination, and Applications. The sections on Separations are of general interest and include methods based on precipitation, ion-exchange, chromatography, and liquid-liquid extraction. Molecular absorption and fluorescence techniques are described in the sections on determinations, and the emphasis is on the use of well-established reagents. Several reagents that have been recently introduced for the determination of trace levels of metals are also critically reviewed at the end of each section on methods of determination. Important applications of these methods to the determination of trace metals in complex organic and inorganic materials are described in detail at the end of each chapter

  7. Polarographic determination of trace amounts of thorium

    Energy Technology Data Exchange (ETDEWEB)

    Zaofan Zhao; Xiaohua Cai; Peibiao Li; Handong Yang

    1986-07-01

    A sensitive linear-sweep polarographic method for the determination of thorium is described. It is based on the thorium complex with Xylidyl Blue I (XBI) in a medium containing ethylenediamine, 1, 10-phenanthroline, oxalic acid and ninhydrin, at pH 10.5-11.5. The complex has been proved to be Th(XBI)/sub 2/, with log ..beta..'=9.6. The method can be used to determine trace amounts of thorium over the range 3.5x10/sup -8/-3x10/sup -6/M. The detection limit is 1x10/sup -8/M. A solvent extraction procedure is necessary to eliminate interference from several cations. The method has been applied to determination of traces of thorium in minerals, with good results.

  8. Determination of Trace Elements in Thai Cereal

    International Nuclear Information System (INIS)

    Permnamtip, Vorapot; Busamongkol, Arporn; Laoharojanaphand, Sirinart; Chaiyasith, Suwan

    2007-08-01

    Full text: Trace elements were analyzed in Thai cereal, e.g. rice and bean, by using neutron activation analysis (NAA). The selected cereals are major food items for Thai population. The data obtained from this work will be useful for nutrition and safety consumption of Thai cereal. Trace elements verified include Al, As, Br, Ca, Cd, Cl, Cr, Cu, Fe, I, K, Mg, Mn, Mo, Se, Sn, V and Zn. It was found that Al, As, Br, Cl, Cu, Fe, Mn, Zn, Ca, K and Mg are presented in the range of 2.2 to 35.7, 0.15 to 0.21, 0.44 to 13.5, 55.6 to 640.3, 16.3 to 16.5, 158.9 to 161.1, 12.2 to 55.7, 8.2 to 58.1 (g/g (ppm) , 0.02 to 0.28, 0.09 to 1.99 and 0.03 to 0.26 %, respectively. For Cd, Cr, I, Mo, Se, Sn and V were not found in sample because the concentrations were lower than detection limit. Precision and accuracy were determined by analyzing standard reference materials: NIST 1568a, NIST 8704, ACSP DORM-1, NIES No.9 and NMIJ 7302 to a

  9. Age determination of trace plutonium using liquid scintillation counting and α-spectrometry

    International Nuclear Information System (INIS)

    Chen Yan; Chang Zhiyuan; Zhao Yonggang; Li Jinghuai; Shu Fujun

    2010-01-01

    Liquid scintillation counting combined with α-spectrometry through measuring 241 Pu/ 241 Am ratio to determine the age of trace Pu was studied. The technique was explored for the age determination of nanogram grade Pu sample on the basis of Pu/Am separation. The ages of two Pu samples-one with known and the other with unknown age were determined by the method. The determined age by the method is in agreement with the reference value. The established method for determining the age of trace Pu can be adopted in the verification activities of nuclear safeguards and nuclear arms control. (authors)

  10. INAA Application for Trace Element Determination in Biological Reference Material

    Science.gov (United States)

    Atmodjo, D. P. D.; Kurniawati, S.; Lestiani, D. D.; Adventini, N.

    2017-06-01

    Trace element determination in biological samples is often used in the study of health and toxicology. Determination change to its essentiality and toxicity of trace element require an accurate determination method, which implies that a good Quality Control (QC) procedure should be performed. In this study, QC for trace element determination in biological samples was applied by analyzing the Standard Reference Material (SRM) Bovine muscle 8414 NIST using Instrumental Neutron Activation Analysis (INAA). Three selected trace element such as Fe, Zn, and Se were determined. Accuracy of the elements showed as %recovery and precision as %coefficient of variance (%CV). The result showed that %recovery of Fe, Zn, and Se were in the range between 99.4-107%, 92.7-103%, and 91.9-112%, respectively, whereas %CV were 2.92, 3.70, and 5.37%, respectively. These results showed that INAA method is precise and accurate for trace element determination in biological matrices.

  11. Determination of trace elements in airborne particulate matter. Pt. 2

    International Nuclear Information System (INIS)

    Pamuk, F.; Kahraman, N.; Kut, D.

    1975-04-01

    Several trace elements are being introduced into the atmosphere from various sources. Since many of the trace elements are highly toxic, the concentrations of them should be measured and controlled continuously for public health. Concentrations of trace elements have been determined in air samples collected from seven different districts of Ankara by the use of instrumental neutron activation analysis and atomic absorption spectrophotometer. (Pamuk, F.; Kahraman, N.; Kut, D.)

  12. Problems of determination of principle of psychological profile of unknown criminal person in investigational activity

    Directory of Open Access Journals (Sweden)

    Galina Getman

    2017-03-01

    By the author of the article of analysis different determinations of «psychological profile of unknown criminal person» were subjected. They are set positive lines and separate positions that in opinion of author are not expedient and important are subjected to criticism. That is why, the author points in conclusions the argued positions in relation to the necessity of the use of psychological profile of  unknown criminal person during investigation of criminal realizations in activity of investigator.

  13. Structure Determination of Unknown Organic Liquids Using NMR and IR Spectroscopy: A General Chemistry Laboratory

    Science.gov (United States)

    Pavel, John T.; Hyde, Erin C.; Bruch, Martha D.

    2012-01-01

    This experiment introduced general chemistry students to the basic concepts of organic structures and to the power of spectroscopic methods for structure determination. Students employed a combination of IR and NMR spectroscopy to perform de novo structure determination of unknown alcohols, without being provided with a list of possible…

  14. The separation and determination of trace elements in iron ore

    International Nuclear Information System (INIS)

    Jones, E.A.

    1977-01-01

    The separation, concentration, and determination of trace elements in iron ores are described. After the sample has been dissolved, the iron is separated by liquid-liquid extraction with a liquid cation-exchanger, di-(2-ethylhexyl) phosphoric acid. The trace elements aluminium, cadmium, calcium, chromium, cobalt, copper, lead, magnesium, manganese, mercury, potassium, sodium, vanadium, and zinc are determined in the aqueous phase by atomic-absorption spectrophotometry

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

    Science.gov (United States)

    Smith, K. Christopher; Garza, Ariana

    2015-01-01

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

  16. Trace elements determination in human hair

    International Nuclear Information System (INIS)

    Carrion, Jose

    1995-01-01

    Concentrations of Cu, Zn, Pb, Mg, Ca, Na, K, Mn, Cr, Ni, Co, V, Cd and Al, in human hair sampled from 23 young men during 24 months were determined by atomic absorption spectroscopy. Additional determination of mercury and volatile elements were made by using accessory MHS-10. Statistical treatment of data is presented for each person and element. The pre-treatment of hair carried out with an organic solvent to remove the superficial pollutants is explained. (The author)

  17. Determination of Sugar and Some Trace Metals Content in Selected ...

    African Journals Online (AJOL)

    Ten brands of commercial fruit juices were analyzed for pH, specific gravity, total solids, reducing sugar and total sugar trace metals contents. The pH was determined using a Hanna pH meter. Sugar content was determined using the Lane and Eynon method. Sodium and potassium were determined by flame photometry ...

  18. Application of trace element analysis to determine trace element concentrations in the field of medicine

    International Nuclear Information System (INIS)

    Kasperek, K.; Feinendegen, L.E.

    1976-01-01

    Applied trace elements research in medicine requires a sensitive and efficient technique of trace elements analysis such as, e.g., neutron activation analysis. Essential trace elements act as stabilisators (iron in haem), structural elements (silicium in fibrous tissue), in hormones (iodine in thyroid hormone), in vitamins (cobalt in vitamin B 12), and in enzymes. Most of the essential trace elements act as coenzymes or in coenzymes or directly as metabolic catalysators. For example, selenium deficiency in PKU and maple syrup patients receiving dietary treatment can be detected by determining the selenium content of the serum, while low selenium values in the whole blood indicate liver cirrhosis. Acrodermatitis enteropathica can be diagnosed by determinig zinc in the serum, and pancreatic insufficiency by determining zinc in the pancreatic juice. Zinc also plays a part in disturbances of growth, in the healing of wounds, and in the insulin metabolism. Cobalt is important in some types of anaemia and in myocardiopathies. Trace elements are also necessary in the treatment of diseases, e.g. iron cobalt in some types of anaemia, and zinc in the delayed healing of wounds in the postoperative phase and in acrodermatitis enteropathica. Chromium is now being tested for the treatment of diabetes mellitus, and fluorides may be of interest in the treatment of osteoporosis. Finally, trace elements are important in the aetiology of acute poisoning, in nutrition, and in environmental protection. (orig./AK) [de

  19. Application of trace element analysis to determine trace element concentrations in the field of medicine. [Neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Kasperek, K; Feinendegen, L E

    1976-01-01

    Applied trace elements research in medicine requires a sensitive and efficient technique of trace elements analysis, such as neutron activation analysis. Essential trace elements act as stabilizators (iron in haem), structural elements (silicon in fibrous tissue), in hormones (iodine in thyroid hormone), in vitamins (cobalt in vitamin B 12), and in enzymes. Most of the essential trace elements act as coenzymes or in coenzymes or directly as metabolic catalyzers. For example, selenium deficiency in PKU and maple syrup patients receiving dietary treatment can be detected by determining the selenium content of the serum, while low selenium values in the whole blood indicate liver cirrhosis. Acrodermatitis enteropathica can be diagnosed by determinig zinc in the serum, and pancreatic insufficiency by determining zinc in the pancreatic juice. Zinc also plays a part in disturbances of growth, in the healing of wounds, and in the insulin metabolism. Cobalt is important in some types of anaemia and in myocardiopathies. Trace elements are also necessary in the treatment of diseases, e.g. iron cobalt in some types of anaemia, and zinc in the delayed healing of wounds in the postoperative phase and in acrodermatitis enteropathica. Chromium is now being tested for the treatment of diabetes mellitus, and fluorides may be of interest in the treatment of osteoporosis. Finally, trace elements are important in the aetiology of acute poisoning, in nutrition, and in environmental protection.

  20. Determination of trace impurities in materials

    International Nuclear Information System (INIS)

    Parashar, D.C.

    1991-01-01

    Research work done at the National Physical Laboratory to develop new methods which are more specific and/or more sensitive has been reviewed. These methods are based on the use of existing facilities viz. atomic absorption spectrophotometry, uv-visible spectrophotometry, gas chromatography and conventional chemical methods. It is possible to determine impurities like boron at 5ppb level, phosphorus at 100 ppb and oxygen non-stoichiometry in 1:2:3 compounds with higher accuracy. Boron is determined spectrophotometrically by forming a complex with curcumin and phosphorus is determined indirectly by atomic absorption spectrophotometry by forming phosphomolybdate complex with antimony or bismuth which have 1:1 ratio with phosphorus in the complex. Gas chromatographic technique has been used to evaluate the oxygen non-stoichiometry in high temperature superconductors (1:2:3 compound) where the HTc sample is dissolved in dilute nitric acid in helium environment and the oxygen released is determined using thermal conductivity detector. (author). 19 refs., 3 figs., 4 tabs

  1. Spectrochemical determination of impurities and noble metal traces in carnallite

    International Nuclear Information System (INIS)

    Goldbart, Z.; Carmi, U.; Harrel, A.

    1978-02-01

    A spectrochemical method was developed for the determination of impurities and noble metal traces in carnallite by DC arc excitation. The investigated sample is brought to a standard form of potassium-magnesium sulphate mixed with graphite. Detection limits of 1-10 ppm were determined for 27 elements; the dynamical detection range is 1-400 ppm

  2. Determination of trace metals in river sediment

    International Nuclear Information System (INIS)

    Smith, R.

    1984-01-01

    This study forms part of the NIWR's series of interlaboratory comparison studies involving southern African laboratories engaged in water and wastewater analysis, and is concerned with the analysis by 21 laboratories of a standard reference sample of river sediment for arsenic, cadmium, cobalt, copper, lead, manganese, mercury, nickel and zinc. The results obtained are evaluated and discussed, along with some of the advantages and disadvantages of various sample pretreatment techniques. The mean values of the results obtained for Cu, Hg, Pb, Ni and Zn were found to be in good agreement with the certified values for the standard reference sample, but those for Cd and Mn were considerably lower than the corresponding certified values. A fairly wide range of acid extraction or digestion procedures for pretreatment of the sample was used by the participating laboratories, most of whom employed direct flame atomic absorption spectrophotometry for the measurement of Cd, Co, Cu, Pb, Mn, Ni, and Zn. The few laboratories who determined As and Hg did so mainly by means of vapour generation/atomic absorption techniques

  3. Trace determination of uranium in fertilizer samples by total ...

    Indian Academy of Sciences (India)

    Uranium is reported to be present in phosphate fertilizers. The recovery of uranium from the fertilizers is important because it can be used as fuel in nuclear reactors and also because of environmental concerns. For both these activities suitable method of uranium determinations at trace levels in these fertilizers are required.

  4. Determination of trace elements in urban airborne particulates (PM ...

    African Journals Online (AJOL)

    Assessment of the air quality in Newcastle upon Tyne, UK was performed by determining the trace element content in airborne particulates (PM10). Samples were collected over a 12 month period (March 2011 to April 2012) using two high volume air sampler provided with a PM10 size selective inlet. The concentrations of ...

  5. Determination of trace elements in electronic materials by NAA

    International Nuclear Information System (INIS)

    Kobayashi, Kenji

    1986-01-01

    Trace amounts of elements in electronic materials were determined by instrumental neutron activation analysis (INAA), re-activation analysis and substoichiometric radioactivation analysis using gamma-ray spectrometry. Ten elements (Cr, Cu, Fe, Zn, Co, Eu, Ir, Sb, Sc, Tb) in gallium arsenide single crystal were determined by INAA and substoichiometric radioactivation analysis. Trace level of chromium (10 13 atoms/cm 3 ) and zinc (10 14 atoms/cm 3 ) in gallium arsenide single crystal were determined by INAA. The chromium concentrations in horizontal Bridgmangrown semi-insulating gallium arsenide ingot were ranged from 1.2 x 10 16 atoms/cm 3 at seed end to 3.5 x 10 16 atoms/cm 3 at tail end. The trace determinations of iron (10 14 atoms/cm 3 ) and copper (10 14 atoms/cm 3 ) in silicon, gallium arsenide and indium phoshide single crystals were carried out by substoichiometric radioactivation analysis. The reactivation analysis for the multielement determination of indium phosphide single crystal was carried out and nineteen elements were determined simultaneously by gamma-ray spectrometry. Eleven elements (Ag, As, Br, Co, Cr, Fe, K, Mn, Sb, Sc, Zn) in four NIES standard reference materials (Pond Sediment, Chlorella, Mussel and Tea Leaves) and seven elements (Co, Cr, Eu, Fe, Sc, Tb, Yb) in two NBS glasses (SRM-615 and SRM-613) were determined by INAA and substoichiometric radioactivation analysis and the analytical results obtained by the methods were in good agreement with certified values by NIES and NBS. (author)

  6. The determination of an unknown boundary condition in a fractional diffusion equation

    KAUST Repository

    Rundell, William

    2013-07-01

    In this article we consider an inverse boundary problem, in which the unknown boundary function ∂u/∂v = f(u) is to be determined from overposed data in a time-fractional diffusion equation. Based upon the free space fundamental solution, we derive a representation for the solution f as a nonlinear Volterra integral equation of second kind with a weakly singular kernel. Uniqueness and reconstructibility by iteration is an immediate result of a priori assumption on f and applying the fixed point theorem. Numerical examples are presented to illustrate the validity and effectiveness of the proposed method. © 2013 Copyright Taylor and Francis Group, LLC.

  7. Experimental determination of the empirical formula and energy content of unknown organics in waste streams

    Energy Technology Data Exchange (ETDEWEB)

    Shizas, I. [Univ. of Toronto, Dept. of Civil Engineering, Toronto, Ontario (Canada); Kosmatos, A. [Ontario Power Generation, Toronto, Ontario (Canada); Bagley, D.M. [Univ. of Toronto, Dept. of Civil Engineering, Toronto, Ontario (Canada)

    2002-06-15

    Two experimental methods are described in this paper: one for determining the empirical formula, and one for determining the energy content of unknown organics in waste streams. The empirical formula method requires volatile solids (VS), chemical oxygen demand (COD), total organic carbon (TOC), and total Kjeldahl nitrogen (TKN) to be measured for the waste; the formula can then be calculated from these values. To determine the energy content of the organic waste, bomb calorimetry was used with benzoic acid as a combustion aid. The results for standard compounds (glucose, propionic acid, L-arginine, and benzoic acid) were relatively good. The energy content measurement for wastewater and sludges had good reproducibility (i.e. 1.0 to 3.2% relative standard deviation for triplicate samples). Trouble encountered in the measurement of the empirical formulae of the waste samples was possibly due to difficulties with the TOC test; further analysis of this is required. (author)

  8. Experimental determination of the empirical formula and energy content of unknown organics in waste streams

    International Nuclear Information System (INIS)

    Shizas, I.; Kosmatos, A.; Bagley, D.M.

    2002-01-01

    Two experimental methods are described in this paper: one for determining the empirical formula, and one for determining the energy content of unknown organics in waste streams. The empirical formula method requires volatile solids (VS), chemical oxygen demand (COD), total organic carbon (TOC), and total Kjeldahl nitrogen (TKN) to be measured for the waste; the formula can then be calculated from these values. To determine the energy content of the organic waste, bomb calorimetry was used with benzoic acid as a combustion aid. The results for standard compounds (glucose, propionic acid, L-arginine, and benzoic acid) were relatively good. The energy content measurement for wastewater and sludges had good reproducibility (i.e. 1.0 to 3.2% relative standard deviation for triplicate samples). Trouble encountered in the measurement of the empirical formulae of the waste samples was possibly due to difficulties with the TOC test; further analysis of this is required. (author)

  9. Spectrographic determination of traces of halogens; Dosage de traces d'halogenes par la methode spectrographique

    Energy Technology Data Exchange (ETDEWEB)

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

    1961-07-01

    Hollow cathode source is employed for determining traces of halogens (fluorine - chlorine) in the uranium oxide U{sub 3}O{sub 8} qualitatively, detection of at least 40 ppm of fluorine, as alkali fluoride and 125 ppm of chlorine, is possible. (author) [French] Un tube a decharge a cathode creuse a ete utilise pour la determination spectrographique des halogenes (fluor - chlore) presentes a l'etat de traces dans un oxyde d'uranium U{sub 3}O{sub 8}. On a pu deceler qualitativement des teneurs de 40 ppm de fluor sous forme de fluorures alcalins. En ce qui concerne le chlore, la plus faible teneur decelee a ete de 125 ppm. (auteur)

  10. ICP-AES determination of trace elements in carbon steel

    International Nuclear Information System (INIS)

    Sengupta, Arijit; Rajeswari, B.; Kadam, R.M.; Babu, Y.; Godbole, S.V.

    2010-01-01

    Full text: Carbon steel, a combination of the elements iron and carbon, can be classified into four types as mild, medium, high and very high depending on the carbon content which varies from 0.05% to 2.1%. Carbon steel of different types finds application in medical devices, razor blades, cutlery and spring. In the nuclear industry, it is used in feeder pipes in the reactor. A strict quality control measure is required to monitor the trace elements, which have deleterious effects on the mechanical properties of the carbon steel. Thus, it becomes imperative to check the purity of carbon steel as a quality control measure before it is used in feeder pipes in the reactor. Several methods have been reported in literature for trace elemental determination in high purity iron. Some of these include neutron activation analysis, atomic absorption spectrometry and atomic emission spectrometry. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is widely recognized as a sensitive technique for the determination of trace elements in various matrices, its major advantages being good accuracy and precision, high sensitivity, multi-element capability, large linear dynamic range and relative freedom from matrix effects. The present study mainly deals with the direct determination of trace elements in carbon steel using ICP-AES. An axially viewing ICP spectrometer having a polychromator with 35 fixed analytical channels and limited sequential facility to select any analytical line within 2.2 nm of a polychromator line was used in these studies. Iron, which forms one of the main constituents of carbon steel, has a multi electronic configuration with line rich emission spectrum and, therefore, tends to interfere in the determination of trace impurities in carbon steel matrix. Spectral interference in ICP-AES can be seriously detrimental to the accuracy and reliability of trace element determinations, particularly when they are performed in the presence of high

  11. Determination of Trace Concentration in TMD Detectors using PGAA

    Directory of Open Access Journals (Sweden)

    Tomandl I.

    2015-01-01

    Full Text Available Transmutation detectors could be alternative to the traditional activation detector method for neutron fluence dosimetry at power nuclear reactors. This new method require an isotopically highly-sensitive, non-destructive in sense of compactness as well as isotopic content, precise and standardly used analytical method for trace concentration determination. The capability of Prompt Gamma-ray Activation Analysis (PGAA for determination of trace concentrations of transmuted stable nuclides in the metallic foils of Ni, Au, Cu and Nb, which were irradiated for 21 days in the reactor core at the LVR-15 research reactor in Řež, is reported. The PGAA measurements of these activation foils were performed at the PGAA facility at Forschungs-Neutronenquelle Heinz Maier-Leibnitz (FRMII in Garching.

  12. Spectrographic Determination of Trace Constituents in Rare Earths

    International Nuclear Information System (INIS)

    Capdevila, C.; Alvarez, F.

    1962-01-01

    A spectrographic method was developed for the determination of 18 trace elements in lanthanum, cerium, praseodimium, neodimium and samarium compounds. The concentrations of the impurities cover the range of 0,5 to 500 ppm. Most of these impurities are determined by the carrier distillation method. Several more refractory elements have been determined by total burning of the sample with a direct current arc or by the conduction briquet excitation technique with a high voltage condensed spark. The work has been carried out with a Hilger Automatic Large Quartz Spectrograph. (Author) 5 refs

  13. Trace element impurity determination in aspirin tablets by INAA

    International Nuclear Information System (INIS)

    Miyoshi, E.K.; Saiki, M.

    2009-01-01

    Instrumental neutron activation analysis (INAA) was applied to assess trace element concentrations in six samples of aspirin tablets acquired in Sao Paulo city, Brazil. Concentrations of the elements Br, Ca, Co, Cr, Fe, K, La, Na, Sc and Zn were determined. Comparisons were made between the results obtained with published data for aspirins from foreign countries. Certified reference materials, INCT-MPH-2 Mixed Polish Herbs were analyzed for quality control of the analytical results. (author)

  14. Determination of trace elements in chicken feeds in Khartoum state

    International Nuclear Information System (INIS)

    Hassan, Salma Yahya Mohammed

    2017-03-01

    Trace elements are very important for chicken because thy contribute in biochemical processes required for normal growth, development and formation of the eggshell. The deficiency or the elevation of these trace elements may affect the normal physiological activity and biochemical process of their bodies. In this study the concentrations of trace elements in chicken feed samples were determined by X RF spectrometry. The results showed that there were 9 trace elements in sample ( K, Ca Mn, Fe Cu Zn, Pb, Rb, Sr) the mean concentration were K ( 2.12 x 10 4 ), Ca (2.22x10 4 ), Mn (48.1). Fe (191), Cu(9.81), Zn (24.6), Pb (1.63), Rb (7.79), Sr(4.09) ppm. Comparing the trace elements concentrations obtained in this study with the recommended values showed that some of them e.g Mn, Cu, Zn, Fe were found higher concentration than the recommended values, which stipulated by national research council NRC European Union. While lead concentration was in the permissible limit (5mg/kg). However, the statistical Alan's revealed than there were no significant difference between all concentrations of trace elements in the two types of chicken feeds i.e layer and broiler. The pearson correlation test displayed a strong correlation between K-Rb (0.885), Mn-Zn (0.874). The negative correlation between Mn-Rb (0.680), K-Mn (0.6000), K-Ca (0.565), Zn-Rb (-0.541). Ca-Rb (0.458) were found . Further investigations were performed using the principal component analysis (PCA) which involved the extraction of principal factor to study the total variance in the feed samples in terms of the trace elements concentrations in each. The obtained results revealed that the first principal component have a positive correlation with the elements Ca, Mn, Pb, and Zn, while K and Rb showed negative correlation with it. Similarly, the second principal compound showed positive correlation with the elements Mn, PB and Zn, while Ca and Sr showed negative, on the perth hand the third component was found to

  15. [Determination and correlation analysis of trace elements in Boletus tomentipes].

    Science.gov (United States)

    Li, Tao; Wang, Yuan-zhong; Zhang, Ji; Zhao, Yan-li; Liu, Hong-gao

    2011-07-01

    The contents of eleven trace elements in Boletus tomentipes were determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The results showed that the fruiting bodies of B. tomentipes were very rich in Mg and Fe (>100 mg x kg(-1)) and rich in Mn, Zn and Cu (>10 mg x kg(-1)). Cr, Pb, Ni, Cd, and As were relatively minor contents (0.1-10.0 mg x kg(-1)) of this species, while Hg occurred at the smallest content (< 0.1 mg x kg(-1)). Among the determined 11 trace elements, Zn-Cu had significantly positive correlation (r = 0.659, P < 0.05), whereas, Hg-As, Ni-Fe, and Zn-Mg had significantly negative correlation (r = -0.672, -0.610, -0.617, P < 0.05). This paper presented the trace elements properties of B. tomentipes, and is expected to be useful for exploitation and quality evaluation of this species.

  16. Chronocoulometric determination of trace levels of uranium in rocks

    International Nuclear Information System (INIS)

    Cantagallo, M.I.C.; Gutz, I.G.R.

    1990-01-01

    The chronocoulometric method for the determination of trace levels of uranium, based on the catalytic nitrate reduction was applied with real and synthetic samples. Reference materials with complex matrices like rocks were first solubilized by hot digestion under pressure in a PTFE bomb. When necessary, an adapted liquid-liquid extraction procedure was used for previous separation of interferents. The obtained results are in good agreement with the values obtained with other techniques such as X-ray fluorescence, mass spectrometry -isotope dilution and apithermal activation analysis. (author) [pt

  17. Direct Position Determination of Unknown Signals in the Presence of Multipath Propagation.

    Science.gov (United States)

    Du, Jianping; Wang, Ding; Yu, Wanting; Yu, Hongyi

    2018-03-17

    A novel geolocation architecture, termed "Multiple Transponders and Multiple Receivers for Multiple Emitters Positioning System (MTRE)" is proposed in this paper. Existing Direct Position Determination (DPD) methods take advantage of a rather simple channel assumption (line of sight channels with complex path attenuations) and a simplified MUltiple SIgnal Classification (MUSIC) algorithm cost function to avoid the high dimension searching. We point out that the simplified assumption and cost function reduce the positioning accuracy because of the singularity of the array manifold in a multi-path environment. We present a DPD model for unknown signals in the presence of Multi-path Propagation (MP-DPD) in this paper. MP-DPD adds non-negative real path attenuation constraints to avoid the mistake caused by the singularity of the array manifold. The Multi-path Propagation MUSIC (MP-MUSIC) method and the Active Set Algorithm (ASA) are designed to reduce the dimension of searching. A Multi-path Propagation Maximum Likelihood (MP-ML) method is proposed in addition to overcome the limitation of MP-MUSIC in the sense of a time-sensitive application. An iterative algorithm and an approach of initial value setting are given to make the MP-ML time consumption acceptable. Numerical results validate the performances improvement of MP-MUSIC and MP-ML. A closed form of the Cramér-Rao Lower Bound (CRLB) is derived as a benchmark to evaluate the performances of MP-MUSIC and MP-ML.

  18. Indirect Spectrophotometric Determination of Trace Quantities of Hydrazine

    Energy Technology Data Exchange (ETDEWEB)

    Shabani, A. M. Haji; Dadfarnia, S.; Dehghan, K. [Yazd University, Yazd (Iran, Islamic Republic of)

    2004-02-15

    An indirect, sensitive and accurate method for the determination of trace amounts of hydrazine is described. The method is based on the oxidation of hydrazine by a known excess of iodate in the presence of hydrochloric acid. The unreacted iodate is used in the oxidation of hydroxylamine to nitrite. Sulfanilic acid is diazotized by the nitrite formed. The resulting diazonium ion is coupled with N-(1-naphthyl)ethylenediamine to form a stable azo dye, which shows an absorption maximum at 540 nm. Hydrazine can be determined in the range of 20-400 ng mL{sup -1} with a detection limit of 3.1 ng mL{sup -1}. The relative standard deviation for 50, 200 and 400 ng mL{sup -1} of hydrazine is 2, 1.5 and 1.3%, respectively (n = 10). The method was applied to the determination of hydrazine in water samples

  19. Determination of trace arsenic on hanging copper amalgam drop electrode.

    Science.gov (United States)

    Piech, Robert; Baś, Bogusław; Niewiara, Ewa; Kubiak, Władysław W

    2007-04-30

    Hanging copper amalgam drop electrode has been applied for trace determination of arsenic by cathodic stripping analysis. Detection limit for As(III) as low as 0.33nM (0.02mug/L) at deposition time (240s) could be obtained. For seven successive determinations of As(III) at concentration of 5nM relative standard deviation was 2.5% (n=7). Interferences from selected metals and surfactant substances were examined. Absence of copper ions in sample solution causes easier optimization and makes method less vulnerable on contamination. The developed method was validated by analysis of certified reference materials (CRMs) and applied to arsenic determinations in natural water samples.

  20. Kinetic Spectrophotometric Determination of Trace Amounts of Sulfide

    Energy Technology Data Exchange (ETDEWEB)

    Barzegar, Mohsen [Tarbiat Modarres University, Tehran (Iran, Islamic Republic of); Jabbari, Ali [K. N. Toosi University, Tehran (Iran, Islamic Republic of); Esmaeili, Majid [Razi University, Kermanshah (Iran, Islamic Republic of)

    2003-09-15

    A method for the determination of trace amount of sulfide based on the addition reaction of sulfide with methyl green at pH 7.5 and 25 .deg. C is described. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of the dyestuff at 637 nm by the initial rate and fixed time method. The calibration graph is linear in the range 30-1200 ppb. The theoretical limit of detection was 0.014 ppm. Seven replicate analysis of a sample solution containing 0.70 ppm sulfide gave a relative standard deviation of 1.5%. The interfering effects of various ions on sulfide determination have been reported and procedures for removal of interference have been described. The proposed method was applied successfully to the determination of sulfide in tap and wastewater samples.

  1. Kinetic Spectrophotometric Determination of Trace Amounts of Sulfide

    International Nuclear Information System (INIS)

    Barzegar, Mohsen; Jabbari, Ali; Esmaeili, Majid

    2003-01-01

    A method for the determination of trace amount of sulfide based on the addition reaction of sulfide with methyl green at pH 7.5 and 25 .deg. C is described. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of the dyestuff at 637 nm by the initial rate and fixed time method. The calibration graph is linear in the range 30-1200 ppb. The theoretical limit of detection was 0.014 ppm. Seven replicate analysis of a sample solution containing 0.70 ppm sulfide gave a relative standard deviation of 1.5%. The interfering effects of various ions on sulfide determination have been reported and procedures for removal of interference have been described. The proposed method was applied successfully to the determination of sulfide in tap and wastewater samples

  2. Plutonium-236 traces determination in plutonium-238 by α spectrometry

    International Nuclear Information System (INIS)

    Acena, M.L.; Pottier, R.; Berger, R.

    1969-01-01

    Two methods are described in this report for the determination of plutonium-236 traces in plutonium-238 by a spectrometry using semi-conductor detectors. The first method involves a direct comparison of the areas under the peaks of the α spectra of plutonium-236 and plutonium-238. The electrolytic preparation of the sources is carried out after preliminary purification of the plutonium. The second method makes it possible to determine the 236 Pu/ 238 Pu ratio by comparing the areas of the α peaks of uranium-232 and uranium-234, which are the decay products of the two plutonium isotopes respectively. The uranium in the source, also deposited by electrolysis, is separated from a 1 mg amount of plutonium either by a T.L.A. extraction, or by the use of ion-exchange resins. The report ends with a discussion of the results obtained with plutonium of two different origins. (authors) [fr

  3. Spectrographic determination of trace impurities in reactor grade aluminium

    International Nuclear Information System (INIS)

    Chandola, L.C.; Machado, I.J.

    1975-01-01

    A spectrographic method enabling the determination of 21 trace impurities in aluminium oxide is described. The technique involves mixing the sample with graphite buffer in the ratio 1:1, loading it in a graphite electrode and arcing it for 30 sec. in a dc arc to 10 A current against a pointed graphite cathode. The spectra are photographed on Ilford N.30 emulsion employing a large quartz spectrograph. The aluminium line at 2669.2 A 0 serves as the internal standard. The impurities determined are Ag, B, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Mg, Mo, Ni, Pb, Sb, Si, Sn, Ti, V and Zn. The sensitivity varies from 5 to 100 ppm and the precision from +- 5 to +- 22% for different elements. A method for converting aluminium metal to aluminium oxide is described. It is found that boron is not lost during this conversion. (author)

  4. Direct Position Determination of Unknown Signals in the Presence of Multipath Propagation

    Science.gov (United States)

    Yu, Hongyi

    2018-01-01

    A novel geolocation architecture, termed “Multiple Transponders and Multiple Receivers for Multiple Emitters Positioning System (MTRE)” is proposed in this paper. Existing Direct Position Determination (DPD) methods take advantage of a rather simple channel assumption (line of sight channels with complex path attenuations) and a simplified MUltiple SIgnal Classification (MUSIC) algorithm cost function to avoid the high dimension searching. We point out that the simplified assumption and cost function reduce the positioning accuracy because of the singularity of the array manifold in a multi-path environment. We present a DPD model for unknown signals in the presence of Multi-path Propagation (MP-DPD) in this paper. MP-DPD adds non-negative real path attenuation constraints to avoid the mistake caused by the singularity of the array manifold. The Multi-path Propagation MUSIC (MP-MUSIC) method and the Active Set Algorithm (ASA) are designed to reduce the dimension of searching. A Multi-path Propagation Maximum Likelihood (MP-ML) method is proposed in addition to overcome the limitation of MP-MUSIC in the sense of a time-sensitive application. An iterative algorithm and an approach of initial value setting are given to make the MP-ML time consumption acceptable. Numerical results validate the performances improvement of MP-MUSIC and MP-ML. A closed form of the Cramér–Rao Lower Bound (CRLB) is derived as a benchmark to evaluate the performances of MP-MUSIC and MP-ML. PMID:29562601

  5. Direct Position Determination of Unknown Signals in the Presence of Multipath Propagation

    Directory of Open Access Journals (Sweden)

    Jianping Du

    2018-03-01

    Full Text Available A novel geolocation architecture, termed “Multiple Transponders and Multiple Receivers for Multiple Emitters Positioning System (MTRE” is proposed in this paper. Existing Direct Position Determination (DPD methods take advantage of a rather simple channel assumption (line of sight channels with complex path attenuations and a simplified MUltiple SIgnal Classification (MUSIC algorithm cost function to avoid the high dimension searching. We point out that the simplified assumption and cost function reduce the positioning accuracy because of the singularity of the array manifold in a multi-path environment. We present a DPD model for unknown signals in the presence of Multi-path Propagation (MP-DPD in this paper. MP-DPD adds non-negative real path attenuation constraints to avoid the mistake caused by the singularity of the array manifold. The Multi-path Propagation MUSIC (MP-MUSIC method and the Active Set Algorithm (ASA are designed to reduce the dimension of searching. A Multi-path Propagation Maximum Likelihood (MP-ML method is proposed in addition to overcome the limitation of MP-MUSIC in the sense of a time-sensitive application. An iterative algorithm and an approach of initial value setting are given to make the MP-ML time consumption acceptable. Numerical results validate the performances improvement of MP-MUSIC and MP-ML. A closed form of the Cramér–Rao Lower Bound (CRLB is derived as a benchmark to evaluate the performances of MP-MUSIC and MP-ML.

  6. New trace element determinations in the fingernails of ALS patients

    Energy Technology Data Exchange (ETDEWEB)

    Van Dalsem, D.J.; Ehmann, W.D. [Univ. of Kentucky, Lexington, KY (United States); Robinson, L. [Oak Ridge National Laboratory, TN (United States)

    1996-12-31

    Amyotrophic lateral sclerosis (ALS) afflicts 2 of every 100,000 people in the United States each year. A well-known example of ALS today is Stephen Hawking. He is a theoretical physicist, the author of A Brief History of Time, and is virtually immobilized by ALS. Diseases that cause progressive paralysis because of motor neuron degeneration in the central nervous system are termed motor neuron disorders (MND). Amyotrophic lateral sclerosis is a common form of MND. Pain-free, progressive muscular weakness is the most common clinical symptom. There is chronic weakness with atrophy of the affected muscles by the time the disease is diagnosed. Atrophy eventually results in wheelchair confinement and then only bed without the ability to speak or swallow. Death often occurs as a result of respiratory problems. Unlike other neurodegenerative diseases, in ALS the patient`s bladder and bowel control, eye movement, and mental faculties are preserved. The question today is whether or not certain trace elements are involved in the etiology or pathogenesis of ALS. A collaborative study was undertaken by the University of Kentucky and Oak Ridge National Laboratory (ORNL) using neutron activation analysis (NAA) to study trace element concentrations in ALS patients fingernails to determine if there existed statistically significant imbalances.

  7. Kinetic method of determination of rhodium trace amounts

    International Nuclear Information System (INIS)

    Kalinina, V.E.; Lyakushina, V.M.; Rybina, A.E.

    1978-01-01

    A catalytic action of rhodium compounds has been detected and studied in the reaction of copper (2) tellurate oxidation with hypobromite to ditelluratocuprate (3) in an alkaline medium. The relationships between the reaction rate and concentrations of copper, tellurate, and hypobromite have been established. The optimum concentrations of the used compounds have been found: Csub(Cu(2))=4x10 -5 g-ion/l; Csub(OHsup(-))=3.0 g-ion/l; Csub(Te)=1.4x10 -2 g-ion/l; Csub(NaBrO)=2.17x10 -3 M. It has been established for chloride, sulphate, and perchlorate solutions of rhodium (3) and (4) that the reaction sensitivity increases by 2-3-fold with a temperature rise from 25-60 deg C. The technique of determining rhodium traces has been developed based on its catalytic action. The low limit of determined rhodium amounts is about 10 -3 mkg/ml

  8. Use of X-Ray Fluorescence Spectrometry to Determine Trace ...

    African Journals Online (AJOL)

    This paper deals with application of X-ray fluorescence spectrometry for the detection of trace elements in graphic. An X-ray spectrometer was constructed and used to carry out measurements on graphite spheres impregnated with different chemical elements. The intensities of the lines of these trace elements, as function of ...

  9. The determination of a neutron source position in an unknown homogeneous medium: The planar case

    International Nuclear Information System (INIS)

    Dubinski, S.; Talmor, A.; Presler, O.; Tshuva, A.; Yaar, I.; Orion, I.; Alfassi, Z.B.

    2005-01-01

    The possibility of localization of an unknown neutron source in various bulky homogeneous media (box) was studied. For the planar case, two 3 He detectors on the opposite faces of the box were used. A constant polypropylene shield around the box and detectors was used to eliminate the varying contribution from the environment to increase count rates of the detectors and to protect the experimentalist. It is shown that the location of a single small neutron emitting source in a large box can be found to a better than 7% by using two neutron detectors positioned on parallel faces of the box, coplanar with the source. The localization requires measurement of the count rate of both the unknown source and an extra source positioned on one of the faces of the box. The localization is based on the finding that the ratio of the count rates of the two detectors is an exponential function of the distance of the source from one of the detectors

  10. Determination of trace elements by resonant ionization mass spectrometry (RIMS)

    International Nuclear Information System (INIS)

    Ruster, W.; Ames, F.; Rehklau, D.; Mang, M.; Muehleck, C.; Rimke, H.; Sattelberger, P.; Herrmann, G.; Trautmann, N.; Kluge, H.J.; Otten, E.W.

    1988-01-01

    A resonant ionization mass spectrometer has been developed as an analytical tool for the detection of trace elements, especially of plutonium and other radionuclides. The sample, deposited on a rhenium filament, is evaporated by electrical heating and the atoms of the element under investigation are selectively ionized by laser light delivered from three dye lasers pumped by a copper vapour laser. The resulting photoions are detected in a time-of-flight spectrometer with a channelplate detector. For plutonium a mass resolution of M/ΔM=1500 was obtained and an overall detection efficiency of 4x10 -6 was determined for stepwise excitation and ionization via autoionizing states. With a laser light bandwidth of 3-5 GHz neighbouring isotopes could be suppressed by a factor of 20 due to isotope shifts in the excitation transitions. The isotope composition of synthetic samples was measured and good agreement was found with mass spectroscopic results. The influence of the hyperfine structure on the isotope ratios is discussed. (orig.)

  11. Spectroscopic Determination of Trace Contaminants in High Purity Oxygen

    Science.gov (United States)

    Hornung, Steven D.

    2011-01-01

    Oxygen used for extravehicular activities (EVA) must be free of contaminants because a difference in a few tenths of a percent of argon or nitrogen content can mean significant reduction in available EVA time. These inert gases build up in the extravehicular mobility unit because they are not metabolized or scrubbed from the atmosphere. Measurement of oxygen purity above 99.5% is problematic, and currently only complex instruments such as gas chromatographs or mass spectrometers are used for these determinations. Because liquid oxygen boil-off from the space shuttle will no longer be available to supply oxygen for EVA use, other concepts are being developed to produce and validate high purity oxygen from cabin air aboard the International Space Station. A prototype optical emission technique capable of detecting argon and nitrogen below 0.1% in oxygen was developed at White Sands Test Facility. This instrument uses a glow discharge in reduced pressure gas to produce atomic emission from the species present. Because the atomic emission lines from oxygen, nitrogen, and argon are discrete and in many cases well-separated, trace amounts of argon and nitrogen can be detected in the ultraviolet and visible spectrum. This is a straightforward, direct measurement of the target contaminants and may lend itself to a device capable of on-orbit verification of oxygen purity. System design and optimized measurement parameters are presented.

  12. Microscopic age determination of human skeletons including an unknown but calculable variable

    DEFF Research Database (Denmark)

    Wallin, Johan Albert; Tkocz, Izabella; Kristensen, Gustav

    1994-01-01

    estimation, which includes the covariance matrix of four single equation residuals, improves the accuracy of age determination. The standard deviation, however, of age prediction remains 12.58 years. An experimental split of the data was made in order to demonstrate that the use of subgroups gives a false...

  13. Concentration of 24 Trace Elements in Human Heart Tissue Determined by Neutron Activation Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Wester, P O

    1964-06-15

    By means of neutron-activation analysis, human heart tissue from autopsy of 20 victims of traumatic accidents has been investigated with respect to the concentration of 24 different trace elements. A recently developed ion-exchange technique combined with gamma spectrometry has been used, which permits simultaneous determination of a large number of trace elements. The following trace elements have been determined quantitatively: Ag, As, Au, Ba, Br; Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Hg, La, Mo, Pt, Rb, Sb, Se, Se, Sm, Zn, W. In some heart samples, Hf and Os were determined qualitatively. The mean and standard deviation are given for the elements Cu, Fe, Se and Zn, Since none of the other quantitatively determined trace elements were normally distributed, the median is given as the central value. When possible, comparisons with values from other investigations have been made. No marked differences in the trace-element concentrations with age or sex could be detected.

  14. Concentration of 24 Trace Elements in Human Heart Tissue Determined by Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Wester, P.O.

    1964-06-01

    By means of neutron-activation analysis, human heart tissue from autopsy of 20 victims of traumatic accidents has been investigated with respect to the concentration of 24 different trace elements. A recently developed ion-exchange technique combined with gamma spectrometry has been used, which permits simultaneous determination of a large number of trace elements. The following trace elements have been determined quantitatively: Ag, As, Au, Ba, Br; Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Hg, La, Mo, Pt, Rb, Sb, Se, Se, Sm, Zn, W. In some heart samples, Hf and Os were determined qualitatively. The mean and standard deviation are given for the elements Cu, Fe, Se and Zn, Since none of the other quantitatively determined trace elements were normally distributed, the median is given as the central value. When possible, comparisons with values from other investigations have been made. No marked differences in the trace-element concentrations with age or sex could be detected

  15. Determining trace element in hair of children with mental retardation

    International Nuclear Information System (INIS)

    Wang Zhilan; Gu Bomei; Jia Meixiang

    1992-01-01

    Seven trace elements in the hair come from 29 mental retardation children and 29 normal children have been analysed by INAA and XRF. There are significant differences for Fe and Sc between the two groups. The average value of Pb in the hair of the mental retardation children is higher than that of the normal children. Although Zn is very important for children growing, there is no significant difference between two children groups

  16. Determination of toxic trace elements in body fluid reference samples

    International Nuclear Information System (INIS)

    Gills, T.E.; McClendon, L.T.; Maienthal, E.J.; Becker, D.A.; Durst, R.A.; LaFleur, P.D.

    1974-01-01

    The measurement of elemental concentration in body fluids has been widely used to give indication of exposures to certain toxic materials and/or a measure of body burden. To understand fully the toxicological effect of these trace elements on our physiological system, meaningful analytical data are required along with accurate standards or reference samples. The National Bureau of Standards has prepared for the National Institute for Occupational Safety and Health (NIOSH) a number of reference samples containing selected toxic trace elements in body fluids. The reference samples produced include mercury in urine at three concentration levels, five elements (Se, Cu, As, Ni and Cr) in freeze-dried urine at two levels, fluorine in freeze-dried urine at two levels and lead in blood at two concentration levels. These reference samples have been found to be extremely useful for the evaluation of field and laboratory analytical methods for the analysis of toxic trace elements. In particular the use of at least two calibration points (i.e., ''normal'' and ''elevated'' levels) for a given matrix provides a more positive calibration for most analytical techniques over the range of interest for occupational toxicological levels of exposure. (U.S.)

  17. Trace elements in natural drugs determined by INAA

    International Nuclear Information System (INIS)

    Chen Kehshaw; Tseng Chialiang; Lin Tehsien

    1993-01-01

    Natural drugs are widely used for diuretic, phlegm elimination and stomach invigoration purposes. Seventy-five of the most common remedies used by Chinese people have been subjected to trace element survey analysis by instrumental neutron activation. Within this large number of different natural products, fourteen trace elements (K, Sc, Cr, Fe, Co, Zn, Br, Rb, Cs, La, Sm, Eu, Au and Th) are commonly detected. Among these elements, Fe had the highest concentration followed by Zn, and Rb, Sm, Eu and Au were found to have the lowest concentrations. Although the three groups of natural drugs exhibit a widely different therapeutic action, the concentration ranges of the fourteen elements were very similar. While this suggests no apparent specific role for the trace elements in the drug function, parallels are drawn between the known drug related functions of Rb, Zn, Br, Fe, Co and K and the levels of elements found in the natural drugs. It is concluded that the various natural drugs also provide human benefits through supplements of essential elements such as Fe, Zn, Cr, Sc, Rb and Co. (author) 13 refs.; 5 tabs

  18. Determination of trace elements in cockle Anadara Granosa L. using INAA

    International Nuclear Information System (INIS)

    Ibrahim, Noorddin

    1994-01-01

    This study determines the trace metal content in Anadara Granosa L., a popular seafood amongst South-East-Asians. Using the technique of instrumental neutron activation analysis (INAA) identification has been made of the presence of 17 trace metals including elements which are classified as toxic (As, Br, Cs) and those which are rare-earths (Eu, Ce, Lu, Tb, Yb). (author)

  19. Determination of refractory trace elements in Chinese meteorites by RNAA

    International Nuclear Information System (INIS)

    Kraehenbuehl, U.; Burger, M.

    1989-01-01

    Some refractory trace elements are important target elements for spallation reactions in meteorites. These elements also serve to characterize the investigated meteorites. The elements Ti, Y, Zr, Hf, W and Ta were measured after radiochemical separation in chondrites from China. After acid digestion of the irradiated samples, the group separations were obtained by precipitation reactions. The necessary radiochemical purification of the pure β emitter Y was realized on a Lewatite OC 1026 column. For all the other elements discrete gamma radiation was measured. (orig.)

  20. Accuracy of trace element determinations in alternate fuels

    Science.gov (United States)

    Greenbauer-Seng, L. A.

    1980-01-01

    A review of the techniques used at Lewis Research Center (LeRC) in trace metals analysis is presented, including the results of Atomic Absorption Spectrometry and DC Arc Emission Spectrometry of blank levels and recovery experiments for several metals. The design of an Interlaboratory Study conducted by LeRC is presented. Several factors were investigated, including: laboratory, analytical technique, fuel type, concentration, and ashing additive. Conclusions drawn from the statistical analysis will help direct research efforts toward those areas most responsible for the poor interlaboratory analytical results.

  1. Simultaneous Determination of 30 Trace Elements in Cancerous and Noncancerous Human Tissue Samples with Gamma-ray Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Samsahl, K; Brune, D; Wester, P O

    1963-10-15

    The following trace elements were quantitatively determined by gamma-ray spectrometry in T samples of non-cancerous and 5 samples of cancerous human tissue: P, Ca, Cr, Fe, Co, Cu, Zn, As, Se, Br, Rb, Mo, Ag, Cd, Sb, Cs, La, Au, and Hg. In some of the samples the following elements were qualitatively determined: Ti+Sc, Ga, Sr, In, Ba, Ce, Hf, Os, Pt, and U. Most of the trace elements were found to be present in much higher concentrations in the non-cancerous than in the corresponding cancerous liver samples. In a typical run one sample each of cancerous and non-cancerous tissue was irradiated together with standards of the elements to be determined in a thermal flux of 2.10{sup 13} n/cm{sup 2}/sec. for 24 hours. The radioactive trace elements were separated into 16, and in some cases 18, groups by means of a chemical group separation method. Subsequently, the gamma spectrometric measurements were performed. Two persons can manage the chemical separations and measure the different activities from a run in 1,5 days. A new method of comparing unknown samples with standards was developed.

  2. Determination of trace Np and Pu by ICP-MS with extraction chromatography in emergency situations

    International Nuclear Information System (INIS)

    Yanqin, Ji; Qing, Tian; Baoming, Shen; Xianzhang, Shao

    2008-01-01

    Full text: An accurate determination of radioculides from various sources in the environmental samples is essential for assessment of the potential hazards and suitable countermeasures both in case of accidents, authorised release and routine surveillance. However, the concentrationof neptunium and plutonium is extremely low in environmental samples, and such samples have a complex matrix composition, which is to be taken into account for a proper analysis. Conventional radiochemical methods such as alpha spectrometry, neutron activation analysis, liquid, liquid scintillation system, fission track and gamma spectrometry for the quantitative determination of neptunium and plutonium often require complicated and time-consuming sample preparation and separation procedures. Due to the large amount of the complex and often unknown matrix, the analysis may also be covered by naturally occurring radionuclides. With the development of new analysis techniques, non-radioactive methods are increasingly used for the determination of trace or ultra-trace radionuclides in environmental samples. Inductively coupled plasma mass spectrometry (ICP-MS) is one of the most suitable analysis techniques for the measurement of the long-lived radionuclides with its high sensitivity, low detection limits, short analysis time, less chemical interferences and multi-elemental capability. The throughput is therefore very high (approx.100 samples a day). The main objective of the present study was to set up of a simple, fast separation procedure to measure Np and Pu in the environmental samples ICP-MS. An unique extraction chromatographic column (TOA: tri-n-octylamine on Teflon powder) with a two-stage sample loading was prepared to separate Np and Pu from the environmental matrix. Np and Pu were efficiently retained in 4 M HNO 3 medium on the column and easiy eluted with 0.02 M oxalic acid 0.16 M HNO 3 at 95 C degree. The separated solutions were free from most of the matrix elements and were

  3. Quantitative determination of minor and trace elements in rocks and soils by spark source mass spectrometry

    International Nuclear Information System (INIS)

    Ure, A.M.; Bacon, J.R.

    1978-01-01

    Experimental details are given of the quantitative determination of minor and trace elements in rocks and soils by spark source mass spectrometry. The effects of interfering species, and corrections that can be applied, are discussed. (U.K.)

  4. Non-destructive determination of trace elements. Final progress report

    International Nuclear Information System (INIS)

    Anderson, D.L.; Gordon, G.E.; Zoller, W.H.; Walters, W.B.; Lindstrom, R.M.

    1984-05-01

    In the course of this project we have successfully designed, built, and tested the first neutron beam facility dedicated to routine multielement neutron capture prompt-γ activation analysis (PGAA). This technique is capable of accurately measuring concentrations of up to 20 elements in a number of sample types, and is an extremely valuable complement to instrumental neutron activation analysis (INAA) and other analytical methods. We have found PGAA to have some major advantages over INAA: (1) the sample is subjected to neutron fluxes about five orders of magnitude less than in PGAA, with essentially no radiation or heating damage; (2) as the data are taken during sample irradiation, analyses can be performed immediately instead of waiting up to four weeks as in INAA; (3) it is capable of measuring all major elements, except oxygen, in many samples, including H, C, N, and Si, which cannot be done by INAA; and (4) it is especially sensitive for the trace elements B, Cd, Sm and Gd. In addition, we have characterized the overall capabilities of PGAA and the corrections necessary to make it an extremely accurate technique. We have applied PGAA in a number of studies in which it has proved to be extremely valuable and, at times, even providing crucial information that other techniques were incapable of supplying. 1 fig., 6 tabs

  5. Spectroscopic Determination of Trace Contaminants in High-Purity Oxygen

    Science.gov (United States)

    Hornung, Steven

    2013-01-01

    Oxygen used for extravehicular activities (EVAs) must be free of contaminants because a difference in a few tenths of a percent of argon or nitrogen content can mean significant reduction in available EVA time. These inert gases build up in the extravehicular mobility unit because they are not metabolized or scrubbed from the atmosphere. A prototype optical emission technique capable of detecting argon and nitrogen below 0.1% in oxygen has been developed. This instrument uses a glow discharge in reduced-pressure gas to produce atomic emission from the species present. Because the atomic emission lines from oxygen, nitrogen, and argon are discrete, and in many cases well-separated, trace amounts of argon and nitrogen can be detected in the ultraviolet and visible spectrum. This is a straightforward, direct measurement of the target contaminants, and may lend itself to a device capable of on-orbit verification of oxygen purity. A glow discharge is a plasma formed in a low-pressure (1 to 10 Torr) gas cell between two electrodes. Depending on the configuration, voltages ranging from 200 V and above are required to sustain the discharge. In the discharge region, the gas is ionized and a certain population is in the excited state. Light is produced by the transitions from the excited states formed in the plasma to the ground state. The spectrum consists of discrete, narrow emission lines for the atomic species, and broader peaks that may appear as a manifold for molecular species such as O2 and N2, the wavelengths and intensities of which are a characteristic of each atom. The oxygen emission is dominated by two peaks at 777 and 844 nm.

  6. Trace determination of uranium in fertilizer samples by total ...

    Indian Academy of Sciences (India)

    the fertilizers is important because it can be used as fuel in nuclear reactors and also because of en- vironmental concerns. ... The amounts of uranium in four fertilizer samples of Hungarian origin were determined by ... TXRF determination of uranium from phosphate fertilizers of Hungarian origin and the preliminary results ...

  7. General procedure for the determination of trace amounts of iodine in natural water samples of unknown composition by spectrophotometric titration

    International Nuclear Information System (INIS)

    Pesavento, M.; Profumo, A.

    1985-01-01

    Concentrated hydrochloric acid is added to samples of natural waters containing 2 x 10 -7 to 5 x 10 -5 M iodine and the solutions are then oxidised with hydrogen peroxide on a boiling water-bath. They are then reduced with sodium sulphite, which is subsequently removed by bubbling a stream of inert gas through the solution. All of the inorganic iodine, now present in the solution in the -1 oxidation state, can be titrated spectrophotometrically with standard potassium iodate solution, following a method previously described in which interferences from oxidants and reductants are eliminated. (author)

  8. General procedure for the determination of trace amounts of iodine in natural water samples of unknown composition by spectrophotometric titration

    Energy Technology Data Exchange (ETDEWEB)

    Pesavento, M.; Profumo, A. (Pavia Univ. (Italy). Dip. di Chimica Generale)

    1985-02-01

    Concentrated hydrochloric acid is added to samples of natural waters containing 2 x 10/sup -7/ to 5 x 10/sup -5/ M iodine and the solutions are then oxidised with hydrogen peroxide on a boiling water-bath. They are then reduced with sodium sulphite, which is subsequently removed by bubbling a stream of inert gas through the solution. All of the inorganic iodine, now present in the solution in the -1 oxidation state, can be titrated spectrophotometrically with standard potassium iodate solution, following a method previously described in which interferences from oxidants and reductants are eliminated.

  9. Determination of trace elements in KRISS biological CRMs by INAA

    International Nuclear Information System (INIS)

    Cho, Kyung Haeng; Park, Kwang Won; Zeisler, Rolf

    2005-01-01

    Two biological Certified Reference Materials (CRMs), KRISS 108-04-001 (oyster tissue) and 108-05-001 (water dropwort stem), were prepared by Korea Research Institute of Standards and Science (KRISS) during FY '01. The certified values of these materials had been determined by Isotope Dilution Mass Spectrometry (IDMS) for six elements (Cd, Cr, Cu, Fe, Pb and Zn). Additional analytical works are now progressing to certify the concentrations of a number of the environmental and nutrimental elements in these CRMs. The certified values in a CRM are usually determined by using a single primary method with confirmation by other method(s) or using two independent critically-evaluated methods. Instrumental Neutron Activation Analysis (INAA) plays an important role in determination of certified values. INAA procedure was used in determination of 20 elements in these two biological CRMs to acquire the concentration information and the results were compared with KRISS certified values

  10. Determination of traces of phosphorus using isotope exchange

    International Nuclear Information System (INIS)

    Zeman, A.; Kratzer, K.

    1976-01-01

    A simple and selective radioanalytical method for the determination of phosphorus (0.015 - 5 μg in a 5 ml sample), based on the heterogeneous isotope exchange, has been developed. The sample containing phosphorus is shaken in the presence of molybdate with a standard solution of tetraphenylarsonium molybdophosphate labelled with phosphorus-32 in 1-2 dicloroethan. From the distribution of the activity between the aqueous and organic phases the amount of phosphorus in the sample can be determined. (Authors)

  11. PIXE determination of essential trace elements in some traditional Chinese medicines

    International Nuclear Information System (INIS)

    Xiao, L.; Qin, J.F.

    1990-01-01

    The essential trace elements in 30 traditional Chinese medicines, (24 tonics and 6 nontonics) were determined by proton-induced X-ray emission. The authors' previous suggestion that traditional Chinese medicines may be classified by the order of magnitude of their essential trace elements, thus indicating their pharmacological effects, is not justified. The pharmacological effect of a trace element or its essentiality may be dependent on some ligand that can be chelated with it. A nonlinear mapping algorithm, however, shows that the 30 traditional Chinese medicines are nearly separated into two groups, indicating their tonic or nontonic pharmacological effects

  12. Determination of uranium traces in fuel cans of nuclear reactors

    International Nuclear Information System (INIS)

    Acosta L, C.E.; Benavides M, A.M.; Sanchez P, L.A.; Nava S, G.F.

    1997-01-01

    The objective of this work is to quantify the uranium content that as impurity can be found in zircon and zircaloy alloys which are used in the construction of fuel cans. The determination of this serves as a quality control measure due to that the increment of uranium content in alloy, diminishing the corrosion resistance. The fluorimetric method was used to do this determination. It is a very sensitive, reliable, rapid method also high reproducibility and repeatability as well as low detection limits (0.25 mg/kg). (Author)

  13. Integration of Solid-phase Extraction with Electrothermal Atomic Absorption Spectrometry for Determination of Trace Elements

    OpenAIRE

    NUKATSUKA, Isoshi; OHZEKI, Kunio

    2006-01-01

    An enrichment step in a sample treatment is essential for trace analysis to improve the sensitivity and to eliminate the matrix of the sample. Solid-phase extraction (SPE) is one of the widely used enrichment technique. Electrothermal atomic absorption spectrometry (ETAAS) is a well-established determination technique for trace elements. The integration of SPE with ETAAS leads to further improvement of sensitivity, an automation of the measurement and the economy in the sample size, amounts o...

  14. Characterization of prehistoric pottery from the Tremiti Isles by trace elements determination

    International Nuclear Information System (INIS)

    Brandone, A.; Fumo, P.; Giacco, M.; Oddone, M.; Riganti, V.; Baldi, M

    1993-01-01

    The potteries found on the Tremiti Isles (Italy, Adriatic Sea) have been characterized through their trace elements content. The goal of the work was to find out the number of ore deposits that supplied the clay used to manufacture the pottery. Neutron activation analysis has been employed for trace elements content determinations; the results have been statistically evaluated, clusterized and discussed. (author) 13 refs.; 1 fig.; 3 tabs

  15. Report on intercomparison A-13 of the determination of trace elements in freeze dried animal blood

    International Nuclear Information System (INIS)

    Pszonicki, L.; Hanna, A.N.; Suschny, O.

    1983-03-01

    This document deals with the comparative evaluation of the analytical data on the trace elements in beef blood obtained by 38 laboratories in 23 countries. The evaluations were based on 799 laboratory mean values of concentration of 41 elements. It was one of the series of IAEA intercomparisons on the determination of trace elements in animal materials. It was organized for the purpose of assisting the participating laboratories to check the accuracy of their work and to prepare a new reference material

  16. New trace element determinations in the fingernails of ALS patients

    Energy Technology Data Exchange (ETDEWEB)

    Van Dalsem, D.J.; Robinson, L. [Oak Ridge National Lab., TN (United States); Ehmann, W.D. [Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry

    1996-02-01

    ORNL`s High Flux Isotope Reactor was used in a neutron activation analysis experiment to determine selected elemental composition of fingernails from patients afflicted with amyotrophic lateral sclerosis (AL). While no statistical difference were found in aluminium a suggestive difference was observed for copper concentrations.

  17. Uranium coulometric titration. Application to the determination of traces

    International Nuclear Information System (INIS)

    Bergey, C.

    After a description of the device, the means developed to improve the titration method are presented. Coulometry enables to determine U with an accuracy of 0,1% in samples of only several tenths of a milligram. This method is rapid but not intended for routine analysis [fr

  18. New trace element determinations in the fingernails of ALS patients

    International Nuclear Information System (INIS)

    Van Dalsem, D.J.; Robinson, L.; Ehmann, W.D.

    1996-01-01

    ORNL's High Flux Isotope Reactor was used in a neutron activation analysis experiment to determine selected elemental composition of fingernails from patients afflicted with amyotrophic lateral sclerosis (AL). While no statistical difference were found in aluminium a suggestive difference was observed for copper concentrations

  19. Kinetic spectrophotometric determination of trace amounts of selenium and vanadium

    Energy Technology Data Exchange (ETDEWEB)

    Safavi, A.; Sedghy, H.R.; Shams, E. [Dept. of Chemistry, Shiraz Univ. (Iran)

    1999-11-01

    A sensitive kinetic spectrophotometric method has been developed for the determination of Se(IV) over the range of 45 to 4000 ng in 10 mL of solution. The method is based on the catalytic effect of Se(IV) on the reduction reaction of bromate by hydrazinium dichloride, with subsequent reaction of Ponceau S with products of the above reaction (chlorine and bromine), causing color changing of Ponceau S. Method development includes optimization of time interval for measurement of slope, pH, reagents concentration, and temperature. The optimized conditions yielded a theoretical detection limit of 33 ng/10 mL of solution of Se(IV). The interfering effects were studied and removed. The method was applied to the determination of selenium in spiked water, Kjeldahl tablet, selenium tablet, and shampoo. Vanadium(V) has an inhibition effect on the catalyzed reaction of bromate and hydrazine by selenium. Using this effect, V(V) can be determined in the range of 70 to 2500 ng in 10 mL of solution. The optimization procedure includes pH and selenium concentration. An extraction method was used for interference removal. The method was applied to the determination of vanadium in petroleum. (orig.)

  20. Determination of uranium traces in nuclear cans of nuclear reactors

    International Nuclear Information System (INIS)

    Acosta L, E.; Benavides M, A.M.; Sanchez P, L.

    1996-01-01

    To quantify the uranium content as impurity can be found in zirconium alloys and zircaloy, utilized to construct the sheaths containing fuels of the reactors of nuclear plants. The determination by fluorescence spectroscopy was employed as quality control measurement, at once the corrosion resistance, diminish with the increase of the uranium content in the alloys. (Author)

  1. Developing methods of determining unknown roational periods of asteroids via observations of (3122) Florence by the Harvard Observing Project

    Science.gov (United States)

    Abrams, Natasha Sarah; Bieryla, Allyson; Gomez, Sebastian; Huang, Jane; Lewis, John; Todd, Zoe; Alam, Munazza; Carmichael, Theron; Garrison, Lehman H.; Weaver, Ian; Chen, Chen; McGruder, Chima; Medina, Amber

    2018-06-01

    (3122) Florence is an asteroid that made the headlines with its close approach to Earth in late 2017. It is one of the biggest and brightest near-Earth asteroids that has been discovered and it has recently been found to have two moons. By observing the light reflected off an asteroid, we can measure its brightness over time and determine the rotational period of the asteroid. An asteroid’s rotational period can reveal information about its physical characteristics, such as its shape, and further our knowledge about processes that contribute to asteroid rotation in general. The Harvard Observing Project (HOP) is an initiative that allows undergraduates to learn about observational astronomy and take part in formal data collection and analysis. Over the course of the fall 2017 semester, HOP obtained four multi-hour, continuous observations in the R-band of the asteroid using the Harvard University 16-inch Clay Telescope. In our analysis, we reduced the images and performed astrometry and photometry on the data. The asteroid’s light curve was produced using AstroImageJ and we used the Python package gatspy to determine its rotational period. We found the rotational period to be 2.22 hours +/- 0.25, which agrees with the known rotational period of 2.3580 hours +/- 0.0002. This spring 2018 semester we are applying our methods to data collected on asteroids with unknown rotational periods and plan to present our findings.

  2. Determination of fluorine trace amounts in metallic uranium

    Energy Technology Data Exchange (ETDEWEB)

    Kukisheva, T N; Bolshakova, A S; Yefimova, N S

    1976-05-01

    A simple and rapid method was proposed for the determination of fluorine in metallic uranium without the removal of the latter. The method is based on the weakening of the color intensity of a complex of zirconium with xylenol orange in the presence of fluorine in a 1 N solution with respect to hydrochloric acid. For preparation for photometry, the solution to be analyzed is neutralized with ammonia to a pH of approximately 3. It is suggested that a complex of sulfosalicylic acid with uranium (VI) be used as the indicator in neutralization. The required acidity in the solution subjected to photometry is provided by the addition of a 5 N hydrochloric acid solution of zirconium. The coefficient of variation V/sub 15/ (at a fluorine content 3x10/sup -3/%) is 10%. In 7 h, 15-20 determinations can be performed.

  3. Indirect spectrophotometric determination of trace cyanide with cationic porphyrins.

    Science.gov (United States)

    Ishii, H; Kohata, K

    1991-05-01

    Three highly sensitive methods for the determination of cyanide have been developed, based on the fact that the complexation of silver ions with three cationic porphyrins, 5,10,15,20-tetrakis-(1-methyl-2-pyridinio)porphine [T(2-MPy)P], 5,10,15,20-tetrakis(1-methyl-3-pyridinio)porphine [T(3-MPy)P] and 5,10,15,20-tetrakis(1-methyl-4-pyridinio)porphine [T(4-MPy)P], in alkaline media is inhibited by cyanide and the decrease in absorbance of the silver(II) complex is proportional to the cyanide concentration. Sensitivities of the procedures developed are 0.133, 0.126 and 0.234 ng/cm(2), respectively for an absorbance of 0.001. Cadmium(II), copper(II), mercury(II), zinc(II), iodide and sulfide interfere with the cyanide determination. One of the proposed methods was applied to the determination of cyanide in waste-water samples, with satisfactory results.

  4. Determination of trace elements in drinking tea by various analytical techniques

    International Nuclear Information System (INIS)

    Wang Chufang; Ke Chenghsiung; Yang Jenqyann

    1993-01-01

    Tea has been one of the most popular simulating beverages which is both heavily produced and consumed in Taiwan. The determination of minor or trace elements in drinking tea and tea leaves is therefore important for estimating the daily intake of Taiwanese considered as a safety indicator. In order to accurately and precisely determine the concentrations of trace elements in samples, several analytical methods such as AAS, NAA and ICP-AES are suggested. This paper attempts to utilize all three methods to determine the concentrations of minor or trace elements in different types of tea leaves and the extracts percolated from them. The influence of fermentation processes on the concentration levels of minor or trace elements in tea samples is investigated. Because only free metal ions are bioavailable for the human body, it is necessary to determine their concentrations in drinking tea. The dissolution of trace elements in drinking tea is therefore studied by simulating the common Chinese style of tea percolation. Concentrations of thirteen elements including Zn, Mn, Ca, Cu, Ni, Al, K, Mg, Cd, Pb, Na, Co and Sc are determined. (author) 14 refs.; 1 fig.; 6 tabs

  5. Determination of trace metals in natural fresh waters

    International Nuclear Information System (INIS)

    Holm, K.; Borg, H.; Korhonen, M.

    1989-06-01

    The determination method still most widely used is atomic absorption spectrometry with graphite furnace. The natural levels of several elements are however too low to be accurately determined without any preconcentration. Besides, in sea water, the high salt content causes matric effects, which require time consuming separation steps as solvent extraction or ion exchange. The report describes two procedures for preconcentration of fresh water samples, freeze-drying and replicate injections in the furnace, respectively. The procedures are designed to be used on a routine basis. All water samples are collected in polypropylene bottles which are soaked before use in HCl 1+1, rinsed and allowed to stand until use filled with 0.1 M HNO 3 . The samples are preserved by addition of conc. HNO 3 (2 ml/l, sub boiling distilled). In the freeze-drying procedure, the samples are weighed and frozen in the pre-weighed polypropylene sampling bottles and evaporated to about one tenth of the original volume in the vaccum chamber of a freeze dryer. The samples are then weighed again for determination of the concentration factor and alayzed by graphite furnace AAS. When using the other procedure, the water samples are directly injected into the frunace for several times (2-8) before atomization and measurement of the absorption signal. The drying and ashing step is allowed to proceed after every injection. Comparisons of the two procedures have shown good agreement. The advantage of the replicate injection technique is primarily that the concentration factor is more esily controlled and repeated than by the freeze drying procedure. Further, the latter procedure sometimes suffers from precipitates being formed during the evaporation,especially in humic waters rich in iron. (12 figs., 7 tabs., 14 refs.)

  6. Flow injection kinetic spectrofluorimetric determination of trace amounts of osmium

    Science.gov (United States)

    Tang, Bo; Zhang, Hui; Wang, Yan

    2005-07-01

    A flow injection (FI) kinetic spectrofluorimetric method is described for the determination of osmium(IV) and the possible mechanism of catalytic reaction is discussed. The method is based on the fluorescence enhancing reaction of o-vanillin furfuralhydrazone (OVFH) with potassium bromate, which is catalyzed by Os(IV) in water medium at pH 6.10 and 45 °C. OVFH is newly synthesized and its ionization, IR and elemental analysis are established. Under these experimental conditions, the oxidized product of OVFH has excitation and emission maxima at 337 and 490 nm, respectively. The linear range of this method is 0-600 ng ml -1 with the R.S.D. of 1.2%. The detection limit is 1.0 ng ml -1 of Os(IV). A high analysis rate of 24 samples h -1 is obtained by the FI method. The proposed method is applied successfully to determine Os(IV) in synthetic mixture and mineral samples, and the results are well consistent with the standard values.

  7. Trace Level Determination of Polyether Ionophores in Feed

    Science.gov (United States)

    Rokka, Mervi; Jestoi, Marika; Peltonen, Kimmo

    2013-01-01

    A liquid chromatography-mass spectrometric method was developed and validated to determine six polyether ionophores (lasalocid sodium, monensin sodium, salinomycin sodium, narasin, maduramicin ammonium alpha, and semduramicin sodium) in feed samples. The method developed was very straightforward, involving extraction with 84% acetonitrile of the coccidiostats from the feed samples and filtration of the raw extract prior to chromatographic analysis. Method validation included the determination of selectivity, linearity, specificity, repeatability, the limit of detection, limit of quantification, decision limit (CCα), detection capability (CCβ), and recovery. Feed samples from the Finnish national feed control programme and suspected carry-over samples from a feed manufacturer were analysed in parallel with an existing liquid chromatography method coupled with ultraviolet detection. All feed control samples were negative in LC-UV, but with the developed MS method, monensin, salinomycin, and narasin were detected at concentrations of <0.025–0.73 mg/kg, <0.025–0.027 mg/kg, and <0.025–1.6 mg/kg, respectively. In suspected carry-over samples after an output of 2.0 tonnes of unmedicated feed in the pelletizer line, the concentrations of monensin, salinomycin, and narasin varied from undetected to 16 mg/kg. In the mixer line, after 3.2 tonnes of unmedicated feed output, the concentrations of monensin, salinomycin, and narasin varied from undetected to 2.4 mg/kg. PMID:23484082

  8. Determination of trace elements in the human substantia nigra

    Energy Technology Data Exchange (ETDEWEB)

    Morawski, M. [Paul-Flechsig-Institut fuer Hirnforschung, Universitaet Leipzig, Jahnallee 59, 04109 Leipzig (Germany)]. E-mail: morm@medizin.uni-leipzig.de; Meinecke, Ch. [Fakultaet fuer Physik und Geowissenschaften, Universitaet Leipzig, Linnestrasse 5, 04105 Leipzig (Germany); Reinert, T. [Fakultaet fuer Physik und Geowissenschaften, Universitaet Leipzig, Linnestrasse 5, 04105 Leipzig (Germany); Doerffel, A.C. [Paul-Flechsig-Institut fuer Hirnforschung, Universitaet Leipzig, Jahnallee 59, 04109 Leipzig (Germany); Riederer, P. [Klin. Neurochemie, Abt. Psychiatrie, Universitaet Wuerzburg, Fuechsleinstrasse 15, 97080 Wuerzburg (Germany); Arendt, T. [Paul-Flechsig-Institut fuer Hirnforschung, Universitaet Leipzig, Jahnallee 59, 04109 Leipzig (Germany); Butz, T. [Fakultaet fuer Physik und Geowissenschaften, Universitaet Leipzig, Linnestrasse 5, 04105 Leipzig (Germany)

    2005-04-01

    'The gain in brain is mainly in the stain' was long time a key sentence for research in neurodegenerative disease. However, for a quantification of the element concentrations (especially iron) in brain tissue, standard staining methods are insufficient. Advanced physical methods allow a quantitative elemental analysis of brain tissue. The sophisticated ion beam analysis provides a quantitative determination of elemental concentrations with a subcellular spatial resolution using a scanning proton beam focussed down to below 1 {mu}m that induces characteristic X-rays in the specimen (PIXE - particle induced X-ray emission). Histochemical and biochemical determinations of total iron content in brain regions from idiopathic Parkinson's disease have demonstrated an increase of iron in parkinsonian substantia nigra pars compacta but not in the pars reticulata, however without a clear cellular classification. For the first time, we have differentially investigated the intra- and extraneuronal elemental concentrations (especially iron) of the human substantia nigra pars compacta versus pars reticulata with detection limits in the range of 50 {mu}mol/l. Thus, we could compare the neuronal iron concentration in human brain sections of healthy and parkinsonian brain tissue. Clear differences in the iron concentration and distribution could be disclosed. Additionally, we could show in situ that the increased intraneuronal iron content is linked to neuromelanin.

  9. Spectrographic determination of traces of boron in steels

    International Nuclear Information System (INIS)

    Alduan, F.A.; Roca, M.

    1976-01-01

    A spectrographic method has been developed to determine quantitatively boron in steels in the 0.5 to 250 ppm concentration range. The samples are dissolved in acids and transformed into oxides, avoiding boron losses by the addition of mannitol. For the fluoride evolution of boron in the dc arc the following compounds have been considered: CuF 2 , LiF, NaF, and SrF 2 . CuF 2 , at a concentration of 10%, provides the highest line-to-background intensity ratio. An arc current of 5 amperes eliminates the interference from iron spectrum on the most sensitive boron line - B 2497.7 A. Variations in chromium and nickel contents have no effect on the analytical results. (author)

  10. Determination of Trace Elements in Patients With Chronic Hepatitis B

    Directory of Open Access Journals (Sweden)

    Vahid Hosseini

    2011-10-01

    Full Text Available Chronic Hepatitis B virus (HBV infection is a major liver disease worldwide and its clinical manifestations are linked to immune response. The purpose of this study was to evaluate the relationship between selenium, copper, and zinc in comparison with transaminase level in chronic HBV patients. Serum samples of the HBV infected patients were obtained from Tooba medical center, Sari, Iran. Sixty patients were enrolled in this study (36 men and 24 women, mean age: 39.6 ± 12.2 years. The concentration of zinc, selenium, copper and transaminases were determined using an autoanalyzer system. Concentrations of selenium (0.273 ±0.056 μg/dl and zinc (2.1±0.037 was elevated in patients with low transaminase levels as were significantly different in comparison with patients with high transaminase level (P<0.05. Serum copper concentration was similar in two groups of patients. Elevated levels of transaminase concentrations were independently associated with low zinc and selenium concentrations in chronic HBV patients. It is concluded that serum zinc and selenium levels are associated with less hepatic damage in chronic HBV patients and might have a protective role during liver injury.

  11. The Determination of Uranium and Trace Metal Impurities in Yellow Cake Sample by Chemical Method

    International Nuclear Information System (INIS)

    Busamongkol, Arporn; Rodthongkom, Chouvana

    1999-01-01

    The purity of uranium cake is very critical in nuclear-grade uranium (UO 2 ) and uranium hexafluoride (UF 6 ) production. The major element in yellow cake is uranium and trace metal impurities. The objective of this study is to determine uranium and 25 trace metal impurities; Aluminum, Barium, Bismuth, Calcium, Cadmium, Cobalt, Chromium, Copper, Iron, Potassium, Iithium, Magnesium, Manganese, Molybdenum, Sodium, Niobium, Nickel, Lead, Antimony, Tin, Strontium, Titanium, Vanadium, Zinc and Zirconium, Uranium is determined by Potassium dichromate titration, after solvent extraction with Cupferon in Chloroform, Trace metal impurities are determined by solvent extraction with Tributyl Phosphate in Carbon-tetrachloride ( for first 23 elements) and N-Benzoyl-N-Phenylhydroxylamine in Chloroform ( for last 2 elements), then analyzed by Atomic Absorption Spectrophotometer (AAS) compared with Inductively Couple Plasma Spectrophotometers (ICP). The accuracy and precision are studied with standard uranium octaoxide

  12. Zeta functions and regularized determinants related to the Selberg trace formula

    DEFF Research Database (Denmark)

    Momeni, Arash; Venkov, Alexei

    determinants of one dimensional Schroedinger operator for harmonic oscillator. We decompose the determinant of the automorphic Laplacian into a product of the determinants where each factor is a determinant representation of a zeta function related to Selberg's trace formula. Then we derive an identity...... connecting the determinants of the automorphic Laplacians on different Riemannian surfaces related to the arithmetical groups. Finally, by using the Jacquet-Langlands correspondence we connect the determinant of the automorphic Laplacian for the unit group of quaternions to the product of the determinants......For a general Fuchsian group of the first kind with an arbitrary unitary representation we define the zeta functions related to the contributions of the identity, hyperbolic, elliptic and parabolic conjugacy classes in Selberg's trace formula. We present Selberg's zeta function in terms...

  13. [Determination of polysaccharide from Chinese medicine Morinda officinalis how and its trace elements analysis].

    Science.gov (United States)

    Wu, Yong-Jun; Liu, Jie; Wu, Yu-Ming; Liu, Li-E; Zhang, Hong-Quan

    2005-12-01

    Polysaccharide was extracted from morinda officinalis how by back-flowing with 80% ethanol for 1 h, and the method of improved phenol-sulfuric acid spectroscopy was adopted to determine the content of morinda officinalis how polysaccharide. As for its trace elements, the atomic absorption spectroscopy was used to detect the content of Zn, Fe and Cu, which were compared with its fake; and cold atomic fluorometry was applied to determine the trace mercury. The results were satisfactory, which can give reference about the effective components of morinda officinalis how, and will help to exploit it.

  14. Determination of trace elements in maifanite by outer cover electrode atomic emission spectrometry

    Institute of Scientific and Technical Information of China (English)

    LI Jianqiang; LU Yiqiang; JIANG Wei

    2005-01-01

    Maifanite is a nature medicinal stone used in many fields for long time. The research on it showed that there are many trace elements in maifanite. In this paper, 36 trace elements in maifanite were determined by outer cover electrode atomic emission spectrometry, and the determination conditions were studied systematically. The results show that the concentrafions of elements, which are beneficial to human health, are higher, and the elements harmful to people health such as As, Cd, Hg, Cr, and Pb are tiny in maifanite. The precision and the accuracy were also discussed.

  15. Determination of trace gold in rocks and minerals by neutron activation analysis

    International Nuclear Information System (INIS)

    Zhao Yunlong; Zhou Suqing; Liang Yutang

    1988-05-01

    The determination of trace gold in rocks and minerals by neutron activation analysis is described. Two methods are used for pre-separating and concentrating the trace gold in geological samples. one of the methods is that the samples are dissolved in aqua regia solution; activated carbon paper pulp filter is used for pre-separating and concentrating trace gold by dynamic adsorption method; then the activated carbon containing gold was ashed at 650 ∼ 700 deg c. The other method is that the samples are dissolved in aqua regia solution; the polyurethane foam plastic filled with activated carbon is used for pre-separating and concentrating trace gold by dynamic adsorption method; then the foam plastic containing gold was ashed at 650 deg c. The gold in ashes is determinated by neutron activation analysis. The detection limit is 0.004ng/g. The accuracy of the method is examined by gold in reference standard material. The results of this method are in good agreement with the recommended value. For analysis of the trace gold by the methods of instrumental neutron activation analysis and epithermal neutron activation analysis, the interference of 411.8 keV γ-ray from 153 Sm, 152 Eu and fission products of uranium and the correction methods are discussed

  16. Trace elements in Turkish tobacco determined by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Guelovali, M.C.; Guenduez, G.

    1983-01-01

    The concentration of 20 trace elements in nine brands of Turkish cigarette tobacco and in a brand of pipe tobacco ash has been determined by instrumental neutron activation analysis. The percent transference of elements into smoke has been estimated from the amounts remaining in the ash. (author)

  17. Application of neutron activation analysis to trace elements determinations in lung samples

    International Nuclear Information System (INIS)

    Rogero, S.O.

    1991-01-01

    The purpose of this work was to apply the instrumental neutron activation analysis method to determine trace elements in lung samples from smokers and non smokers. Samples of lung tissues and lymph nodes from pulmonary hilum analyzed were collected from autopsies by researchers from Faculdade de Medicina da USP. (author)

  18. Determination of trace elements in biological material by neutron activation analysis

    International Nuclear Information System (INIS)

    Tran Van, L.; Teherani, D.K.

    1989-01-01

    Eighteen trace elements in biological materials [grass (Imperata cylindrica), mimosa plant (Mimosa pudica), rice] by neutron activation method were determined. In the comparative analysis the content of the same element was different in each material, although they were collected at the same place and the same sampling method was applied. (author) 4 refs.; 1 fig.; 1 tab

  19. Determination of trace elements (Fe, Cu and Zn) in serum and tail ...

    African Journals Online (AJOL)

    Strong and poor relationships between the levels of trace elements in blood, tissue and hair have been determined in various studies. The horses in this study have been fed with dry straw and artificial feed in winter months, with fresh grass in autumn and spring. The purpose was to investigate possible changes in the ...

  20. Trace metal contaminants in sediments and soils: comparison between ICP and XRF quantitative determination

    Directory of Open Access Journals (Sweden)

    Congiu A.

    2013-04-01

    Full Text Available A mineralization method HCl-free for heavy metals analysis in sediments and soils by DRC-ICP-MS was developed. The procedure, which uses concentrated nitric, hydrofluoric acid and hydrogen peroxide, was applied for the analysis of arsenic, cadmium, chromium, nickel and vanadium. The same samples were then analyzed, as pressed pellets, by wavelength dispersive X ray fluorescence (WD-XRF using the dedicated PANalytical Pro Trace solution for the determination of trace elements. Comparison of ICP and XRF data showed good agreement for the elements under investigation, unless for chromium in soils, which recovery was not complete.

  1. Determination of trace elements by INAA in urban air particulate matter and transplanted lichens

    International Nuclear Information System (INIS)

    Bergamaschi, L.; Rizzio, E.; Profumo, A.; Gallorini, M.

    2005-01-01

    Lichens as biomonitors and neutron activation analysis as analytical technique have been employed to evaluate the trace element atmospheric pollution in the metropolitan area of the city of Pavia (Northern Italy). Transplanted lichens (Parmelia sulcata and Usnea gr. hirta) and air particulate matter have been monthly collected and analyzed during the winter 2001-2002. INAA and ET-AAS have been used for the determination of 28 elements in air particulate matter and 25 elements in lichens. Trace metals concentrations as well as the corresponding enrichment factors were evaluated and compared. (author)

  2. Determination of trace elements in cigarette and tobacco by neutron activation analysis

    International Nuclear Information System (INIS)

    Nouchpramool, S.

    1988-01-01

    The objective of this work is to determine the concentration of 22 trace elements in cigarette and tobacco by instrumental neutron activation analysis in which multielements can be analyzed simultaneously with high sensitivity and reliability as well as easy and rapid. It is well known that, trace toxic elements with high concentration may be harmful for health of smokers. Since they might damage the respiratory system and might cause other diseases. The finding for this report can be used as the basis of further study on toxic of trace elements to the smoker. The results of this analysis show that the bromine content in all samples is significantly high, but the concentration of the other elements are varying from one to another. Bromine concentration might come from soil and/or smoked tobacco leaves with methyl bromide as fungicide

  3. Determination of trace elements in ground water by two preconcentration methods using atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Elhag, A. Y.

    2004-01-01

    This is a comparative study between two different methods of preconcentration done to separate the trace elements cadmium, nickel. chromium, manganese, copper, zinc, and lead in drinking (ground) water samples taken from different locations in Gezira State, central Sudan (the map); these methods are (coprecipitation) with aluminium hydroxide and by Ammonium Pyrrolidine Dithiocarbamate (APDC) using Methyl Isobutyl Ketone (MIBK) as an organic solvent; and subsequent analysis by Atomic Absorption Spectrometry (AAS) for both methods. The result of comparison showed the superiority of the (APDC) coprecipitation method over the aluminium hydroxide coprecipitation method in the total percentage recoveries of the studied trace elements in drinking (ground) water samples, such results confirm previous studies. This study also involves direct analysis of these water samples by atomic absorption spectrometry to determine the concentrations of trace elements Cadmium, Nickel, Chromium, Manganese, Copper, Zinc and Lead and compare it to the corresponding guide line values described by the World Health Organization and the maximum concentrations of trace elements in drinking water permitted by the Sudanese Standards and Metrology Organizations (SSMO), where the concentrations of some elements in some samples were found to be different than the described values by both of the organizations. The study includes a trial to throw light on the effect of the proximity of the water samples sources to the Blue Nile river on its trace elements concentrations; no relation was proved to exist in that respect.(Author)

  4. Integrated luminometer for the determination of trace metals in seawater using fluorescence, phosphorescence and chemiluminescence detection

    OpenAIRE

    Worsfold, P. J.; Achterberg, E. P.; Bowie, A. R.; Cannizzaro, V.; Charles, S.; Costa, J. M.; Dubois, F.; Pereiro, R.; San Vicente, B.; Sanz-Medel, A.; Vandeloise, R.; Donckt, E. Vander; Wollast, P.; Yunus, S.

    2002-01-01

    The paper describes an integrated luminometer able to perform fluorescence (FL), room temperature phosphorescence (RTP) and chemiluminescence (CL) measurements on seawater samples. The technical details of the instrumentation are presented together with flow injection (FI) manifolds for the determination of cadmium and zinc (by FL), lead (RTP) and cobalt (CL). The analytical figures of merit are given for each mainfold and results are presented for the determination of the four trace metals i...

  5. Determination of artificial and natural radionuclides and others trace elements in environmental samples form Antarctica

    International Nuclear Information System (INIS)

    Schuch, L.A.; Godoy, J.M.; Nordemann, D.J.R.

    1994-01-01

    The results of the radioactive elements concentrations, determined by gamma spectrometry and the others trace elements determined by neutron activation analysis of several environmental samples (soils, marine sediments, algae mosses and lichens) in Comandante Ferraz Antartica Station are presented. The high concentrations of Cs-137 were found in lichens and mosses samples and the soils and sediments showed concentrations of natural radionuclides. (C.G.C.). 8 refs, 1 fig, 3 tabs

  6. Determination of some trace elements in biological samples using XRF and TXRF techniques

    International Nuclear Information System (INIS)

    Khuder, A.; Karjou, J.; Sawan, M. K.

    2006-07-01

    XRF and TXRF techniques were successfully used for the multi-element determination of trace elements in whole blood and human head hair samples. This was achieved by the direct analysis using XRF technique with different collimation units and by the optimized chemical procedures for TXRF analysis. Light element of S and P were preferably determined by XRF with primary x-ray excitation, while, elements of K, Ca, Fe, and Br were determined with a very good accuracy and precision using XRF with Cu- and Mo-secondary targets. The chemical procedure dependent on the preconcentration of trace elements by APDC was superiorly used for the determination of traces of Ni and Pb in the range of 1.0-1.7 μg/dl and 11-23 μg/dl, respectively, in whole blood samples by TXRF technique; determination of other elements as Cu and Zn was also achievable using this approach. Rb in whole blood samples was determined directly after the digestion of samples using PTFE-bomb for TXRF analysis. (author)

  7. The Determination Of Trace Element Levels In Diet By Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Kukuh, Ratnawati; Djojosubroto, Harjoto

    2002-01-01

    Trace element levels in foodstuff are normally low. Although the levels are low, certain trace elements which are called essential trace elements have an important role in metabolism process. Deficiency or intoxication of essential trace elements may lead to abnormal health. In this study the levels of Zn, Fe, AI, Mn, and Co in diet samples were determined by neutron activation analysis, and then the daily intakes of these elements were estimated. The samples were prepared by duplicate diet method, representing those that were consumed by population from West, Central and East Java. Following the collection the respective samples were blended, then were freeze dried at-54 o c. The elemental quantification were performed by neutron activation analysis. The traceability of the determination was ensured using standard reference material NIST-SRM-1548a. The results show that the daily intake for Zn were 2.8-22.8 mg/day (reference value were 5- 40 mg/day), Fe were 3.1-26.5 mg/day (reference value were 6-40 mg/day), AI were 4,2-32.9 mg/day (reference value were 2-45 mg/day), Mn were 1.0-5,6 mg/day (reference value were 0.4-10,0 mg/day), and Co were 0,005-0,074 mg/day (reference value were 0.005 -1.8 mg/day

  8. Report on the intercomparison for the determination of trace elements in Lake Sediment (SL-1)

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1979-02-01

    The determination of trace element concentrations including those of the rare-earths in geological samples has gained much importance during the past decade. Knowledge of the concentrations of specific elements and of their ratios have proved essential for the understanding of the development of geological strata. With increasing use of instruments in analysis, reference samples have become essential for their calibration and various international organizations have issued reference materials to monitor precision and accuracy in chemical determinations. The IAEA has in the past organized several intercomparisons and prepared reference samples of geochemical materials. The present report deals with a recent intercomparison on the determination of trace elements in Lake Sediment (Sl-1) carried out in 1977-1978 and involving the participation of 43 institutes who returned a total of 2535 individual results on 43 elements.

  9. Determination of trace amount of formaldehyde base on a bromate-Malachite Green system.

    Science.gov (United States)

    Tang, Yufang; Chen, Hao; Weng, Chao; Tang, Xiaohui; Zhang, Miaoling; Hu, Tao

    2015-01-25

    A novel catalytic kinetic spectrophotometric method for determination of trace amount of formaldehyde (FA) has been established, based on catalytic effect of trace amount of FA on the oxidation of Malachite Green (MG) by potassium bromate in presence of sulfuric acid medium, and was reported for the first time. The method was monitored by measuring the decrease in absorbance of MG at 617 nm and allowed a precise determination of FA in the range of 0.003-0.08 μg mL(-1), with a limit of detection down to 1 ng mL(-1). The relative standard deviation of 10 replicate measurements was 1.63%. The method developed was approved to be sensitive, selective and accurate, and adopted to determinate free FA in samples directly with good accuracy and reproducibility. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. XRF determination of trace and major elements using a single-fused disc

    International Nuclear Information System (INIS)

    Thomas, I.R.; Haukka, M.T.

    1978-01-01

    A new fusion method using lithium metaborate, suitable for the determination of major and trace elements by X-ray fluorescence analysis (XRF), has proven to be of comparable accuracy to other XRF methods for the ten major rock-forming oxides. The very low dilution allows determination of trace elements with a decrease in sensitivity of about a factor of 2 compared with XRF determination using pressed-powder pellets. A feature of the method is the flexibility of sample preparation allowed: the matrix-correction parameters may be used for a wide range of dilutions (sample/flux ratios), no 'Loss' correction is necessary, and imperfect or inhomogeneous discs may be crushed and pressed pellets made of the glass powder when required. Considerable savings in the time during preparation, analysis and correction of results are possible with current automation because of streamlining procedures

  11. Determination of trace and ultra-trace elements in Dergaon meteorite by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Balaram, V.; Gnaneswara Rao, T.; Anjaiah, K.V.; Phukon, N.; Majumdar, A.C.

    2003-01-01

    In this paper, a detailed methodology for high precision measurement of several trace and ultra-trace elements including REE and PGE have been presented using effective sample preparation techniques and inductively coupled plasma mass spectrometry. Discussion is focussed on aspects, such as total dissolution and recovery of all elements, minimization of oxide and doubly-charged and other polyatomic ion interferences, calibration by matrix matching standards, accuracy and precision

  12. Determination of trace elements in seawater using Mg-scavenger as preconcentration agent, and neutron activation analysis

    International Nuclear Information System (INIS)

    Andersen, B.

    1986-01-01

    In order to determine trace elements in seawater, a preconsentration method based on coprecipitation on Mg(OH) 2 is presented. Different parameters influencing the carrying effects have been investigated using model solutions and radioactive tracers. The deposit and solution are separated by filtration. Filter with deposit is stored in quarts ampules for later determination of trace elements by means of neutron activation analysis

  13. Significant improvement of accuracy and precision in the determination of trace rare earths by fluorescence analysis

    International Nuclear Information System (INIS)

    Ozawa, L.; Hersh, H.N.

    1976-01-01

    Most of the rare earths in yttrium, gadolinium and lanthanum oxides emit characteristic fluorescent line spectra under irradiation with photons, electrons and x rays. The sensitivity and selectivity of the rare earth fluorescences are high enough to determine the trace amounts (0.01 to 100 ppM) of rare earths. The absolute fluorescent intensities of solids, however, are markedly affected by the synthesis procedure, level of contamination and crystal perfection, resulting in poor accuracy and low precision for the method (larger than 50 percent error). Special care in preparation of the samples is required to obtain good accuracy and precision. It is found that the accuracy and precision for the determination of trace (less than 10 ppM) rare earths by fluorescence analysis improved significantly, while still maintaining the sensitivity, when the determination is made by comparing the ratio of the fluorescent intensities of the trace rare earths to that of a deliberately added rare earth as reference. The variation in the absolute fluorescent intensity remains, but is compensated for by measuring the fluorescent line intensity ratio. Consequently, the determination of trace rare earths (with less than 3 percent error) is easily made by a photoluminescence technique in which the rare earths are excited directly by photons. Accuracy is still maintained when the absolute fluorescent intensity is reduced by 50 percent through contamination by Ni, Fe, Mn or Pb (about 100 ppM). Determination accuracy is also improved for fluorescence analysis by electron excitation and x-ray excitation. For some rare earths, however, accuracy by these techniques is reduced because indirect excitation mechanisms are involved. The excitation mechanisms and the interferences between rare earths are also reported

  14. Method to determine trace elements in water samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Kueppers, G.; Erdtmann, G.

    1981-05-01

    For the determination of trace elements in water by neutron activation analysis irradiation porcedures and chemical separation procedures have been developed. Irradiation in melted quarz glass ampoules in the presence of a platinum wire (for recombination of the oxyhydrogen gas produced by radiolysis) proved successfull with different variants of the irradiation methods, as long irradiation periods without pressure build-up could be achieved. Possible falsifications of the analysis results were investigated in detail (losses by absorption on vessel walls etc.). The irradiated samples can be measured directly with a gamma ray spectrometer and from the radionuclides found the trace element contents may be calculated. More sensitive determinations are possible if the radionuclides are chemically separated. Procedures for removing the matrix activities, for the separation of the radionuclides in groups of elements and for the isolation of single elements have been developed. For especially sensitive determination of some elements selective separation procedures for antimony, cadmium, selenium, mercury and uranium have been developed. The analytical procedures described have been applied to trace element determinations in river water, glacier ice and water solutions from technical processes. (orig./RB) [de

  15. Determination of the trace TBP in industrial feed liquid by gas chromatography

    International Nuclear Information System (INIS)

    Gao Yuehua; Jiang Junqing; Mu Ling; Yang Songtao

    2012-01-01

    The determination of the trace TBP in kerosene of the industrial feed liquid by gas chromatography is studied in the paper. It first takes the purification treatment for the kerosene containing trace TBP. The plutonium is removed by 0.2 mol/L ferrous sulfamate-1 mol/L nitric acid using the back-extraction. The uranium and the nitric acid in the organic phase are removed by the deionized water. The impurity which affect the measurement of the TBP and is harmful to the gas chromatograph are eliminated. Then the content of the TBP of the organic phase can be determined by gas chromatography. Results show that the measuring range of the content of the TBP is 0.02% ∼ 2%. The precision of the method is better than 5% and the recovery is between 95%∼106%. (authors)

  16. Trace elements in Turkish tobacco determined by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Gulovali, M.C.

    1977-01-01

    This study was undertaken to determine the concentration of trace elements in nine different brands of Turkish cigarette tobacco, pipe tobacco and tobacco ash. Instrumental neutron activation analysis was employed, and a gamma-ray spectrometer consisting of 40 cm 3 Ge(Li) detector coupled to 1024 and 4096-channel analyzers were used. Samples were irradiated at a thermal neutron flux of about 10 13 cm -2 sec -1 . Concentrations of Na, K, Sc, Cr, Fe, Co, Zn, As, Se, Br, Rb, Sb, Cs, Ba, La, Ce, Eu, Hf, Hg and Th were determined in tobacco and ash; percent transference of these elements into ash were calculated. It was found out that trace elements in cigarette tobacco are left in the ash but only a small percentage is transferred into the smoke

  17. Determination of trace elements by neutron activation analysis using dinonylnaphtalene sulfonic acid as a preconcentrating agent

    International Nuclear Information System (INIS)

    Yang, M.H.; Chen, P.Y.; Tseng, C.L.; Yeh, S.J.; Weng, P.S.

    1977-01-01

    Dinonylnaphthalene sulfonic acid (HD) has been used as a preconcentrating agent to enrich trace metal ions and to separate the interfering elements such as Na, K, Cl and Br, which normally exist in the natural aqueous systems. Experiments were performed by extracting the ions in the aqueous medium with HD in n-hexane and subsequently backextracted into a minimal volume of acid solution. Factors influencing the extraction efficiency of the ions of interest were investigated. The preconcentration technique has been successfully applied to the determination by neutron activation analysis of trace elements in natural water and biological materials. Both short-lived nuclides (Mg, Al, Ca, Mn) and long-lived nuclides (Sm, Eu, Zn, La, Cr, Sc, Fe, Co) in the ppb-level concentrations were determined. (T.G.)

  18. Determination of trace elements in BCR single cell protein via destructive neutron activation analyses

    International Nuclear Information System (INIS)

    Tjioe, P.S.; Goeij, J.J.M. de; Nooijen, J.L.; Kroon, J.J.

    1978-10-01

    The amount of some trace elements in single cell protein (SCP), a product of BP Research Centre at Sunbury-at-Thames, England, was determined by neutron activation analysis. The SCP-samples were irradiated in the reactor of the Interuniversity Reactor Institute at Delft in a neutron flux of 1.0x10 13 n/cm 2 s for 12 hours. Samples of Bowen's Kale were used as reference material. After a decay of two or three days the samples were chemically destroyed, and the trace elements were separated. The quantity of the following elements was determined by measuring the γ-activity by means of a scintillation counter: antimony, cadmium, mercury, arsenic and selenium. The amounts of these elements in the SCP and in the reference material were tabled

  19. Determination of 11 trace elements in U3O8 CRMs by ICP-AES

    International Nuclear Information System (INIS)

    Liu Husheng

    1994-01-01

    The TBP extractant-containing resin and extraction chromatography technique were used to separate 11 trace elements in U 3 O 8 CRMs. The sample was separated at a flow rate of 0.5 mL/min with 3 mol/L HNO 3 as medium. A model 975 ICP direct reading spectrometer was used to determine the trace elements of Ca, Cd, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb and Sn in U 3 O 8 CRMs. The lowest quantitatively determinable concentration of impurities in U 3 O 8 CRMs are 0.02-1.6 μg/g. The RSD is less than 10%. The proposed method provides excellent and accurate analytical data for the U 3 O 8 samples prepared as certified reference materials (CRMs)

  20. Determination of trace elements in ceramic uranium dioxide pellets powders CRMs by ICP-AES

    International Nuclear Information System (INIS)

    Liu Husheng; Li Jun

    1997-01-01

    The 237-quaternary ammonium extraction resin chromatography is used to the separation of 6 trace elements in ceramic uranium dioxide pellets powders, which are used as certified reference materials (CRMs). The sample is dissolved in 6.5 mol/L HNO 3 and uranium is separated by chromatographic column. the 6 trace elements Al, Ba, Co, Ta, Ti and V contained in the elutriant are determined by using ICP directly reading spectrometer. For a 300 mg sample, the lowest determinable concentration of impurities in ceramic UO 2 pellets powders CRMs is (0.016-0.250) x 10 -6 . The relative standard deviation is less than 7.5%. The proposed method provides excellent and accurate analytical data for the ceramic UO 2 pellets powders samples (CRMs)

  1. Informative importance of determination of trace elements in biologocal mediums in patients with endocrine pathology

    Directory of Open Access Journals (Sweden)

    Ирина Николаевна Андрусишина

    2015-07-01

    Full Text Available Aim. The changes of mineral metabolism in human organism caused by the deficiency or excess of trace elements in environment (air, food stuffs, water can lead to disorder of functional status of organism.An excess or deficiency of the certain metals disturb the balance of metabolic processes in organism that causes the different changes in endocrine system too. That is why the aim of research was to detect the peculiarities of distribution of macro and trace elements in patients with different endocrine pathology and to show the reasonability of the complex approach in assessment of microelementoses at hyperthyroidism and diabetes mellitus.Methods. The balance of 15 macro and trace elements in different biological mediums (hairs, whole blood, blood serum, urine was studied using EAAS and AES-ICP methods.Result. There was demonstrated the high informative importance of determination of K, Mg, Mn, Cr, Zn at pancreas pathology and Cr, Mn, Se, Zn- at thyroid pathology in human. There was detected that endocrine pathology is characterized with the surplus accumulation of Al, As and Pb in organism of examined patients.Conclusions. To increase the reliability and efficiency of the clinical diagnostics of endocrine human pathology there was demonstrated the high informative importance of the complex approach in choice of biological mediums at assessment of the trace elements imbalance. 

  2. Development of a choronocoulometric method for determining traces of uranium using the catalytic nitrate reduction

    International Nuclear Information System (INIS)

    Cantagallo, M.I.C.; Gutz, I.G.R.

    1990-01-01

    With the aim of improving the sensitivity of the electroanalytical determination of uranium at trace levels. The uranium catalyzed reduction of nitrate on mercury electrode and the technique of chronocoulometry were used. Several experimental parameters were investigated (electrolyte composition, potential program, integration time, blank correction, temperature, previous separation) and adequate conditions were selected for the analytical determination. Under these conditions it was possible to exceed the best reported sensitivity for the catalytic determination, extending the detection limit to 3.10 -10 M. Exploratory study of the combination of this procedure with pre-concentration of uranium ions on the electrode revealed a detection limit ten limes lower. (author) [pt

  3. Spectrographic Determination of Trace Constituents in Rare Earths; Determinacion espectrografica de impurezas en tierras raras

    Energy Technology Data Exchange (ETDEWEB)

    Capdevila, C; Alvarez, F

    1962-07-01

    A spectrographic method was developed for the determination of 18 trace elements in lanthanum, cerium, praseodimium, neodimium and samarium compounds. The concentrations of the impurities cover the range of 0,5 to 500 ppm. Most of these impurities are determined by the carrier distillation method. Several more refractory elements have been determined by total burning of the sample with a direct current arc or by the conduction briquet excitation technique with a high voltage condensed spark. The work has been carried out with a Hilger Automatic Large Quartz Spectrograph. (Author) 5 refs.

  4. The determination of some trace elements in sulphide concentrates by spectrophotometry

    International Nuclear Information System (INIS)

    Shelton, B.J.; Komarkova, E.; Josephson, M.; Cook, E.B.T.; Dixon, K.

    1977-01-01

    The report describes the determination of trace amounts (as low as 1 to 10 p.p.m. depending on the element) of arsenic, germanium, molybdenum, nickel, phosphorus, selenium, tellurium, tin, and titanium in sulphide concentrates. The proposed methods, which are detailed in the appendices, are adaptations of established procedures that were modified to allow for the complex nature of the concentrates to be analysed

  5. Determination of trace element impurities in aspirin tablets by neutron activation analysis

    International Nuclear Information System (INIS)

    Iskander, F.Y.; Klein, D.E.; Bauer, T.L.

    1986-01-01

    Twenty-five trace and minor elements in five different Egyptian aspirin brands (Aspo, Askin, Aspocid, Aspeol and Rivo) were determined by instrumental neutron activation analysis. It was concluded that the concentration of As, Ba, Br, Co, Cr, Fe (except in Aspocid), Mg, Mn, Rb, Se, Sr and Zn in the Egyptian brands is below or within the concentration range reported for these elements in 16 American aspirin and aspirin-like brands. (author)

  6. Optimization of experimental conditions in uranium trace determination using laser time-resolved fluorimetry

    International Nuclear Information System (INIS)

    Baly, L.; Garcia, M.A.

    1996-01-01

    At the present paper a new sample excitation geometry is presented for the uranium trace determination in aqueous solutions by the Time-Resolved Laser-Induced Fluorescence. This new design introduces the laser radiation through the top side of the cell allowing the use of cells with two quartz sides, less expensive than commonly used at this experimental set. Optimization of the excitation conditions, temporal discrimination and spectral selection are presented

  7. Determination of five trace elements in leaves in Nanfang sweet orange by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Li Fangqing

    2006-01-01

    The five trace elements of copper, zinc, manganese, iron and cobalt in leaves of Nanfang sweet orange are determined by flame atomic absorption spectrometry. The technique is simple, precise and sensitive. The effect of the type of digesting solution (mixed acid), the ratio of mixed acid, the volume of digesting solution and the time of digesting are investigated in details. The results show that leaves of Nanfang sweet orange contain higher amount of iron and zinc. (authors)

  8. Determination of trace amounts of selenium in minerals and rocks by flemeless atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Capdevila, C.; Alduan, F.A.

    1980-01-01

    The determination of trace amounts of selenium in silicate rocks and feldspart by solvent extraction and graphite furnace atomic-absorption spectrometry has been studied. Sodium diethyl-ditiocarbamate and ammonium pyrrolidinedithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted into carbon tetrachloride as the sodium diethylditiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (author)

  9. X-ray fluorescence analysis for trace element determination in foodstuff chemistry

    International Nuclear Information System (INIS)

    Wildanger, W.

    The physical fundamentals of X-ray fluorescence analysis are given and the routine spectrometers described. The basic principles are given of analytical methods used in qualitative and quantitative fluorescence analyses. Examples are given of the use of the method in a number of fields and the possibility and usefulness is discussed for the determination of trace elements in foodstuffs. The preparation of samples, preliminary concentration of components and calibration methods are discussed. (M.K.)

  10. Determination of trace elements in chewing gum by neutron activation analysis

    International Nuclear Information System (INIS)

    Dietz, M.L.

    1990-01-01

    Six trace elements of nutritional or toxicological interest (Al, Ca, Cl, Mn, Na and Sr) were determined in three different brands of chewing gum by instrumental neutron activation analysis. For the particular brands of gum examined, none of the detected elements was found to be present at a level representing a substantial contribution to the total dietary intake of the element for an American adult. (author) 11 refs.; 3 tabs

  11. Determination of trace metals in Cladophora glomerata: C. glomerata as a potential biological monitor

    Energy Technology Data Exchange (ETDEWEB)

    Keeny, W.L.; Breck, W.G.; Vanloon, G.W.; Page, J.A.

    1976-01-01

    A differential pulse anodic stripping voltammetry method has been developed for the determination of Zn, Cd, Pb and Cu in Cladophora glomerata. The method has been applied to samples taken in August from a remote island in Lake Ontario (Main Duck) and a shore site near Kingston, Ontario (Deadman Bay). It is postulated that C. glomerata can act as a biological monitor, concentrating the trace metals present in the aqueous environment with a reasonably constant CF for each element.

  12. Trace elements in the diets of Turkish children determined by INAA

    International Nuclear Information System (INIS)

    Aras, N.K.; Mauerhofer, E.; Naidu, R.K.; Arcasoy, A.; Denschlag, H.O.

    1992-01-01

    The role of toxic and essential trace elements in human diet is increasingly important because of environmental problems and the increasingly sophisticated industrial treatment of food products. Instrumental neutron activation analysis (INAA) is particularly well suited for multielement determinations. In order to test and demonstrated the usefulness of the method in connection with the fast pneumatic tube system of the Mainz TRIGA reactor, the authors have analyzed six diet samples of Turkish children

  13. Trace Elements in Human Myocardial Infarction Determined by Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Wester, P.O.

    1965-05-01

    By means of neutron activation analysis, injured and adjacent uninjured human heart tissue from 12 autopsy cases with myocardial infarction are investigated with respect to the concentration of 23 trace elements. The bulk elements K, Na and P are also determined. A recently developed ion-exchange technique, combined with subsequent y-spectrometry, is used. The following trace elements are determined: Ag, As, Au, Ba, Br, Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Hg, La, Mo, Rb, Sb, Sc, Se, Sm, Zn and W. In the injured tissue compared to the uninjured, calculation on a wet weight basis showed a decrease in Co, Cs, K, Mo, P, Rb and Zn, and an increase in Br, Ca, Ce, La, Na, Sb and Sm. The differences in Ca, La, Mo, P and Zn are dependent on the age of the myocardial infarction, and the regression lines for these elements are given. The concentration of the trace elements in uninjured tissue from infarcted hearts is compared to the concentration of these elements in normal heart tissue, determined in a previous study. In the uninjured tissue from infarcted hearts a decrease is found in Cu and Mo, and an increase in As and Ce

  14. Trace Elements in Human Myocardial Infarction Determined by Neutron Activation Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Wester, P O

    1965-05-15

    By means of neutron activation analysis, injured and adjacent uninjured human heart tissue from 12 autopsy cases with myocardial infarction are investigated with respect to the concentration of 23 trace elements. The bulk elements K, Na and P are also determined. A recently developed ion-exchange technique, combined with subsequent y-spectrometry, is used. The following trace elements are determined: Ag, As, Au, Ba, Br, Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Hg, La, Mo, Rb, Sb, Sc, Se, Sm, Zn and W. In the injured tissue compared to the uninjured, calculation on a wet weight basis showed a decrease in Co, Cs, K, Mo, P, Rb and Zn, and an increase in Br, Ca, Ce, La, Na, Sb and Sm. The differences in Ca, La, Mo, P and Zn are dependent on the age of the myocardial infarction, and the regression lines for these elements are given. The concentration of the trace elements in uninjured tissue from infarcted hearts is compared to the concentration of these elements in normal heart tissue, determined in a previous study. In the uninjured tissue from infarcted hearts a decrease is found in Cu and Mo, and an increase in As and Ce.

  15. Laser-time resolved fluorimetric determination of trace of boron in U3O8

    International Nuclear Information System (INIS)

    Xu Yongyuan; Wang Yulong; Wang Qin

    1988-01-01

    In this work, a laser-time resolved fluorimetric determinatin of trace of boron in U 3 O 8 had been developed. The boron complex with dibenzoyl methane (DBM) in a suitable medium is excited by a small nitrogen laser and emits the delay fluorescence with lifetime of 2 ms which is much longer than that of the fluorescence of uranium. Since the fluorescence of uranium doesn't interfere with determination of boron in the time resolved fluorimetric method boron need not be separated from uranium in advance. Thus the determination is very rapid and simple. The limit of determination is 0.02 ngB/ml. When 10 mgU is taken, 0.01 ppm of boron in uranium can be determined. Several samples of U 3 O 8 with boron content from 0.04 to 0.5 ppm have been determined by using this method. The results of determination have been accordant with other methods

  16. Determination of trace amounts of impurities in molybdenum by spark source and glow discharge mass spectrometry

    International Nuclear Information System (INIS)

    Saito, Morimasa

    1994-01-01

    For the determination of trace and ultra-trace amounts of impurities in high-purity molybdenum, spark source mass spectrometry and glow discharge mass spectrometry were studied. In spark source mass spectrometry using the metal probe method, the liquid-helium cryogenic pump was used in order to protect the surface of the samples from oxidation. The theoretical relative sensitivity factors (Mo=1) calculated from physical properties were used. The analytical results obtained for molybdenum tablet and high-purity molybdenum were in good agreement with those obtained by other methods (atomic absorption spectrometry and others). In glow discharge mass spectrometry, the relative sensitivity factors were calculated by using the results obtained by spark source mass spectrometry and atomic absorption spectrometry, and this method was applied to the determination of ultra-trace amounts of impurities in ultra high-purity molybdenum and gave the satisfactory results. The detection limits (2σ, n=10) in the integration time of 600 s for U and Th were 0.6 ppb and 0.3 ppb, and the values for Al, Si, Cr, Mn and Cu were in the range of 10 ppb to 0.5 ppb. (author)

  17. Determination of trace amounts of cadmium in zirconium and its alloys by graphite furnace AAS

    International Nuclear Information System (INIS)

    Takashima, Kyoichiro; Toida, Yukio

    1994-01-01

    Trace amount of cadmium in zirconium and its alloys was determined by graphite furnace atomic absorption spectrometry (GF-AAS) after ion exchange separation. A 2g chip sample was decomposed with 20ml of hydrofluoric acid (1+9) and a few drops of nitric acid. A trace amount of cadmium was separated from zirconium by strongly acidic cation-exchange resin (MCI GEL CK 08P) using 50ml of hydrochloric acid as an eluent. The solution was gently evaporated to dryness on an electric hot plate heater and under an infrared lamp. The residue was dissolved in 1ml of nitric acid (1+14) and diluted to 10ml in a volumetric glass flask with distilled water. Ten microliters of this solution was injected into a graphite furnace and then atomized at 2200degC for 4s in argon at a flow rate of 3.0l/min. Acids used in the analytical procedure were purified by azeotropic distillation and cation-exchange resin. The limit of determination (3σ BK ) for cadmium was 0.5ngCd/g and the relative standard deviation (RSD) at 1ngCd/g level was less than 20% for the GF-AAS. The accuracy of this technique was confirmed by NIST SRM 1643b (trace elements in water). (author)

  18. Studies of effects on determination of trace hydrogen in U-Nb alloy

    International Nuclear Information System (INIS)

    Zou Lexi; Li Yingqiu; Liu Jun; Wu Lunqiang; Qi Lianzhu; Bian Min

    2002-01-01

    The affecting factors for determination of trace hydrogen in U-Nb alloy are studied. The status of samples affects greatly the measured hydrogen content, which has the higher value for scrap sample than cylinder sample. The hydrogen content in cylinder is closer to real value in U-Nb alloy. The hydrogen in U-Nb alloy is mainly from surface adsorption. The results of hydrogen determined by vacuum thermal evolved method, in which the relative standard uncertainty is less than 28%, are in agreement with those by inert-gas fusion method

  19. Determination of trace elements in bottled water in Greece by instrumental and radiochemical neutron activation analyses

    International Nuclear Information System (INIS)

    Soupioni, M.J.; Symeopoulos, B.D.; Papaefthymiou, H.V.

    2006-01-01

    Four different bottled water brands sold in Greece in the winter of 2001-2002 were analyzed for a wide range of chemical elements, using neutron activation analysis (NAA). The elements Na and Br were determined instrumentally (INAA), whereas the other metals and trace elements radiochemically (RNAA). The results indicated that the mean level of all the elements determined in the samples were well within the European Union (EU) directive on drinking water and accomplish the drinking water standards of the World Health Organisation (WHO) as well as of the Food and Drug Administration (FDA). (author)

  20. Trace element determination in tomato puree using particle induced X-ray emission and Rutherford backscattering

    International Nuclear Information System (INIS)

    Romero-Davila, E.; Miranda, J.

    2004-01-01

    Particle induced X-ray emission (PIXE) and Rutherford backscattering spectrometry (RBS) were used to determine the concentrations of trace elements in samples of 12 tomato puree brands sold in the Mexican market. While RBS offered information about the main elements present in the matrix, PIXE gave results on trace elements. As a whole, data for 17 elements (C, N, O, Na, Mg, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, and Zn) were obtained. To evaluate the results, a comparison with brands from USA, Japan, Colombia, and Chile was carried out, using tomato purees produced following the domestic technology recipe. Additionally, the results were considered in the light of the Codex Alimentarius and the Mexican standard. It was found that all of the brands fall within the limits established by these standards, being of the same order of magnitude as the foreign brands. (author)

  1. Determination of short-lived trace elements in environmental samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Wardani, S.; Sihombing, E.; Hamzah, A.; Rochidi; Hery, P.S.; Hartaman, S.; Iman, J.

    1998-01-01

    Concentration of a short-lived trace elements in environmental samples were determined by neutron activation analysis, a counting loss often occur due to the high counting rate. A Pile-Up Rejecter (PUR) electric circuit was installed in counting a short-lived trace elements by a γ-ray spectrometer in order to correct a counting loss. The samples were irradiated for 30∼60 seconds at neutron flux of 3.5 x 10 12 n.cm -2 .s -1 , then the samples cooled for 120 second and counted for 180 second using this system. The nuclides concentration in the varieties environmental samples have a difference analysis result, was more accurate and precise, which the measured result would be 30 % more higher by PUR system than the result would be counted using a conventional γ-ray spectrometry method

  2. Determination of trace and toxic elements in marine sediments collected from the strait of Malacca, Malaysia

    International Nuclear Information System (INIS)

    Wee Boon Siong; Abdul Khalik Hj. Wood

    2007-01-01

    The Strait of Malacca has been a major route for international trade with heavy traffic of large vessels navigating through the narrow waterway everyday. Beside, the Strait of Malacca has some natural ecosystem which requires proper protection from human activities. Therefore, the Malaysian government has initiated a project to monitor the pollution level at the Strait of Malacca. As a result, sampling expeditions had been conducted to collect marine samples to be analyzed for trace and toxic elements as well as organic pollutions and radionuclides. The focus of this report is to determine trace and toxic element concentration in surface sediment samples collected from 18 sampling locations at the Strait of Malacca was reported. (author)

  3. Determination of trace elements in coffee beans and instant coffee of various origins by INAA

    International Nuclear Information System (INIS)

    Zaidi, J.H.; Fatima, I.; Arif, M.; Qureshi, I.H.

    2006-01-01

    Extensive use of coffee, by one-third of world's population, entails the evaluation of trace element contents in it. Instrumental neutron activation analysis (INAA) was successfully employed to determine the concentration of 20 trace elements (essential, toxic and nonessential) in four samples of coffee beans of various origins and two instant coffee brands most commonly consumed in Pakistan. Base-line values of certain toxic and essential elements in coffee are provided. The daily intake of essential and toxic elements through coffee was estimated and compared with the recommended values. The cumulative intake of Mn is four times higher than the recommended value and that of toxic elements is well below the tolerance limits. (author)

  4. Determination of several trace elements in Chinese herbs with epithermal neutral activation analysis

    International Nuclear Information System (INIS)

    Chen, Chien-Yi; Chang Lai, Sheng-Pin

    2002-01-01

    For purpose of medication and health, Chinese herbs have been long adopted throughout oriental communities. Thus, more than ten trace elements in herbal medicines that are frequently consumed by children in central Taiwan were analyzed herein to explore the importance of various herbs. These elements are considered beneficial to human health in many folds. INAA was applied to determine the concentrations of elements as Al, Cl and Sc, while ENAA analyzed As, Cd, Mn, and Sb in this work. Among various local herbs, the elemental concentrations varied from 10 4 to 10 -3 μg/g. The experimental results suggest that the ENAA method can be applied successfully to analyze trace elements of As, Cd, Mn, and Sb in herbs. Yet, thirteen elements were verified, and a quantified index AT was introduced to help classifying the elements. The ATs in various Chinese herbs are also discussed herein and the accuracy is in excellent agreement with values reported in previously published data. (author)

  5. Trace element composition and distribution in micron area of dinosaur eggshell fossils determined by proton microprobe

    International Nuclear Information System (INIS)

    Chen Youhong; Zhu Jieqing; Wang Xiaohong; Wang Yimin

    1997-01-01

    The scanning proton microprobe and micro-PIXE quantitative analysis technique have been used to determine composition and distribution of the trace elements in micron areas of dinosaur eggshell fossils from the stratum of Upper Cretaceous system at Nanxiong Basin in Guangdong Province, China. The study shows that the trace elements mainly include Ti, V, Cr, Mn, Co, Ni, Cu, Zn, As, Rb, Sr, Y, Zr, Sb, Ba and Pb in the micron area, but they present different distributions. While the element Sr is mainly enriched in the near surface layer, others mainly reside in the near inner layer. A preliminary discussion on the reason of the dinosaur extinction is given based on the above study

  6. Trace element composition and distribution in micron area of dinosaur eggshell fossils determined by proton microprobe

    International Nuclear Information System (INIS)

    Chen Youhong; Zhu Jieqing; Wang Xiaohong; Wang Yimin

    1997-01-01

    The scanning proton microprobe and micro-PIXE quantitative analysis technique have been used to determine composition and distribution of the trace elements in micron areas of dinosaur eggshell fossils from the stratum of Upper Cretaceous system at Nanxiong Basin in Guangdong Province, China. The study shows that the trace elements mainly include Ti, V, Cr, Mn, Co, Ni, Cu, Zn, As, Rb, Sr, Y, Zr, Sb, Ba and Pb in the micron area, but they present different distributions. While the elements Sr is mainly enriched in the near surface layer, others mainly reside in the near inner layer. A preliminary discussion on the reason of the dinosaur extinction is given based on the above study

  7. Determination of trace elements in plant samples using XRF, PIXE and ICP-OES techniques

    International Nuclear Information System (INIS)

    Ahmed, Hassan Elzain Hassan

    2014-07-01

    The purpose of this study is to determine trace element concentration (Ca, Cu, Cr, K,Fe, Mn,Sr, and Za) in some sudanese wild plants namely, Ziziphus Abyssinica and Grewia Tenax. X-ray fluorescence ( X RF), particle-induced x-ray emission ( PIXE) and inductively coupled plasma-optical emission spectroscopy (ICP-OES) techniques were used for element determination. A series of plants standard references materials were used to check the reliability of the different employed techniques as well as to estimate possible factors for correcting the concentration of some elements that deviated significantly from their actual concentration. The results showed that, X RF, PIXE and ICP-OES are equally competitive methods for measuring Ca,K, Fe, Sr and Zn elements. Unlikely to ICP-OES seems to be superior techniques tend to be appropriate methods for Cu determination in plant samples however, for Mn element PIXE and ICP-OES are advisable techniques for measuring this element rather than X RF method. On the other hand, ICP-OES seems to be the superior techniques over PIXE and X RF methods for Cr and Ni determination in plant samples. The effect of geographical location on trace elements concentration in plants has been examined through determination of element in different species of Grewia Tenax than collected from different location. Most of measured elements showed similarity indicating there is no significant impact of locations on the difference of element contents. In addition, two plants with different genetic families namely, Ziziphus Spina Christi and Ziziphus Abyssinica were collected from the same location and screened for their trace element content. It was found that there were no difference between the two plants for Ca, K, Cu, Fe, and Sr element. However, significant variations were observed for Mn and Zn concentrations implying the possibility of using of those two elements for plant taxonomy purposes.(Author)

  8. Report on intercomparison V-8 of the determination of trace elements in rye flour

    International Nuclear Information System (INIS)

    Pszonicki, L.; Veglia, A.; Dybczynski, R.; Suschny, O.

    1982-01-01

    The participants were requested to determine as many elements as they could from among the following 29: As, Be, Ca, Cd, Cl, Co, Cr, Cu, F, Fe, Ga, Hg, I, K, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Si, Sn, Tl, U, V and Zn. While six of these elements (Be, Ga, Sn, Tl, U, V) were not determined by any laboratory, some participants on the other hand determined several elements which had not been ordered for such as As, Al, Au, Ba, Br, Cs, Eu, La, N, Rb, S, Sc, Sr, Ti and Y. In total, 34 laboratories submitted results of 1,207 individual determinations (301 laboratory means) on 38 elements. The methods most often employed in this intercomparison were neutron activation analysis (47% of all results) and atomic absorption (20%). The results of the intercomparison demonstrated again the difficulties in the determination of trace elements in organic materials. The agreement between participating laboratories was in general poor

  9. A new method for the determination of unknown neutron fluence for 14.0 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Malik, Fariha [Physics Reasearch Division, PINSTECH, Nilore, Islamabad (Pakistan)]. E-mail: fariha@pinstech.org.pk; Khan, Ehsan U. [Department of Physics, CIIT, Islamabad (Pakistan); Qureshi, Imtinan [Physics Reasearch Division, PINSTECH, Nilore, Islamabad (Pakistan); Husaini, Syed N. [Physics Reasearch Division, PINSTECH, Nilore, Islamabad (Pakistan); Ahmad, Waqar [Physics Reasearch Division, PINSTECH, Nilore, Islamabad (Pakistan); Rajput, Usman [Physics Reasearch Division, PINSTECH, Nilore, Islamabad (Pakistan); Raza, Qaiser [Applied Physics Division, PINSTECH, Nilore, Islamabad (Pakistan)

    2006-11-15

    Measuring the correct neutron fluence in various energy intervals in and around the neutron sources is important for the purpose of personnel and environmental neutron dosimetry. In this paper, we present a new method for the measurement of the fluence of mono-energetic neutrons having the energy of 14.0 MeV. The samples exposed to neutrons from the 14.0 MeV neutron generator at PINSTECH with various fluence values ranging from 10{sup 7} to 10{sup 10} n cm{sup -2} were etched for 10 min in 6 N NaOH at 70.0{+-}1.0 {sup o}C and the transmittance of UV radiation was measured using a spectrophotometer. This procedure was repeated 20 times after etching the same sample each time for increasing time intervals till the stage when transmittance reached the constant minimum value. An exponential decay of the transmittance has been observed with respect to the increasing etching time interval in each of the samples exposed to various neutron fluence. Further, it has also been observed that there is a linear relationship between the transmittance decay constant and neutron fluence. Hence, the linear graph can be used as a calibration for measuring the unknown fluence of 14.0 MeV neutrons.

  10. Determination of trace amounts of boron in steel by high frequency plasma torch spectrometry

    International Nuclear Information System (INIS)

    Akiyoshi, Takanori; Tsukamoto, Takako

    1978-01-01

    Trace amount of boron in steel were determined by means of emission spectrometry using high frequency plasma torch. The sensitivity of this method depended on the kind of solvent used, and methyl alcohol gave the best sensitivity. The determination limit of boron in methanol was 0.002 μg/ml. The established method utilized the high sensibility of the plasma torch and the easy distillation of boron in methanol as trimethyl-borate (B(OCH 3 ) 3 ). The sample was dissolved by acids and dehydrated by hot H 2 SO 4 and H 3 Po 4 . After cooling and addition of methanol (60 ml), the solution was distilled to obtain 40 ml of the distillate. The amount of boron in the distillate was determined by the intensity of the spectral line of B 2497.73 A excited by plasma torch. This method was rapid and accurate, particularly in determining trace amounts of boron and the determination range of boron in steel was 0.2 to 150 ppm. This method was also appliciable to stainless steels and other alloys. (auth.)

  11. The quantitative determination of trace elements in giant unicellular plants by particle-induced X-ray emission

    International Nuclear Information System (INIS)

    Navarrete-Dominguez, V.R.; Yoshihara, K.; Tanaka, N.

    1982-01-01

    Particle-induced X-ray emission (PIXE) was applied for the determination of trace elements in biologically interesting materials, giant unicellular plants. It was found that the PIXE method had advantages in multi-element trace analysis of a single cell of the sample plant. (author)

  12. Worldwide Interlaboratory Comparison on the Determination of Trace Elements in the IAEA-457 Marine Sediment Sample

    International Nuclear Information System (INIS)

    2016-01-01

    The primary goal of the IAEA Environment Laboratories is to assist Member States in the use of both stable and radioisotope analytical techniques to understand, monitor and protect the environment. In this context, the major impact of large coastal cities on marine ecosystems is an issue of primary concern for the IAEA and the IAEA Environment Laboratories. The marine pollution assessments required to understand such impacts depend on accurate knowledge of contaminant concentrations in various environmental compartments. Through the IAEA Environment Laboratories, the IAEA has been assisting national laboratories and regional laboratory networks since the early 1970s through the provision of a reference material programme for the analysis of radionuclides, trace elements and organic compounds in marine samples. Quality assurance and quality control are two fundamental requirements to ensure the reliability of analytical results. Data that are not based on adequate quality assurance and quality control can be erroneous, and their misuse can lead to poor environmental management decisions. In this regard, the IAEA has a long history of organizing interlaboratory studies, which have evolved to include an increasing array of potential contaminants in the marine environment. Relevant activities comprise global interlaboratory comparison, regional proficiency tests, the production of marine reference materials and the development of reference methods for trace elements and organic pollutants analysis in marine samples. This publication summarizes the results of the IAEA-457 interlaboratory comparison on the determination of trace elements in a marine sediment sample

  13. Determination of trace elements concentrations in Grewia tenax plants collected from Darfur Region-Sudan

    International Nuclear Information System (INIS)

    Alzain, H. A; Ebrahim, A. M; Salih, A. M; Ali Altom, M. S.

    2016-01-01

    This study is aimed to determine trace elements concentrations (Ca, Cu, Cr, K,Fe, Mn, Ni, Sr and Zn) in Grewia tenax collected from Darfur state western of Sudan. X- ray fluorescence (X RF) technique was used to determine elements concentration. A series of plant standard reference materials(ISE 2012-1) were used to check the reliability of employed technique by comparing the obtained results with the certified values, to estimate possible factors for correcting the concentration of some elements. The results showed that, X RF is a suitable method for measuring Ca, Cu, K, Fe, Mn, Sr and Zn elements. On the other hand, X RF for Cr and Ni determination in plant samples, these elements have showed a deviation from their certified values. Concentration of Fe was about 35 mg/kg in Grewia tenax samples where as K and Ca showed maximum levels about 16000 and 8500 mg/kg respectively, Cu showed minimum concentration about 10 mg/kg. The effect of geographical location on trace elements concentration in plants has been examined through determination of element in different species of Grewia tenax that collected from different locations in Darfur region. Most of the measured elements showed that there is no significant impact of locations on the difference of element contents.(Author)

  14. Determination of phosphorus traces in platinum alloys by two-phase isotope exchange

    International Nuclear Information System (INIS)

    Vlacil, F.

    1980-01-01

    The method of ZEMAN and KRATZER for the determination of phosphorus traces by means of two-phase isotope exchange was modified for the determination of phosphorus in pure platinum or pure platinum alloys. It was found that Pt, Rh, Ag and As do not interfere with the determination. Among the elements usually present in platinum metal or platinum alloys, only gold interferes. It was removed by extraction from 7M HCl by MIBK and AmOAc. Hydrochloric acid also interferes but it can be removed by evaporation. The analytical procedure is given for the solution obtained by pressure decomposition of the sample (0.5 g) in a steel bomb with PTFE inlay. It is possible to determine > 2 ppm P (approximate error -10%). If using calibration dependence instead of the well known equation for isotope exchange it is not necessary to know the content of P in the standard solution labelled with 32 P. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1978-01-01

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

  16. The determination of trace elements in uranium ores by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    De Villiers, W. van Z.

    1983-11-01

    The determination of 17 trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Rb, Sr, Th, U, V, Y, Zn and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated in this study. The determination of major elements was also necessary for the calculation of mass absorption coefficients. Initially a method was developed for the determination of the elements of interest in unmineralised silicates. Correction for absorption of radiation by the sample were made by means of mass absorption coefficients which were obtained from the relation between the inverse of the mass absorption coefficient and the intensity of the Compton scattering peak. The Feather and Willis method was used for determining the background intensity at the peak positions as well as for mass absorption coefficients. It was observed that the background intensity in the region of the uranium lines increases with increasing uranium content of the sample

  17. Report on intercomparison IAEA/W-4 of the determination of trace elements in simulated fresh water

    International Nuclear Information System (INIS)

    Pszonicki, L.; Hanna, A.N.; Suschny, O.

    1985-05-01

    The report presents results of a laboratory intercomparison on the determination of trace elements in simulated fresh water. 20 trace elements were analyzed by 38 laboratories from 21 countries. The results of the reported comparison confirm the agreement of the nominal concentration values of trace elements in the IAEA/W-4 simulated fresh water with the determined values of these elements. They also confirm that concentrated solutions of this type can be stored in quartz ampoules without any noticeable changes due to the adsorption of trace components on the quartz wall of vessels for considerable time. The concentration values of trace elements could be certified and the material IAEA/W-4 simulated fresh water issued as a reference material. 84% of all results were obtained either by atomic absorption or by atomic emission spectroscopy

  18. Texture one zero Dirac neutrino mass matrix with vanishing determinant or trace condition

    Science.gov (United States)

    Singh, Madan

    2018-06-01

    In the light of non-zero and relatively large value of rector mixing angle (θ13), we have performed a detailed analysis of texture one zero neutrino mass matrix Mν in the scenario of vanishing determinant/trace conditions, assuming the Dirac nature of neutrinos. In both the scenarios, normal mass ordering is ruled out for all the six possibilities of Mν, however for inverted mass ordering, only two are found to be viable with the current neutrino oscillation data at 3σ confidence level. Numerical and some approximate analytical results are presented.

  19. Adsorptive stripping voltammetric determination of trace amounts of lead in environmental water samples with complicated matrix

    Directory of Open Access Journals (Sweden)

    Grabarczyk M.

    2013-04-01

    Full Text Available A sensitive, simple and fast adsorptive stripping voltammetric procedure for trace determination of lead in environmental water samples has been developed. The method is based on adsorptive accumulation of the Pb(II-cupferron complex onto a hanging mercury drop electrode, followed by the reduction of the adsorbed species by a voltammetric scan using differential pulse modulation. The interference from surface active substances was eliminated by adsorption of interferents onto an Amberlite XAD-16 resin. Optimumconditions for removing the surfactants by mixing the analysed sample with resin were evaluated. The accuracy of the method was tested by analyzing certified reference material (SPS-WW1 Waste Water.

  20. Trace element determination in soft tissues of marine bivalves by activation analysis

    International Nuclear Information System (INIS)

    Fukushima, M.; Tamate, H.; Nakano, Y.

    2003-01-01

    Trace elements in soft tissues of marine bivalves were determined by neutron activation analysis (NAA) and photon activation analysis (PAA). Elemental levels of Ag, As, Br, Co, Cu, Fe, I, Mn, Ni, Rb, Se, and Zn in the organs of giant ezoscallos, rock oysters, and giant crams were obtained. The metal-bound proteins were extracted from the mantles and hepatopancreases of rock oysters. By irradiating the fraction obtained by HPLC gel chromatography, the possibility for the existence of an Ag bound protein in the mantles was found. (author)

  1. Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

    International Nuclear Information System (INIS)

    Pourreza, N.

    2004-01-01

    Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

  2. A Fast Radiochemical Method for the Determination of Some Essential Trace Elements in Biology and Medicine

    International Nuclear Information System (INIS)

    Samsahl, K.

    1964-12-01

    A method has been developed for the determination with neutron-activation analysis of the following trace elements in soft biological tissues: Br, Ca, Cl, Cu, K, Mg, Mn, Mo, Na, P, Sr and Zn. The method consists in performing a short-term irradiation of the samples with a high thermal neutron flux, followed by fast chemical separations and gamma-spectrometric measurements. The chemical separations and the measurements of short-lived nuclides from a run are finished within 70 min, after the end of irradiation

  3. Determination of trace elements in human brain tissues using neutron activation analysis

    International Nuclear Information System (INIS)

    Leite, R.E.P.; Jacob-Filho, W.; Grinberg, L.T.; Ferretti, R.E.L.

    2008-01-01

    Neutron activation analysis was applied to assess trace element concentrations in brain tissues from normal (n = 21) and demented individuals (n = 21) of both genders aged more than 50 years. Concentrations of the elements Br, Fe, K, Na, Rb, Se and Zn were determined. Comparisons were made between the results obtained for the hippocampus and frontal cortex tissues, as well as, those obtained in brains of normal and demented individuals. Certified reference materials, NIST 1566b Oyster Tissue and NIST 1577b Bovine Liver were analyzed for quality of the analytical results. (author)

  4. Preliminary investigation on determination of radionuclide distribution in field tracing test site

    International Nuclear Information System (INIS)

    Tanaka, Tadao; Mukai, Masayuki; Takebe, Shinichi; Guo Zede; Li Shushen; Kamiyama, Hideo.

    1993-12-01

    Field tracing tests for radionuclide migration have been conducted by using 3 H, 60 Co, 85 Sr and 134 Cs, in the natural unsaturated loess zone at field test site of China Institute for Radiation Protection. It is necessary to obtain confidable distribution data of the radionuclides in the test site, in order to evaluate exactly the migration behavior of the radionuclides in situ. An available method to determine the distribution was proposed on the basis of preliminary discussing results on sampling method of soils from the test site and analytical method of radioactivity in the soils. (author)

  5. Determination of trace elements in tea by wavelength dispersive X-ray fluorescence spectroscopy

    International Nuclear Information System (INIS)

    Gong Chunhui; Zeng Guoqiang; Ge Liangquan; Li Jun; Wen Ziqiang

    2013-01-01

    Background: Measuring trace elements in tea can determine its nutritional value, verify the authenticity and place of origin, and detect the poisonous and harmful elements remaining in tea due to the application of chemical fertilizers and pesticides. Purpose: In order to reduce the time for sample preparation and the costs of equipment maintenance, wavelength dispersive X-ray fluorescence (WDXRF) spectroscopy was used to determine the trace elements in tea which is rapid, non-destructive and accurate. The contents of more than 20 elements can be measured simultaneously. Methods: Sample pieces were made by the sample preparation method of boric acid rebasing. To avoid the exogenous environmental pollution subjected in the growth of tea, we removed the residual dust of the tea by cleaning it. According to the principle that the standard samples should be similar types with the samples to be analyzed to select standard samples. The curves were built by SuperQ, which contained compiling the measurement conditions, establishing the measurement conditions, checking the angles, determining the measurement times, checking PHD and adding the contents and the names of sample pieces. The accuracy of the method can be obtained by comparing the measured values with the trace element contents of standard samples. The contents of trace elements in tea determined by WDXRF can be used to classify the tea attribution and the tea species through cluster analysis of SPSS software. Results: (1) The results show that the biggest relative standard deviation is 0.43% of Pb, and the precision is very good. (2) Five kinds of tea are taken separately in Fujian and Yunnan, measured three times with the established working curves. And tree diagram of cluster analysis can be obtained with SPSS software to analyze the measured average values with cluster analysis, coupling method between groups and Minkowski distance measurement techniques. It can be seen that in the tree diagram, when the

  6. A Fast Radiochemical Method for the Determination of Some Essential Trace Elements in Biology and Medicine

    Energy Technology Data Exchange (ETDEWEB)

    Samsahl, K

    1964-12-15

    A method has been developed for the determination with neutron-activation analysis of the following trace elements in soft biological tissues: Br, Ca, Cl, Cu, K, Mg, Mn, Mo, Na, P, Sr and Zn. The method consists in performing a short-term irradiation of the samples with a high thermal neutron flux, followed by fast chemical separations and gamma-spectrometric measurements. The chemical separations and the measurements of short-lived nuclides from a run are finished within 70 min, after the end of irradiation.

  7. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed...... by superior performance and versatility. In fact, two approaches are conceivable: The analyte-loaded ion-exchange beads might either be transported directly into the graphite tube where they are pyrolized and the measurand is atomized and quantified; or the loaded beads can be eluted and the eluate forwarded...

  8. Trace aluminium determination and sampling problems of archeological bone employing destructive neutron activation analysis

    International Nuclear Information System (INIS)

    Blotcky, A.J.; Rack, E.P.; Recker, R.R.; Leffler, J.A.; Teitelbaum, S.

    1978-01-01

    A destructive neutron activation analysis procedure was developed for determining trace aluminium content in bone. The method is based on a carefully planned sample preparation, irradiation at a neutron flux for 3.1x10 11 nxcm -2 xs -1 for 5 minutes, and chemical separation based on ion exchange. It was found that bone samples soaked in aluminium containing soil gave highly elevated aluminium values as a result of the aluminium adsorption into the bone matrix. The maximum aluminium content values for prehistoric bones are larger than those of modern bones and comparable to aluminium levels present in bone from renal patients. (T.G.)

  9. Determination of trace elements of Egyptian crops by neutron activation analysis Pt. 3

    International Nuclear Information System (INIS)

    Sherif, M.K.; Awadallah, R.M.; Amrallah, A.H.

    1980-01-01

    Multielemental neutron activation analysis was used for the determination of Al, As, Au, Br, Ca, Cd, Co, Cr, Cu, Fe, La, Mn, Mo, Sb, Se, W and Zn in African tea and lady's fingers (Malvaceae Family), ginger (Zingiperanceae Family), canella bark (Laureceae Family), black pepper (Piperaceae Family), cucumber seeds and vegetable marrow seeds (Cucurbitaceae Family), tomatos seed (Solanaceae Family), safflower seeds (Compositae Family), jew's mallow seed (Tiliaceae Family) and sesame (Pedaliaceae Family). Trace elements determination was made for the analysis of destructive (using super pure nitric acid and adsorbing the metal-APDC and metal-Dz complexes on activated charcoal) and nondestructive (dry seeds) samples. The method is simple, precise and sensitive for the determination of microamounts of the elements (ppm to ppb). (author)

  10. Abstracts book of 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements

    International Nuclear Information System (INIS)

    1995-01-01

    The 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements has been held in Poznan 27-28 April 1995. The new versions of analytical methods have been presented for quantitative determination of trace elements in biological, environmental and geological materials. Also the number of special techniques for sample preparation enables achievement the best precision of analytical results have been shown and discussed

  11. Selenium and Trace Element Distribution in Astragalus Plants: Developing a Differential Pulse Polarographic Method for Their Determination

    OpenAIRE

    SOMER, Güler; ÇALIŞKAN, A. Cengiz

    2007-01-01

    Astragalus plants have a wide range of applications in pharmaceuticals (gum tragacanth), as thickening agents in foods, and may have applications in controlling cancer cells. They are used as feed for animals and they are indicator plants for selenium. Because of their use in health-related areas it is very important to determine their selenium and trace element content with high accuracy. A new differential pulse polarographic method was established for trace element determination (...

  12. Determination of trace metals and analysis of arsenic species in tropical marine fishes from Spratly islands.

    Science.gov (United States)

    Li, Jingxi; Sun, Chengjun; Zheng, Li; Jiang, Fenghua; Wang, Shuai; Zhuang, Zhixia; Wang, Xiaoru

    2017-09-15

    Trace metal contents in 38 species of tropical marine fishes harvested from the Spratly islands of China were determined by microwave digestion and inductively coupled plasma mass spectrometry analysis. Arsenic species were determined by high-performance liquid chromatography and inductively coupled plasma mass spectrometry analysis. The average levels of Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Pb, and U in the fish samples were 1.683, 0.350, 0.367, 2.954, 36.615, 0.087, 0.319, 1.566, 21.946, 20.845, 2.526, 3.583, 0.225, 0.140, and 0.061mg·kg -1 , respectively; Fe, Zn, and As were found at high concentrations. The trace metals exhibited significant positive correlation between each other, with r value of 0.610-0.852. Further analysis indicated that AsB (8.560-31.020mg·kg -1 ) was the dominant arsenic species in the fish samples and accounted for 31.48% to 47.24% of the total arsenic. As(III) and As(V) were detected at low concentrations, indicating minimal arsenic toxicity. Copyright © 2017. Published by Elsevier Ltd.

  13. Trace Elements in the Conductive Tissue of Beef Heart Determined by Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Wester, P.O.

    1965-08-01

    By means of neutron activation analysis, samples of four beef hearts taken from the bundle of His and adjacent ventricular muscle, the AV node and adjacent atrial muscle are investigated with respect to the concentration of 23 trace elements. The bulk elements K, Na and P are also determined. A recently developed ion-exchange technique, combined with subsequent γ-spectrometry, is used. The following trace elements are determined: Ag, As, Au, Ba, Br, .Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Hg, La, Mo, Rb, Sb, Sc, Se, Sm, W and Zn. In the conductive tissue compared to adjacent muscle tissue, calculations on a wet weight basis show a lower concentration of Cs, Cu, Fe, K, P, Rb and Zn in the former, and a higher concentration of Ag, Au, Br, Ca and Na. The mean differences (μg/g wet tissue), as well as their degree of significance, between the bundle of His and adjacent tissue from the ventricular septum, between the AV node and adjacent atrial muscle, between the ventricular septum and the right atrium, and between the bundle of His and the AV node are given for the elements Cu, Fe, K, Na, P and Zn

  14. Trace element determinations in brain tissues from normal and clinically demented individuals

    International Nuclear Information System (INIS)

    Saiki, Mitiko; Genezini, Frederico A.; Leite, Renata E.P.; Grinberg, Lea T.; Ferretti, Renata E.L.; Suemoto, Claudia; Pasqualucci, Carlos A.; Jacob-Filho, Wilson

    2013-01-01

    Studies on trace element levels in human brains under normal and pathological conditions have indicated a possible correlation between some trace element concentrations and neurodegenerative diseases. In this study, analysis of brain tissues was carried out to investigate if there are any differences in elemental concentrations between brain tissues from a normal population above 50 years of age presenting Clinical Dementia Rating (CDR) equal to zero (CDR=0) and that cognitively affected population ( CDR=3). The tissues were dissected, ground, freeze-dried and then analyzed by instrumental neutron activation analysis. Samples and elemental standards were irradiated in a neutron flux at the IEA-R1 nuclear research reactor for Br, Fe, K, Na, Rb, Se and Zn determinations. The induced gamma ray activities were measured using a hyperpure Ge detector coupled to a gamma ray spectrometer. The one-way ANOVA test (p< 0.05) was used to compare the results. All the elements determined in the hippocampus brain region presented differences between the groups presenting CDR=0 and CDR=3. In the case of frontal region only the elements Na, Rb and Zn showed differences between these two groups. These findings proved the correlation between elemental levels present in brain tissues neurodegenerative diseases. Biological standard reference materials SRM 1566b Oyster Tissue and SRM 1577b Bovine Liver analyzed for quality control indicated good accuracy and precision of the results. (author)

  15. Trace Elements in the Conductive Tissue of Beef Heart Determined by Neutron Activation Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Wester, P O

    1965-08-15

    By means of neutron activation analysis, samples of four beef hearts taken from the bundle of His and adjacent ventricular muscle, the AV node and adjacent atrial muscle are investigated with respect to the concentration of 23 trace elements. The bulk elements K, Na and P are also determined. A recently developed ion-exchange technique, combined with subsequent {gamma}-spectrometry, is used. The following trace elements are determined: Ag, As, Au, Ba, Br, .Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Hg, La, Mo, Rb, Sb, Sc, Se, Sm, W and Zn. In the conductive tissue compared to adjacent muscle tissue, calculations on a wet weight basis show a lower concentration of Cs, Cu, Fe, K, P, Rb and Zn in the former, and a higher concentration of Ag, Au, Br, Ca and Na. The mean differences ({mu}g/g wet tissue), as well as their degree of significance, between the bundle of His and adjacent tissue from the ventricular septum, between the AV node and adjacent atrial muscle, between the ventricular septum and the right atrium, and between the bundle of His and the AV node are given for the elements Cu, Fe, K, Na, P and Zn.

  16. Semi-quantitative spectrographic determination of traces of elements in igneous rocks

    International Nuclear Information System (INIS)

    Costa, M.Q. da; Eichhoff, H.-J.

    1982-01-01

    A semi-quantitative spectrographic technique based on Harveys'method, using background radiation as internal standard is described for the analysis of trace elements in igneous rocks by the total energy method. A certain amount of the sample was completely vapourized in a DC arc with anodic excitation under argon and oxygen atmosphere, using graphite electrodes of standard dimensions. In the processed film, selected lines and adjancent backgrounds were evaluated by densitometry and the corresponding intensity ratios were calculated. Sensitivity factors were determined for the analytical lines of Co, Cu, Ga, Ni, Sc, Sr, V, Y, Zn, and Zr in geological standards (G-2, BCR-1, AGV-1, GSP-1) from the United States Geological Survey. Matrix effects between samples and standards were minimized by using the above mentioned geological standards. An average value of the sensitivity factors was employed for the calculation of the concentration of the elements in the samples. A comparison between the results obtained by this method and those from the analysis of zinc by atomic absorption is presented. This method enabled the analyses of igneous rock samples having SiO2 contents between 40 and 80%, with an error in the determinations of trace elements less than 30%.(Author) [pt

  17. Electrochemical preconcentration and hydride generation methods for trace determination of selenium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Bye, R.

    1986-01-01

    The use of atomic absorption spectrometry in combination with two different preconcentration/separation techniques for the determination of trace concentrations of selenium is described. Electrochemical preconcentration onto a platinum electrode with a subsequent atomization of selenium is discussed briefly. Several parameters are considered such as the presence of depolarizers, and the temperature of the electrolyzed solutions. Special attention is payed to the efficiency of the atomization step, and a method to improve this is proposed. Applications of the technique to real samples are also reported. Secondly, the separation of the selenium as the volatile selenium hydride from the sample solution is considered. Several papers in this thesis deal with commonly occurring interferants as nickel and copper and with ways of minimizing or avoiding the interferring effects, whereas other papers relate to more theoretical aspects of the hydride generation process. New methods for the determination of selenium in technical samples with high contents of nickel and copper are also presented

  18. A radioagent method for determination of traces of phosphorus in high-purity silicon

    International Nuclear Information System (INIS)

    Chen, P.Y.; Chen, J.S.; Sun, H.J.; Yang, M.H.

    1985-01-01

    The feasibility of the determination of phosphorus at the extreme trace levels in high-purity silicon by radioreagent method is explored. After silicon dissolution with hydrofluoric and nitric acids and matrix volatilization, 12-molybdophosphoric acid is formed by the addition of the reagent, sup(99)MoOsub(4)sup(2-), in nitric acid medium and then extracted into isobutyl acetate. By plotting the phosphorus content against the radioactivity of sup(99)Mo in the organic phase, a linear relationship persisting down to 5 ng is obtained. Special effort was made to eliminate the unreacted sup(99)MoOsub(4)sup(2-) reagent and the optimal control of phosphorus blank introduced through the multistage analytical procedure in order to ensure reliable determination of phosphorus at the ppb level. (author)

  19. Liquid-Liquid Extraction and Determination of Trace Elements in Iron Minerals by Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Taseska, Milena; Stafilov, Trajche; Makreski, Petre; Jacimovic, Radojko; Jovanovski, Gligor

    2006-01-01

    Various trace elements (cadmium, chromium, cobalt, nickel, manganese) in some iron minerals were determined by flame (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). The studied minerals were chalcopyrite (CuFeS 2 ), hematite (Fe 2 O 3 ) and pyrite (FeS 2 ). To avoid the interference of iron, a method for liquid-liquid extraction of iron and determination of investigated elements in the inorganic phase was proposed. Iron was extracted by diisopropyl ether in hydrochloride acid solution and the extraction method was optimized. Some parameters were obtained to be significantly important: Fe mass in the sample should not exceed 0.3 g, the optimal concentration of HCI should be 7.8 mol 1 -1 and ratio of the inorganic and organic phase should be 1: 1. The procedure was verified by the method of standard additions and by its applications to reference standard samples. The investigated minerals originate from various mines in the Republic of Macedonia. (Author)

  20. Levels of trace elements in different varieties of wheat determined by Atomic Absorption Spectroscopy

    International Nuclear Information System (INIS)

    Mohamed, A.E.; Taha, G.M.

    2003-01-01

    Trace elements Ag, Au, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn were determined in six wheat samples purchased from the open market in different localities (Egypt, Saudi Arabia, Yemen, Oman, Dubai and Australia). The dried powdered samples were decomposed in HNO3-HClO4 acids mixtures and elements were determined using recording atomic absorption spectrophotometer. The results were within the safety baseline of all the assayed elements. Certified biological standards, Brown's Kale (BK), Orchard Leaves (OL) and tomato leaves (TOML) were used to assure the accuracy of results. However, Co, Pb and Sr were absent from samples except the Egyptian samples. The obtained databases were statistically treated. Several significant and strong positive correlation coefficients (r=0.506-1.00) between the groups of elements were observed. On the other hand, strong negative correlations (r=0.492-0.873) between another group of elements were also shown. (author)

  1. Determination of trace amounts of tin in geological materials by atomic absorption spectrometry

    Science.gov (United States)

    Welsch, E.P.; Chao, T.T.

    1976-01-01

    An atomic absorption method is described for the determination of traces of tin in rocks, soils, and stream sediments. A dried mixture of the sample and ammonium iodide is heated to volatilize tin tetraiodide -which is then dissolved in 5 % hydrochloric acid, extracted into TOPO-MIBK, and aspirated into a nitrous oxide-acetylene flame. The limit of determination is 2 p.p.m. tin and the relative standard deviation ranges from 2 to 14 %. Up to 20 % iron and 1000 p.p.m. Cu, Pb, Zn, Mn, Hg, Mo, V, or W in the sample do not interfere. As many as 50 samples can be easily analyzed per man-day. ?? 1976.

  2. Activation analytical determination of essential and toxic trace elements in biological material

    International Nuclear Information System (INIS)

    Schelenz, R.

    1980-01-01

    In order to determine the essential trace elements Hg, Ag, Cu and Se in food (potatoes, milk powder) and biological standard materials (fruit tree leaves), simple, fast radiochemical separation methods are worked out. Following oxidative decomposition and destillation of Hg, the elements silver, copper and selenium are found in the destillation residue and can be electrochemically enriched on an amalgamated Cu foil (determination of Ag and Se in the concentration range of 10 -9 to 10 -8 g, of Cu in the range of 10 -12 to 10 -10 g), whilst the matrix elements Na, K, P are adsorbed on a column with 3 different inorganic ion exchangers. The eluate of the ion exchanger can be added directly to the multielement gamma spectroscopy. The possiblity of working purely instrumentally is demonstrated by 2 examples: multielement analysis of human hair and river water. (RB) [de

  3. Particle induced X-ray emission and complementary nuclear methods for trace element determination; Plenary lecture

    Energy Technology Data Exchange (ETDEWEB)

    Johansson, S A.E. [Lund Univ. (Sweden). Dept. of Nuclear Physics

    1992-03-01

    In this review the state-of-the-art of particle induced X-ray emission (PIXE) methods for the determination of trace elements is described. The developmental work has mostly been carried out in nuclear physics laboratories, where accelerators are available, but now the increased interest has led to the establishment of other dedicated PIXE facilities. The reason for this interest is the versatility, high sensitivity and multi-element capability of PIXE analysis. A further very important advantage is that PIXE can be combined with the microbeam technique, which makes elemental mapping with a spatial resolution of about 1 {mu}m possible. As a technique, PIXE can also be combined with other nuclear reactions such as elastic scattering and particle-induced gamma emission, so that light elements can be determined. The usefulness of PIXE is illustrated by a number of typical applications in biology, medicine, geology, air pollution research, archaeology and the arts. (author).

  4. Application of the radioreagent method to the determination of trace quantities of lead

    International Nuclear Information System (INIS)

    Figueiredo, A.M.G.; Saiki, M.; Lima, F.W. de

    1983-01-01

    The radioreagent method of analysis was applied to determine trace quantities of lead in several types of samples. This method is based on the extraction of radioactive cobalt, displaced by lead from the cobalt chelate of ethylenediaminetetraacetate labeled with 60 Co, into a tetracycline-benzyl alcohol solution. The radioactivity of the released cobalt, extracted into the organic phase, measured by menas of a single channel gamma-ray analyzer coupled to a Na(T1) scintillation detector, is proportional to the lead concentration. The elements which might interfere with the analysis were removed by a chemical separation procedure of lead using dithizone. The method was applied for lead determination in air samples, gasoline and samples from the International Atomic Energy Agency, namely: simulated air filter (Air-3), fresh water (W-3), dried animal whole blood(A-2) and calcinated animal bone (A3/1). The sensitivity, accuracy and precision of the method were also discussed. (Author) [pt

  5. Experimental determination of trace-element partitioning between pargasite and a synthetic hydrous andesitic melt

    Science.gov (United States)

    Brenan, J. M.; Shaw, H. F.; Ryerson, F. J.; Phinney, D. L.

    1995-10-01

    In order to more fully establish a basis for quantifying the role of amphibole in trace-element fractionation processes, we have measured pargasite/silicate melt partitioning of a variety of trace elements (Rb, Ba, Nb, Ta, Hf, Zr, Ce, Nd, Sm, Yb), including the first published values for U, Th and Pb. Experiments conducted at 1000°C and 1.5 GPa yielded large crystals free of compositional zoning. Partition coefficients were found to be constant at total concentrations ranging from ˜ 1 to > 100 ppm, indicating Henry's Law is oparative over this interval. Comparison of partition coefficients measured in this study with previous determinations yields good agreement for similar compositions at comparable pressure and temperature. The compatibility of U, Th and Pb in amphibole decreases in the order Pb > Th > U. Partial melting or fractional crystallization of amphibole-bearing assemblages will therefore result in the generation of excesses in 238U activity relative to 230Th, similar in magnitude to that produced by clinopyroxene. The compatibility of Pb in amphibole relative to U or Th indicates that melt generation in the presence of residual amphibole will result in the long-term enrichment in Pb relative to U or Th in the residue. This process is therefore incapable of producing the depletion in Pb relative to U or Th inferred from the Pb isotopic composition of MORB and OIB. Comparison of partition coefficients measured in this study with previous values for clinopyroxene allows some distinction to be made between expected trace-element fractionations produced during dry (cpx present) and wet (cpx + amphibole present) melting. Rb, Ba, Nb and Ta are dramatically less compatible in clinopyroxene than in amphibole, whereas Th, U, Hf and Zr have similar compatibilities in both phases. Interelement fractionations, such as DNb/DBa are also different for clinopyroxene and amphibole. Changes in certain ratios, such as Ba/Nb, Ba/Th, and Nb/Th within comagmatic suites may

  6. Determination of several trace elements in Chinese herbs with epithermal neutral activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Chien-Yi [Chung Shan Medical Univ., Inst. of Biochemistry, Taiwan (China); Chang Lai, Sheng-Pin [Chung Shan Medical Univ. Hospital, Dept. of Nuclear Medicine Chief, Taiwan (China)

    2002-04-01

    For purpose of medication and health, Chinese herbs have been long adopted throughout oriental communities. Thus, more than ten trace elements in herbal medicines that are frequently consumed by children in central Taiwan were analyzed herein to explore the importance of various herbs. These elements are considered beneficial to human health in many folds. INAA was applied to determine the concentrations of elements as Al, Cl and Sc, while ENAA analyzed As, Cd, Mn, and Sb in this work. Among various local herbs, the elemental concentrations varied from 10{sup 4} to 10{sup -3} {mu}g/g. The experimental results suggest that the ENAA method can be applied successfully to analyze trace elements of As, Cd, Mn, and Sb in herbs. Yet, thirteen elements were verified, and a quantified index AT was introduced to help classifying the elements. The ATs in various Chinese herbs are also discussed herein and the accuracy is in excellent agreement with values reported in previously published data. (author)

  7. Photoresponsive molecularly imprinted hydrogel casting membrane for the determination of trace tetracycline in milk.

    Science.gov (United States)

    Wang, Qiang; Lv, Zhen; Tang, Qian; Gong, Cheng-Bin; Lam, Michael Hon Wah; Ma, Xue-Bing; Chow, Cheuk-Fai

    2016-03-01

    This study aimed to develop a photoresponsive molecularly imprinted hydrogel (MIH) casting membrane for the determination of trace tetracycline (TC) in milk. This MIH casting membrane combined the specificity of MIHs, the photoresponsive properties of azobenzene, and the portable properties of a membrane. Photoresponsive TC-imprinted MIHs were initially fabricated and then cast on sodium dodecyl sulfonate polyacrylamide gel. After TC removal, a photoresponsive MIH casting membrane was obtained. The photoresponsive properties of the MIH casting membrane were robust, and no obvious photodegradation was observed after 20 cycles. The MIH casting membrane displayed specific affinity to TC upon alternate irradiation at 365 and 440 nm; it could quantitatively uptake and release TC. The TC concentration (0.0-2.0 × 10(-4) mol l(-1)) in aqueous solution displayed a linear relationship with the photoisomerization rate constant of azobenzene within the MIH casting membrane. As such, a quick detection method for trace TC in aqueous foodstuff samples was established. The recovery of this method for TC in milk was investigated with a simple pretreatment of milk, and a high recovery of 100.54-106.35% was obtained. Therefore, the fabricated membrane can be used as a portable molecular sensor that can be easily recycled. Copyright © 2015 John Wiley & Sons, Ltd.

  8. Determination of trace elements: Neutron-activation analysis in geochemistry and cosmochemistry

    International Nuclear Information System (INIS)

    Kolesov, G.M.

    1994-01-01

    Geochemistry, like cosmochemistry, open-quotes studies chemical elements hor-ellipsis of the crust and hor-ellipsis the Earth hor-ellipsis their history, their distribution hor-ellipsis their genetic hor-ellipsis connectionsclose quotes and is based on data on the abundance and distribution of elements obtained by various analytical methods. Neutron-activation analysis (NAA) plays a particular role in this respect. This is due to its high sensitivity (detection limit as small as 10 -14 g), which makes possible the use of samples of arbitrary mass, and also due to the possibility of obtaining information about composition without destruction of the object, conserving, if required, the unique material under investigation. Of the most interest are the data on the contents for a number of trace elements (at a level of 10 -7 - 10 -4 %), among which are rare-earth elements (REE), U, Th, Zr, Hf, Ta, W, Ga, Ni, Rb, Cs, platinum-group metals, Ag, Au, etc. These elements are considered as indicators of geochemical processes associated with the genesis and evolution of solar system bodies in early and more recent stages of evolution; they are also used to study processes and phenomena at zone boundaries: river-sea, ocean-atmosphere, and so on. The aim of this work is to show the capabilities of NAA in the determination of trace elements

  9. Determination of trace metals in coastal seawater around Okinawa and its multielement profiling analysis

    International Nuclear Information System (INIS)

    Itoh, Akihide; Ishigaki, Teruyuki; Arakaki, Teruo; Yamada, Ayako; Yamaguchi, Mami; Kabe, Noriko

    2009-01-01

    In the present study, trace metals in coastal surface seawater around Okinawa were determined by inductively coupled plasma mass spectrometry (ICP-MS) with chelating disk preconcentration. As a result, the concentrations of V, Mn, Co, Ni, Cu, Zn, Mo, Cd, Pb, and U were obtained in the range from 10 μgL -1 to 0.001 μgL -1 for 6 samples. In addition, multielement profiling analyses were carried out using analytical values obtained in order to elucidate the features of trace metals in each coastal sea area. For coastal surface seawater near an urban area, the analytical values for Zn, Cu, Mn, and Pb were higher by more than 10-fold the literature values for open-surface seawater, and those of Cd were also relatively high. Such a trend concerning the multi-element profile was almost similar to the literature values for coastal seawater of the main island of Japan. On the other hand, the analytical values of most elements for coastal surface seawater near a suburb area were in the range from 0.5 to 5 fold, compared to the literature values for open surface seawater. From multielement profiling analyses for nutrient type elements in marine chemistry, it was suggested that the concentrations of Zn and Cd in a coral sea area normalized to literature values for open surface-seawater were higher than those of Ni and Cu. (author)

  10. Trace water vapor determination in nitrogen and corrosive gases using infrared spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Espinoza, L.H.; Niemczyk, T.M. [Univ. of New Mexico, Albuquerque, NM (United States). Dept. of Chemistry; Stallard, B.R.; Garcia, M.J. [Sandia National Labs., Albuquerque, NM (United States)

    1997-06-01

    The generation of particles in gas handling systems as a result of corrosion is a major concern in the microelectronics industry. The corrosion can be caused by the presence of trace quantities of water in corrosive gases such as HCl or HBr. FTIR spectroscopy has been shown to be a method that can be made compatible with corrosive gases and is capable of detecting low ppb levels of water vapor. In this report, the application of FTIR spectroscopy combined with classical least squares multivariate calibration to detect trace H{sub 2}O in N{sub 2}, HCl and HBr is discussed. Chapter 2 discusses the gas handling system and instrumentation required to handle corrosive gases. A method of generating a background spectrum useful to the measurements discussed in this report, as well as in other application areas such as gas phase environmental monitoring, is discussed in Chapter 3. Experimental results obtained with the first system are presented in Chapter 4. Those results made it possible to optimize the design options for the construction of a dedicate system for low ppb water vapor determination. These designs options are discussed in Chapter 5. An FTIR prototype accessory was built. In addition, a commercially available evacuable FTIR system was obtained for evaluation. Test results obtained with both systems are discussed in Chapter 6. Experiments dealing with the interaction between H{sub 2}O-HCl and potential improvements to the detection system are discussed in Chapter 7.

  11. Determination of isoniazid concentration in rabbit vertebrae by isotope tracing technique in conjunction with HPLC.

    Science.gov (United States)

    Liu, Peng; Fu, Zhaozong; Jiang, Jianming; Yuan, Liang; Lin, Zhen

    2013-09-01

    Medications compounded with isoniazid (INH) are usually applied to surgical sites at the completion of surgery to locally kill postoperative residual tubercle bacilli. However, the distribution and elimination of INH in the vertebrae in vivo are not known. In this study, isotope tracing was used in conjunction with high-pressure liquid chromatography (HPLC) to address this. INH and technetium-99 m-labeled INH were applied to the vertebrae of rabbits. After 2 and 6 h, osseous tissues containing INH, as determined by radionuclide imaging, were collected for detection with HPLC. The results showed that INH mainly stayed around the vertebrae 6 h after its application and did not permeate widely into the blood or other organs, except for the kidneys. The standard deviations of INH concentrations in the technetium-99 m-INH group were approximately four-fold smaller than those in the INH group. This method of coupling isotope tracing and HPLC can effectively limit experimental error during sample collection, allowing accurate and reliable identification of the concentration levels of INH in osseous tissues in vivo. Copyright © 2013 John Wiley & Sons, Ltd.

  12. Photometric determination of trace cadmium in waste water drained from uranium mining and water-metallurgy

    International Nuclear Information System (INIS)

    Zhu Zihui; Gu Gang; Xu Quanxiu

    1987-09-01

    Cadmium (Cd) ions react with dithizone to form a pink to red color that can be extracted with chloroform and measured photometrically. Dithizone method is one of standard method to determine trace Cd in the environmental waste water. This method, however, can not be suitable for measuring the trace Cd in the waste water drained from uranium mining and water-metallurgy factory, because this kind of waste water contains magnesium ions as high as 1500 mg/L. One more discomfort is that the method needs to use a large amount of potassium cyanide. The authors, therefore, used potassium fluorine as a precipitator that removed the excess magnesium ions in the experimental system, and try to reduce the amount of potassium cyanide to 1/20 of original usage. The experimental results indicated that the modified method as mentioned above was very satisfactory either to simulated samples or to actual samples of waste water drained from uranium mining and water-metallurgy plants. In Summary, this modified method has higher sensitivity with minimun detectable quantity of 0.02 ppm and it is accurate and reproducible with recovery rate of 100 ± 5%

  13. Trace elements determinations in cancerous and non-cancerous human tissues using instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Choi, Insup.

    1989-01-01

    Recent improvements in analyzing techniques when coupled to the growing knowledge of trace element biochemistry provide a powerful tool to investigate the relationship between trace elements and cancer. It is hoped that selective delivery or restriction of specific minerals may aid in cancer prevention or treatment. Tissues were collected at the time of surgery of various cancer patients including colon cancer and breast cancer. Three kinds of tissues were taken from a patient; cancerous, noncancerous, and transitional tissue obtained from a region located between the cancer and healthy tissues. A total of 57 tissues were obtained from 19 cancer patients. Seven of them were colon cancer patients, and 5 of them were breast cancer patients. Nine elements were determined using instrumental activation analysis. Cancerous colon tissue had significantly higher concentrations of selenium and iron than healthy tissues. Cancerous breast tissue had significantly higher concentrations of selenium, iron, manganese, and rubidium than healthy tissues. Iron can be enriched in cancer tissue because cancer tissue retains more blood vessels. Selenium is enriched in cancer tissue, possibly in an effort of the body to inhibit the growth of tumors. The manganese enrichment can be explained in the same manner as selenium considering its suspected anticarcinogenicity. It is not certain why rubidium was enriched in cancer tissue. It could be that this is the result of alteration of cell membrane permeability, change in extracellular matrix, or increased metabolism in cancer tissue

  14. Determination of Trace Elements In Soil and Plants In Coastal Basin of Syria By Using Instrumental Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Kassem, A.

    2004-01-01

    Instrumental neutron activation analysis (INAA) methods have been used for the determination of some major, minor and trace elements (As, Cr, Co, Ni, Zn, Sb, Sc Ce, Ti, Fe, Mn and V) in some kinds of plant leaves with their soil. Accuracy of measurements have been evaluated by analyzing a number of plant and soil reference materials, precision have been estimated by triplicate the sample as well as the reference. The obtained accurate and reliable data in microgram quantities of some trace elements in plants and soil will serve as baseline values and will be helpful to monitor the changes in the trace elements content of soil and plant leaves. (Author)

  15. The determination of minor isotope abundances in naturally occurring uranium materials. The tracing power of isotopic signatures for uranium

    Energy Technology Data Exchange (ETDEWEB)

    Ovaskainen, R

    1999-11-01

    Atomic Energy Agency (IAEA) from uranium milling and mining facilities (Australia, Canada, Gabon, Namibia, Czech Republic, France), were determined. These signatures form the basic register. The isotopic signatures are feasible in identifying the sample origin and in separating naturally occurring or background contributions from local anthropogenic sources. With the comparison of fingerprints of unknown samples to the isotopic fingerprints of samples of known origin, it is possible to trace back unknown samples to their origin or at least to exclude suspected origins in the case of non-identity of fingerprints. This was successfully demonstrated with a number of samples of unknown origin, which were measured during the study. Generally, no significant variability was observed in the n({sup 235}U)/n({sup 238}U) ratios except in the well known case of samples originating from Oklo (Gabon). Small variations in the n({sup 234}U)/n({sup 238}U) amount ratios were understood from the radiochemical mother-daughter relationship of the two isotopes involved. The detection limit for the n({sup 236}U)/n({sup 235}U) amount ratio (DL = 0.000001) was derived from blank measurements. The limit of quantitation 0.000003 was calculated as LQ=3DL. When the measured ratio exceeded the quantitation limit, the presence of {sup 236}U is explained. (orig.) 99 refs.

  16. The determination of minor isotope abundances in naturally occurring uranium materials. The tracing power of isotopic signatures for uranium

    International Nuclear Information System (INIS)

    Ovaskainen, R.

    1999-01-01

    facilities (Australia, Canada, Gabon, Namibia, Czech Republic, France), were determined. These signatures form the basic register. The isotopic signatures are feasible in identifying the sample origin and in separating naturally occurring or background contributions from local anthropogenic sources. With the comparison of fingerprints of unknown samples to the isotopic fingerprints of samples of known origin, it is possible to trace back unknown samples to their origin or at least to exclude suspected origins in the case of non-identity of fingerprints. This was successfully demonstrated with a number of samples of unknown origin, which were measured during the study. Generally, no significant variability was observed in the n( 235 U)/n( 238 U) ratios except in the well known case of samples originating from Oklo (Gabon). Small variations in the n( 234 U)/n( 238 U) amount ratios were understood from the radiochemical mother-daughter relationship of the two isotopes involved. The detection limit for the n( 236 U)/n( 235 U) amount ratio (DL = 0.000001) was derived from blank measurements. The limit of quantitation 0.000003 was calculated as LQ=3DL. When the measured ratio exceeded the quantitation limit, the presence of 236 U is explained. (orig.)

  17. Selberg trace formula for bordered Riemann surfaces: Hyperbolic, elliptic and parabolic conjugacy classes, and determinants of Maass-Laplacians

    International Nuclear Information System (INIS)

    Bolte, J.

    1992-08-01

    The Selberg trace formula for automorphic forms of weight m ε- Z, on bordered Riemann surfaces is developed. The trace formula is formulated for arbitrary Fuchsian groups of the first kind which include hyperbolic, elliptic and parabolic conjugacy classes. In the case of compact bordered Riemann surfaces we can explicitly evaluate determinants of Maass-Laplacians for both Dirichlet and Neumann boundary-conditions, respectively. Some implications for the open bosonic string theory are mentioned. (orig.)

  18. Cell-selective determination of trace elements in testis by SR-XRF analysis with nanoprobe

    International Nuclear Information System (INIS)

    Homma-Takeda, Shino; Nishimura, Yoshikazu; Watanabe, Yoshito; Yukawa, Masae; Ueno, Shunji; Terada, Yasuko

    2005-01-01

    Organotin compounds are widely used in industry and its environmental contamination by these compounds has recently become a concern. It is known that they act as endocrine disruptors but details of the dynamics of Sn in reproductive organs are still unknown. In the present study, we attempted to determine Sn in the testis of rats exposed to tributyltin chloride (TBTC) cell-selectively by synchrotron radiation X-ray florescence analysis with nanoprobe. TBTC was orally administered to rats at a dose of 45 μmol/kg per day for 3 days. One day later, Sn was detected in spermatozoa at the stage VIII seminiferous tubule, which are the final step of spermatogenesis in the testis. Sn levels in the microdissectioned seminiferous tubules determined by inductively coupled argon plasma-mass spectrometry were approximately equivalent to that in the testis. These data indicate that Sn accumulates in germ cells as well as in spermatozoa in a short period of TBTC exposure. (author)

  19. 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

  20. Determination of trace elements in the reproduction systems of some rare animals using pixe

    Science.gov (United States)

    Suqing, Chen; Nengming, Wang; Jianxuan, Chen; Dazhong, Zhang

    In order to search for the significance of artificial feeding, reproduction and heredity, trace elements in the reproductive systems of some rare animals, including giant panda, lesser panda, marmot and river deer, have been determined. Typcial X-ray spectra of various samples are given. The elemental contents in ovary and testis of the giant panda and the lesser panda are calculated by means of yttrium as an internal standard. Elemental relative concentrations are calculated from peak areas in the spectra for thick samples. It is found that for the concentration of the elements Cr, Mn, Fe, Ni, Cu, As in the ovary there exist no significant different between the giant panda and the lesser panda. The concentration of Zn, however, shows a remakable difference. The importance of zinc in biological processes is discussed.

  1. Determination of trace amounts of cadmium in sea water by a flameless atomic absorption method

    International Nuclear Information System (INIS)

    Yamazoe, Seigo; Oshima, Shozo

    1975-01-01

    Determination of trace amounts of cadmium in sea water has been developed by a flameless atomic absorption method using a carbon rod atomizer. Sea water is diluted with isopropyl alcohol and the white salt formed is removed by filtration, then the filtrate is fed to the instrument as a sample for measurement. A complete separation of the salt is not needed in this pre-treatment. The effect of the residual salt can be avoided by separating the atomic absorption of cadmium and the molecular absorption of the residual salt by means of controlling the temperature and the time of ashing and atomization of the sample in the carbon rod. The repeatability and the accuracy are 2.0--8.5% in the coefficient of variation and 0.8--5.3% respectively. (auth.)

  2. Preparation of an estuarine sediment quality control material for the determination of trace metals

    Directory of Open Access Journals (Sweden)

    Hatje Vanessa

    2006-01-01

    Full Text Available Quality Control Materials (QCM have being used routinely in daily laboratory work as a tool to fill the gap between need and availability of Certified Reference Materials (CRM. The QCM are a low-cost alternative to CRMs, and they are in high demand, especially, for the implementation of quality control systems in laboratories of several areas. This paper describes the preparation of a QCM for the determination of trace metals in estuarine sediments and the results of an interlaboratory exercise. Homogeneity and stability studies were performed and analysis of variance was carried out with the results. No statistical significant differences were observed in the concentrations of Co, Cr, Cu, Mn, Pb and Zn between- or within bottle results. Neither the storage nor temperature affected the results. Therefore, the QCM produced is considered homogeneous and stable and can be used for statistical control charts, evaluation of reproducibility and interlaboratory exercises.

  3. Determination of some toxic trace elements in Indian tobacco and its smoke

    International Nuclear Information System (INIS)

    Shaikh, A.N.; Khandekar, R.N.; Anand, S.J.S.; Mishra, U.C.

    1992-01-01

    Toxic trace metals like mercury, arsenic and cadmium have been determined in widely used Indian chewing tobacco and cigarette tobacco by neutron activation followed by sequential radiochemical separation (RNAA). Differential Pulse Anodic Stripping Voltammetry (DPASV) has been used for the estimation of lead, cadmium and copper in cigarette tobacco and its smoke aerosols. The reliability of the data has been assured by analyzing standard reference materials, bovine liver (NBS-1577) and orchard leaves (NBS-1571), and intercomparison of the Pb, Cd and Cu values by three techniques, namely, RNAA, DPASV and Energy Dispersive X-ray Fluorescence technique (EDXRF). The levels of Hg, Cd, As, Pb, and Cu in cigarette and chewing tobacco and the estimated intake of Cd, Cu and Pb to the smoker are presented and discussed. (author) 12 refs.; 3 tabs

  4. Determination of trace elements in acid rain by reversed phase extraction chromatography and neutron activation

    International Nuclear Information System (INIS)

    Rao, R.R.; Goski, D.G.; Chatt, A.

    1991-01-01

    A preconcentration neutron activation analysis (PNAA) method has been developed for the simultaneous determination of selected trace elements in acid rain and other water samples. The method consists of preconcentration of the elements by reversed phase extraction chromatography using oxine-loaded Amberlite XAD-2 resin. Nearly 100% recoveries were obtained for Co, Cu, Hg, V and Zn at pH 6.0 and for Cd at pH 7.0. Manganese gave incomplete recoveries at the pH range of 4.0-8.0 studies. Various factors that can influence preconcentration of the elements have been investigated in detail. The precision and accuracy of measurements have been evaluated by analyzing certified reference materials. The detection limits have been found to be of the order of ppb. The PNAA method has been applied to a number of acid rain and other water samples

  5. Thermometric Titration for Rapid Determination of Trace Water in Jet Fuel

    Directory of Open Access Journals (Sweden)

    Jian-Qiang Hu

    2017-01-01

    Full Text Available Water content in jet fuels is detected by thermometric titration (TMT, and the optimal detected system is 2,2-dimethoxypropane as titrant, cyclohexane and isopropanol as titration solvents, and methanesulfonic acid as catalyst in this method. The amounts of oil, concentration and delivery rate of titrant, volumes, and the reliability and accuracy of thermometric titration were emphasized. The results show that the accuracy, validity, and reliability of TMT are excellent by different indicated spiked water contents. The obtained results between TMT and Karl Fischer titration have been proven to be in accord. But, the duration of titration merely spends 3–5 min in the whole process, greatly shortening the detected time. Therefore, rapid and accurate determination of trace water in a jet fuel can be realized by TMT.

  6. Trace quantities of uranium in some indian chewing tobaccos as determined by fission track analysis

    International Nuclear Information System (INIS)

    Rana, N.P.S.; Singh, P.; Azam, A.; Naqvi, A.H.; Srivastava, D.S.

    1996-01-01

    The sandwiched pellet technique using Makrofol-E plastic track detectors has been employed to determine trace quantities of uranium in nine brands of flavored chewing tobaccos consumed by the Indian population. In this technique the nuclear reaction, 235 U(n,f), is used for the quantitative estimation of uranium. The maximum value of uranium (1.88 ppm) has been found in raw tobacco leaves (Surti), while the minimum (0.13 ppm) in Tulsi (Double Zero brand). Other seven brands showed intermediate values of U-contents which are also reported in this paper. These values are compared with the U-contents reported in the literature for other forms of tobaccos. (author). 9 refs., 2 figs., 1 tab

  7. (F)UV Spectroscopy of K648: Abundance Determination of Trace Elements

    Science.gov (United States)

    Mohamad-Yob, S. J.; Ziegler, M.; Rauch, T.; Werner, K.

    2010-11-01

    We present preliminary results of an ongoing spectral analysis of K 648, the central star of the planetary nebula Ps 1, based on high resolution FUV spectra. K 648, in M 15 is one of only four known PNe in globular clusters. The formation of this post-AGB object in a globular cluster is still unclear. Our aim is to determine Teff, log g, and the abundances of trace elements, in order to improve our understanding of post-AGB evolution of extremely metal-poor stars, especially PN formation in globular clusters. We analyzed FUSE, HST/STIS, and HST/FOS observations. A grid of stellar model atmospheres was calculated using the Tübingen NLTE Model Atmosphere Package (TMAP).

  8. Determination of rare earths and traces of other elements by neutron activation analysis

    International Nuclear Information System (INIS)

    Atalla, L.T.; Mantovani, M.S.M.; Marques, L.S.

    A complete methodology for a multielemental analysis in geological material using the neutron activation technique was developed. 21 trace elements (9 of which are rare earths) were determined using thermal and epithermal neutron irradiations. Instrumetnal and radiochemical processing, applied to BCR-1 and G-2 geological standards, are described. Statistical tests carried out on G-2 data show an error smaller than 15% referring to all elements except Cr, Sb and Yb. The observed differences between are discussed. The good precision attained in this method is confirmed by its application to BCR-1 standard, which presents errors smaller than 4% for all elements except Nd, due to its intrinsic properties. The results from the present work are compared with those from other laboratories. (C.L.B.) [pt

  9. Determination of trace and toxic elements in Koran rice CRM by INAA, ICP and AAS

    International Nuclear Information System (INIS)

    Yong Sam Chung; Young Ju Chung; Kyung Haeng Cho; Joung Hae Lee

    1997-01-01

    Trace and toxic elements in Certified Reference Material (CRM) made of Korean rice at the Korea Research Institute of Standards and Science have been analyzed by Instrumental Neutron Activation Analysis (INAA). Data intercomparison from the measurement with those of Atomic Absorption Spectrometry (AAS) and Induced Coupled Plasma Spectrometry (ICPS) has been studied. The powdered samples were sterilized at 1.5 x 10 6 rad in the bottles using a 60 Co source after sieving and spiking to specific elements such as As, Cd, Cr, Cu and Hg and then the homogeneity of samples was assessed. Rice flour (SRM 1568a) and standard solutions made by the National Institute of Standards Technology (NIST) were used to construct the calibration curves for the INAA and the chemical methods, respectively. The uncertainties and concentration of constituent elements were determined and the possibility of their use for analytical quality control was considered. (author)

  10. 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.

  11. [Fluorescence Determination of Trace Se with the Hydride-K13-Rhodamine 6G System].

    Science.gov (United States)

    Liang, Ai-hui; Li, Yuan; Huang, Shan-shan; Luo, Yang-he; Wen, Gui-qing; Jiang, Zhi-liang

    2015-05-01

    Se is a necessary trace element for human and animals, but the excess intake of Se caused poison. Thus, it is very important to determination of Se in foods and water. The target of this study is development of a new, sensitive and selective hydride generation-molecular fluorescence method for the determination of Se. In 0. 36 mol . L-1 sulfuric acid, NaBH4 as reducing agent, Se (IV) is reduced to H2 Se. Usin3-g I solution as absorption liquid3, I- is reduced to I- by H2Se. When adding rhodamine 6G, Rhodamine 6G and I3- form association particles, which lead to the fluorescence intensity decreased. When Se(IV) existing, Rhodamine 6G and I3- bind less, And the remaining amount of Rhodamine 6G increase. So the fluorescence intensity is enhanced. The analytical conditions were optimized, a 0. 36 ml . L-1 H2SO4, 21. 6.g . L-1 NaBH4, 23.3 µm . L-1 rhodamine 6G, and 50 µmol . L-1 KI3 were chosen for use. When the excitation wavelength is at 480nm, the Rayleigh scattering peak does not affect the fluorescence recording, and was selected for determination of Se. Under the selected conditions, Se(IV) concentration in the 0. 02~0. 60 µg . mL-1 range and the increase value of the fluorescence intensity (ΔF) at 562 nm linear relationship. The linear regression equation is ΔF562 nm =12. 6c + 20. 9. The detecton limit was 0.01 µ.g . L-1. The influence of coexistence substances on the hydride generatin-molecular fluorescence determination of 5. 07 X10(-6) mol . L-1 Se(IV) was considered in details. Results showed that this new fluorescence method is of high selectivity, that is, 0. 5 mmol. L-1 Ba2+, Ca2+, Zn2+ and Fe3+, 0. 25 mmol . L-1 . Mg2+, 0. 05 mmol . L-1 K+, 0. 2 mmol . L-1 Al3+, 0. 025 mmol . L-1 Te(VI) do not interfere with the determination. The influence of Hg2+, CD2+ and Cu2+ that precipitate with Se(IV), can be eliminated by addition of complex reagent. This hydride generation-molecular fluorescence method has been applied to determination of trace Se in water

  12. Determination of minor-and trace elements in magnesite samples, by activation analysis

    International Nuclear Information System (INIS)

    Sepulveda Munita, C.J.A.

    1979-01-01

    A method employing activation analysis with thermal neutron was developed for the determination of minor and trace elements in magnesite samples from the states of Ceara and Bahia (Brazil). Ten samples were analyzed. A qualitative analysis of the samples indicated the presence of Mn, Fe, Sc, Ca, Cu, Co and some of the lanthanides. The experimental part includes a non-destructive analysis of manganese and analysis with chemical separation of the other elements, individually or in groups, after sample dissolution, The dissolutions were made with concentrated HCl and the further separations were carried out in 8 N HCl medium. Iron was separated by means of an extraction of HFeCl 4 with isopropyl ether. Scandium and calcium were determined by retention of scandium with di-(2-ehylhexyl) phosphoric acid (HDEHP). The activities of 46 Sc and 47 Sc (a 47 Ca descendant) were employed for the analysis of scandium and calcium in the sample. In the effluent of the kieselguhr column copper and cobalt were determined, after retention in an anionic resin of the CuCl - 3 and CoCl - 3 complexes. Finally, in the effluent of the resin, the lanthanide group was separated by oxalate precipitation. In the gamma-ray spectrum of this precipitate the elements europium, cerium, samarium and lanthanum were determined. A detailed study of the possible interferences in the neutron activation analysis of the elements analysed was also made. The precision and accuracy of the results obtained and the sensitivity of the method are discussed. (Author) [pt

  13. Application of chronocoulomentry for trace levels uranium determination using catalytic nitrate reduction on mercury electrode

    International Nuclear Information System (INIS)

    Cantagallo, M.I.C.

    1988-01-01

    With the aim of improving the sensitivity of the electro-analytical determination of uranium at trace levels, the uranium catalyzed reduction of nitrate on mercury electrodes was used and the technique of chronocoulometry was compared with other voltammetric techniques. The catalytic process offers high sensitivity in comparison with uranyl reduction in absence of nitrate. The chronocoulometry, virtually unexplored for analytical applications, was found to be specially well suited for determinations based on this kind of electrode process, when using current integration times in the range of several seconds. Under these conditions the interference from diffusion controlled faradaic processes is reduced to a minimum. Several experimental parameters were investigated (eletrolyte composition, potential program, integration time, blank correction, temperature, previous separation) and adequate conditions were selected for the analytical determination of pure and real samples. The proposed method was applied and evaluated with real and, when necessary, an adapted liquid-liquid extraction procedure was used. Reference materials with complex matrices like rocks were first solubilized by hot digestion under pressure. The obtained results are in good agreement with the values obtained with other techniques such as X-ray fluorescence, mass spectrometry-isotope dilution and epithermal netron activation analysis. (author) [pt

  14. Determination of trace levels of iodine in table salt by ICP-TOF MS

    International Nuclear Information System (INIS)

    Waqar, F.; Muhammad, B.; Hakim, M.; Jan, S.

    2012-01-01

    An ion exchange method was established for the effective removal of sodium matrix for iodine determination by ICP-TOF-MS technique. Since the direct determination of trace level analytes in the presence of heavy matrix is not recommended by this technique. Therefore, the removal of matrix is essentially required to achieve better detection limits and to avoid memory effects. The extraction system was designed for the removal of matrix prior to the analysis by ICP-MS, various parameters were optimized to achieve efficient removal of matrix. The accuracy of the method was evaluated by spiking salt samples with known amount of iodine (50 mu g/g) and % recoveries were calculated. The recoveries obtained were > 98% with relative standard deviation (RSD) < 5%. The established method was applied for the analysis of commercially available iodized table salt samples. The results and % recoveries are given. The most commonly used iodo metric titration method is not satisfactory as it has 5-10 % quantitative error. Our method is reliable and could be conveniently applied for the determination of iodine in table salt samples. (Orig./A.B.)

  15. Determination of minor and trace elements in kidney stones by x-ray fluorescence analysis

    Science.gov (United States)

    Srivastava, Anjali; Heisinger, Brianne J.; Sinha, Vaibhav; Lee, Hyong-Koo; Liu, Xin; Qu, Mingliang; Duan, Xinhui; Leng, Shuai; McCollough, Cynthia H.

    2014-03-01

    The determination of accurate material composition of a kidney stone is crucial for understanding the formation of the kidney stone as well as for preventive therapeutic strategies. Radiations probing instrumental activation analysis techniques are excellent tools for identification of involved materials present in the kidney stone. In particular, x-ray fluorescence (XRF) can be very useful for the determination of minor and trace materials in the kidney stone. The X-ray fluorescence measurements were performed at the Radiation Measurements and Spectroscopy Laboratory (RMSL) of department of nuclear engineering of Missouri University of Science and Technology and different kidney stones were acquired from the Mayo Clinic, Rochester, Minnesota. Presently, experimental studies in conjunction with analytical techniques were used to determine the exact composition of the kidney stone. A new type of experimental set-up was developed and utilized for XRF analysis of the kidney stone. The correlation of applied radiation source intensity, emission of X-ray spectrum from involving elements and absorption coefficient characteristics were analyzed. To verify the experimental results with analytical calculation, several sets of kidney stones were analyzed using XRF technique. The elements which were identified from this techniques are Silver (Ag), Arsenic (As), Bromine (Br), Chromium (Cr), Copper (Cu), Gallium (Ga), Germanium (Ge), Molybdenum (Mo), Niobium (Nb), Rubidium (Rb), Selenium (Se), Strontium (Sr), Yttrium (Y), Zirconium (Zr). This paper presents a new approach for exact detection of accurate material composition of kidney stone materials using XRF instrumental activation analysis technique.

  16. Th, U and trace elements determination in Egyiptian Lake sediments by INAA and laser fluorimetry

    International Nuclear Information System (INIS)

    Ismail, S.S.; Grass, F.; Ghods, A.

    1995-01-01

    A study was undertaken to determine element concentrations in Aswan High Dam Lake sediments. Sediment samples were collected from 40 to 500 km upstream of the dam to follow the sedimentation process and the distribution of Th, U and the trace elements in the lake. INAA was applied for the determination of Sm, Ce, Lu, Th, Cr, Yb, Au, Hf, Ba, Nd, Cs, Tb, Sc, Rb, Fe, Zn, Co, Eu, and Sb, while Laser Fluorimetry was applied for U determination. The accuracy and the reproducibility of the techniques were tested with IAEA standard materials (SL, Soil-7). The U values ranged from 4 ppm to 18 ppm, Th values were between 2 and 10 ppm, and showed a very good correlation with the rare earth elements and Fe. The distribution of most of the elements in the lake follows the same trend as the distribution of the clays in the sediments. Ba showed a negative correlation with most of the elements under investigation. (author) 5 refs.; 4 figs.; 7 tabs

  17. The determination of traces of uranium by means of laser fluorometry

    International Nuclear Information System (INIS)

    Venter, R.J.

    1987-11-01

    A method and apparatus were developed to quantitatively determine traces of uranium. A xenon chloride excimer laser was used as an excitation source, which provided various advantages above the conventional light sources. Boxcar integration was used to limit background fluorescence by time-resolved fluorescence spectroscopy. A characteristic wavelength of uranium fluorescence was selected with cut-off filters and a monochromator. The effect of different matrices on the fluorescence of uranium was determined, and the most suitable matrix for quantitative analysis was chosen. A quick and simple method for determining uranium was developed. A combined water sample of industrial effluent was used to evaluate the method. The effect of interfering species, characteristic of the water sample, was examined. A standard addition technique was used to compensate for the effect of the interfering species. The detection limit of uranium in pure water was calculated at three times the standard deviation of the blank sample and was found to be 14 pg/cm 3

  18. Determination of trace elements in fisheries samples by instrumental neutron and photon activation analysis

    International Nuclear Information System (INIS)

    Chattopadhyay, A.; Ellis, K.M.; Nimalasiri Desilva, K.

    1979-01-01

    An instrumental neutron activation analysis (INAA) method has been developed for the simultaneous determination of trace concentrations of up to 23 elements in fisheries samples. The INAA method consists of irradiations of wet and lyophilized cod muscle and liver samples for three different periods at a flux density of 5x10 11 n.cm -2 .s -1 and subsequent measurements after four different decay periods using high-resolution Ge(Li) gamma-ray spectrometry. Concentrations of several essential and toxic elements have been determined. Loss of certain elements during lyophilization has been studied. Elemental distribution in muscles and livers as a function of the age of fish has been investigated. Precision and accuracy of the INAA method have been evaluated by analysing replicate samples, National Bureau of Standards' bovine liver standard reference material, and an intercalibration fish flour sample provided by the International Council for the Exploration of the Sea. A few fish samples have also been analysed by an alternative method, namely instrumental photon activation analysis (IPAA). Elemental concentrations determined by both INAA and IPAA methods are reported here. (author)

  19. Determination of trace quantities of uranium in rocks mass spectrometric isotope dilution technique

    International Nuclear Information System (INIS)

    Kakazu, Mauricio Hiromitu

    1980-01-01

    A detailed experimental investigation on the thermionic emission of uranium deposited on a single flat type rhenium filament has been carried out. The study was aimed at determining the influence of various forms of deposition on the emission sensitivity and thermal stability of U + , UO + and UO 2 + ions. Based on these investigations, a technique, involving an addition of a small quantity of colloidal suspension of graphite on top of the uranyl nitrate sample deposited, was chosen because of its higher, emission sensitivity for uranium metal ions. The experimental parameters of the technique were optimised and the technique was employed in the determination of trace quantities of uranium in rock samples using mass spectrometric isotope dilution method. For the mass spectrometric isotope dilution analysis National Bureau of Standards uranium isotopic standard NBS-U 970 was employed as a tracer, where as the mass discrimination effect in the uranium isotope analysis was corrected using the uranium isotopic standard NBS-U500. Uranium was determined in each of the seven granite samples from Wyoming, USA and two USGS standard rocks. The precision of the analysis was found to be ±1% . The uranium values obtained on the rock samples were compared with the analyses of other investigators. Influence of the sample splitting on the uranium analysis was discussed in the light of the analytical results obtained.(author)

  20. Determination of metal traces in lubricating oils by Aas and Icp-SFMS after microwave digestion

    International Nuclear Information System (INIS)

    Perez B, M. A.; Acosta L, C. E.; Hernandez M, H.; Romero G, E. T.; Lara A, N.; Kuri C, A.

    2016-09-01

    The analysis of lubricating oils allows to monitor the operating conditions of the machines and equipment, their pollution levels, degradation and finally their wear and useful life, as well as to establish a preventive lubrication program as a technical diagnostic maintenance tool. The useful life of oil is the period of functional time has in the machine until the antioxidants are consumed, producing large changes in the physical (density and viscosity) and chemical properties of the base oil, resulting in a wear of the components that make up the machine. The present work includes a theoretical as well as analytical basis for determining the content of metallic elements (Ag, Al, Cu, Fe, Mg, Sn and Zn) at trace level in used lubricating oils. A simple and rapid method of analysis is proposed, consisting mainly of the pretreatment of the sample by acidic digestion with a microwave oven. Subsequently an open digestion in a heating plate is carried out to dryness and recovered with concentrated HNO 3 . For the quantitative analysis two analytical techniques were used: flame atomic absorption spectroscopy (Aas) and magnetic sector mass spectrometry with inductively coupled plasma source (Icp-SFMS). In both cases, the proposed method offers a good linearity and sensitivity for each of the trace elements under study. The accuracy of the method expressed as relative standard deviation ranges from 1.4 to 2.3%. In relation to the accuracy measurement, an oil was also analyzed as a certified reference material (Conostan 500 mg/L), with the concentration of certified Mg, obtaining satisfactory results. (Author)

  1. Determination of trace elements in total particulate matter of cigarette smoke by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Mishra, U.C.; Shaikh, G.N.

    1985-01-01

    Cigarette smoke contains many trace elements hazardous for human body. Tobacco samples were analyzed for their trace element contents and the results were reported earlier. This paper presents results on the trace element content analyzed in cigarette smoke using an automatic smoking machine developed in laboratory to simulate actual smoking pattern. The trace element levels in the total particulate matter samples of the cigarette smoke collected on filter papers were measured and compared with those of cigarette smoke condensate reported in the literature. Both methods of collection give comparable results. (author)

  2. Determination of trace element mineral/liquid partition coefficients in melilite and diopside by ion and electron microprobe techniques

    Science.gov (United States)

    Kuehner, S. M.; Laughlin, J. R.; Grossman, L.; Johnson, M. L.; Burnett, D. S.

    1989-01-01

    The applicability of ion microprobe (IMP) for quantitative analysis of minor elements (Sr, Y, Zr, La, Sm, and Yb) in the major phases present in natural Ca-, Al-rich inclusions (CAIs) was investigated by comparing IMP results with those of an electron microprobe (EMP). Results on three trace-element-doped glasses indicated that it is not possible to obtain precise quantitative analysis by using IMP if there are large differences in SiO2 content between the standards used to derive the ion yields and the unknowns.

  3. A new atomization cell for trace metal determinations by tungsten coil atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Donati, G.L., E-mail: georgedonati@yahoo.com.br [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States); Wildman, R.B.; Jones, B.T. [Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 (United States)

    2011-02-28

    A new metallic atomization cell is used for trace metal determinations by tungsten coil atomic absorption spectrometry and tungsten coil atomic emission spectrometry. Different protecting gas mixtures are evaluated to improve atomic emission signals. Ar, N{sub 2}, CO{sub 2} and He are used as solvents, and H{sub 2} and C{sub 2}H{sub 2} as solutes. A H{sub 2}/Ar mixture provided the best results. Parameters such as protecting gas flow rate and atomization current are also optimized. The optimal conditions are used to determine the figures of merit for both methods and the results are compared with values found in the literature. The new cell provides a better control of the radiation reaching the detector and a small, more isothermal environment around the atomizer. A more concentrated atomic cloud and a smaller background signal result in lower limits of detection using both methods. Cu (324.7 nm), Cd (228.8 nm) and Sn (286.3 nm) determined by tungsten coil atomic absorption spectrometry presented limits of detection as low as 0.6, 0.1, and 2.2 {mu}g L{sup -1}, respectively. For Cr (425.4 nm), Eu (459.4 nm) and Sr (460.7 nm) determined by tungsten coil atomic emission spectrometry, limits of detection of 4.5, 2.5, and 0.1 {mu}g L{sup -1} were calculated. The method is used to determine Cu, Cd, Cr and Sr in a water standard reference material. Results for Cu, Cd and Cr presented no significant difference from reported values in a 95% confidence level. For Sr, a 113% recovery was obtained.

  4. A simple spectrophotometric determination of trace amounts of vanadium using thionin

    Directory of Open Access Journals (Sweden)

    Tom Cherian

    2005-12-01

    Full Text Available A simple and sensitive spectrophotometric method has been developed for the determination of trace amounts of vanadium using thionin as a chromogenic reagent. The proposed method is based on the reaction of vanadium(V with potassium iodide in acid medium to liberate iodine, which bleaches the violet colour of thionin and is measured at 600 nm. This decrease in absorbance is directly proportional to the vanadium(V concentration and obeys Beer's law in the range of 0.2-10 μgmL-1 of V(V. The molar absorptivity, Sandell's sensitivity, detection limit and quantitation limit of the method were found to be 2.298 x 104 Lmol-1cm-1, 0.52 x 10-2 μgcm-2, 0.035 μgmL-1 and 0.11 μgmL-1, respectively. The optimum reaction conditions and other analytical conditions were evaluated. The effect of interfering ions on the determination is described. The developed method has been successfully applied to the analysis of the vanadium in synthetic and alloy samples.

  5. Determination of Trace Antimony (III by Adsorption Voltammetry at Carbon Paste Electrode

    Directory of Open Access Journals (Sweden)

    Nongyue He

    2005-05-01

    Full Text Available This work presents a sensitive method for the determination of trace antimonybased on the antimony-pyrogallol red (PGR adsorption at a carbon paste electrode (CPE.The optimal conditions were to use an electrode containing 25% paraffin oil and 75%high purity graphite powder as working electrode, a 0.10 mol/L HCl solution containing3.0×10-5 mol/L PGR as accumulation medium and a 0.20 mol/L HCl solution aselectrolyte with an accumulation time of 150 s and a reduction time of 60 s at -0.50 Vfollowed with a sweep from -0.50 V to 0.20 V. The mechanism of the electrode reactionwas discussed. Interferences of other metal ions were studied as well. The detection limitwas 1×10-9 mol/L. The linear range was from 2.0×10-9 mol/L to 5.0×10-7 mol/L.Application of the proposed method to the determination of antimony in water andhuman hair samples gave good results.

  6. Determination of trace elements and heavy metals in sediment using x-ray fluorescence

    International Nuclear Information System (INIS)

    Sidahmed, Muataz Ahmed Ibrahem

    2014-01-01

    In this study, 30 sediment samples were taken randomly from the area of Suba south of Khartoum state. Trace elements and heavy metal were determined in sediments samples using x-ray fluoresce spectroscopy (X RF). K, Ca, Ti, Mn, Fe, Cu, Zn, Pb, Rb, Sr, and Zr were determined by X RF. Standard Reference Material (SRM) from international Atomic Energy Agency (IAEA-Soil-7) has been used to achieve accuracy of X RF method. Measured values were found in agreements with certified values. The average elemental concentrations of K, Ca, Ti, Mn, Fe, Cu, Zn, Pb, Rb, Sr, and Zr were 5882.7, 20703.3, 6264.3, 460.97, 26713.3, 7.7, 43.4, 18.6, 28.6, 144.8, and 173.06, respectively. Correlation between elements was performed also cluster analysis was used to check the similarly between the samples result. The result of study were compared with previous studies and the concentrations of some elements found to be similar.(Author)

  7. Intercomparison and determination of trace elements in urban dust by neutron activation analysis

    International Nuclear Information System (INIS)

    Chung, Yong Sam; Moon, Jong Hwa; Kim, Sun Ha; Park, Kwang Won; Kang, Sang Hun

    2000-01-01

    Trace elements in air samples artificially loaded on filters with urban dust and the bulk material of urban dust as an environmental sample were determined non-destructively using instrumental neutron activation analysis. Standard reference material (Urban Dust, SRM 1648) of the National Institute of Standard and Technology was used for the analytical quality control. The relative error for 37 elements was less than 15% and the standard deviation was less than 10%. 29 elements in the urban dust and 21 elements in the loaded filter sample were determined respectively. To evaluate the proficiency and reliability of the measurement, data intercomparison was performed and 39 analytical laboratories participated in the analysis using different analytical methods; neutron activation analysis, particle induced X-ray emission analysis, X-ray fluorescence analysis and atomic absorption spectrometry. Z-scores were calculated using the standard deviation of the laboratory's mean as target standard deviation, and a good result was obtained that the values fall between-1 and +1 except some elements. (author)

  8. Determination of arsenic and other trace elements in cosmetics by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Gonzalez Cepeda, A.M.; Cienfuegos Silva, E.E.

    1978-01-01

    A general survey of trace-elements in different types of cosmetics, in particular arsenic, was carried out in order to detect elements that might be detrimental to human health. The samples were analyzed by instrumental neutron activation analysis and high-resolution gamma-ray spectrometry with Ge(Li) detectors. Different amounts of Br and Sb, detected in almost all the samples, produced interferencies in the determination of As when the 559 KeV photopeak was used. Since the triplet formed could not be resolved by the Ge(Li) detector, a mathematical procedure was developed using the 776 KeV gamma-ray emission of 82-Br and various factors found experimentally. This procedure was checked using laboratory-made samples of known concentrations and the results obtained had good precision and accuracy. In addition to arsenic the elements Co, Cr, Br, Sc, Fe and Zn were also quantitatively determined. Those cosmetics made from inorganic raw materials have an As concentration higher than those elaborated from organic materials. (EC)

  9. Studies of trace element determinations in nails by neutron activation analysis method

    International Nuclear Information System (INIS)

    Aguiar, Amilton Reinaldo; Saiki, Mitiko

    1996-01-01

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

  10. Significance of combinative determination of urinary type IV collagen and trace albumin in type 2 diabetics

    International Nuclear Information System (INIS)

    Yang Libin

    2004-01-01

    In order to evaluate the diagnostic value of combinative determination of urinary trace albumin(Alb) and urinary type IV collagen (C-IV) for early damage of renal function in type 2 diabetics, 24-hr urine was collected each from 30 normal subjects and 165 type 2 diabetics, and RIA was carried out to determine simultaneously Alb and C-IV (concentration method). The results showed: (1) the content of Alb in 24-hr urine of normal subjects was 6.45±2.04 mg/24 hrs, and that of C-IV was 86.68 ± 11.98 μg/L; (2) The type 2 diabetics were divided into A and B groups according to their Alb content in 24-hr urine. In group A(n=130) the Alb content was ≥30 mg/24 hrs and their C-IV was 120.03 ± 34.02 μg/L, whereas in group B(n=35) the corresponding values were < 30 mg/24 hrs and 97.14 ± 24.93 μg/L, respectively. Conclusion: When the Alb content of type 2 diabetics is still within the normal upper limit, the level of C-IV has already been elevated in part of them, indicating C-IV level can be more able to reflect early damage of renal function in type 2 diabetics than Alb content does. (authors)

  11. Determination of trace elements in drinking water by neutron activation analysis

    International Nuclear Information System (INIS)

    Munita, C.S.; Abe, R.M.; Andrade e Silva, L.G. de.

    1988-10-01

    The concentracao of Hg, Cr, Zn, Fe and Co has been determined in fresh drinking water by a combination of preconcentration and neutron activation analysis. In order to preconcentrate the trace metals, a Chelex-100 resin in the NH + - form has been employed and it was not necessary to use special NH 4 + - form has been employed and it was not necessary to use special agents for the adsorption of the elements which are practically quantitatively retained by the resin. The retention of each element during the preconcentration was investigated using radioactive tracers. Selenium is known as a strongly interferent element for the analysis since the (n,Π) produced 75 Se has a Π-line at 0.279 MeV which coincides with the only Π-line of 203 Hg. The separation was made by a selective retention of mercury. After the sample had passed through the resin, the column was transfered to a polythylene envelope and irradiated at a neutron flux of about 5.10 12 ncm -2 s -1 for 8 h. For Hg the resin was irradiated in quartz ampoules. The samples were counted 15 days after the irradiation. The present method is superior to most other Chelex-100 separation procesures where elements of interest are eluted from the resin prior determinations thereby introducing the possibility of additional reagent blanks and incomplete as well as non-reproducible recoveries. (author) [pt

  12. Derivative spectrophotometric determination of trace amounts of Tungsten(VI) in real water samples

    International Nuclear Information System (INIS)

    Viswanatha, C.; Ramakrishna Reddy, K.; Devanna, N.; Praveen Kumar, M.D.

    2012-01-01

    2,4-Dimethoxybenzaldehydeisonicotinoylhydrazone (DMBHIH) has been synthesized and characterized with IR, NMR and Mass Spectroscopic methods. A simple and derivative spectrophotometric method has been developed for the determination of trace amounts of W(VI). The reagent forms a yellow coloured water soluble complex with W(VI) in basic medium (pH 8.0). The molar absorptivity and Sandell's sensitivity of coloured species are 3.43 x 10 4 L.mol -1 cm -1 and 0.0049 μg/cm 2 respectively. Beer's law is obeyed in the range 0.4113-6.2138 μg/ml of W(VI) at λ max 394 nm. W(VI) forms 1:1 complex with DMBHIH and stability constant of the complex was 5.22x10 6 . The first and second derivative amplitude was measured at 453 nm and 468 nm. The developed method applied for the determination of W(VI) in alloys and biological samples. (author)

  13. The use of nuclear related analytical techniques for the determination of ingestion and body content of trace elements

    International Nuclear Information System (INIS)

    Djojosubroto, H.; Santoso, D.; Widjajakusuma, B.

    1998-01-01

    A number of observations revealed that various human disease states are associated with measurable abnormalities of trace element levels. Until present there is no data on trace element levels in human tissues and dietary intake representing the population in Indonesia. Trace element level in various biological materials, especially human serum related to health syndrome (e.g. acute myocardial infarction and goiter prevalences) was performed by National Atomic Energy Agency in cooperation with relevant institutes. The present study is concerned with determination of ingestion and organ content of trace elements of importance in radiological protection (Cs, Sr, I, Th and U). Quantitation of the elements in the samples will be determined by neutron activation analysis, complemented by nuclear related analytical techniques, e.g. inductively coupled plasma - mass spectrometry and atomic absorption spectrometry. Samples to be analyzed consist of (a) total diets and individual staple foodstuffs, (b) autopsy specimens of liver, lung, kidney, muscle, thyroid and bone, and (c) drinking water. It seems difficult for us to define nationally representative specimens of total diets and individual staple foodstuffs. Based on these facts, in the first year activity samples of dietary intake from various socio economic levels of population in West Java will be collected. Human tissue sample is obtained from autopsy of normal persons who are killed in traffic accident or homicide victim. Traces of Th and U in drinking water are determined by neutron activation analysis following preconcentration of these elements in chelating resin Chlelex 100. (author)

  14. Determination of trace elements in wool fibre by instrumental neutron activation analysis and relation between trace element contents and quality of wool

    International Nuclear Information System (INIS)

    Eozyol, H.

    1990-01-01

    Wool samples were analyzed by neutron activation analysis and 17 elements, Al, Ag, Au, As, Br, Ca, Co, Cr, Cu, Fe, La, Mg, Mn, Na, Sb, Se and Zn were measured quantitatively. The presence of seven others, Ce, Eu, I, Mo, Te and W was noted. Since several elements, such as Cd, Hg and Pb could not be conveniently determined by NAA, Atomic Absorption Spectroscopy (AAS) was used instead. Cu and Zn were also analyzed by NAA and AAS to compare these two methods. Mechanical properties of samples were measured and the relations between the trace element contents and properties were investigated. (author) 16 refs.; 7 tabs

  15. Cloud point extraction and spectrophotometric determination of mercury species at trace levels in environmental samples.

    Science.gov (United States)

    Ulusoy, Halil İbrahim; Gürkan, Ramazan; Ulusoy, Songül

    2012-01-15

    A new micelle-mediated separation and preconcentration method was developed for ultra-trace quantities of mercury ions prior to spectrophotometric determination. The method is based on cloud point extraction (CPE) of Hg(II) ions with polyethylene glycol tert-octylphenyl ether (Triton X-114) in the presence of chelating agents such as 1-(2-pyridylazo)-2-naphthol (PAN) and 4-(2-thiazolylazo) resorcinol (TAR). Hg(II) ions react with both PAN and TAR in a surfactant solution yielding a hydrophobic complex at pH 9.0 and 8.0, respectively. The phase separation was accomplished by centrifugation for 5 min at 3500 rpm. The calibration graphs obtained from Hg(II)-PAN and Hg(II)-TAR complexes were linear in the concentration ranges of 10-1000 μg L(-1) and 50-2500 μg L(-1) with detection limits of 1.65 and 14.5 μg L(-1), respectively. The relative standard deviations (RSDs) were 1.85% and 2.35% in determinations of 25 and 250 μg L(-1) Hg(II), respectively. The interference effect of several ions were studied and seen commonly present ions in water samples had no significantly effect on determination of Hg(II). The developed methods were successfully applied to determine mercury concentrations in environmental water samples. The accuracy and validity of the proposed methods were tested by means of five replicate analyses of the certified standard materials such as QC Metal LL3 (VWR, drinking water) and IAEA W-4 (NIST, simulated fresh water). Copyright © 2011 Elsevier B.V. All rights reserved.

  16. use of x-ray fluorescence spectrometry to determine trace elements ...

    African Journals Online (AJOL)

    NIJOTECH

    Abstract. This paper deals with application of X-ray fluorescence spectrometry for the detection of trace elements in graphic. An X-ray spectrometer was constructed and used to carry out measurements on graphite spheres impregnated with different chemical elements. The intensities of the lines of these trace elements, ...

  17. Trace metal determinations by total-reflection x-ray fluorescence analysis in the open Atlantic Ocean

    International Nuclear Information System (INIS)

    Schmidt, D.; Gerwinski, W.; Radke, I.

    1993-01-01

    The Intergovernmental Oceanographic Commission (IOC), as a major component of its programme ''Global Investigation of Pollution in the Marine Environment'' (GIPME), maintains a long-standing project on ''Open Ocean Baseline Studies of Trace Contaminants''. Initially, the Atlantic Ocean and trace metals were selected. Four deep-water stations in the Cape Basin, Angola Basin, Cape Verde Abyssal Plain and Seine Abyssal Plain were regularly sampled for at least 36 depths. Additional samples were taken between stations. Samples were distributed to participants and a similar number of additional laboratories. As a central part of our own contribution to the project, we determined the trace heavy metals manganese, nickel, copper, zinc and lead and the lighter selenium by total-reflection X-ray fluorescence analysis. For the TXRF, the pre-enrichment of the trace metals and the separation from the salt matrix were performed by complexation with sodium dibenzyldithiocarbamate and reverse-phase chromatography. Generally, very low levels of trace elements were found in filtered and unfiltered water samples from these remote areas of the open Atlantic Ocean. Typical examples of the distributions of trace metal concentrations on depth profiles from the four deep-water stations as well as intercomparisons between the stations are presented. (author)

  18. Determination of trace element contents in grass samples for cattle feeding using NAA techniques

    Energy Technology Data Exchange (ETDEWEB)

    Yusof, Alias Mohamad; Jagir Singh, Jasbir Kaur

    1987-09-01

    An investigation on trace elements contents in six types of grass samples used for cattle feeding have been carried out using NAA techniques. The grass samples, Mardi Digit, African Star, Signal, Guinea, Setaria and Setaria Splendida were found to contain at least 19 trace elements in varying concentrations. The results were compared to the figures obtained from available sources to ascertain the status as to whether the grass samples studied would satisfy the minimum requirements of trace elements present in grass for cattle feeding or otherwise. Preference made on the suitability of the grass samples for cattle feeding was based on the availability and abundance of the trace elements, taking into account factors such as the degree of toxicity, inadequate amounts and contamination due to the presence of other trace elements not essential for cattle feeding.

  19. Determination of trace element contents in grass samples for cattle feeding using NAA techniques

    International Nuclear Information System (INIS)

    Alias Mohamad Yusof; Jasbir Kaur Jagir Singh

    1987-01-01

    An investigation on trace elements contents in six types of grass samples used for cattle feeding have been carried out using NAA techniques. The grass samples, Mardi Digit, African Star, Signal, Guinea, Setaria and Setaria Splendida were found to contain at least 19 trace elements in varying concentrations. The results were compared to the figures obtained from available sources to ascertain the status as to whether the grass samples studied would satisfy the minimum requirements of trace elements present in grass for cattle feeding or otherwise. Preference made on the suitability of the grass samples for cattle feeding was based on the availability and abundance of the trace elements, taking into account factors such as the degree of toxicity, inadequate amounts and contamination due to the presence of other trace elements not essential for cattle feeding. (author)

  20. Trace element determination study in human hair by neutron activation analysis

    International Nuclear Information System (INIS)

    Frazao, Selma Violato

    2008-01-01

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

  1. Determination of essential trace elements in wine by neutron activation analysis

    International Nuclear Information System (INIS)

    Daniele, Anna Paula

    2016-01-01

    Several studies have been carried out for determining essential elements in foodstuffs, including wine, due to its important nutritional role in human body functions. It was shown that daily consumption of wine in moderation contributes significantly to the needs of essential elements in human body such as Ca, Co, Cr, Fe, K, Mg, Mn, Zn, V, among others, and has health benefits in the prevention of numerous diseases and longer life expectancy, related in particular to the intake of antioxidants such as polyphenolic compounds. Trace elements are good indicators of origin of wines and their concentrations can be used as criteria to ensure authenticity, quality and show that the tolerance limits established by law were respected throughout the production process. However, although Brazilian wine industry is among the 15 largest in the world, analytical studies for organic and inorganic compounds of wine content are still small when compared to other major producers. In this sense, this study aimed to evaluate some procedures of wine sample preparation to determine essential elements by Instrumental Neutron Activation Analysis (INAA) and compare the results with those determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP OES). Three sample preparation procedures were studied: freeze-drying, evaporation and dry ashing. The parameters studied were precision, accuracy and detection limit. ANOVA and Tukey-Kramer tests were applied to verify the statistical differences between the mean values obtained by the three wine preparation procedures for INAA with those means obtained by ICP OES. It was noticed that about 60% of results obtained by freeze-drying agreed with those obtained by ICP OES. (author)

  2. Determination of trace elements in tea leaves by neutron activation analysis

    International Nuclear Information System (INIS)

    Kasrai, M.; Shoushtarian, M.J.; Bozorgzadeh, M.H.

    1977-01-01

    Instrumental neutron-activation analysis has been employed to determine 14 trace elements in two brands of Iranian and foreign tea. A popular local brand (Ghoncheh) and a foreign brand (Lipton tea bags) were randomly purchased. The samples were dried in an oven (100 deg C) and used without further treatment. In order to measure the concentration of elements in tea solution, weighed amounts of tea were mixed with double-distilled boiling water. After cooling the leaves were separated by centrifugation. Aliquots of clear solution were dried for analysis. Three sets of standards containing the following elements using the spec-pure materials were prepared: (a) Cl, Mn, Na, K; (b) Br, La, Au; (c) Cr, Fe, Rb, Sc, Cs, Zn, Co. In each irradiation, one set of standards, along with the sample, was neutron irradiated at a thermal flux of approximately 2x10 13 ncm -2 sec -1 in the Research Reactor of the Nuclear Research Centre. The period of irradiation ranged from 10 min to 4 hrs, depending on the radionuclides to be measured. The transference ratio of the elements into solution, when tea is leached by percolation, is also reported. It was found that some elements are totally transferred into solution and some are partially retained by the leaves. (T.G.)

  3. Determination of trace elements in Turkish tea leaves by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Demiralp, R.

    1986-01-01

    The human body continuously assimilates a variety of inorganic elements from food and the environment. Some of these elements are closely related to human health and disorder. Tea is one of the most popular stimulating beverages which is consumed by low and high income family groups in many countries. Instrumental neutron activation analysis is one of the preferred methods because information on a large number of elements can be obtained simultaneously. Five packets each of the seven commonly used brands of tea were obtained from the market. In order to determine the transfer of trace elements into the drinkable portion about 2-3g. of the tea leaves were boiled in hot water for 2 min. After filtration the used tea leaves were dried at 65 deg. C in an oven and a portion, about 200mg was used for analysis. Samples and standards were irradiated 10 min. and 2 hrs. at pneumatic system and central thimble in the TRIGA MARK-II research reactor. After irradiation, the activities of samples and standards were measured with a aoaxial Ge detector coupled to a spectroscopic amplifier. A Canbera 90 model multi- channel analyzer with an 8K memory was used for pulse height analysis. The system has a resolution of 2.0 KeV. for the 1332.5 KeV gamma ray of 60 Co. The activity of the sample and standard was compared and the element contst of the sample was calculated. (author)

  4. Determination of water traces in various organic solvents using Karl Fischer method under FIA conditions.

    Science.gov (United States)

    Dantan, N; Frenzel, W; Küppers, S

    2000-05-31

    Flow injection methods utilising the Karl Fischer (KF) reaction with spectrophotometric and potentiometric detection are described for the determination of the trace water content in various organic solvents. Optimisation of the methods resulted in an accessible (linear) working range of 0.01-0.2% water for many solvents studied with a typical precision of 1-2% R.S.D. Only 50 mul of organic solvent was injected and the sampling frequency was about 120 samples per h. Since the slopes of the calibration curves were different for different solvents appropriate calibration was required. Problems associated with spectrophotometric detection and caused by refractive index changes were pointed out and a nested-loop configuration was proposed to overcome this kind of interference. The potentiometric method with a novel flow-through detector cell was shown to surpass the performance of spectrophotometric detection in any respect. The characteristics of the procedures developed made them well applicable for on-line monitoring of technical solvent distillations in an industrial plant.

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

    International Nuclear Information System (INIS)

    Yamane, Takeshi; Fukasawa, Tsutomu

    1976-01-01

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

  6. Trace determination of 90Sr and 89Sr in environmental samples by collinear resonance ionization spectroscopy

    International Nuclear Information System (INIS)

    Lantzsch, J.; Bushaw, B. A.; Bystrow, V. A.; Herrmann, G.; Kluge, H.-J.; Niess, S.; Otten, E. W.; Passler, G.; Schwalbach, R.; Schwarz, M.; Stenner, J.; Trautmann, N.; Wendt, K.; Yushkevich, Y. V.; Zimmer, K.

    1995-01-01

    Collinear resonance ionization spectroscopy has been developed as a sensitive technique for fast trace detection of 90 Sr and 89 Sr in the environment. A detection limit for 90 Sr of 10 7 atoms in the presence of 10 17 atoms in the presence of 10 17 atoms of stable Strontium has been achieved, while the applicability of the method has been demonstrated on real world samples. After collection and chemical separation, strontium is surface ionized, accelerated to 33keV and mass separated. The ions are neutralized and the emerging fast atoms interact with an argon ion laser beam (γ=364 nm) in a quasi-collinear geometry. Optical excitation starts from the long-lived 5s4d 3 D2 state of strontium, which is populated in the charge exchange process, and the fast atoms are selectively excited into the high-lying 5s23f 3 F3 Rydberg state. The Rydberg-atoms are subsequently field-ionized and detected by a channeltron detector after energy selection. The described method was successfully used to determine the 90 Sr-content in air samples collected near Munich during the Chernobyl reactor accident in April 1986

  7. Determination of trace impurities in high purity water by emission spectroscopy and flame photometry

    International Nuclear Information System (INIS)

    Charbel, M.Y.; Lordello, A.R.

    1985-01-01

    A spectrochemical method for the determination of trace amounts of Fe, Mg, Mn, Sn, Cr, Bi, Ni, Ca, Na, Zn, Sr, Al, Ba and Cu in high purity water is described. In addition Na, Li and K are measured by flame photometry. The standards used in the spectrochemical method are prepared by evaporation in hot plate of 50 mL standard solution in Teflon becker to dryness, the residue being dissolved with 500 μL hot HCl (1:1). Four hundred μL of this solution is evaporated under infra-red lamp on Apiezon treated flat top graphite electrodes. The residue is submitted to a direct current arc excitation. The accuracy is estimated by the spectrochemical method with a direct procedure sample preparation. The relative standard deviation varies from +- 4% to +- 27%. For the elements Na, Li and K standard solutions are concentrated fiftyfold by a simple evaporation procedure and then measured by flame photometry. The standard deviation and accuracy are given. (Author) [pt

  8. The spectrographic determination of minor and trace elements in copper, lead, and zinc concentrates

    International Nuclear Information System (INIS)

    Breckenridge, R.L.; Russell, G.M.; Watson, A.E.

    1976-01-01

    This report deals with the development of a method for the determination, by an emission-spectrographic technique, of magnesium, manganese, aluminium, silver, calcium, chromium, cobalt, titanium, antimony, cadmium, molybdenum, zirconium, nickel, boron, vanadium, arsenic, beryllium, tin, germanium, and bismuth in copper, lead, and zinc sulphide concentrates. The method involves the preparation of complex standards in which the volatile elements arsenic, antimony, cadmium, tin, and bismuth are incorporated as sulphide compounds at temperatures of 800 degrees Celsius in evacuated silica tubes together with a synthetic sulphide matrix. These standards are then mixed with the other minor and trace elements to form composite standards. The conditions for excitation with a direct-current arc, and the analytical lines for the elements and internal standards, are given. The procedure is rapid and convenient, and involves the minimum of sample preparation. The accuracy is about 10 per cent, and the method has a coefficient of variation for the various elements of between 2 and 13 per cent

  9. Determination of Tetracycline and Fluoroquinolone Antibiotics at Trace Levels in Sludge and Soil

    Directory of Open Access Journals (Sweden)

    Marie-Virginie Salvia

    2015-01-01

    Full Text Available This work describes the development of a sensitive analytical method to determine simultaneously traces of tetracycline and fluoroquinolone antibiotics in sludge and soil, based on PLE extraction, followed by SPE purification and finally an analysis by LC-MS/MS. Recoveries were greater than 87% in the case of fluoroquinolones and between 25.4 and 41.7% for tetracyclines. Low relative standard deviations (<15% were obtained in both matrices. The limits of quantification were comprised between 1.1 and 4.6 ng/g and between 5 and 20 ng/g in soil and sludge, respectively. The method was then successfully applied to the analysis of the target antibiotics in sludge as well as soil that received spreading. The substances most frequently found and with the highest levels were fluoroquinolones with concentrations exceeding 1,000 ng/g in several samples of sludge and up to 16 ng/g in soil.

  10. Trace and ultratrace analysis methods for the determination of phosphorus by flow-injection techniques.

    Science.gov (United States)

    Motomizu, Shoji; Li, Zhen-Hai

    2005-04-15

    Trace (phosphorus determination by flow-injection analysis are reviewed. Most of the methods cited in this review are fundamentally based on the reaction of orthophosphate with molybdate to form heteropoly acids, such as molybdenum yellow and molybdenum blue, and some of the methods are based on the formation of such secondary reactions as ion associates and their aggregates with bulky cations, such as cationic dyes and quaternary ammonium ions. The heteropoly acids themselves can be measured by spectrophotometry, and the ion associate formed with a cationic dye, Malachite Green (MG), can be measured based on the coloration of MG. Light scattering detection methods can be used for measuring the aggregates of ion associates formed with bulky cations. Highly sensitive detection of phosphorus can be accomplished by fluorophotometry; Rhodamine B (RB) and its analogues react with molybdophosphate to form ion associates, which shows fluorescence quenching of RB: LOD is about 5 nM. The detection method based on the chemiluminescence of luminal oxidized with molybdophosphoric acids is probably the most sensitive of all the detection methods reported so far: LOD of the method is as low as 1nM. The LOD of the molybdenum blue method can be improved by using a liquid core waveguide: LOD is 0.5 nM.

  11. Features of the spectroscopic determination of the isotope composition of trace amounts of hydrogen in helium

    International Nuclear Information System (INIS)

    Nemets, V.M.; Petrov, A.A.; Solov'ev, A.A.

    1986-01-01

    The investigation of the magnitude of the isotope effect in the intensiti of the beta lines of the Balmer series was carried out with the excitation of a high-frequency discharge in a quartz tube having a diameter of ca.6.5 at pressures of the gaseous mixture ranging from 1 to 70 kPa. From the experimental results here it follows that as the isotopes of hydrogen are diluted with helium, the value of K decreases from 1.2-1.1 to 0.84-0.86, and the maximum of the plots of K= f(P) broaden and move toward higher pressures. In order to account for the laws obtained, the authors examined a set of elementary processes and reactions for which the isotope-related differences in the rate constants (alpha) can influence the relative concentrations of the excited atoms of the isotopes of hydrogen in a discharge. The physical model presented in this paper of the shaping of the isotope effects in the atomic spectrum of hydrogen makes it possible to account for the observed laws governing the excitation of a discharge in a mixture of the isotopes of hydrogen with helium and thus greatly facilitates the selection of the optimal conditions for the excitation of the analytical spectrum in devising procedures for the spectroscopic isotope determination of trace impurities of hydrogen in helium

  12. Application of radio-reagent method in the determination of lead trace amounts

    International Nuclear Information System (INIS)

    Figueiredo, A.M.G.

    1983-01-01

    A radiometric method for trace analysis of lead was established, based on the displacement reaction between lead and the complex cobalt - ethylenediaminetetracetate labelled with 60 Co (Co* - EDTA), which is named radioreagent. The radioactive cobalt displaced by lead is separated from the excess of radioreagent by the solvent extraction technique, using a solution of tetracycline (Tc) in benzyl alcohol. The activity of the extracted cobalt is then measured by means of a single-channel gamma-ray analyser coupled to a NaI (Tl) scintillation detector, the activity being proportional to the lead concentration, in a range from 2.5 to 150 μg. The interference of several elements (V, Th, Sc, Fe, La, Yb, Cu, Cd, Zn, Mn, Ni, Co, Al and Sn) was investigated by means of a previous separation between lead and these interfering elements. The analyses of artificial samples containing lead and the interfering elements gave a yield of 91.1 + - 3.2 %. The detection limit achieved by the method was 3.3 μg of lead. The radioreagent method was applied to lead analysis of samples from IAEA, namely: simulated air filter (Air-3), fresh water (W-3), dried animal blood (A-2) and calcinated animal bone (A-3/1). Lead was also determined in gasoline samples and air samples, these latter collected in the surroundings of the IPEN/CNEN/SP (Brazil). (Author) [pt

  13. A new method for determination of trace amount thorium-spectrophotometric determination of thorium in aqueous phase by chlorophosphonazo-mA

    International Nuclear Information System (INIS)

    Xia Yuanxian; Qian Hesheng

    1986-01-01

    In this paper the spectrophotometric method for determination of trace amount of thorium in weak acidic medium by chlorophosphonazo-mA is described. The composition of the complex was estimated to be 1:4 by slope ratio method. The apparent molar absorption of thorium at 675 nm is 9.2 x 10 4 . Beer's law is obeyed for 0-12.0 μg of thorium in 10 ml solution. The coefficient of variation for thorium is 0.88%. The method has been applied to the determination of trace amounts of thorium in the extraction process of thorium

  14. Optimization of trace elements determination (Arsenic and chromium) in blood and serum of human by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ahmadi Faghih, M. A.; Aflaki, F.

    2003-01-01

    Trace elements play an important role in the bio physiology of cells by affecting their growth and contributions to various biological processes such as wound healing. Determination of toxic trace elements in biological fluids is an important subject of interest for toxicological purposes. Increasing the concentration of these elements in the blood levels, cause serious diseases in patients. Recently instrumental analysis procedures such as atomic absorption spectrometry have been used in clinical measurements for determination of many toxic trace elements in the biological samples. In this paper we are reporting the study of various methods of blood and serum samples preparation for determining the toxic trace elements of Arsenic and Chromium. The measurement of this elements performed by using electrothermal atomic absorption spectrometry. The best and reliable results for Chromium analysis was achieved by injection of diluted serum samples, where the samples were diluted with H CI 0.1N. In Arsenic analysis, the best results obtained by extraction with aqueous solution of TCA. For determining all of these elements the RSD% was less than 5%

  15. Contributions te the study of methods and factors affecting the spectrophotometric determination of boron traces with carmin uranium compounds

    International Nuclear Information System (INIS)

    Fernandez Cellini, R.; Gasco Sanchez, L.

    1956-01-01

    The study of some factors affecting the spectrophotometric determination of boron traces with carmin is made; the influence of carmin from different origin, the stability of complex carmin-boric acid in relation with the sulphuric acid concentration, the interference produced by ion nitrate, and the ion uraline and light influence are discussed. (Author) 36 refs

  16. Internal standard method for determination of gallium and some trace elements in bauxite by neutron activation analysis

    International Nuclear Information System (INIS)

    Chen, S.G.; Tsai, H.T.

    1983-01-01

    A method is described for the determination of gallium and other trace elements such as Ce, Cr, Hf, Lu and Th in bauxite by the technique of neutron activation analysis using gold as internal standard. Isopropyl ether was used as organic extractant radioactive gallium from the sample. This method yields very good accuracy with a relative error of +-3%. (author)

  17. Determination of trace elements and screening of metalloproteins in human blood and tissues

    International Nuclear Information System (INIS)

    Prohaska, K.

    2003-02-01

    ). For the very low concentrations of trace element in blood fractions (e.g. Co, Cr, or Ni) the GFAAS had to be used. The simultaneous ICP-OES was applied for the determination of Ca, Mg, P, Fe, Cu, and Zn in whole blood. Line selection was performed in the complex sample matrix. In digested freeze-dried blood the simultaneous lines showed no interferences for Ca, Cu, Fe, Mg, P, S, and Zn. Only for Co serious interference occurred in the matrix. The method was not suitable for the determination of Cd, Cr, Mn, Mo, Nb, Ni, Pb, Ti, and V in the blood samples, because the LODs of the ICP-OES method were too high for this purpose. (author)

  18. Determination of trace levels of nickel and manganese in soil, vegetable, and water

    Energy Technology Data Exchange (ETDEWEB)

    Khani, Rouhollah; Shemirani, Farzaneh [School of Analytical Chemistry, University College of Science, University of Tehran, Tehran (Iran, Islamic Republic of)

    2010-12-15

    A simple and reliable method for rapid and selective extraction and determination of trace levels of Ni{sup 2+} and Mn{sup 2+} was developed by ionic liquid (IL) based dispersive liquid-liquid microextraction coupled to flame atomic absorption spectrometry (FAAS) detection. The proposed method was successfully applied to the preconcentration and determination of nickel and manganese in soil, vegetable, and water samples. After preconcentration, the settled IL-phase was dissolved in 100 {mu}L of ethanol and aspirated into the FAAS using a home-made microsample introduction system. Injection of 50 {mu}L of each analyte into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Effective parameters such as pH, amount of IL, volume of the disperser solvent, concentration of the chelating agent, and effect of salt concentration were inspected by a (2{sup 5-1}) fractional factorial design to identify the most important parameters and their interactions. Under optimum conditions, preconcentration of 10 mL sample solution permitted the detection of 0.93 {mu}g L{sup -1} Ni{sup 2+} and 0.52 {mu}g L{sup -1} Mn{sup 2+} with enrichment factors 77.2 and 82.6 for Ni{sup 2+} and Mn{sup 2+}, respectively. The accuracy of the procedure was evaluated by analysis of a certified reference material (CRM TMDW-500, drinking water). (Copyright copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  19. New technique for the determination of trace noble metal content in geological and process materials

    Energy Technology Data Exchange (ETDEWEB)

    Mitkin, V.N. E-mail: mit@che.nsk.su; Zayakina, S.B.; Anoshin, G.N

    2003-02-03

    A new two-step sample preparation technique is proposed for the instrumental determination of trace quantities of noble metals (NM) in refractory geological and process materials. The decomposition procedure is based on the oxidizing fluorination of samples with subsequent sulfatization (OFS) of the sample melt or cake. Fluorination of samples is accomplished using a mixture of KHF{sub 2}+KBrF{sub 4} or KHF{sub 2}+BrF{sub 3} depending on the ratio of sample mass to oxidizing mixture. Both cakes and melts can result using this procedure. Sulfatization of resulting fluorides is completed using concentrated sulfuric acid heated to 550 deg. C. Validation studies using certified geostandard reference materials (GSO VP-2, ZH-3, Matte RTP, HO-1, SARM-7) have shown that the proposed method is fast, convenient and most often produces non-hygroscopic homogeneous residues suitable for analysis by atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). Results obtained for NM concentrations in reference materials agreed with certified concentration ranges and results obtained using other methods of analysis. The OFS procedure combined with direct current plasma d.c. plasma AES achieved the following limits of detection (LOD) for the noble metals: Ag, Au, Pd, 1-2x10{sup -6}; Pt, 5x10{sup -6}; and Ru, Rh, Ir, Os, 1-3x10{sup -7} wt.%. Using graphite furnace AAS (GFAAS) combined extraction pre-concentration the following LODs for NMs were achieved: Pt, Ru, 1x10{sup -6}; Pd, Rh, 1x10{sup -7}; and Au, Ag, 1-2x10{sup -8} wt.%. The relative standard deviation for NM determinations (S{sub r}) was dependent on NM concentration and sample type, but commonly was in the range of 3-15% for d.c. plasma AES and 5-30% for GFAAS.

  20. Determination of trace amounts of uranium in a reprocessing plant by solution spectrofluorimetry

    International Nuclear Information System (INIS)

    Mauchien, P.; Cauchetier, Ph.

    1983-01-01

    To establish inventory tables accurately and satisfy safeguards requirements - and also to ensure satisfactory operation of a reprocessing plant - it is essential to determine the uranium content of numerous solutions where the uranium is present only in trace quantities. For this purpose a method is proposed which relies on the fluorescence of uranyl solutions exposed to ultra-violet radiation. After a brief theoretical summary, the parameters which influence the measurements most strongly are enumerated: medium, temperature, nature of the matrix, and choice of wavelength of the incident radiation. It is then apparent that the measurement must be performed by internal calibration (using the proportional addition method) and that it is useful to obtain a fluorescence spectrum which enables us to verify the presence of uranium. The applications of this method at the La Hague plant are described, where it has been used since October 1981 by shift teams, notably to check the following points: the attack acid (before receiving the fuel), the foot of the first-cycle column, the carbonated solvent washing solution and the solutions of the effluent treatment unit. It is in fact used throughout the plant, even for checking uranium in PuO 2 oxide. The method makes it possible to avoid organic reagents such as pyridine and, in many cases, cumbersome effluent-generating separations. Determinations are possible - to give one example - by simple dilution in the fission-product concentrates and in plutonium solutions where the Pu/U ratio is as great as 1000/1. In pure solutions the detection limit with the equipment used at present is a few μg per litre in the measuring tank. In general, the accuracy is a few per cent. (author)

  1. Determination of the side-reaction coefficient of desferrioxamine B in trace-metal-free seawater

    Directory of Open Access Journals (Sweden)

    Johan Schijf

    2016-07-01

    Full Text Available Electrochemical techniques like adsorptive cathodic stripping voltammetry with competitive ligand equilibration (ACSV-CLE can determine total concentrations of marine organic ligands and their conditional binding constants for specific metals, but cannot identify them. Individual organic ligands, isolated from microbial cultures or biosynthesized through genomics, can be structurally characterized via NMR and tandem MS analysis, but this is tedious and time-consuming. A complementary approach is to compare known properties of natural ligands, particularly their conditional binding constants, with those of model organic ligands, measured under suitable conditions. Such comparisons cannot be meaningfully interpreted unless the side-reaction coefficient (SRC of the model ligand in seawater is thoroughly evaluated.We conducted series of potentiometric titrations, in non-coordinating medium at seawater ionic strength (0.7 M NaClO4 over a range of metal:ligand molar ratios, to study complexation of the siderophore desferrioxamine B (DFOB with Mg and Ca, for which it has the highest affinity among the major seasalt cations. From similar titrations of acetohydroxamic acid in the absence and presence of methanesulfonate (mesylate, it was determined that Mg and Ca binding to this common DFOB counter-ion is not strong enough to interfere with the DFOB titrations. Stability constants were measured for all DFOB complexes with Mg and Ca including, for the first time, the bidentate complexes. No evidence was found for Mg and Ca coordination with the DFOB terminal amine. From the improved DFOB speciation, we calculated five SRCs for each of the five (deprotonated forms of DFOB in trace-metal-free seawater, yet we also present a more convenient definition of a single SRC that allows adjustment of all DFOB stability constants to seawater conditions, no matter which of these forms is selected as the 'component' (reference species. An example of Cd speciation in

  2. Guidelines for the determination of selected trace metals in aerosols and in wet precipitation

    International Nuclear Information System (INIS)

    1988-01-01

    This publication describes sampling and analytical procedures suitable for the collection and analysis of representative samples of atmospheric aerosols and wet precipitation for selected trace metals. 11 refs, 2 tabs

  3. Trace element determination in beauty products by k0-instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Sneyers, L.; Verheyen, L.; Vermaercke, P.; Bruggeman, M.

    2009-01-01

    A recent study on trace elements in beauty products and cosmetics sold on the Asian market has shown the presence of high levels of U, Th and rare earth elements in so called 'Hormesis cosmetics'. For the purpose of comparison, some more information about trace elements in European cosmetics would be useful. In this paper the results obtained using k 0 -standardised Instrumental Neutron Activation Analysis (k 0 -INAA) for more than 20 trace elements in 20 different beauty products collected from the European market are presented. We found traces of Ba, As and Sb which is in breach with European legislation. For some of the other elements like Cr and Co further speciation is needed in order to evaluate their presence in beauty products. (author)

  4. Survey of currently available reference materials for use in connection with the determination of trace elements in biological materials

    International Nuclear Information System (INIS)

    Parr, R.M.

    1983-09-01

    Elemental analysis of biological materials is at present the subject of intensive study by many different research groups throughout the world, in view of the importance of these trace elements in health and medical diagnosis. IAEA and other organizations are now making a variety of suitable reference materials available for use in connection with the determination of trace elements in biological materials. To help analysts in making a selection from among these various materials, the present report provides a brief survey of data for all such biological reference materials known to the author. These data are compiled by the author from January 1982 to June 1983

  5. INAA for the determination of trace elements and evaluation of their enrichment factors in lichens of high altitude areas

    International Nuclear Information System (INIS)

    Bergamaschi, L.; Rizzio, E.; Giaveri, G.; Profumo, A.; Gallorini, M.; Giordani, L.

    2005-01-01

    Trace element (TE) characterization and analysis in epiphytic lichens collected in different areas of the Himalayas (Nepal) and of the Alps (Italy) is presented. The results give information for the assessment of TE distribution present in the two different areas. The evaluation of the enrichment factors may provide information for many elements about their association to long-distance atmospheric transport phenomena. To this purpose, samples of superficial soils, collected in the same areas of those of the lichens, have also been analyzed. Most of the trace elements were determined by instrumental neutron activation analysis (INAA), while lead and cadmium measurements were carried out with electrothermal atomic absorption spectroscopy (ET-AAS). (author)

  6. Trace element determination in fingernails, hair and blood serum in patients with Crohn's disease using neutron activation analysis

    International Nuclear Information System (INIS)

    Buschmann, H.

    1984-01-01

    The determination of trace elements and electrolyte concentrations in blood serum, hair and fingernails of 16 patients with Crohn's disease was carried out by means of instrumental neutron activation analysis. In the serum a significant decline in the zinc content could be registered, while the remaining trace elements remained in the normal range. The parenteral nutrition also showed a zinc deficiency. There was, however, also an iron deficiency. The studies of the hair and fingernails gave the following results: Rubidium and antimony in the normal range; zinc, selenium, iron and cobalt below normal values. (orig./PW) [de

  7. Neurient: An Algorithm for Automatic Tracing of Confluent Neuronal Images to Determine Alignment

    Science.gov (United States)

    Mitchel, J.A.; Martin, I.S.

    2013-01-01

    A goal of neural tissue engineering is the development and evaluation of materials that guide neuronal growth and alignment. However, the methods available to quantitatively evaluate the response of neurons to guidance materials are limited and/or expensive, and may require manual tracing to be performed by the researcher. We have developed an open source, automated Matlab-based algorithm, building on previously published methods, to trace and quantify alignment of fluorescent images of neurons in culture. The algorithm is divided into three phases, including computation of a lookup table which contains directional information for each image, location of a set of seed points which may lie along neurite centerlines, and tracing neurites starting with each seed point and indexing into the lookup table. This method was used to obtain quantitative alignment data for complex images of densely cultured neurons. Complete automation of tracing allows for unsupervised processing of large numbers of images. Following image processing with our algorithm, available metrics to quantify neurite alignment include angular histograms, percent of neurite segments in a given direction, and mean neurite angle. The alignment information obtained from traced images can be used to compare the response of neurons to a range of conditions. This tracing algorithm is freely available to the scientific community under the name Neurient, and its implementation in Matlab allows a wide range of researchers to use a standardized, open source method to quantitatively evaluate the alignment of dense neuronal cultures. PMID:23384629

  8. Application of neutron activation analysis to trace element determinations in lung samples

    International Nuclear Information System (INIS)

    Rocero, Sizue Ota

    1992-01-01

    The purpose of this work was to apply the instrumental neutron activation analysis method to determine trace elements in lung samples from smokers and non smokers. Samples of lung tissues and lymph nodes from pulmonary hilum analyzed were collected from autopsies by researchers from the Medicine College of the University of Sao Paulo, SP, Brazil. Adequate conditions for preparation and analysis of samples were previously established. The preparation of samples consisted of homogenization, lyophilization and sterilization in 60 Co source. The samples and standards were irradiated in the IEA-R1 reactor under thermal neutron flux of 3.7 x 10 11 n.cm -2 .s -1 for 30 min to determine Cl, K, Mn and Na and for 16 h under flux of 10 19 n.cm -2 .s -1 for the determination of Au, Br, Ce, Co, Cr, Cs, Eu, Fe, Hf, La, Rb, Sb, Sc, Se, Th and Zn. The counting were carried out with a hiperpure (ge) detector connected to a 4096 channels analyzer and a microcomputer. the results obtained for lung sample analyses indicated a good reproducibility of the method for most of the elements determined with relative standard deviations lower than 10.5%. The accuracy of the method was evaluated by analyzing reference materials such as IAEA Animal Muscle H-4, NIST Bovine Liver 1577a, IUPAC Bowen's Kale and NIES Vehicle Exhaust Particulates. The results obtained from these analyzes agreed with the values of the literature for several elements with relative errors less than 20%. Less precise and accurate results were obtained for elements with concentrations at the Mup/Kg levels. Elemental concentrations obtained in the lung tissue analyses were within the range of reference values for normal subjects presented in the literature, except for the Cl concentrations for non smokers, Hf in both groups and Sb for the smokers. By comparing results obtained for lung samples from smokers and non smokers, the concentrations of Ce, Cr and Sb were higher in lungs from smokers and the others elements were

  9. Determination of trace elements in soil and plants in the Orontes basin of Syria by using instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Kassem, A.; Sarheel, A.; Al-Somel, N.

    2004-01-01

    Instrumental neutron activation analysis (INAA) have been used for the determination of some major, minor and trace elements (As, Cr, Co, Ni, Zn, Sb, Sc, Ce, Ti, Fe, Mn and V) in various plant leaves together with their soil. The accuracy of the measurements have been evaluated by analyzing a number of plant and soil reference materials, precision have been estimated by triplicate analysis of the sample as well as that of the reference material. The obtained accurate and reliable data of some trace elements on microgram level for plants and soil will serve as baseline values and will be helpful to monitor the changes in the trace element content of soil and plant leaves. (author)

  10. Official Methods for the Determination of Minerals and Trace Elements in Infant Formula and Milk Products: A Review.

    Science.gov (United States)

    Poitevin, Eric

    2016-01-01

    The minerals and trace elements that account for about 4% of total human body mass serve as materials and regulators in numerous biological activities in body structure building. Infant formula and milk products are important sources of endogenic and added minerals and trace elements and hence, must comply with regulatory as well as nutritional and safety requirements. In addition, reliable analytical data are necessary to support product content and innovation, health claims, or declaration and specific safety issues. Adequate analytical platforms and methods must be implemented to demonstrate both the compliance and safety assessment of all declared and regulated minerals and trace elements, especially trace-element contaminant surveillance. The first part of this paper presents general information on the mineral composition of infant formula and milk products and their regulatory status. In the second part, a survey describes the main techniques and related current official methods determining minerals and trace elements in infant formula and milk products applied for by various international organizations (AOAC INTERNATIONAL, the International Organization for Standardization, the International Dairy Federation, and the European Committe for Standardization). The third part summarizes method officialization activities by Stakeholder Panels on Infant Formula and Adult Nutritionals and Stakeholder Panel on Strategic Food Analytical Methods. The final part covers a general discussion focusing on analytical gaps and future trends in inorganic analysis that have been applied for in infant formula and milk-based products.

  11. Trace elements determination in Syrian honey using x-ray fluorescence technique

    International Nuclear Information System (INIS)

    Khuder, A.; Ahmad, M.; Saour, G.

    2009-05-01

    Major and trace elements of S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Rb, Sr in 27 Syrian honey samples, which collected from different areas in the country, in addition to 3 imported honey samples, were determined by dry ashing method for XRF analysis. The samples were diluted and homogenized with a binder made from cellulose powder. The analyzed elements were divided into three groups, relating to the secondary targets used for X-ray excitation. The internal standard method for XRF analysis with a Mo secondary target was used for the determination of the first group of elements: Sr, Rb, Se, As, Zn, Cu, Ni, and Fe. While, the external standard method for XRF analysis with Cu and Ti secondary targets was used for the determination of the second: Mn, Cr, Ti, Ca, K, and third: Cl, and S group of elements, respectively. The results were accurate with a relative standard error less than 4.2 %. The problem of element loss was overcome by the complete drying of honey samples before their ashing. The moisture content was obtained using mass loss and refractive index methods. As a result, the lower limits of detection (LLD) obtained by Mo-XRF was in the range from 0.011 μg Sr/g to 0.064 μg Fe/g, resulting for samples containing 0.1 % ash and collecting live time 1000 s; while, LLD obtained by Cu-XRF was in the range 0.014 μg Mn/g to 0.057 μg K/g. LLD for S and Cl using Ti secondary target was with values of 0.503 μg/g and 1.96 μg/g, respectively. The enhancement factor obtained by drying method for XRF was in the range from 147 to 1667. Normal concentration of elements in Syrian honey was obtained. The concentration of elements was comparable to those obtained by other workers for honeys in different countries. Elements of K, Ca, and Cl were predominantly distributed in all Syrian honey samples. Elements of Sr, Zn, Cu, Fe, Ti, and S were well distributed in all honey samples. While, the concentrations of Rb, Ni, Mn, Cr elements in some honey samples were below the

  12. Determination of trace elements in Katana (Japanese sword) by neutron activation analysis with multidimensional γ-ray spectrometry

    International Nuclear Information System (INIS)

    Okada, Y.; Hirai, S.; Ohya, S.; Kimura, Atsushi; Hatsukawa, Yuichi; Toh, Yosuke; Koizumi, Mitsuo; Oshima, Masumi

    2006-01-01

    In this study, we tried to measure trace elements (As and Sb) in Katana (Japanese swords) by multidimensional γ-ray spectrometry method (GEMINI-II) and conventional counting method for neutron activation analysis (NAA). The determined values by GEMINI-II and conventional counting were in good agreement with. Using the multidimensional γ-ray spectrometry (GEMINI-II) to determine As and Sb was improved by 7 times and 10 times compared with the conventional counting method. (author)

  13. Determination of trace amounts of metals in saline water by energy-dispersive XRF (with the Na-DDTC preconcentration)

    International Nuclear Information System (INIS)

    Holynska, B.; Bisiniek, K.

    1975-01-01

    A simple method for the determination of trace concentrations of metals in saline water is described. The analytical procedure involves the separation of metal ions of Cu(2), Zn(2), Hg(2) and Fe(3) by precipitation with diethyldithiocarbamate (DDTC). The radioisotope X-ray fluorescence method using Si/Li detector has been applied for the determination of metal ions closed in the DDTC deposition. (author)

  14. Neutron activation analysis applied to the determination of trace elements in human nails

    International Nuclear Information System (INIS)

    Aguiar, Amilton Reinaldo

    2001-01-01

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

  15. Principle of neutron activation analysis and its use for determination of trace elements in sediment

    International Nuclear Information System (INIS)

    Verma, Rakesh

    2012-01-01

    information. Their chemical characterization is needed to understand the natural and anthropogenic influence on the bodies of water. Nuclear analytical techniques such as NAA and X-ray fluorescence spectrometry (XRF) have been used for determination of various elements in sediment. Recently we have participated in the inter-laboratory comparison organized by International Atomic Energy Agency for the determination of trace elements in sediment sample. The results of analysis will be discussed. (author)

  16. Minerals and trace elements determination in diets by neutron activation analysis

    International Nuclear Information System (INIS)

    Eiras, Maria Izabel O.; Favaro, Debora I.T.; Ribeiro, Marisilda; Cozzolino, Silvia M.F.

    2002-01-01

    In the present study 12 diets, each one consisting of a pool of seven day diets, composed by four meals: breakfast, lunch, dinner and snack, adequate in energy and macro nutrients according to the RDA (Recommended Daily Allowance) recommendations, were elaborated and offered to a group of 12 men (19-42 years). The diets were collected by duplicate portion technique and dried by two different processes: freeze drying and 60 deg C ventilated oven drying. In the total, 24 diets were analyzed. The content of some minerals and trace elements (Ca, Fe, Mg, Mn, Na, Se and Zn) were determined by Instrumental Neutron Activation Analysis. The validation of methodology was made by analysis of the reference materials Typical Diet (NIST SRM 1548 a ), Orchard Leaves (NIST SRM 1541) and Peach Leaves (NIST SRM 1547). The results observed by two different drying processes used were statistically compared by test T of Student. It was possible to conclude that the concentration means can be considered as statistically equal, within a significance level of 0.05. The daily intake values calculated from the concentration results were: 712 (± 59) mg Ca/day; 10.7 (± 0.8) mg Fe/ day; 3387 (± 16) mg K/ day; 275 (± 6) mg Mg/ day; 3.0 (± 0.5) mg Mn/ day; 3656 (± 699) mg Na/ day; 42 (± 6) μg Se/ day e 11.6 (± 2.4) mg Zn/ day. The calculated intake was compared to the new daily recommended values set by RDA (National Research Council-USA) for the range age of individuals studied. It was possible to conclude that the diets were adequate in Fe and Zn and inadequate for the other elements. Concerning the minerals Na and K we verified high daily intake levels and this was already observed in other Brazilian regional diets. (author)

  17. Determination of trace elements in tailpipe fish produced in artificial farms and from white and blue nile

    International Nuclear Information System (INIS)

    Ahmed, Zeinb Khalil Elsaim

    2017-01-01

    In this study, an analytical protocol of x-ray fluorescence spectroscopy was used to determine the concentration of 13 trace elements, potassium (K), antimony (Sb), iron (Fe), copper (Cu), zinc (Zn), lead (Pb), bromine (Br), rubidium (Rb), strontium (Sr), mercury (Hg), chromium (Cu), manjense (Mn), and calcium (Ca), in tilapa fish. A total of 70 samples covering 35 fish samples collected from different states includes Eldamazine for blue nile samples and the Mawrada market for the white nile samples and 5 artificial fish farms samples were collected from Om badda in Omdurman and Bahry state for three farms Alsamraband Aldorshab and from Alshagra state in Khartoum, during may to June 2016. The trace elements detected in all samples, and the concentration in part million (ppm). The concentrations of trace elements followed the sequence of, K, Ca, Fe, Zn, Cu, Sr, Rb, Pb, but Cr, Hg and Ni were observed in one fish fram (farm A). The analysis included two tissues (flesh and gills), because most people in Sudan consume the flesh and gills, specially in the small fishes, consider as good indicators for the trace elements, and toxic compounds in general. The analysis indicated that the white nile fishes have higher l eves of most of the trace elements compared to the blue nile, e.g. Fe (560±186) in the white nile, whereas in the blue nile, (188±63). On the other hand , the artificial tilapia farms showed significant variations in the trace elements concentrations. The analysis revealed that a higher concentrations of most of the trace elements in gill tissues than flesh, e.g. Fe (1673±1453) in the flesh, and (9768±1175) in the gills. These results indicated that the gill accumulated higher levels of heavy metals than other organs, because they acted as a depot tissue. In addition, the post hoc test was performed following (Dunnett tests), using the blue nile group as a control group, since it has the lowest trace elements concentrations, among the river nile fishes in

  18. Report on the intercomparison run Soil-5 for the determination of trace elements in soil

    Energy Technology Data Exchange (ETDEWEB)

    Dybczynski, R; Tugsavul, A; Suschny, O

    1978-01-01

    he knowledge of the elemental composition of soil, and especially its trace element content is of interest to many investigators active in various fields of research. Among these concerned are not only agricultural chemists and soil scientists, but also biochemists, environmentalists, nutritionists and others. The increased recognition of the essentially on one hand and toxicity on the other, of certain trace elements towards animals and man, has led to intensified studies of the pathways of trace elements in nature, particularly in the environmental research. Not only atmosphere, hydrosphere and biological tissues, but also soil is examined. Essential and toxic trace elements may pass from soil to plants (by which they are sometimes effectively concentrated) and further through food chains to Man. The interest in the analysis of soil for the content of many trace and also some major elements is therefore rapidly increasing. Hence, there seems to be an obvious need for a reference material with established 'recommended values' of as many elements as possible which could be used for checking the quality of analytical work of the laboratories engaged in soil analyses. At the same time well-characterized soil, containing high levels of minerals can be also of interest for geochemists as a complement to already existing geochemical reference samples.

  19. Essential trace elements content in a sudanese meal of cooked Hibiscus Sp. leaves as determined by both X-ray florescence and atomic absorption spectroscopy techniques

    International Nuclear Information System (INIS)

    Mohamed, S.M; Taha, M.H.

    2003-01-01

    Essential trace elements content of a Sudanese meal of cooked Karkadi plant leaves (Hibiscus Sp)was determined and found to be several folds higher than the average trace element content of Sudanese food as determined in twenty nine daily consumed mixed diets. Therefore, this plant can act as a promising natural supplement in cases of deficiency provided it is grown in a trace element rich soil. (Author)

  20. World-wide intercomparison exercise for the determination of trace elements in Fucus sample IAEA-140. Report no. 64

    International Nuclear Information System (INIS)

    Coquery, M.; Carvalho, F.P.; Horvat, M.; Azemard, S.

    1997-09-01

    The accurate and precise determination of trace elements in marine samples is fundamental to pollution assessment in coastal and marine environments. Analyses of sea plants are important to investigate the uptake of toxic elements along the trophic chain and sea plants may be used as indicators for water pollution and to compare the levels of contamination of different aquatic environments. IAEA. together with UNEP and the Intergovernmental Oceanographic Commission (IOC) work closely with other producers of Reference Materials in order to assure a continuous supply of these vital compounds for quality assurance procedures. A full catalogue of materials is published regularly. The Marine Environmental Studies Laboratory (MESL) of IAEA-MEL has conducted intercomparison exercises on trace elements for over twenty years as part of its contribution to IAEA's Analytical Quality Control Service, UNEP's Regional Seas Programme. and, occasionally, in association with the IOC GIPME (Global Investigation of the Pollution in the Marine Environment) programme. This report describes the performance of laboratories in one intercomparison run conducted during 1996 that was organized for the determination of trace elements in a marine macro algae (Fucus sp.) sample. This study was intended to give laboratories responsible for trace element analyses of marine materials an opportunity for checking their analytical performance

  1. Determination of trace impurities in iron-based alloy using neutron activation analysis

    International Nuclear Information System (INIS)

    Zaidi, J.H.; Waheed, S.; Ahmad, S.

    2000-01-01

    A radiochemical neutron activation analysis procedure has been developed and applied to investigate 40 major, minor, and trace impurities in iron-based alloy. A comparison of RNAA and INAA indicated a significant improvement in the detection limits. The extensive use of these alloys in the heavy mechanical industry, manufacturing of aircraft engines, nuclear applications, medical devices and chemical equipment requires their precise characterization. The concentration of iron in the iron-based alloy was found to be 86.7%, whereas Ca, Cr, K, Mg, Mn, V and W were the other constituents of the alloy, which constituted to around 12.89%. The rest of the elements were present in minor or trace levels. Most of the rare earth elements were also present in trace amounts. (orig.)

  2. Accelerator SIMS, a technique for the determination of stable trace elements in ultrapure materials

    Energy Technology Data Exchange (ETDEWEB)

    Ender, R.M.; Suter, M. [Eidgenoessische Technische Hochschule, Zurich (Switzerland); Doebeli, M.; Synal, H.A. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    A new sputtering chamber with special precautions against sample contamination from the surroundings of the sample has been added to the AMS beamline of the tandem accelerator. This allows the detection of trace element concentrations in ultrapure materials below the ppb range in many cases. (author) 1 fig., 2 refs.

  3. Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

    Roč. 99, S (2005), s489-s491 ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] Institutional research plan: CEZ:AV0Z40310501 Keywords : solid sampling * electrothermal atomic absorption spectrometry * trace analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

  4. Determination of Trace Level Triclosan in Water by Online Preconcentration and HPLC-UV Diode Array

    Science.gov (United States)

    An online high performance liquid chromatography (HPLC) method for the detection and quantification of trace levels of triclosan in water is discussed. Triclosan, an anti-bacterial agent, and related compounds have been shown to reach municipal waste waters through the disposal ...

  5. Known knowns, known unknowns and unknown unknowns in prokaryotic transposition.

    Science.gov (United States)

    Siguier, Patricia; Gourbeyre, Edith; Chandler, Michael

    2017-08-01

    Although the phenomenon of transposition has been known for over 60 years, its overarching importance in modifying and streamlining genomes took some time to recognize. In spite of a robust understanding of transposition of some TE, there remain a number of important TE groups with potential high genome impact and unknown transposition mechanisms and yet others, only recently identified by bioinformatics, yet to be formally confirmed as mobile. Here, we point to some areas of limited understanding concerning well established important TE groups with DDE Tpases, to address central gaps in our knowledge of characterised Tn with other types of Tpases and finally, to highlight new potentially mobile DNA species. It is not exhaustive. Examples have been chosen to provide encouragement in the continued exploration of the considerable prokaryotic mobilome especially in light of the current threat to public health posed by the spread of multiple Ab R . Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Extraction inductively coupled plasma-optical emission spectrometry (ICP-OES). Determination of traces of phosphorus in tungsten

    International Nuclear Information System (INIS)

    Bauer, G.; Wegscheider, W.; Mueller, K.

    1989-01-01

    A method for the separation and preconcentration of traces of phosphorus from tungsten was developed. Solid phase extraction of the phosphovanadomolybdate complex performed on a micro-column was applied. Phosphorus was determined by optical emission spectroscopy (OES) with inductively coupled plasma (ICP) excitation. A limit of detection of 0,4 μg/g P with respect to the solid phase is obtained. By directly coupling the extraction/elution step to the ICP instrument a detection limit of 0,06 μg/g P in W was achieved. Besides, the complexity of spectral evaluation in ICP-OES determinations of traces in spectralline-rich matrices is discussed. (Authors)

  7. Determination of trace aluminum by fluorescence quenching method based on catalysis of potassium chlorate oxidizing alizarin red

    Science.gov (United States)

    Shao-Qin, Lin; Xuan, Lin; Shi-Rong, Hu; Li-Qing, Zeng; Yan, Wang; Li, Chen; Jia-Ming, Liu; Long-Di, Li

    2005-11-01

    A new method for the determination of trace aluminum has been proposed. It is based on the fact that alizarin red can emit strong and stable fluorescence at 80 °C for 30 min and Al 3+ can effectively catalyze potassium chlorate oxidizing alizarin red to form non-fluorescence complex which cause the fluorescence quenching. The linear dynamic range of this method is 0.040-4.00 ng l -1 with a detection limit of 5.3 pg l -1. The regression equation can be expressed as Δ If = 8.731 + 21.73 c (ng l -1), with the correlation coefficient r = 0.9992 ( n = 6). This sensitive, rapid and accurate method has been applied to the determination of trace aluminum(III) in human hair and tea samples successfully. What is more, the mechanism of catalyzing potassium chlorate oxidizing alizarin red by the fluorescence quenching method is also discussed.

  8. Determination of Trace and Volatile Element Abundance Systematics of Lunar Pyroclastic Glasses 74220 and 15426 Using LA-ICP-MS

    Science.gov (United States)

    McIntosh, E. Carrie; Porrachia, Magali; McCubbin, Francis M.; Day, James M. D.

    2017-01-01

    Since their recognition as pyroclastic glasses generated by volcanic fire fountaining on the Moon, 74220 and 15426 have garnered significant scientific interest. Early studies recognized that the glasses were particularly enriched in volatile elements on their surfaces. More recently, detailed analyses of the interiors of the glasses, as well as of melt inclusions within olivine grains associated with the 74220 glass beads, have determined high H2O, F, Cl and S contents. Such elevated volatile contents seem at odds with evidence from moderately volatile elements (MVE), such as Zn and K, for a volatile- depleted Moon. In this study, we present initial results from an analytical campaign to study trace element abundances within the pyroclastic glass beads. We report trace element data determined by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for 15426 and 74220.

  9. Report on the intercomparison runs for the determination of trace and minor elements in cabbage material. IAEA-359

    International Nuclear Information System (INIS)

    Campbell, M.J.; Radecki, Z.; Trinkl, A.; Burns, K.I.

    2000-04-01

    In 1989, the IAEA decided to produce a cabbage plant reference material that could be characterised for certain agrochemical residues. The cabbage plants (Brassica oleracea var. Sabauda) were grown from seed in Seibersdorf, Austria. The plants were treated with ten different agrochemical products during their growing period. Subsequently, it was decided that the material would also be valuable as a reference material for trace element analysis and quality control purposes. The property values for the trace metal content of the cabbage material, designated IAEA 359, were to be ascribed on the basis of information received from international intercomparison exercises. In parallel, it was decided to despatch the material as part of a joint IAEA-NIST (National Institute of Standards and Technology, USA) project to certify the trace and minor element contents of a spinach reference material (NIST 1570a), in which it was to serve as a quality control material. A similar rationale was used to justify inclusion of IAEA 359 in a small scale exercise for a preliminary characterisation of another IAEA reference material, IAEA 336 Lichen. Between 1992 and 1993, the material was used in 4 projects (2 large scale and 2 smaller scale) where its trace element contents were determined. This report deals with the statistical evaluation of the pooled analytical data from these exercises

  10. Determination of trace impurities in high-purity iron using salting-out of polyoxyethylene-type surfactants

    Energy Technology Data Exchange (ETDEWEB)

    Matsumiya, Hiroaki, E-mail: h-matsu@numse.nagoya-u.ac.jp [Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603 (Japan); Sakane, Yuto; Hiraide, Masataka [Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603 (Japan)

    2009-10-19

    To an iron sample solution was added polyoxyethylene-4-isononylphenoxy ether (PONPE, nonionic surfactant, average number of ethylene oxides 7.5) and the surfactant was aggregated by the addition of lithium chloride. The iron(III) matrix was collected into the condensed surfactant phase in >99.9% yields, leaving trace metals [e.g., Ti(IV), Cr(III), Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Pb(II), and Bi(III)] in the aqueous phase. After removing the surfactant phase by centrifugation, the remaining trace metals were concentrated onto an iminodiacetic acid-type chelating resin. The trace metals were desorbed with dilute nitric acid for the determination by inductively coupled plasma-mass spectrometry or graphite-furnace atomic absorption spectrometry. The proposed separation method allowed the analysis of high-purity iron metals for trace impurities at low {mu}g g{sup -1} to ng g{sup -1} levels.

  11. A pilot test of methods for determination of trace metals bound to colloids in surface waters

    Energy Technology Data Exchange (ETDEWEB)

    Nilsson, Kersti (Geosigma AB (Sweden))

    2011-01-15

    Two methods have been tested for the determination of trace metals associated with colloid species in surface waters, using test water from Eckarfjaerden (PFM000070) in Forsmark; 1) fractionation (ultra filtration) using special membrane filters with cut-offs of 1 kD and 5 kD and 2) filtration using a system of standard membrane filters with varying pore sizes connected in series. Both methods were somewhat modified compared to previous methods for colloid determination in groundwater within the site investigations at Forsmark and Laxemar (PLU). The results show that, in general, the largest amounts of metals associated with a colloid phase were recovered in the fraction between 1kD and 5 kD which indicates that the metal ions are associated with low molecular weight organic acids. Similar amounts were recovered on the filters in the filtration experiment. A minor part of the colloidal phase metals was recovered in the fraction larger than 5 kD i.e. metal ions associated with larger organic acids or colloidal size clay minerals. The metals present preferably as colloids in the fractionation experiment were: iron, thorium, cerium, uranium, neodymium, titanium, zirconium and yttrium. The filtering experiment showed larger parts of titanium and aluminum in the colloid phase than the fractionation experiment while the iron and cerium portions were equal and the uranium, yttrium and neodymium portions were lower. The results from the fractionation test showed that the dissolved parts were large for barium, manganese, strontium and rubidium. In the filtration test, uranium, yttrium and rubidium, were also present mainly as dissolved ions. The detection limit for filter analysis of thorium was high, and the part of thorium present as colloids was determined to <50%. Issues and methodological problems: - Severe contamination caused interpretation difficulties for several metal ions, especially chromium, nickel and zinc. - Both methods are time consuming and difficult to

  12. Application of anion-exchange techniques to the determination of traces of molybdenum in sea-water

    International Nuclear Information System (INIS)

    Kiriyama, T.; Kuroda, R.

    1984-01-01

    A combined ion-exchange spectrophotometric method has been developed for the determination of molybdenum in sea-water. Molybdenum is sorbed strongly on Amberlite CG 400 (Cl - ) at pH 3 from sea-water containing ascorbic acid and is easily eluted with 6 M nitric acid. Molybdenum in the effluent can be determined spectrophotometrically with potassium thiocyanate and stannous chloride. The combined method allows selective and sensitive determination of traces of molybdenum in sea-water. The precision of the method is 2% at a molybdenum level of approx. 10 μg/l. (author)

  13. Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Alduan, F. A.; Capdevilla, C.

    1980-01-01

    The determination of trace amounts of selenium In silicate rocks and feldspar by solvent extraction and graphite furnace atomic-absorption spectrometry has been stu- died. Sodium diethyl-ditio carbamate and ammonium pyrrolidine dithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted Into carbon tetrachloride as the sodium diethyldithiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (Author) 7 refs

  14. Possibilities of High Resolution Inductively Coupled Plasma Optical Emission Spectrometry in the Determination of Trace Elements in Environmental Materials

    Directory of Open Access Journals (Sweden)

    Nikolaya Velitchkova

    2013-01-01

    Full Text Available This paper presents new quantitative data for the spectral interferences obtained by high resolution 40.68 MHz radial viewing inductively coupled plasma optical emission spectrometry (HR-ICP-OES in the determination of Zn, Cd, Sb, Cu, Mn, Pb, Sn, Cr, U, and Ba in environmental materials in the presence of a complex matrix, containing Al, Ca, Fe, Mg, and Ti. The -concept for quantification of spectral interferences was used. The optimum line selection for trace analysis of a variety of multicomponent matrices requires the choice of prominent lines, which are free or negligibly influenced by line interference problems. The versatility of -concept as basic methodology was experimentally demonstrated in the determination of trace of elements in soil and drinking water. The detection limits are lower in comparison with corresponding threshold concentration levels for soil and drinking water in accordance with environmental regulations. This paper shows the possibilities of present day ICP-OES equipment in the direct determination of trace elements (without preconcentration of impurities in environmental samples.

  15. Vertical distribution of particulate trace elements in a street canyon determined by PIXE analysis

    International Nuclear Information System (INIS)

    Raunemaa, T.; Hautojaervi, A.; Kaisla, K.; Gerlander, M.

    1981-01-01

    Suspended particles in a street canyon were investigated by collecting air particulate matter on thin filters at heigths 2.3 to 20.5 m. The weather parameters and traffic characteristics were registered during the collection. Quantitative analysis of 15 trace elements from AI to Pb was carried out by the PIXE method using 1.8-2.0 MeV protons. The concentration of lead was found to decrease exponentially when going from street level to roof level. Almost all the trace elements analyzed were found to fall into two groups with different vertical distributions. The collected matter above 10 m height was found to be due mainly to combustion originated motor vehicle exhaust, the matter below 10 m to soil originated dust. (orig.)

  16. Report on intercomparison IAEA/V-10 of the determination of trace elements in hay powder

    International Nuclear Information System (INIS)

    Pszonicki, L.; Hanna, A.N.

    1985-07-01

    Hay plays an important role in the natural production circle of human nutrition. The level of its pollution is an important factor which can effect various branches of the food industry. The aim of the reported exercise organized by the IAEA was to provide the participating laboratories an opportunity to check their analytical performance by comparing their results with the results of other laboratories and to establish the concentration level of trace elements for certification purposes. The hay powder was analyzed by 50 laboratories from 25 countries for 42 elements. Neutron activation, atomic absorption, atomic emission and X-ray spectroscopy were predominantly used as analytical methods. The results provided by the participants of the reported intercomparison exercise have enabled to certify the concentration of eighteen trace and minor elements and to establish non-certified information values for the concentration of an additional twelve elements in Hay Powder IAEA/V-10

  17. A survey of Trace Metals Determination in Hospital Waste Incinerator in Lucknow City, India

    Directory of Open Access Journals (Sweden)

    Ranjan Kumar

    2004-08-01

    Full Text Available Information on the elemental content of incinerator burning of human organ, animal and medical waste is scanty in India Nineteen trace elements were analyzed in the incinerator ash from four major hospitals, one municipal waste incinerator and two R & D laboratories engaged in animal experiment in Lucknow city. Concentrations of Zinc and Lead were found to be very high in comparison to other metals due to burning of plastic products. The source of Ca, P and K are mainly bone, teeth and other animal organs. A wide variation in trace concentration of several toxic elements have been seen due to variation in initial waste composition, design of the incinerator and operating conditions.

  18. Determination of trace amounts of chemical warfare agent degradation products in decontamination solutions with NMR spectroscopy.

    Science.gov (United States)

    Koskela, Harri; Rapinoja, Marja-Leena; Kuitunen, Marja-Leena; Vanninen, Paula

    2007-12-01

    Decontamination solutions are used for an efficient detoxification of chemical warfare agents (CWAs). As these solutions can be composed of strong alkaline chemicals with hydrolyzing and oxidizing properties, the analysis of CWA degradation products in trace levels from these solutions imposes a challenge for any analytical technique. Here, we present results of application of nuclear magnetic resonance spectroscopy for analysis of trace amounts of CWA degradation products in several untreated decontamination solutions. Degradation products of the nerve agents sarin, soman, and VX were selectively monitored with substantially reduced interference of background signals by 1D 1H-31P heteronuclear single quantum coherence (HSQC) spectrometry. The detection limit of the chemicals was at the low part-per-million level (2-10 microg/mL) in all studied solutions. In addition, the concentration of the degradation products was obtained with sufficient confidence with external standards.

  19. Report on intercomparison V-9 of the determination of trace elements in cotton cellulose

    International Nuclear Information System (INIS)

    Pszonicki, L.; Hanna, A.N.; Suschny, O.

    1983-03-01

    Trace elements in plants are being investigated in many laboratories using nuclear techniques, mainly neutron activation analysis. To enable these laboratories to check the accuracy of their work and to provide data needed in the certification of a batch of reference material, the IAEA has organized several intercomparisons of analytical results of plants. This report deals with the comparative evaluations of the results on cotton cellulose powder. A total of 27 laboratories from 19 countries submitted 377 laboratory means on 57 elements

  20. Determination of trace elements in a cigarette paper by neutron activation analysis

    International Nuclear Information System (INIS)

    Abedinzadeh, Z.; Khalkhali, Zh.; Razeghi, M.; Parsa, B.

    The concentration of 19 trace elements in a cigarette paper (Zig-Zag Paper Company, France) which is used in making different brands of Iranian cigarettes, has been measured by neutron activation analysis, employing a high-resolution Ge(Li) detector. They include Na, K, Ca, Sc, Cr, Mn, Fe, Co, Zn, Br, Sr, Sb, Ba, Ce, Eu, Gd, Au, Hg, and Th. (author)

  1. Determination of trace U in beverages and mineral water using SSNTD (solid state nuclear track detector)

    International Nuclear Information System (INIS)

    Lin Junying; Zheng Liping; Cheng Yulin; Hao Xiuhong

    1991-01-01

    Trace U in beverages and mineral water has been estimated using the fission track analysis technique. The U contents in beverages vary from 0.26 ± 0.03 to 1.65 ± 0.07 ppb, with an average of 0.93 ± 0.05 ppb. The mean U content in mineral water is 9.20 ± 0.16 ppb, which is 10 times higher than that in other beverages

  2. Determination of trace lithium in uranium compounds by adsorption on activated alumina using a micro-column method.

    Science.gov (United States)

    Luo, Ming-Biao; Li, Bo-Ping; Yang, Zhi; Liu, Wei; Sun, Yu-Zhen

    2008-08-01

    A novel method using a micro-column packed with active alumina as solid phase was proposed for separation of trace lithium from uranium compounds prior to determination. The method is based on a preliminary chromatographic separation of the total amount of uranium. This separation involves passing the solution containing sodium carbonate through active alumina and then eluting the trace lithium retained by the solid phase with a solution of sulfuric acid. Two modes, off-line and on-line micro-column preconcentration, were performed. In conjunction with atomic absorption spectrometry, this on-line preconcentration technique allows a determination of lithium at 10(-9) level. Both off-line and on-line mode operation conditions were investigated in separation and determination of trace lithium by micro-column method (length of column bed, flow rate, etc.). The adsorption capacity of activated alumina was found to be 343 microg g(-1) for lithium. Under the optimal operation condition, the detection limit (DL) of on-line preconcentration corresponding to three times the standard deviation of the blank (S/N = 3) was found to be 1.3 ng mL(-1) and the RSD of this method is 3.32% (n = 5). The on-line calibration graph was linear over the range 20 - 200 ng mL(-1). A good preconcentration factor 820 was achieved by experiment under the on-line mode. The developed method was applied to the analysis of trace lithium in nuclear grade uranium compounds.

  3. Determination of trace elements in airborne particulates by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Jung, Yong Sam; Jung, Yung Joo; Jung, Eui Sik; Cho, Seung Yun

    1995-01-01

    Trace elements in airborne particulates were analyzed by instrumental neutron activation analysis(INAA) under the optimum analytical condition. Neutron irradiation for sample was done at the irradiation hole(neutron flux, 1 x 10 13 n/cm 2 s) of TRIGA MARK-III research reactor in the Korea Atomic Energy Research Institute. For the verification of the analytical method, NIST SRM-1648 and NIES CRM No.8 were chosen and analyzed. The accuracy and precision of the analysis of 40 and 24 trace elements in the samples were compared with the certified and reported values, respectively. The analytical method was found to be reliable enough when the analytical data of NIES sample were compared with those of different countries. In the analytical result of two or both of standard reference materials, relative standard deviation was within the 15% except a few elements and the relative error was within the 10%. We used this method to analyze 30 trace elements in airborne particulates collected with the high volume air sampler(PM-10) at two different locations and also confirmed the possibility to use this method as a routine monitoring tool to find out environmental pollution sources. 3 figs., 8 tabs., 19 refs. (Author)

  4. Total reflection X-ray fluorescence as a convenient tool for determination of trace elements in microscale gasoline and diesel

    Science.gov (United States)

    Zhang, Airui; Jin, Axiang; Wang, Hai; Wang, Xiaokang; Zha, Pengfei; Wang, Meiling; Song, Xiaoping; Gao, Sitian

    2018-03-01

    Quantitative determination of trace elements like S, Fe, Cu, Mn and Pb in gasoline and S in diesel is of great importance due to the growing concerns over air pollution, human health and engine failure caused by utilization of gasoline and diesel with these harmful elements. A method of total reflection X-ray fluorescence (TXRF) was developed to measure these harmful trace elements in gasoline and diesel. A variety of factors to affect measurement results, including TXRF parameters, microwave-assisted digestion conditions and internal standard element and its addition, were examined to optimize these experimental procedures. The hydrophobic treatment of the surface of quartz reflectors to support the analyte with neutral silicone solutions could prepare thin films of gasoline and diesel digestion solutions for subsequent TXRF analysis. The proposed method shows good potential and reliability to determine the content of harmful trace elements in gasoline and diesel with high sensitivity and accuracy without drawing different standard calibration curves, and can be easily employed to screen gasoline and diesel in routine quality control and assurance.

  5. Methodology for determination of trace elements in mineral phases of iron banded formation by LA-ICP-MS

    International Nuclear Information System (INIS)

    Sousa, Denise V.M. de; Nalini Junior, Herminio A.; Sampaio, Geraldo M.S.; Abreu, Adriana T. de; Lana, Cristiano de C.

    2015-01-01

    The study of the chemical composition of mineral phases of iron formation (FF), especially of trace elements, is an important tool in the understanding of the genesis of these rocks and the contribution of the phases in the composition of whole rock. Low mass fraction of such elements in the mineral phases present in this rock type requires a suitable analytical procedure. The laser ablation technique coupled with ICP-MS (LA-ICP-MS) has been widely used for determination of trace elements in geological samples. Thus, the aim of this study is to develop calibration curves for determination of trace elements (Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in mineral phases of banded iron formations by LA-ICP-MS. Several certified reference materials (CRM) were used for calibrate the equipment. The analytical conditions were checked by CRM NIST SRM 614. The results were satisfactory, since the curves showed good linearity coefficients, good accuracy and precision of results. (author)

  6. Determination of trace elements in Ethiopian, Vietnamese, and Japanese women using high-resolution IC-PMS.

    Science.gov (United States)

    Tekeste, Zinaye; Amare, Bemnet; Asfaw, Fanaye; Fantahun, Bereket; van Nguyen, Nhien; Nishikawa, Takeshi; Yabutani, Tomoki; Okayasu, Takako; Ota, Fusao; Kassu, Afework

    2015-10-01

    Humans and other living organisms require small quantities of trace elements throughout life. Both insufficient and excessive intakes of trace elements can have negative consequences. However, there is little information on serum level of trace elements in different populations. This study examines serum levels of trace elements in Ethiopian, Japanese, and Vietnamese women. Random samples of healthy women who were referred for routine hospital laboratory examinations in the cities of Hanoi, Sapporo, and Gondar were invited to participate in the study. Serum levels of magnesium, zinc, copper, iron, selenium, and calcium were determined using an inductively coupled plasma mass spectrometer. Furthermore, body mass index of each study participant was determined. The mean ± SD serum concentrations of zinc (μg/dL), copper (μg/dL), iron (μg/dL), selenium (μg/dL) and calcium (mg/dL), respectively, were 76.51 ± 39.16, 152.20 ± 55.37, 385.68 ± 217.95, 9.15 ± 4.21, and 14.18 ± 3.91 in Ethiopian women; 111.49 ± 52.92, 105.86 ± 26.02, 155.09 ± 94.83, 14.11 ± 3.41, and 11.66 ± 2.51 in Vietnamese women; and 60.69 ± 9.76, 107 ± 156, 268 ± 128, 8.33 ± 3.65, and 11.18 ± 0.68 in Japanese participants. Ethiopian women had significantly higher level of serum calcium than Vietnamese and Japanese women (both P Vietnamese women was higher than in women from Japan, the difference was not statistically significant (P > 0.05). Furthermore, compared with Japanese women, Ethiopian women had significantly high iron and copper concentrations (P Vietnamese than Ethiopian women. The study revealed a remarkable difference in serum concentrations of trace elements in women from different countries, implying differences in trace elements in the food or soil. Copyright © 2015 Elsevier Inc. All rights reserved.

  7. Determination of trace amounts of cerium in silicate rocks based on its candoluminescence in a calcium oxide based matrix

    International Nuclear Information System (INIS)

    Belcher, R.; Nasser, T.A.K.; Polo-Diez, L.; Townshend, A.

    1977-01-01

    A very sensitive method for the determination of cerium (above 10 ng ml -1 ) has been developed (Belcher et al., Analyst;100:415(1975)), based on the measurement of the green candoluminescence produced by cerium in a calcium oxide-calcium sulphate matrix, with sulphuric acid as a coactivator, when the matrix is inserted into a hydrogen-nitrogen-air flame. This paper describes the application of this method to the determination of trace amounts of cerium in rocks. It involves the fusion of the sample with lithium metaborate, and does not require the isolation of cerium from other components of the rock, before measuring the candoluminescence intensity of the cerium. (author)

  8. An ICP-AES method for the determination of trace metals in uranium by solvent extraction using KSM-17

    International Nuclear Information System (INIS)

    Jacob, Mary; Radhakrishnan, K.; Dhami, P.S.; Kulkarni, V.T.; Joshi, M.V.; Patwardhan, A.B.; Ramanujam, A.; Mathur, J.N.

    1994-01-01

    This paper describes the studies carried out for the determination of trace metallic impurities in uranium solutions. Uranium matrix is separated from the impurity elements by its selective extraction using 2-ethylhexyl hydrogen 2-ethylhexyl phosphonate (KSM-17, equivalent to PC88A). The aqueous phase is analysed for trace impurities by inductively coupled argon plasma atomic emission spectrometry. The studies also include recovery of impurities at various acidities and spectral interferences of uranium over the analyte element channels. Based on the above studies, a method has been standardised for the analysis of nineteen elements in uranium solutions. The relative standard deviation of the method for various elements is in the range of +- 1-5%. (author). 7 refs., 8 tabs., 1 fig

  9. Determination of several trace metals in biological materials by PIXE analysis after solvent extraction and polystyrene-film collection

    International Nuclear Information System (INIS)

    Iwata, Yoshihiro; Korenaga, Tatsumi; Suzuki, Nobuo

    1991-01-01

    Traces of vanadium, manganese, iron, cobalt, nickel, copper, and zinc were quantitatively extracted with diethyldithiocarbamate (DDTC) in benzene from a digested solution of biological materials and the metal-DDTC complexes were collected into a small amount of polystyrene foam produced by lyophilization of the benzene extract after addition of polystyrene. The polystyrene foam was dissolved in benzene and spread on Mylar film. After drying, a polystyrene film containing metal-DDTC complexes was produced on Mylar film, and then the polystyrene film was peeled from the Mylar film. This film was subjected to PIXE analysis. This method was applied to NBS SRM 1572 citrus leaves and a marine macroalgal sample, and 6 trace metals were simultaneously and accurately determined. (author)

  10. Graphite electrodes modified by 8-hydroxyquinolines and its application for the determination of copper in trace levels

    Directory of Open Access Journals (Sweden)

    Sousa Eliane R. de

    2006-01-01

    Full Text Available Surface modification by 8-hydroxyquinoline-5-sulfonic acid (8-HQS or 8-hydroxyquinoline (8-HQ on a graphite electrode through irreversible adsorption is reported in this paper. Cyclic voltammetry was used to characterize the surface behavior. The modified surface exhibited an affinity to chelating Cu(II in the solution, forming a Cu(II complex, which was employed for Cu(II trace analysis. Of the metals Zn, Ni, Pb, Co, and Cd, none presented interference until excess concentration of 10 times. Significant interference could be observed from Co(II, Cd(II and Fe(II for an excess concentration of 100 times on the analyte. A differential pulse voltammetry, combined with a preconcentrating-stripping process and a standard addition method was used for the analysis. A detection limit for trace copper determination in water, such as 5.110-9 mol L-1, was obtained.

  11. Trace element determination using static high-sensitivity inductively coupled plasma optical emission spectrometry (SHIP-OES).

    Science.gov (United States)

    Engelhard, Carsten; Scheffer, Andy; Nowak, Sascha; Vielhaber, Torsten; Buscher, Wolfgang

    2007-02-05

    A low-flow air-cooled inductively coupled plasma (ICP) design for optical emission spectrometry (OES) with axial plasma viewing is described and an evaluation of its analytical capabilities in trace element determinations is presented. Main advantage is a total argon consumption of 0.6 L min(-1) in contrast to 15 L min(-1) using conventional ICP sources. The torch was evaluated in trace element determinations and studied in direct comparison with a conventional torch under the same conditions with the same OES system, ultrasonic nebulization (USN) and single-element optimization. A variety of parameters (x-y-position of the torch, rf power, external air cooling, gas flow rates and USN operation parameters) was optimized to achieve limits of detection (LOD) which are competitive to those of a conventional plasma source. Ionic to atomic line intensity ratios for magnesium were studied at different radio frequency (rf) power conditions and different sample carrier gas flows to characterize the robustness of the excitation source. A linear dynamic range of three to five orders of magnitude was determined under compromise conditions in multi-element mode. The accuracy of the system was investigated by the determination of Co, Cr, Mn, Zn in two certified reference materials (CRM): CRM 075c (Copper with added impurities), and CRM 281 (Trace elements in rye grass). With standard addition values of 2.44+/-0.04 and 3.19+/-0.21 microg g(-1) for Co and Mn in the CRM 075c and 2.32+/-0.09, 81.8+/-0.4, 32.2+/-3.9 for Cr, Mn and Zn, respectively, were determined in the samples and found to be in good agreement with the reported values; recovery rates in the 98-108% range were obtained. No influence on the analysis by the matrix load in the sample was observed.

  12. Neutron activation analysis for environmental trace element research determination of elemental composition of sediments in the Sea of Galillee, Israel

    Energy Technology Data Exchange (ETDEWEB)

    Lavi, N; Ne` eman, E; Brenner, S; Butenko, V [Tel Aviv Univ. (Israel). Medical School

    1996-12-01

    The aims of this work were to: a) demonstrate the effectiveness of instrumental neutron activation analysis for determining the background concentrations of trace elements in the sediments collected from the Sea of Gallile. b) determine the advantage factors for epithermal neutron irradiation. c) determine the contribution of silicon to the total {sup 28}Al activity by the {sup 28}Si(n,p){sup 28}Al reaction. c) check the validity of the method by determining the elemental content of U.S. NBS Standard Reference Material SRM-1633a (fly ash). d) calculate the average enrichment factors for the elements in sediments . e) determine the concentrations of the artificial radionuclides {sup 134}Cs, {sup 137}Cs and the naturally occurring radionuclides {sup 40}K, {sup 226}Ra and {sup 232}Th (authors).

  13. Determination of traces of fluorine and hydrofluoric acid in the atmosphere

    International Nuclear Information System (INIS)

    Francois, H.; Grand-Clement, A.M.; Faltot, G.

    1963-01-01

    As some publications highlighted hazards related to the presence of dispersed fluorine and hydrofluoric acid in the atmosphere, the authors, after a brief recall of some measurement devices presented in some publications, present an experimental set-up which aims at measuring traces of these compounds in the atmosphere. They notably describe the preparation of a controlled fluorine atmosphere, discuss the efficiency of the absorption-based trap, report the study of the electrolytic analysis cell, discuss its calibration. They also report the study of the influence of temperature and of the presence of disturbing ions

  14. Comparison of three analytical methods for the determination of trace elements in whole blood

    International Nuclear Information System (INIS)

    Ward, N.I.; Stephens, R.; Ryan, D.E.

    1979-01-01

    Three different analytical techniques were compared in a study of the role of trace elements in multiple sclerosis. Data for eight elements (Cd, Co, Cr, Cu, Mg, Mn, Pb, Zn) from neutron activation, flame atomic absorption and electrothermal atomic absorption methods were compared and evaluated statistically. No difference (probability less than 0.001) was observed in the elemental values obtained. Comparison of data between suitably different analytical methods gives increased confidence in the results obtained and is of particular value when standard reference materials are not available. (Auth.)

  15. Determination of trace elements in poly(methyl methacrylate) by neutron activation analysis

    International Nuclear Information System (INIS)

    Kobayashi, M.

    1979-01-01

    The results are reported of the neutron activation analysis of poly(methyl methacrylate) polymerized with a redox system of chromium (II) acetate and p-chlorobenzyl peroxide in dimethylformamide at 30 0 C. Since the polymer was originally synthesized in experiments for kinetic studies, the results indicate an arbitrary background of purity of polymers obtained in a laboratory. Samples were irradiated for 28m and gamma spectra detected trace amounts of chlorine, aluminum, vanadium, magnesium, manganese, potassium, copper, zinc, sodium, bromine, lanthanum, gold, and chromium. 2 figures, 1 table

  16. A Fast Radiochemical Method for the Determination of Some Essential Trace Elements in Biology and Medicine

    Energy Technology Data Exchange (ETDEWEB)

    Samsahl, K

    1966-02-15

    An anion-exchange method based on fast selective sorption steps from mixtures of sulfuric, hydrobromic, and hydrochloric acid solutions has been developed for the separation of five different groups of radioactive trace elements in neutron-irradiated biological material. The separations are performed automatically with a simple proportioning pump apparatus. The apparatus allows the exact adjustment of influent solutions to the series of ion-exchange columns. The practical application of the method is described in detail. The successful use of the method is practically independent on the level of Na activity present in the sample.

  17. Latest approaches on green chemistry preconcentration methods for trace metal determination in seawater--a review.

    Science.gov (United States)

    La Colla, Noelia Soledad; Domini, Claudia Elizabeth; Marcovecchio, Jorge Eduardo; Botté, Sandra Elizabeth

    2015-03-15

    Evaluation of trace metal levels in seawater samples is undertaken regularly by research groups all over the world, leading to a growing demand for techniques involving fewer toxic reagents, less time-consuming protocols and lower limits of detection. This review focuses on providing a brief but concise description of the latest methodologies developed to this end, outlining the advantages and disadvantages of the various protocols, chelating and dispersive agents and instruments used. Conclusions are drawn on the basis of the articles reviewed, highlighting improvements introduced in order to enhance the performance of the protocols. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. The determination of trace elements in new food grain SRM's using neutron activation analysis

    International Nuclear Information System (INIS)

    Gills, T.E.; Gallorini, M.; Rook, H.L.

    1978-01-01

    Potentially toxic metals in the food chain that can lead to deleterious effects on human health have been well documented. Because of the toxicity of some metals, levels of 1 ppm or less must be routinely monitored in foods to ensure human safety. To ensure the accuracy of measurement, NBS in a cooperative interagency agreement with the Food and Drug Administration is involved in developing and certifying selected elements in food grain as a part of the Standard Reference Material program. Both instrumental and radiochemical neutron activation analysis were used to analyze two food grain standard reference materials (Rice and Wheat Flours) for trace element certification. (author)

  19. Determination of trace elements in Mesozoic dykes of the Serra do Mar by neutron activation

    International Nuclear Information System (INIS)

    Vicentini, Caio M.; Marques, Leila S.

    2013-01-01

    The analysis of trace elements such as rare earths, Th, U, Ta, Hf, Ba, Rb and Ba, is a very important tool for petrogenetic studies. In order to study these processes in dykes of Enxame Serra do Mar (Coast of Sao Paulo and Rio de Janeiro), belonging to the Parana Magmatic Province (PMP), one of the most significant provinces of continental basalts in the world, were perform analyzes by neutron activation in these dikes. The technique, employed in Centro de Reator de Pesquisa of the Instituto de Pesquisas Energeticas e Nucleares, provided concentrations of trace elements with accuracy levels of 10% and 9%, which are suitable for petrogenetic studies. Due to the low concentrations of the elements analyzed, the experimental routine sample preparation processes covered very careful to avoid contamination. The samples investigated can be divided into four groups: basic rocks (SiO 2 500; basic rocks with Ti / Y 2 2 > 63%). Dikes of intermediate and acid composition only occur at the Sao Sebastiao Island and adjacent coastal region. The concentrations of major and minor elements, as well as the abundance patterns of rare earths and other incompatible elements of these more differentiated rocks, show significant similarities with the type of the volcanic Chapeco, suggesting similar genesis, in other worlds, including also processes of crustal contamination

  20. Modified emission-transmission method for determining trace elements in solid samples using the XRF techniques

    International Nuclear Information System (INIS)

    Poblete, V.; Alvarez, M.; Hermosilla, M.

    2000-01-01

    This is a study of an analysis of trace elements in medium thick solid samples, by the modified transmission emission method, using the energy dispersion X-ray fluorescence technique (EDXRF). The effects of absorption and reinforcement are the main disadvantages of the EDXRF technique for the quantitative analysis of bigger elements and trace elements in solid samples. The implementation of this method and its application to a variety of samples was carried out using an infinitely thick multi-element white sample that calculates the correction factors by absorbing all the analytes in the sample. The discontinuities in the masic absorption coefficients versus energies association for each element, with medium thick and homogenous samples, are analyzed and corrected. A thorough analysis of the different theoretical and test variables are proven by using real samples, including certified material with known concentration. The simplicity of the calculation method and the results obtained show the method's major precision, with possibilities for the non-destructive routine analysis of different solid samples, using the EDXRF technique (author)

  1. Determination of trace elements in kidneys, livers and brains of rats with sealer implants by ICP-MS

    International Nuclear Information System (INIS)

    Simsek, Neslihan; Akinci, Levent; Alan, Hilal; Gecör, Orhan; Özan, Ülkü

    2017-01-01

    Following root canal treatment, sealers may contact periapical tissue. The purpose of this study was to evaluate the systemic toxic effects of epoxy resin-based sealers (AH Plus and Obtuseal). Inductively coupled plasma-mass spectrometry (ICP-MS) was used to measure levels of trace elements (beryllium, magnesium, aluminium, calcium, chromium, arsenic and lead) in the brain, kidney and liver of rats. Twenty sterilized polyethylene tubes were then filled with AH Plus and Obtuseal and implanted into the dorsal subcutaneous tissue of 10 rats; three unoperated animals were used as a control group. After 45 days, the rats were sacrificed by cervical dislocation following anaesthesia, and brains, kidneys and livers were removed from all experimental animals. ICP-MS analysis was used to determine levels of trace elements. Data were analysed using Kruskal– Wallis and Connover post hoc tests. No significant differences were found in aluminium and calcium levels, but brains, kidneys and livers showed significantly higher amounts of magnesium and chromium than the corresponding controls. In the kidney and liver samples, arsenic levels were found to be higher than in the control group. Lead was detected at higher levels only in liver samples from the AH Plus group. Beryllium was not detected in any organ. It was concluded that AH Plus and Obtuseal release minimal quantities of trace elements when in contact with subcutaneous tissue, and further studies are needed to understand the systemic effects of these materials

  2. Determination of base-line levels of trace amounts in pulses and spices using neutron activation technique

    International Nuclear Information System (INIS)

    Zaidi, J.H.; Arif, M.; Fatima, I.; Qureshi, I.H.

    1993-01-01

    It has been established that essential trace elements are vitally important for biochemical systems, whereas toxic elements if present in relatively higher amounts adversely affect these systems. Trace elements reach the human body mainly through foodstuffs. The different articles contain varying amount of toxic and essential elements. It is therefore necessary to asses the adequacy and safety of the diet by determining the base-line levels of these elements. In continuation of our previous work, some varieties of pulses and spices were analyzed using neutron activation technique. Among the four varieties of pulses lentil (lens esculenta) was found to contain higher amounts of essential elements and lower amounts of toxic elements. The daily intake of essential and toxic elements through pulses was estimated and compared with the suggested values. The estimated intake of essential elements is adequate and that of toxic elements is well below the tolerance limit. In spices cumin and caraway seeds were found to contain relatively higher amounts of essential as well as toxic elements. The studies showed that food spices were additional source of trace element intake. (author)

  3. Multi-elemental determination of trace elements in deep seawater by inductively coupled plasma mass spectrometry with resin preconcentration

    International Nuclear Information System (INIS)

    Sumida, Takashi; Nakazato, Tetsuya; Tao, Hiroaki

    2003-01-01

    A miniaturized column (ca. 3 mm i.d., 40 mm length), packed with a chelating resin (0.2 g) with iminodiacetic acid groups (Muromac A-1), was tested for the preconcentration of trace elements in seawater. After preconcentration, the column was washed with ammonium acetate buffer (pH 5.5) and water to remove the major elements, such as Ca and Mg, and was then eluted with 4 ml of 2 mol l -1 nitric acid. Twenty-six trace elements were determined by inductively coupled plasma mass spectrometry and inductively coupled plasma emission spectrometry. The necessary volume of the seawater sample was only 200 ml. The recoveries for most of the elements tested were over 90%, although those for Al, V and Th were around 70%. The trueness and precision were evaluated by analyzing a standard reference material of seawater (NASS-4, NRC Canada). The observed values obtained with the present method showed good agreement with the certified values. The present method was also applied to deep seawater samples collected at Muroto, Japan. A difference in the rare earth element pattern, especially the Ce anomaly, between the deep seawater sample and the surface seawater sample was observed, as well as the differences of the concentrations of many trace elements. (author)

  4. DETERMINATION of the TRACE ELEMENT LEVELS in HAIR of SMOKERS and NON-SMOKERS by ICP-MS

    Directory of Open Access Journals (Sweden)

    Elif Varhan Oral

    2016-09-01

    Full Text Available For at least 50 years, determination of the trace element levels in human hair has been used to assess environmental and vocational exposure to toxic elements . As compared to other biological matrices (e.g. blood, urine, human hair is stable and therefore useful as a matrice. In this study, analyses of toxic and essential trace elements, such as Cd, Pb, Cu and Fe, were done in hair samples which we collected from male smokers (10 people and non-smokers (10 people who live in Diyarbakır, Turkey and concentrations in hair samples were compared. Hair samples were washed by a standard procedure proposed by the International Atomic Energy Agency. Then the samples were dried for 16 h at 110°C in an oven. Solubilization procedure was carried out by nitric acid hydrogen peroxide mixture (3:1 in closed vessels in a microwave oven. Trace element analyses were carried out by using inductively coupled plasma-mass spectrometry (ICP-MS  technique. In our study, while concentrations of Cd, Pb, and Fe elements were found to be considerably higher in smokers than non-smokers, similar results were observed in Cu concentrations. The precision and accuracy of the method was evaluated by applying spike method to samples. Analytical recovery results were found between 91.2% and 104.6%.

  5. The catalytic kinetic method for the determination of trace formaldehyde (FA) base on a bromate-eosin Y system

    Science.gov (United States)

    Tang, Yufang; Chen, Hao; Weng, Chao; Tang, Xiaohui; Zhang, Miaoling; Yang, Qiongqiong; Hu, Tao; Cai, Changqun

    A new simple and highly sensitive catalytic kinetic method for the determination of trace amount of FA in food sample has been established. The method was based on the catalytic effect of FA on the oxidation of eosin Y by potassium bromate in present of phosphoric acid. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of eosin Y at 518 nm. Under the optimized experimental conditions, the developed method allowed the determination of FA in the range of 0.03-0.6 μg mL-1 with a good precision, and the limit of detection was down to 0.00988 μg mL-1. The relative standard deviation of five replicate measurements for the determination of FA in concentration 0.12 μg mL-1 was 1.8%. The proposed method was successfully applied to the determination of FA in food directly and satisfactory results were obtained.

  6. Spectrophotometric determination of trace uranium in phosphate ore samples from kurum and uro areas, Nuba mountains, Sudan

    International Nuclear Information System (INIS)

    Mohamed, A. A.; Ali, A. H.; Altayeb, M. A. H.

    2004-01-01

    A method was proposed for the spectrophotometric determination of uranium content in phosphate ores. the method is based on the use of nitrogen (v) acid for leaching the rock, and treatment with ammonium carbonate solution, whereby uranium (Vi) is kept in solution as its carbonate complex. The ion-exchange technique was used for the recovery of uranium. Uranium was determined spectrophotometrically by measurement of the absorbance of the yellow uranium (Vi)-8-hydroxyquinolate complex at λ 425 nm. The procedure was used for the determination of trace uranium content in 30 phosphate ore samples collected from Kurun and Uro areas in Nuba mountains in Sudan. X-ray fluorescence technique was employed for the assessment of the method used. The spectrophotometric method results show a high similarity with those obtained by XRF technique. This agreement indicates that the procedure proposed here has been successfully applied for the determination of uranium in phosphate ores. (Author)

  7. Determination of some trace elements in edible crops grown in Jebel Merra area

    International Nuclear Information System (INIS)

    Mohamed, Abdelmoneim Adam

    2001-11-01

    This preliminary study was conducted in the area of Jebel Merra in South Darfour State, Western Sudan, With the aim of establishing a base-line data on trace element levels in foodstuffs cultivated in the region. 19 samples of vegetables, cereal grains, spices and fruits were collected from farms in Nyala, Derbat, Sunie and Gawa. With the exception of Nyala, the sampling farms were located on hill slopes using turus system as a means for water harvesting. Samples were analyzed for six trace elements, viz., Fe, Mn, Zn, Cu, Co and Cr using Atomic Absorption Spectroscopy (Aas). Comparison of the results with similar data from different parts of Sudan and from some other countries reveals that the foodstuffs grown in this high latitude region are relatively deficient in their elemental content. This salient feature conforms with well-known fact that, the soil in high latitude regions depleted in nutritional plant elements due to the leaching caused by runoff water hence the corresponding concentrations in plants are quite low indicative of state of malnutrition. Categorically speaking, among the vegetables analyzed, okra has shown a high affinity in accumulating Fe (187.49 ppm), Mn (80.31ppm), Cu (7.43 ppm) and Zn (12.74 ppm) comparative to other species. On the other hand, opposite trend was observed with sorghum as the poorest one with respect to its ability in concentrating Fe (55.57 ppm), Mn (4.19 ppm), Zn (5.25 ppm) and Cu (1.26 ppm) relative to millet, Wheat, Lupins and broad beans. With regard to spices covered in this investigation, garlic contains the lowest concentrations of all the elements analyzed and agree well with those found in onion the poorest of all the vegetables. Concentrations obtained were 108.78 ppm (Fe), 3.6 ppm (Mn), 4.6 ppm (Zn), 1.73 ppm (Cu) and 0.1 ppm (Cr) and 0.16 ppm (Co). On individual basis, the highest concentration of Mn was measured in lupins at 143.18 ppm. Cr content in all spices was found to be less than 1 ppm, whereas for Co

  8. Trace elements in sera of patients with hepatitis B: Determination and analysis

    Science.gov (United States)

    Saod, Wahran M.; Darwish, Nadiya T.; Zaidan, Tahseen A.; Alfalujie, Abdul Wahab A.

    2018-04-01

    Chronic Hepatitis B (HBV) is the leading cause of morbidity and mortality worldwide with about 248 million people having HBV infection. Trace elements e.g. copper (Cu), zinc (Zn), selenium (Se) and iron (Fe) are constituent components of many metal proteins and metalloenzymes in human sera. Therefore, the ratios of these trace elements in human sera are often stated to be a good marker for diagnosing various diseases including HBV. The aims of this study are: to compare the level of trace elements in sera of patients infected with HBV and healthy participants, and to evaluate the efficiency of analytical techniques (e.g. Inductively Coupled Plasma-Mass spectrometry (ICP-MS), Atomic Absorption Spectroscopy (hydride generation) (AAS) and Graphite Furnace Atomic Absorption Spectroscopy (GFAAS) that are currently used to detect Fe and Se elements in Patients' human sera. The findings of this study show that the concentration range of copper element between (132.80±28.64 µg/dl) to (105.66±23.20 µg/dl) was significantly higher in HBV infected patients as compared to those in healthy controls (91.27±9.20 µg/dl). Iron concentration range between (206.64±61.60 µg/l) to (170.00±36.71 µg/l) was significantly higher in HBV infected patients as compared to those in healthy controls (158.00±15.13 µg/l). However, patients with HBV had significantly lower serum concentrations of zinc with a concentration range between (111.64±20.90 µg/dl) to (99.25±24.06 µg/dl) as compared to those in healthy controls (113.44±16.38 µg/dl). While selenium concentration range between (64.39±7.39 µg/l) to (51.10±4.96 µg/l) was significantly lower in HBV infected patients as compared to those in healthy controls (67.68±7.60) (μg/l). Moreover, the results of this study suggest that (AAS) technique was the most accurate method to measure the concentration of selenium element, while (UV and ICP-MS) analytical techniques have the same efficiency in measuring the iron concentration.

  9. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hagarová, Ingrid, E-mail: hagarova@fns.uniba.sk; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb–dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l{sup −1} HNO{sub 3}. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l{sup −1}, quantification limit of 0.38 μg l{sup −1}, relative standard deviation of 4.2% (for 2 μg l{sup −1} of Pb; n = 26), linearity of the calibration graph in the range of 0.5–4.0 μg l{sup −1} (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91–96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters. - Highlights: • The potential of coacervates for the extraction of metal ions is examined. • No difficulties in coupling of ETAAS with the proposed CAE are observed. • Achieved preconcentration factor results in enhanced sensitivity. • Analytical performance is confirmed by the reliable determination of trace Pb. • The proposed CAE is ecofriendly and efficient.

  10. Determination of ultra trace arsenic species in water samples by hydride generation atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Ulusoy, Halil Ibrahim, E-mail: hiulusoy@yahoo.com [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey); Akcay, Mehmet; Ulusoy, Songuel; Guerkan, Ramazan [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey)

    2011-10-10

    Graphical abstract: The possible complex formation mechanism for ultra-trace As determination. Highlights: {yields} CPE/HGAAS system for arsenic determination and speciation in real samples has been applied first time until now. {yields} The proposed method has the lowest detection limit when compared with those of similar CPE studies present in literature. {yields} The linear range of the method is highly wide and suitable for its application to real samples. - Abstract: Cloud point extraction (CPE) methodology has successfully been employed for the preconcentration of ultra-trace arsenic species in aqueous samples prior to hydride generation atomic absorption spectrometry (HGAAS). As(III) has formed an ion-pairing complex with Pyronine B in presence of sodium dodecyl sulfate (SDS) at pH 10.0 and extracted into the non-ionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114). After phase separation, the surfactant-rich phase was diluted with 2 mL of 1 M HCl and 0.5 mL of 3.0% (w/v) Antifoam A. Under the optimized conditions, a preconcentration factor of 60 and a detection limit of 0.008 {mu}g L{sup -1} with a correlation coefficient of 0.9918 was obtained with a calibration curve in the range of 0.03-4.00 {mu}g L{sup -1}. The proposed preconcentration procedure was successfully applied to the determination of As(III) ions in certified standard water samples (TMDA-53.3 and NIST 1643e, a low level fortified standard for trace elements) and some real samples including natural drinking water and tap water samples.

  11. The IAEA worldwide intercomparison exercises (1990-1997). Determination of trace elements in marine sediments and biological samples

    International Nuclear Information System (INIS)

    Coquery, M.; Carvalho, F.P.; Azemard, S.; Horvat, M.

    1999-01-01

    Four major worldwide intercomparison exercises for the determination of trace elements in various environmental matrices were completed by the IAEA Marine Environment Laboratory since 1990: SD-M-2/TM, deep sea marine sediment; IAEA-350, tuna fish homogenate; IAEA-356, contaminated coastal sediment and IAEA-140, sea plant (Fucus sp.). These intercomparison exercises aim at enabling individual laboratories to monitor their performance. The results of these exercises allowed us to make an overall evaluation of the quality of data provided for environmental assessment and to identify the trends of analytical performance in the determination of trace elements over the years. The number of participants in each exercise varied between 68 and 130, and permits statistical evaluation of the performance for a number of elements. For each intercomparison exercise, the performance of the participant laboratories was assessed by comparing reported results with established reference values calculating 'Z-scores'. The results show that for each sample matrix, the values reported by some laboratories were far from satisfactory in the earlier exercises, in particular for Cd, Cr and Pb. Nevertheless, over time, a general improvement of performance can clearly be seen for all elements. Moreover, there was a noticeable increase in the number of laboratories with good performance in the two most recent exercises, observed both for biological and for sediment matrices. However, the determination of trace elements such as Cd, Cr, Pb and Hg in low level environmental samples still remains a major challenge to the analysts. For this reason and in order to assess the current performance of laboratories for low environmental levels of contaminants, the future intercomparison exercises will concentrate on low level sediment and fish samples

  12. Advanced functional materials in solid phase extraction for ICP-MS determination of trace elements and their species - A review.

    Science.gov (United States)

    He, Man; Huang, Lijin; Zhao, Bingshan; Chen, Beibei; Hu, Bin

    2017-06-22

    For the determination of trace elements and their species in various real samples by inductively coupled plasma mass spectrometry (ICP-MS), solid phase extraction (SPE) is a commonly used sample pretreatment technique to remove complex matrix, pre-concentrate target analytes and make the samples suitable for subsequent sample introduction and measurements. The sensitivity, selectivity/anti-interference ability, sample throughput and application potential of the methodology of SPE-ICP-MS are greatly dependent on SPE adsorbents. This article presents a general overview of the use of advanced functional materials (AFMs) in SPE for ICP-MS determination of trace elements and their species in the past decade. Herein the AFMs refer to the materials featuring with high adsorption capacity, good selectivity, fast adsorption/desorption dynamics and satisfying special requirements in real sample analysis, including nanometer-sized materials, porous materials, ion imprinting polymers, restricted access materials and magnetic materials. Carbon/silica/metal/metal oxide nanometer-sized adsorbents with high surface area and plenty of adsorption sites exhibit high adsorption capacity, and porous adsorbents would provide more adsorption sites and faster adsorption dynamics. The selectivity of the materials for target elements/species can be improved by using physical/chemical modification, ion imprinting and restricted accessed technique. Magnetic adsorbents in conventional batch operation offer unique magnetic response and high surface area-volume ratio which provide a very easy phase separation, greater extraction capacity and efficiency over conventional adsorbents, and chip-based magnetic SPE provides a versatile platform for special requirement (e.g. cell analysis). The performance of these adsorbents for the determination of trace elements and their species in different matrices by ICP-MS is discussed in detail, along with perspectives and possible challenges in the future

  13. Determination of trace concentration of uranium in soils by the nuclear track technique

    International Nuclear Information System (INIS)

    Islam, G.S.; Abdullah, M.N.A.

    1998-04-01

    Solid state nuclear track detector CR-39 has been used to estimate trace concentration of uranium in soil and sand samples from various places of Bangladesh. Uranium contents in soil samples have been found to vary from ∼3.79 to ∼8.63 ppm and in sand samples from ∼2.39 to ∼6.53 ppm. The mean concentration in soil and in sand samples were found to be ∼4.52 and ∼2.96 ppm respectively. The maximum uranium concentration in soil samples was observed in Sylhet while the uranium concentration of sand was found to be maximum in the sea beach of Cox's Bazar. The implication of results is briefly discussed in the paper. (author)

  14. Ecological and biological determinants of trace elements accumulation in liver and kidney of Pontoporia blainvillei

    Energy Technology Data Exchange (ETDEWEB)

    Seixas, Tercia G. [Departamento de Quimica, PUC-Rio, 22453-900 Rio de Janeiro, RJ (Brazil); Laboratorio de Radioisotopos Eduardo Penna Franca, IBCCF-UFRJ, 21941-902 Rio de Janeiro, RJ (Brazil)], E-mail: tercia@rdc.puc-rio.br; Kehrig, Helena do A. [Laboratorio de Radioisotopos Eduardo Penna Franca, IBCCF-UFRJ, 21941-902 Rio de Janeiro, RJ (Brazil); Fillmann, Gilberto [Departamento de Oceanografia, FURG, 96201-900 Rio Grande, RS (Brazil); Di Beneditto, Ana Paula M.; Souza, Cristina M.M. [Laboratorio de Ciencias Ambientais, CBB-UENF, 28013-602 Campos dos Goytacazes, RJ (Brazil); Secchi, Eduardo R. [Departamento de Oceanografia, FURG, 96201-900 Rio Grande, RS (Brazil); Laboratorio de Tartarugas e Mamiferos Marinhos, Departamento de Oceonagrafia e Museu Oceanografico ' Prof. E.C. Rios' , FURG, 96201-900, Rio Grande, RS (Brazil); Moreira, Isabel [Departamento de Quimica, PUC-Rio, 22453-900 Rio de Janeiro, RJ (Brazil); Malm, Olaf [Laboratorio de Radioisotopos Eduardo Penna Franca, IBCCF-UFRJ, 21941-902 Rio de Janeiro, RJ (Brazil)

    2007-10-15

    The present work tested whether ecological and biological variables have an influence on the assimilation of trace elements by the tissues of a cetacean from the Western South Atlantic Ocean. No significant differences were observed in the concentrations for both sexes. As individuals from the two sampling areas belong to distinct genetic and morphological populations, animals of similar body length were older on the southeastern than on the southern coast. The liver showed the highest concentrations of mercury, whereas the highest levels of cadmium were found in the kidney. Hepatic mercury, cadmium and selenium in individuals from the south coast were about four times as high as those from the southeast coast. However, arsenic in the liver and kidney were similar in both coastal areas. Hepatic mercury, cadmium and selenium concentrations increased with body length in individuals from the southeastern coast, although no significant correlations (P > 0.05) were observed between body length from either area and the renal and hepatic As concentrations. A significant positive linear relationship was observed between molar concentrations of Hg and Se in the liver of all individuals from both areas (r{sup 2} = 0.93; P < 0.001), presenting Se:Hg ratios close to 4. Differences found among the concentrations of Hg, Cd and Se in dolphins from both areas were probably due to the preferred prey, bioavailability of elements in each marine environment, and environment variables (water temperature, net primary production). As a consequence, concentrations of trace elements in the tissues of this species can be considered to be a result of the surrounding environment.

  15. Mass-produced lonophore-based fluorescent microspheres for trace level determination of lead ions.

    Science.gov (United States)

    Telting-Diaz, Martin; Bakker, Eric

    2002-10-15

    The development and characterization of small, uniform, and mass-produced plasticized PVC-based sensing microspheres in view of rapid trace level analysis of lead ions is reported. Micrometer-sized particles obtained via an automated casting process were rendered selective for lead ions by doping them with highly selective components in a manner analogous to traditional optode sensing films. Single particles that contained the lipophilic ionophore N,N,N',N'-tetradodecyl-3-6-dioxaoctane-1-thio-8-oxodiamide (ETH 5493), the chromoionophore ETH 5418 together with a lipophilized indocarbocyanine derivative as internal reference dye (DiIC18), and lipophilic ion-exchanger sites sodium tetrakis[3,5-bistrifluoromethylphenyl]borate, yielded measurable lead responses at the low nanomolar level in pH buffered solutions. The detection limit for single particles was 3 x 10(-9) M at pH 5.7. The microspheres were fabricated via a reproducible formation of polymer droplets within a flowing aqueous phase followed by collection of spherical particles of approximately 13 microm in size. The particles were immobilized and assayed individually in a microflow cell via fluorescence microscopy. Selectivity patterns found were in agreement with those reported earlier for the lead-selective ligand ETH 5493, and all response functions were fully described by theory. In contrast to optode films that necessitated very long equilibration times and large sample volumes in diluted samples of analyte, particles exhibited extremely enhanced equilibrium response times. Thus, for lead sample concentrations at and above 5 x 10(-8) M, response times were approximately 3 min, whereas at the detection limit, complete equilibrium was recorded after just 15 min, with required sample volumes on the order of 1 mL This new class of microspheres appears to be suitable for rapid and sensitive ion detection at trace levels in environmental and biological applications.

  16. Determination of trace elements in various kinds of bean by X-ray spectrometric techniques (1995-96)

    International Nuclear Information System (INIS)

    U Tin Maung Kyi; U Wai Zin Oo

    2001-01-01

    Various kinds of bean such as Peanut, Gram Whole, Black Eye Bean, Small Red Bean, Lab Lab Bean, Green Mung Bean, Filed Pea, Seasame Seed, Sultani, Maize, Butter Bean, Dolichos Lab Lab, Toor Whole, Small Yellow Bean, Cow Pea have been collected and analysed by EDXRF analysis for trace elements. The measurement system consists of a Cd-109 annual excitation source, a Si (Li) detector, H V power supply, a spectrometry amplifier, a multichannel analyser and a personal computer. The samples were prepared as pressed pellets and measured by Emission Transmission Technique. The accuracy was determined by analysing standard reference material, SOIL-7 form IAEA. (author)

  17. Experiments made to separate the trace elements in seawater by extraction and their determination by neutron activation analysis

    International Nuclear Information System (INIS)

    Heuss, E.; Lieser, K.H.

    1979-01-01

    The problems of trace element determination in seawater by neutron activation analysis are discussed. Experiments with tri-n-octylphosphinoxide (TOPO) did not bring satisfactory results because of the strong interference of the bremsstrahlung from 32 P. Experiments with oxin at different pH showed that in each case only few elements are extracted in greater amounts. An extraction apparatus is described making possible the extraction of up to 10 l water by 50 ml of an organic solution. Extraction experiments using different complexing agents were satisfactory but the evaporation of the organic phase to dryness for irradiation was difficult. (author)

  18. On-site Determination of Trace Arsenic by Reflection-Absorption Colorimetry of Molybdenum Blue Collected on a Membrane Filter.

    Science.gov (United States)

    Hasegawa, Yuya; Suzuki, Yasutada; Kawakubo, Susumu

    2017-01-01

    An on-site determination method for trace arsenic has been developed by collecting it as molybdenum blue (MB) in the presence of tetradecyldimethylbenzylammonium chloride on a mixed cellulose ester membrane filter and by measuring reflection absorbance (RA) of MB on the filter using a laboratory-made palm-top size reflection-absorbance colorimeter with a red light-emitting diode. The value of RA was proportional to the amount of arsenic up to 0.5 μg with a detection limit of 0.01 μg. The proposed method was successfully applied to soil extract and hot-spring water samples.

  19. Note: A dual temperature closed loop batch reactor for determining the partitioning of trace gases within CO2-water systems.

    Science.gov (United States)

    Warr, Oliver; Rochelle, Christopher A; Masters, Andrew J; Ballentine, Christopher J

    2016-01-01

    An experimental approach is presented which can be used to determine partitioning of trace gases within CO2-water systems. The key advantages of this system are (1) The system can be isolated with no external exchange, making it ideal for experiments with conservative tracers. (2) Both phases can be sampled concurrently to give an accurate composition at each phase at any given time. (3) Use of a lower temperature flow loop outside of the reactor removes contamination and facilitates sampling. (4) Rapid equilibration at given pressure/temperature conditions is significantly aided by stirring and circulating the water phase using a magnetic stirrer and high-pressure liquid chromatography pump, respectively.

  20. Determination of trace element concentration in infant head hair of Rawalpindi/Islamabad area using INAA technique

    International Nuclear Information System (INIS)

    Zaidi, J.H.; Gill, K.P.

    2004-01-01

    The concentration of 18 minor and trace elements (essential, toxic and nonessential) in infant head hair was determined. The data provide the base-line values of these elements in head hair of infants of low- and medium-income group subjects. The statistical results show that there are significant correlations between some elements such as: Ca-Zn, Ca-Fe, Mg-Ca, Mg-Mn and Mg-Fe. The results obtained have been compared with the data reported in the literature. Our data show compatibility of elemental contents of infant head hair with those from some of the other geological regions but also deviate in some cases. (orig.)

  1. Oesophageal cancer in the Transkei. Determination of trace element concentrations in selected plant material by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Renan, M.J.; Drennan, B.D.; Keddy, R.J.; Sellschop, J.P.F.

    1979-01-01

    The results of the analysis by instrumental neutron activation for the concentration of trace elements in plant materials from certain areas in the Transkei region of southern Africa are presented. These areas are selected for their characteristic high or low incidence of carcinoma of the oesophagus. To broaden the suite of elements for which analysed and to overcome some of the limitations of neutron activation analysis, certain other nuclear analyses and methods are suggested which, if utilized, would increase the number of elements determined, and so improve the information available. (author)

  2. Freeze dried samples of volcanic gases - a new method for the determination of trace elements by NAA

    International Nuclear Information System (INIS)

    Bichler, M.; Sortino, F.

    1997-01-01

    A new routine technique for the determination of trace elements in volcanic gases by NAA is presented. For time and money saving reasons this method is applicable to samples, collected by the conventional method. This technique uses evacuated glass bottles, partly filled with NaOH solution to absorb acidic gas components and CO 2 , which is the main constituent of the incondensable gas fraction at ambient conditions. The application of NAA to samples collected by this method shows two main sources of difficulties: drying of NaOH without loosing volatile elements of interest (in particular Hg and Se) and the high activities of 24 Na after neutron irradiation. The first can be avoided by liquid irradiation, thereby limiting the irradiation time, the second excludes the determination of short and medium lived nuclides because of the high γ-background due to 24 Na. A new freeze drying technique enables the application of long irradiation times and therefore the use of long-lived activation products for analysis. The samples of volcanic gases were collected at the fumarole fields of La Fossa volcano on the island Vulcano. Southern Italy. This technique allows very sensitive determinations of trace elements in volcanic gases and adds highly valuable information to the understanding and modeling of volcanic gas sources. (orig.)

  3. Development of a mass spectrometrical isotope dilution analysis for determination of trace iodine levels and its application for food samples

    International Nuclear Information System (INIS)

    Schindlmeier, W.

    1984-01-01

    A mass spectrometrical isotope dilution procedure for the determination of trace amounts of iodine in various materials was developed using 129 I as indicator isotope, based on the determination of the 129 I/ 127 I isotope relationship. Negative thermionization was used as ionization method. The analysis procedure, which worked with a standard deviation of between 0,1 and 10% (depending on material tested), was used to determine the iodine level of table salt - both iodized and normal salt (3-6 ppm and less than 0,006 ppm respectively), and food samples with an organic matrix. For comparison the iodine levels were also measured with an iodine-selective electrode. Special preparation and separation procedures were done to suit the sample material. A comparison of the levels of iodine concentration in various powdered milks which were measured by international collaborators using varying methods shows the superior reproducibility of the MS-IDA. (RB) [de

  4. Trace element determination in plant material by means of instrumental neutron activation analysis (INAA) with special reference to molybdenum

    International Nuclear Information System (INIS)

    Schnier, C.; Schnug, E.

    1981-01-01

    The instrumental neutron activation analysis (INAA) permits a non-destructive multielement determination of minute trace element concentrations in organic material. No sample preparation except drying is required. Especially for the determination of molybdenum the INAA offers great advantages compared to the methods used in agricultural chemistry where complicated enrichment and extraction steps are needed. Contamination by reagents or loss of elements are not potential sources of errors. The principle, the advantages and disadvantages of INAA are described. The method is demonstrated with the example of celery samples from an experiment with five different nitrogen fertilizers on contaminated soil and of cabbage samples from an uncontaminated region. Besides molybdenum, 19 other elements (Na, K, Ca, Sc, Cr, Fe, Co, Zn, As, Se, Br, Rb, Cd, Sb, Ba, La, W, Au, Th) are determined. (orig.) [de

  5. Determination of rhenium traces in river water by Q-ICP-MS and HR-ICP-MS

    International Nuclear Information System (INIS)

    Uchida, S.; Tagami, K.; Saito, M.

    2003-01-01

    A simple separation method was applied to determine rhenium in river water using Q-ICP-MS and HR-ICP-MS. Re was concentrated from 420-925 ml river water using a TEVA resin minicolumn. Such extraction using a resin could separate Re from most sample matrices and trace elements. Almost 100% recovery was found throughout the method as determined with radioactive multitracers. The HR-ICP-MS was also used for the direct determination because of its low detection limit for Re (0.007 pg/ml). The Re concentration in the river water samples ranged from 0.9 to 6.5 pg/ml and the three analysis results showed good agreement with each other. (author)

  6. Rapid determination of benzene derivatives in water samples by trace volume solvent DLLME prior to GC-FID

    Energy Technology Data Exchange (ETDEWEB)

    Diao, Chun Peng; Wei, Chao Hai; Feng, Chun Hua [South China Univ. of Technology, Guangzhou Higher Education Mega Center (China). College of Environmental Science and Engineering; Guangdong Regular Higher Education Institutions, Guangzhou (China). Key Lab. of Environmental Protection and Eco-Remediation

    2012-05-15

    An inexpensive, simple and environmentally friendly method based on dispersive liquid liquid microextraction (DLLME) for rapid determination of benzene derivatives in water samples was proposed. A significant improvement of DLLME procedure was achieved. Trace volume ethyl acetate (60 {mu}L) was exploited as dispersion solvent instead of common ones such as methanol and acetone, the volume of which was more than 0.5 mL, and the organic solvent required in DLLME was reduced to a great extent. Only 83-{mu}L organic solvent was consumed in the whole analytic process and the preconcentration procedure was less than 10 min. The advantageous approach coupled with gas chromatograph-flame ionization detector was proposed for the rapid determination of benzene, toluene, ethylbenzene and xylene isomers in water samples. Results showed that the proposed approach was an efficient method for rapid determination of benzene derivatives in aqueous samples. (orig.)

  7. Determination of radionuclides and trace elements in marine sediments and biota from the red sea coast

    International Nuclear Information System (INIS)

    Sirelkhatim, Dia Awad

    2002-09-01

    This study presents data on the concentration levels of natural ( 226 Ra, 210 Pb, 210 Po, 238 U, 234 Th and 40 K) and artificial ( 239+240 Pu, 238 Pu, 90 Sr, 137 Cs) radionuclides as well as trace metals (Pb, Sr, Cr, Ni, V, Ba, La, Ce, Rb, Zn, Nb, As, Ti, Mn, Y, Zr, Th, U, and Ga) in multicellular marine algae, molluscs, coral in surface marine sediments collected from the shallower waters of the fringing reefs area and Flamingo Bay near Port Sudan harbour. The analyses were performed using gamma spectrometry, alpha spectrometry, liquid scintillation counting technique, Cerenkov counting technique and X RF.Surface sediments from this coastal region are poor in their trace metals and radionuclide content compared to similar data reported from different coastal areas around the globe and no source of emission has appeared to make any significant contribution. Surface enrichment of 210 Pb and 210 Po with respect to their progenitor 226 Ra is evident from the activity ratios of 210 Pb/ 226 Ra (3.03±1.79) and 210 Po/ 226 Ra (2.23±1.56) indicating sources other than in situ decay of parent nuclide. Activity concentration ranges in mBq/Kg dry weight of the artificial radionuclides studied were found to be from 5.10 to 82 ( 239+240 Pu), from 0.89 to 8.63 ( 238 Pu),and from 29.6 to 389.5 ( 90 Sr). The ratio 239+240 Pu/ 238 Pu which is used for source term identification has confirmed that the origin of anthropogenic radioactivity in the studied area is mainly the global fall-out. 137 Cs was not detected in all samples analysed. Considering 238 U, 234 Th and 40 K, their activity concentration (Bq/Kg dry weight) ranges in sediments are 2.41-6.69, 27.3-79.4 and 462-656, respectively. 234 Th/ 238 U ratio was an order of magnitude higher than unity indicating that the sediments are from high productivity area with a high biogenic flux from the adjacent water. Among marine plants and animals investigated, the coral species, Favites, show substantial concentration of radium at

  8. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Oliveira Souza, Sidnei de; Silvério Lopes da Costa, Silvânio; Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges

    2014-01-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg −1 for Mn to 77.3 mg kg −1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO 3 and H 2 O 2 ) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The ICP OES technique can be

  9. Designing towards the unknown

    DEFF Research Database (Denmark)

    Wilde, Danielle; Underwood, Jenny

    2018-01-01

    the research potential to far-ranging possibilities. In this article we unpack the motivations driving the PKI project. We present our mixed-methodology, which entangles textile crafts, design interactions and materiality to shape an embodied enquiry. Our research outcomes are procedural and methodological......New materials with new capabilities demand new ways of approaching design. Destabilising existing methods is crucial to develop new methods. Yet, radical destabilisation—where outcomes remain unknown long enough that new discoveries become possible—is not easy in technology design where complex......, to design towards unknown outcomes, using unknown materials. The impossibility of this task is proving as useful as it is disruptive. At its most potent, it is destabilising expectations, aesthetics and processes. Keeping the researchers, collaborators and participants in a state of unknowing, is opening...

  10. Determination of trace elements in standard reference materials by the ko-standardization method

    International Nuclear Information System (INIS)

    Smodis, B.; Jacimovic, R.; Stegnar, P.; Jovanovic, S.

    1990-01-01

    The k o -standardization method is suitable for routine multielement determinations by reactor neutron activation analysis (NAA). Investigation of NIST standard reference materials SRM 1571 Orchard Leaves, SRM 1572 Citrus leaves, and SRM 1573 Tomato Leaves showed the systematic error of 12 certified elements determined to be less than 8%. Thirty-four elements were determined in NIST proposed SRM 1515 Apple Leaves

  11. Trace elements in some new Romanian phytotherapeutic drugs determined by neutron activation analysis

    International Nuclear Information System (INIS)

    Preoteasa, E.A.; Salagean, M.; Pantelica, A.; Ionescu-Tirgoviste, C.

    1997-01-01

    Instrumental neutron activation analysis (INAA) has been performed on four new Romanian phytotherapeutic drugs registered us Fitolip, Fitodiab, Retinomion and Neuromion. The drugs were very well tolerated in clinical trials and are used in diabetes and other chronic diseases. They were prepared in the form of tablets made from dried powders of fruits, flowers, leaves and shells of plants used in non-conventional medicine. All four products are reach in various bioactive substances such as flavones, flavonoids, anthocyans, terpenes, rutosides, vitamins and essential fatty acids. Samples and multielemental reference materials were irradiated in a thermal neutron flux of 1.1 x 10 11 n.cm -2 .s -1 and measured with a high resolution Ge(Li) detector. 28 mineral elements were found, including Mg, K, Ca, Na and Fe at percent and sub-percent levels; Cl, Al and Mn between tens and thousands of ppm; Zn, Br, Rb and Ba up to tens of ppm; Cr, Cu, Co and V in the ppm range; and Sc, As, Sb, Cs, Lu, La, Ce, Sm, Hf, Au, Hg and Th up to hundreds of ppb. The intake of mineral elements provided by a cure of 3 pills/day shows the following: 1. None of the toxic elements As and Hg in the four drugs exceeds a noxious level; 2. Mg is the most abundant macro-element and a cure covers 15 - 60 % of the daily requirements; 3. Among essential microelements, Co may provide even more than 100% of the daily requirements; other elements may give small but significant fractions of the necessary daily amounts, e.g. 3-30% for Cr, 5-20% for Mn, and 2-10% for Fe; 4. The supply of Al, the most abundant unessential metal represents 6 - 40 % of the known daily intake. Thus a 3 pills/day cure could contribute positively to the therapy of various diseases by providing Mg, Mn, Cr (a trace element deficient in diabetes), Fe and Co, but higher daily doses could result in a Co oversupply. Further in INAA studies on biological examples from patients taking these new medicines are needed to understand the

  12. Trace elements in several species of crustaceans of Amami Island Group in Japan determined by activation analysis

    International Nuclear Information System (INIS)

    Fukushima, M.; Tamate, H.; Nakano, Y.

    2001-01-01

    Concentration levels of trace elements were determined in several species of subtropical crustaceans from Amami Islands in Japan in order to evaluate the levels of specific accumulation of elements among species. Tissue samples prepared from gill, muscle, hepatopancreas, and testis were irradiated for photon activation analysis (PAA) and neutron activation analysis (NAA). By PAA and NAA, eighteen elements could be determined. The levels of Br and I were extremely high in gills of spiny lobster and shovel-nosed lobster, respectively. A high concentration of Ag was found in the hepatopancreas of spiny lobsters collected from the Amami Island, while this element was not detected in the same species collected from Toba. The results suggest that the distribution of the trace elements in different tissues and species varies according to both species and environmental differences. To study the molecular forms of the elements in tissue, fractions that contained protein-bound elements from the hepatopancreas of spiny lobsters were separated by ultracentrifugation and gel filtration chromatography. Elution profiles of the chromatography suggest that Cu, Fe, and Se were bound to proteins, while Ag was not. (author)

  13. Determination of natural and artificial radionuclides and some trace metals in manufactured food of Syrian infant and their intake rates

    International Nuclear Information System (INIS)

    Al-Masri, M. S.; Nashawati, A.; Amin, Y.; Ibrahim, S.

    2001-06-01

    Natural and artificial radionuclides and some trace metals in some manufactured food of Syrian infant and their intake rates have been determined. Seventeen manufactured food and eleven types of canned milked, were collected from the local market, and chemically and radioactivity analyzed; radium-226, radium-228, potassium-40, lead-210, polonium-210 and trace metals (Pb, Cd, Cu, Zn) being determined. Results have shown that 210 Po concentration varied between 0.38 and 2.89 Bq/Kg in canned milk while the highest concentration in infant food was found to be 1.69 Bq/Kg; other radionuclides concentration being below the limit of detection. Total uranium concentration varied between 2.2 and 10.5 μg/Kg in milk samples and 0.78-6.0 μg/Kg in food stuff samples. In addition, concentration of Pb and Cd in all samples were found to be very low and lower than the lower of limit of detection of the analytical method. (author)

  14. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Sun Mei; Wu Qianghua

    2010-01-01

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL -1 . The relative standard deviation (n = 7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin.

  15. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun Mei, E-mail: sunmei@ustc.edu.cn [Hefei National Laboratory for Physical Sciences on Microscale, University of Science and Technology of China, No. 96, Jinzhai Road, Hefei 230026 (China); Wu Qianghua [Department of Polymer Science and Engineering, University of Science and Technology of China, Hefei 230026 (China)

    2010-04-15

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL{sup -1}. The relative standard deviation (n = 7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin.

  16. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Sun, Mei; Wu, Qianghua

    2010-04-15

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL(-1). The relative standard deviation (n=7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin. 2009 Elsevier B.V. All rights reserved.

  17. Determination of trace elements in seawater by air-flow injection/ICP-MS with chelating resin preconcentration

    International Nuclear Information System (INIS)

    Lee, Kyue-Hyung; Ohshima, Mitsuko; Motomizu, Shoji

    2002-01-01

    Multielement determination of major to trace metals in a deep seawater malt was accomplished by inductively coupled plasma-mass spectrometry (ICP-MS) together with inductively coupled plasma-atomic emission spectrometry (ICP-AES). Major elements, such as Na, K, Mg, and Ca, were measured by ICP-AES and normal continuos nebulization ICP-MS after sample dilution by 10 3 -10 6 fold. Fifteen trace elements in the concentrated metal solutions pretreated with cation-exchange resin or chelating resin could be simultaneously determined by air-flow injection/ICP-mass spectrometry (AFI/ICP-MS). Since the injection volume for AFI/ICP-MS was 25 μl, final samples volumes less than 500 μl were enough for several replicate measurements. Three different preconcentration methods assisted with AFI/ICP-MS were examined and could be successfully applied to a deep seawater malt. The analytical results of rate earth elements (REEs) and Co, Ni, Cu, Zn, Cd, and Pb obtained by AFI/ICP-MS coupled with disk filtration method using iminodiacetate (IDA)-type chelating resin were favorably agreed with the data obtained by AFI/ICP-MS coupled with column preconcentration method using chitosan-based chelating resin. (author)

  18. Stratospheric particles: Synchrotron x-ray fluorescence determination of trace element contents

    International Nuclear Information System (INIS)

    Sutton, S.R.; Flynn, G.J.

    1987-01-01

    The first trace element analyses on stratospheric particles using synchrotron x-ray fluorescence (SXRF) are reported. Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, Se and Br were detected. Concentrations for chondritic particle U2022G1 are within a factor of 1.7 of CI for all elements detected with the exception of Br which is 37 times CI. Chondritic particle W7029*A27 is also near CI for Cr, Mn, Fe, Ni, Cu, Zn and Ge but enriched in Ga, Se, and Br by factors of 5.8, 3.5 and 8.4, respectively. The third particle of the cosmic dust class also showed high Br enriched relative to CI by a factor of 28. Br was also detected at a high level in an aluminum-rich particle classified as probable artificial terrestrial contamination but exhibiting a chondritic Fe/Ni ratio. Br was not detected in a fifth particle also classified terrestrial and exhibiting a crustal Fe/Ni ratio. If the high Br has a pre-terrestrial origin, the ubiquity of the effect suggests that a large fraction of the chondritic interplanetary dust particles derive from a parent body (bodies) not sampled in the meteorite collection. 26 refs., 3 figs., 3 tabs

  19. Determination of some trace elements in Elsaraf Dam area using AAS and XRF

    International Nuclear Information System (INIS)

    Yagob, T. I.; Ahmed, T. E. A.

    2006-12-01

    To screen the plants in Elsaraf dam (Gedaref-Sudan), for their ability to uptake metal ions and the effect of seasonal rain on the availability of these metal ions for plants, trace elements in plant roots and the associated soil were studied in two seasons using atomic absorption spectroscopy and x-ray fluorescence. The nutrient elements, (Fe, Mn, Zn, Cu, Co) showed higher concentrations than toxic elements (Cr, Ni, Cd) in both plant and soil samples. Iron has the highest concentration 549/5660 and 3358/3680 mg/100 g, manganese has shown the second highest concentration followed by nickel and zinc. Copper, cobalt and chromium have shown relatively similar concentrations,while cadmium has the lowest concentration. In general, almost for all elements the soils have shown higher concentration followed by the plant. Estimation of soil/plant transfer factor (CR) that Cyperus rotandus has the highest affinity toward accumulating most of the metal ions, while the rest of plants have shown almost almost similar affinity.(Author)

  20. Ultra-trace determination of plutonium in marine samples using multi-collector inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Lindahl, Patric; Keith-Roach, Miranda; Worsfold, Paul; Choi, Min-Seok; Shin, Hyung-Seon; Lee, Sang-Hoon

    2010-06-25

    Sources of plutonium isotopes to the marine environment are well defined, both spatially and temporally, which makes Pu a potential tracer for oceanic processes. This paper presents the selection, optimisation and validation of a sample preparation method for the ultra-trace determination of Pu isotopes ((240)Pu and (239)Pu) in marine samples by multi-collector (MC) ICP-MS. The method was optimised for the removal of the interference from (238)U and the chemical recovery of Pu. Comparison of various separation strategies using AG1-X8, TEVA, TRU, and UTEVA resins to determine Pu in marine calcium carbonate samples is reported. A combination of anion-exchange (AG1-X8) and extraction chromatography (UTEVA/TRU) was the most suitable, with a radiochemical Pu yield of 87+/-5% and a U decontamination factor of 1.2 x 10(4). Validation of the method was accomplished by determining Pu in various IAEA certified marine reference materials. The estimated MC-ICP-MS instrumental limit of detection for (239)Pu and (240)Pu was 0.02 fg mL(-1), with an absolute limit of quantification of 0.11 fg. The proposed method allows the determination of ultra-trace Pu, at femtogram levels, in small size marine samples (e.g., 0.6-2.0 g coral or 15-20 L seawater). Finally, the analytical method was applied to determining historical records of the Pu signature in coral samples from the tropical Northwest Pacific and (239+240)Pu concentrations and (240)Pu/(239)Pu atom ratios in seawater samples as part of the 2008 GEOTRACES intercalibration exercise. Copyright 2010 Elsevier B.V. All rights reserved.

  1. Ultra-trace determination of plutonium in marine samples using multi-collector inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lindahl, Patric, E-mail: patriclindahl@yahoo.com [Marine Environment Research Department, Korea Ocean Research and Development Institute, 1270 Sadong, Ansan 426-744 (Korea, Republic of); School of Geography, Earth and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth PL48AA (United Kingdom); Keith-Roach, Miranda; Worsfold, Paul [School of Geography, Earth and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth PL48AA (United Kingdom); Choi, Min-Seok; Shin, Hyung-Seon [Division of Earth and Environmental Science, Korea Basic Science Institute, 113 Gwahangno, Yusung-gu, Daejon 305-333 (Korea, Republic of); Lee, Sang-Hoon [Marine Geology and Geophysics Laboratory, Korea Ocean Research and Development Institute, 1270 Sadong, Ansan 426-744 (Korea, Republic of)

    2010-06-25

    Sources of plutonium isotopes to the marine environment are well defined, both spatially and temporally, which makes Pu a potential tracer for oceanic processes. This paper presents the selection, optimisation and validation of a sample preparation method for the ultra-trace determination of Pu isotopes ({sup 240}Pu and {sup 239}Pu) in marine samples by multi-collector (MC) ICP-MS. The method was optimised for the removal of the interference from {sup 238}U and the chemical recovery of Pu. Comparison of various separation strategies using AG1-X8, TEVA, TRU, and UTEVA resins to determine Pu in marine calcium carbonate samples is reported. A combination of anion-exchange (AG1-X8) and extraction chromatography (UTEVA/TRU) was the most suitable, with a radiochemical Pu yield of 87 {+-} 5% and a U decontamination factor of 1.2 x 10{sup 4}. Validation of the method was accomplished by determining Pu in various IAEA certified marine reference materials. The estimated MC-ICP-MS instrumental limit of detection for {sup 239}Pu and {sup 240}Pu was 0.02 fg mL{sup -1}, with an absolute limit of quantification of 0.11 fg. The proposed method allows the determination of ultra-trace Pu, at femtogram levels, in small size marine samples (e.g., 0.6-2.0 g coral or 15-20 L seawater). Finally, the analytical method was applied to determining historical records of the Pu signature in coral samples from the tropical Northwest Pacific and {sup 239+240}Pu concentrations and {sup 240}Pu/{sup 239}Pu atom ratios in seawater samples as part of the 2008 GEOTRACES intercalibration exercise.

  2. Ultra-trace determination of plutonium in marine samples using multi-collector inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lindahl, Patric; Keith-Roach, Miranda; Worsfold, Paul; Choi, Min-Seok; Shin, Hyung-Seon; Lee, Sang-Hoon

    2010-01-01

    Sources of plutonium isotopes to the marine environment are well defined, both spatially and temporally, which makes Pu a potential tracer for oceanic processes. This paper presents the selection, optimisation and validation of a sample preparation method for the ultra-trace determination of Pu isotopes ( 240 Pu and 239 Pu) in marine samples by multi-collector (MC) ICP-MS. The method was optimised for the removal of the interference from 238 U and the chemical recovery of Pu. Comparison of various separation strategies using AG1-X8, TEVA, TRU, and UTEVA resins to determine Pu in marine calcium carbonate samples is reported. A combination of anion-exchange (AG1-X8) and extraction chromatography (UTEVA/TRU) was the most suitable, with a radiochemical Pu yield of 87 ± 5% and a U decontamination factor of 1.2 x 10 4 . Validation of the method was accomplished by determining Pu in various IAEA certified marine reference materials. The estimated MC-ICP-MS instrumental limit of detection for 239 Pu and 240 Pu was 0.02 fg mL -1 , with an absolute limit of quantification of 0.11 fg. The proposed method allows the determination of ultra-trace Pu, at femtogram levels, in small size marine samples (e.g., 0.6-2.0 g coral or 15-20 L seawater). Finally, the analytical method was applied to determining historical records of the Pu signature in coral samples from the tropical Northwest Pacific and 239+240 Pu concentrations and 240 Pu/ 239 Pu atom ratios in seawater samples as part of the 2008 GEOTRACES intercalibration exercise.

  3. Determination of seven trace elements in human milk, powdered cow's milk and infant foods by neutron activation analysis

    International Nuclear Information System (INIS)

    Grimanis, A.P.; Vassilaki-Grimani, M.; Alexiou, D.; Papadatos, C.

    1979-01-01

    The purpose of this study was to apply neutron activation analysis to the determination of seven trace elements (Co, Cr, Cu, Se, Zn, Rb and As) in colostrum, transitional and mature human milk as well as in powdered cow's milk and commercial infant foods, and thus to find out whether non-breast-fed infants received the same or different amounts of these trace elements as breast-fed ones. Ranges and averages for trace elements in mature human milk, expressed as microgrammes per gramme wet weight, varied as follows: Cr 0.018-0.040 and 0.027; Co 0.0013-0.0030 and 0.0020; Cu 0.38-0.50 and 0.46; Se 0.011-0.022 and 0.015; Zn 1.4-1.7 and 1.5; Rb 0.60-0.66 and 0.63; and As 0.0016-0.0060 and 0.0032. The mean concentrations of the essential trace elements Zn, Se, Cu, Cr and Co in colostrum were, respectively, 3.7, 3.2, 2.4, 1.8 and 1.7 times higher than those in mature human milk. No significant differences in Rb and As concentrations were found between colostrum and mature milk. Average values of Zn and Cu in transitional human milk were, respectively, 3.4 and 1.5 times higher than in mature milk. No significant differences for the rest of the elements were found between these two milk samples. The two milk formulas, half-cream and humanized, contained higher mean concentrations of Zn, Rb and As and similar or lower concentrations of Cr, Co and Se than mature human milk. Half-cream is deficient in Cu; mature human milk contains about 9 times more Cu than the half-cream cow's milk. Humanized milk contains a similar mean concentration of Cu as the mature milk. All examined infant foods contained similar or higher concentrations of all elements determined than did the mature human milk

  4. Microwave assisted digestion of atmospheric aerosol samples followed by inductively coupled plasma mass spectrometry determination of trace elements

    Energy Technology Data Exchange (ETDEWEB)

    Swami, K.; Judd, C.D.; Orsini, J.; Yang, K.X. [New York State Dept. of Health, Albany, NY (United States). Wadsworth Center for Labs. and Research; Husain, L. [New York State Dept. of Health, Albany, NY (United States). Wadsworth Center for Labs. and Research; Dept. of Environmental Health and Toxicology, State Univ. of New York, Albany (United States)

    2001-01-01

    A microwave digestion method in a closed vessel was developed for the determination of trace metals in atmospheric aerosols using inductively coupled plasma mass spectrometry (ICP-MS). A recovery study for the elements V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Cd, Sb, and Pb was conducted using multi-elemental standard solutions, NIST 1633b Trace Elements in Coal Fly Ash, and NIST 1648 Urban Particulate Matter. A simple digestion method using only HNO{sub 3}/H{sub 2}O{sub 2}gave good recoveries (90%-108%) for all elements except Cr in SRM 1648, but yielded low recoveries for SRM 1633b. A more robust method using HNO {sub 3}/H {sub 2}O {sub 2}/HF/H {sub 3}BO {sub 3} yielded higher recoveries (82%-103%) for the lighter elements (V - Zn) in SRM 1633b, and improved the Cr recovery in SRM 1648, but decreased the Se recovery in both SRMs. A comparative analysis of aerosol samples obtained at a remote mountain location Nathiagali, Pakistan (2.5 km above mean sea level), and Mayville, New York, downwind from the highly industrialized Midwestern United States, was carried out using Instrumental Neutron Activation Analysis (INAA) for the elements Cr, Mn, Fe, Co, Zn, As, Se, and Sb. The simple digestion method yielded excellent agreement for Cr, Fe, Zn, As, Se, and Sb, with slopes of the ICP-MS vs. INAA regressions of 0.90-1.00 and R {sup 2} values of 0.96-1.00. The regressions for Mn and Co had slopes of 0.82 and 0.84 with R {sup 2} values of 0.83 and 0.82, respectively. Addition of HF/H {sub 3}BO {sub 3} did not improve the correlation for any of the elements and degraded the precision somewhat. The technique provides sensitivity and accuracy for trace elements in relatively small aerosol samples used in atmospheric chemistry studies related to SO {sub 2} oxidation in cloud droplets. The ability to determine concentrations of a very large number of elements from a single analysis will permit source apportionment of various trace pollutants and hence strategies to control the

  5. Trace elements determination in ginseng and ginkgo biloba medicinal plants; Determinacao de elementos traco nos fitofarmacos ginseng e ginkgo biloba

    Energy Technology Data Exchange (ETDEWEB)

    Avino, Simone; Saiki, Mitiko; Fulfaro, Roberto [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil). Lab. de Analise por Ativacao Neutronica

    2002-07-01

    Determinations of trace elements in medicinal plants or in their extracts are of great interest since some elements are components of active constituents or they can affect the plant metabolism and consequently the formation of active constituents. In this work, inorganic components in medicinal drugs, Ginseng e Ginkgo Biloba provided from different laboratories, were analyzed by neutron activation analysis. Elements As, Br, Ca, Cl, Co Cr, Cs, Fe, K, La, Mg, Mn, Na, Rb, Sb, Sc, and Zn, were determined in these samples. Comparisons carried out between the results obtained for samples from different laboratories indicated distinct concentrations for several elements. These results may be attributed to the effect of soil composition and environmental conditions where these plants were cultivated. The precision and accuracy of the results were evaluated by analyzing reference materials Bowen's Kale from IUAPC and Cabbage from IAEA. (author)

  6. Determination of several trace elements in silicate rocks by an XRF method with background and matrix corrections

    International Nuclear Information System (INIS)

    Pascual, J.

    1987-01-01

    An X-ray fluorescence method for determining trace elements in silicate rock samples was studied. The procedure focused on the application of the pertinent matrix corrections. Either the Compton peak or the reciprocal of the mass absorption coefficient of the sample was used as internal standard for this purpose. X-ray tubes with W or Cr anodes were employed, and the W Lβ and Cr Kα Compton intensities scattered by the sample were measured. The mass absorption coefficients at both sides of the absorption edge for Fe (1.658 and 1.936 A) were calculated. The elements Zr, Y, Rb, Zn, Ni, Cr and V were determined in 15 international reference rocks covering wide ranges of concentration. Relative mean errors were in many cases less than 10%. (author)

  7. Determination of trace level anions in reactor cooling water by ion chromatography using a resin of low capacity

    International Nuclear Information System (INIS)

    1988-01-01

    In the field of nuclear technology, IC has been found to be one of the most versatile and efficient analytical technique because of its ability to provide a fast and sensitive analysis of anions. In this work, a separater column packed with a resin of very low capacity was used with a concentration column for the determination of low level of anions present as traces in reactor cooling water. The results of retention times and detection limits were determined using 2.4 mM Na2CO3 / 3mM NaHCO3 mixture as eluent. The interferences of cations and anions such as (Ca)2+, (UO2)2+, (SO4)2+, have been investigated

  8. Characterisation of airborne particles in the assessment of air quality: a case study for trace metal determination

    International Nuclear Information System (INIS)

    Norhayati Mohd Tahir; Poh Seng Chee; Suhaimi Suratman; Noor Azhar Mohamed Shazili; Suhaimi Hamzah; Abd Khalik Wood; Syamsiah Abd Rahman; Mhd Radzi Abas

    2005-01-01

    A study to determine the concentration of total suspended particulate (TSP) and trace metals concentration in the atmospheric particulate was done in Kuala Terengganu town. TSP was collected using high volume sampler. The sampled filter paper were subjected to microwave assisted acid digestion and the metals were determined using inductive couple plasma with optical emission spectrophotometer (ICP-OES). Results indicated a significant spatial variation but generally the TSP concentrations recorded in this study are still below the recommended Malaysia guideline for TSP. Some of the elemental composition of particulate aerosol is clearly correlation and enrichment analyses, the elements could be grouped into two; Pb, Cd and Zn group could be related to the vehicular emission sources whist the Al, Fe, Mn and Cr group appears to be crustal origin. It can also be concluded that the levels of Pb, Cd and Zn in the study area are generally lower than other cities in Malaysia. (Author)

  9. Evaluation of some procedures relevant to the determination of trace elemental components in biological materials by destructive neutron activation analysis

    International Nuclear Information System (INIS)

    Berry, D.L.

    1979-01-01

    The development of a simplified procedure for the analysis of biological materials by destructive neutron activation analysis (DNAA) is described. The sample manipulations preceding gamma ray assay were investigated as five specific stages of processing: (1) pre-irradiation treatment; (2) sample irradiation; (3) removal of the organic matrix; (4) removal of interfering radioactivities; and (5) concentration and separation of analyte activities. Each stage was evaluated with respect to susceptibility to sample contamination, loss of trace elemental components, and compatibility with other operations in the overall DNAA procedures. A complete DNAA procedure was proposed and evaluated for the analysis of standard bovine liver and blood samples. The DNAA system was effective for the determination of As, Cu, Fe, Hg, Mo, Rb, Sb, Se, and Zn without yield determinations and with a minimum turn-around time of approximately 3 days

  10. Evaluation of some procedures relevant to the determination of trace elemental components in biological materials by destructive neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Berry, D.L.

    1979-01-01

    The development of a simplified procedure for the analysis of biological materials by destructive neutron activation analysis (DNAA) is described. The sample manipulations preceding gamma ray assay were investigated as five specific stages of processing: (1) pre-irradiation treatment; (2) sample irradiation; (3) removal of the organic matrix; (4) removal of interfering radioactivities; and (5) concentration and separation of analyte activities. Each stage was evaluated with respect to susceptibility to sample contamination, loss of trace elemental components, and compatibility with other operations in the overall DNAA procedures. A complete DNAA procedure was proposed and evaluated for the analysis of standard bovine liver and blood samples. The DNAA system was effective for the determination of As, Cu, Fe, Hg, Mo, Rb, Sb, Se, and Zn without yield determinations and with a minimum turn-around time of approximately 3 days.

  11. Trace element content of human hair determined using neutron activation analysis as monitor of exposure effects to environmental metals

    International Nuclear Information System (INIS)

    Dutkiewicz, T.; Paprotny, W.; Sokolowska, D.; Kulka, E.; Woyciechowska, E.; Dybczynski, R.; Sterlinski, S.

    1978-01-01

    Determination of 17 trace elements, mainly metals, in small hair samples by neutron activation analysis was elaborated. The number of elements determined in one sample made it possible to assess quickly the exposure of human population in a given region. The hair samples after careful washing according to procedure elaborated previously were irradiated in high reactor neutron flux (approximately 10 14 n.cm -2 .s -1 ). The activities of samples were measured three times (for different decay times) by means of Ge(Li) gamma-ray spectrometer. A new version of the comparator technique, called a triple-single comparator method, was applied for quantitative analysis. The statistical methods used for planning of sampling and preliminary results on evaluation of analytical data are also described. (author)

  12. The determination of low level trace elements in coals by laser ablation-inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Booth, C.A.; Spears, D.A.; Krause, P.; Cox, A.G. [University of Sheffield, Sheffield (United Kingdom). Dept. of Earth Sciences

    1999-11-01

    The rapid determination of elements present in low level concentrations in bituminous coals is possible using laser abalation-inductively coupled plasma-mass spectrometry (l.a.-i.c.p.-m.s.). A wide range of trace elements can routinely be determined using this technique but it is for environmentally sensitive elements, such as As, Cd, Mo, Sb, Se and Hg, that it is of most use due to the low levels of detection. Calibration of the i.c.p.-m.s. was achieved using a series of uncertified coals and the method evaluated using the South African certified coals, Sarm 18, 19 and 20. A critical evaluation of the data obtained shows that for many of the elements studied the results obtained are both accurate and precise, even at very low concentrations, with the limits of detection for all of the elements being in the {mu}g/kg (parts per billion) range. 6 refs., 3 figs., 9 tabs.

  13. Worldwide Laboratory Comparison on the Determination of Trace Elements in IAEA-452 Biota Sample

    International Nuclear Information System (INIS)

    2012-01-01

    The Marine Environmental Studies Laboratory (MESL) of the International Atomic Energy Agency's Environment Laboratories (IAEA-NAEL) has the programmatic responsibility to provide assistance to Member States' laboratories in maintaining and improving the reliability of analytical measurement results, both in trace elements and organic pollutants. This is accomplished through the provision of reference materials of marine origin, validated analytical procedures, training in the implementation of internal quality control, and through the evaluation of measurement performance by the organization of worldwide and regional interlaboratory comparison exercises. For nearly thirty years, the MESL has conducted worldwide laboratory performance studies, also known as interlaboratory comparison. The results have been used to evaluate laboratory performance with respect to a wide range of organic and inorganic pollutants, including methyl mercury. This work has been conducted in collaboration with the UNEP Regional Seas Programme. The goal of interlaboratory comparison is to demonstrate the measurement capabilities of laboratories participating in interlaboratory comparisons (ILCs) and proficiency tests (PTs). The results from ILCs or PTs are of crucial interest for laboratories as these provide clear information of its measurement capabilities. It should be pointed out that the participation is either voluntary or forced by external requirements (e.g. legal, accreditation, control bodies). NAEL's interlaboratory comparison (ILC) and proficiency test (PT) schemes involve comparison of participant's results with an assigned value, which usually is delivered as a consensus value from the overall population of test results. Those exercises are designed to monitor and demonstrate the performance and analytical capabilities of the participating laboratories, and to identify gaps and problem areas where further development is needed. Continued membership has benefits in training and

  14. Determination of trace elements in fresh cow's milk in Khartoum state

    International Nuclear Information System (INIS)

    Mohammed, Elamin Mohammed Abd Allah

    2017-01-01

    Milk and its products are basic foodstuffs and constitute and important source of some vitamins and a lot of minerals. However, increasing or decreasing intake of theses minerals can be harmful. The aim of this study is to measure the concentrations of macro and trace elements in fresh cow's milk namely, Cl, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Pb, Br, Rb and Sr. A total of 40 samples of fresh cow's milk were collected from different dairy farms located around farms located around Khartoum state, 20 of them collected from cows drink ground water, while the other 20 samples their cows drink river water. Samples were then dried by freeze drying, and analyzed by energy dispersive x-ray fluorescence system. A certified reference sample, obtained from International Atomic Energy Agency was used for quality control analysis, to ensure the reliability of the device. The results obtained were expressed as (mean±uncertainty). The obtained results revealed that some elements i, e, Cl, K, Ca showed clear variation in the levels of their concentrations, compared to the relevant previous studies, which sometime found to be higher and lower than the reported values. While the trace element such as Cr, Mn, Fe, Ni, Cu, Zn, Pb, Br showed higher levels. It was observed that the milk samples of cows drink ground water had significantly higher concentration of Marco elements (Cl, K, Ca) than the milk of cows drink river water (at probability level of p-value<0.05). The elements concentration in the milk of cows drink ground water had also higher concentration of Cu and Br, and lower concentration of Fe, Zn, Pb, Rb and Sr than the milk of cows drink river water. However it is not statistically significant. Some elements such as: Cr, Mn and Ni present in high concentration in the milk of cows drink ground water, while they were not detected in the milk of cows drink river water. The statistical test one way analysis of variance (ANOVA) (at probability level of p-value<0.05) showed

  15. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

  16. Accurate determination of ultra-trace levels of Ti in blood serum using ICP-MS/MS

    International Nuclear Information System (INIS)

    Balcaen, Lieve; Bolea-Fernandez, Eduardo; Resano, Martín; Vanhaecke, Frank

    2014-01-01

    Graphical abstract: -- Highlights: •Novel method for determination of Ti at ultra-trace levels in clinical samples (serum). •Novel method based on Ti(NH 3 ) 6 + reaction product ion formation and double mass selection using recently introduced ICP-QQQ instrumentation. •Lowest limits of detection ever obtained using quadrupole-based instrumentation for Ti. •Accurate determination of basal levels of Ti in blood serum. -- Abstract: Ti is frequently used in implants and prostheses and it has been shown before that the presence of these in the human body can lead to elevated Ti concentrations in body fluids such as serum and urine. As identification of the exact mechanisms responsible for this increase in Ti concentrations, and the risks associated with it, are not fully understood, it is important to have sound analytical methods that enable straightforward quantification of Ti levels in body fluids (for both implanted and non-implanted individuals). Until now, only double-focusing sector field ICP-mass spectrometry (SF-ICP-MS) offered limits of detection that are good enough to deal with the very low basal levels of Ti in human serum. This work reports on the development of a novel method for the accurate and precise determination of trace levels of Ti in human serum samples, based on the use of ICP-MS/MS. O 2 and NH 3 /He have been compared as reaction gases. While the use of O 2 did not enable to overcome all spectral interferences, it has been shown that conversion of Ti + ions into Ti(NH 3 ) 6 + cluster ions by using NH 3 /He as a reaction gas in an ICP-QQQ-MS system, operated in MS/MS mode, provided interference-free conditions and sufficiently low limits of detection, down to 3 ng L −1 (instrumental detection limit obtained for the most abundant Ti isotope). The accuracy of the method proposed was evaluated by analysis of a Seronorm Trace Elements Serum L-1 reference material and by comparing the results obtained with those achieved by means of SF

  17. Analytical determination of traced elements in concrete samples used in nuclear reactors of the European Community

    International Nuclear Information System (INIS)

    May, S.; Piccot, D.

    1984-01-01

    In reactor dismantling residual radioacting of concrete used, especially in biological shield can brought problems for treatment and disposal. Radioactivity of concrete from reactors can be forecasted if element content is known. Elements producing long life radionuclides are: chlorine, calcium nickel, cobalt, niobium, europium and samarium. Neutron activation analysis is used for determination of these elements whithout chemical separation for Ca, Co, Eu and Sm and with radiochemical separation for Cl, Ni and Nb. A lot of elements, less interesting are also determined by gamma spectrometry after irradiation. It was possible to determine 29 elements in 21 concrete samples from different European Community reactors

  18. Determination of trace amounts of cerium in paint by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Wong, K.L.

    1981-01-01

    The determination of Ce in paint by inductively coupled plasma atomic emission spectrometry (ICP-OES) is described, and the detection limit of ICP-OES of 0.0004 ppM is compared with that of other methods. The effects of the major elemental components of paint, Si, Pb, Cr, and Na on the ICP-OES determination of Ce were studied. The interference of 400 ppM of the other ions on the determination of 10 ppM Ce was small (0 to 3% error). The method is applicable to the range of 0.2 to 700 ppM Ce

  19. Minor and trace elements in melanins determined by neutron activation analysis

    International Nuclear Information System (INIS)

    Kochanska-Dziurowicz, A.A.; Wilczok, T.; Mosulishvili, L.; Kharabadze, N.

    1986-01-01

    The presence of Au, Br, Sb, Ag, Fe, Zn, Co, Cr, Ni, Hg and Sn determined by neutron activation analysis was demonstrated in melanins isolated from human dark hair, banana peels or prepared synthetically from tyrosine. (author)

  20. Determination of rhenium (7) trace amounts by spectrophotometric titration in medium of mixed solvents

    International Nuclear Information System (INIS)

    Kuznetsov, V.V.; Samorukova, O.L.

    1978-01-01

    The method has been proposed of determining rhenium (7) microamounts by spectrophotometric titration in the medium water-dimethyl-sulphoxide with the reagent nitrochromazo. The method is based on the formation of ionic pairs K + ReO 4 - in water-organic solvents. The results of rhenium determination are satisfactory in a wide concentration range up to 0.3 mkg in 15 ml which makes the method proposed close in sensitivity to photometric methods and much better in reproducibility

  1. Spectrophotometric determination of trace and ultratrace levels of boron in silicon and chlorosilane samples

    International Nuclear Information System (INIS)

    Chen, J.S.; Lin, H.M.; Yang, M.H.

    1991-01-01

    Spectrophotometric methods for the determination of boron in the low μg/g and ng/g range in high-purity silicon and dichloro- and trichlorosilanes were investigated in detail. The procedures established involve dissolution of silicon samples and the hydrolyzed products of chlorosilane samples in hydrofluoric acid-containing reagents followed by evaporation of the silicon matrix as H 2 SiF 6 . The boron retained in the treated sample solution was then determined by a spectrophotometric method using carminic acid as a chromatic reagent. Special effort has been paid to the control of the analytical blank and reproducible determination of boron. The results indicate that addition of mannitol and proper control of the evaporation process are effective in preventing volatilization of boron during the evaporation of silicon matrix and can thus attain high recovery of boron and reproducible analysis. Through meticulous control of the analytical blank and experimental conditions, the limit of detection for boron determination with the established method can be as low as ng/g levels. Application of the methods to the determination of boron in various stages of purification of silicon and trichlorosilane as well as in borophosphosilicate film was conducted. (orig.)

  2. Trace determination of uranium and thorium in biological samples by radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Benedik, Ljudmila; Repinc, Urska; Byrne, Anthony R.; Stegnar, Peter

    2002-01-01

    Radiochemical neutron activation analysis (RNAA) is an excellent method for determining uranium and thorium; it offers unique possibilities for their ultratrace analysis using selective radiochemical separations. Regarding the favourably sensitive nuclear characteristics of uranium and of thorium with respect to RNAA, but the different half-lives of their induced nuclides, two different approaches were used. In the first approach uranium and thorium were determined separately via 239 U, 239 Np and 233 Pa. In the second approach these elements were 239 239 233 determined simultaneously in a single sample using U and/or Np and Pa. Isolation of induced nuclides was based on separation by extraction and/or anion exchange chromatography. Chemical yields were measured in each sample aliquot using added 235 U, 238 Np and 231 Pa radioisotopic tracers. (author)

  3. Determination of trace elements in seawater by neutron activation analysis and electrochemical separation

    International Nuclear Information System (INIS)

    Jorstad, K.; Salbu, B.

    1980-01-01

    The combination of neutron activation analysis and electrolysis at a constant, controlled potential has proved itself to be a useful multielement method for the determination of 28 elements in seawater. After freeze-drying and irradiation, the samples are dissolved and electrolyzed for 1 h. The radioactive species deposited on the mercury cathode allow determination of 14 elements (Ag, As, Au, Cd, Co, Cr, Fe, Ga, Hg, La, Mo, Sb, Se, Zn). Another 14 elements (Ba, Br, Ca, Ce, Cs, Eu, Na, Rb, Sc, Sm, Sr, Th, U, Yb) are quantitatively determined by measuring the activities in the residual solution. To obtain a reproducible electrolysis, radioactive tracers have been used to study the decrease of element concentrations in solution as a function of time of electrolysis, the influence of the initial element concentration on the rate constant k, the effect of cathode material and of the pH in the solution. 4 figures, 4 tables

  4. Determination of x mercury trace amounts in selected foodstuffs by neutron activation analysis

    International Nuclear Information System (INIS)

    Jiranek, V.; Bludovsky, R.

    1976-01-01

    Neutron activation analysis was used for the analysis of dehydrated milk, flour, coffee, tea and rice. The results were compared with those obtained by the photometric determination of mercury by dithizone. Four types of sample distribution by wet ashing were evaluated with regard to mercury volatilization in sample destruction. The samples were irradiated with thermal neutrons, a carrier was added and the samples were dissolved in the mixture of H 2 SO 4 +HClO 4 +HNO 3 . After dilution mercury was extracted using a substoichiometric amount of dithizone dissolved in chloroform. In the extract the radioactivity of 197 Hg was measured by NaI(Tl). At the average 15% accuracy of determination the lower limit of determination is 0.003 μg Hg. (M.K.)

  5. Analytic determination of the activation of essential and toxic trace elements in biological material

    International Nuclear Information System (INIS)

    Schelenz, R.

    1980-01-01

    A neutron activation-analysis technique for the multielement determination in biological material was developed. The individual steps of this procedure comprise radiochemical and also instrumental analytic techniques. After radiochemical separation 34 elements can be determined, after only instrumental procedures 26 elements can be detected in biological material. The radiochemical analysis of 34 elements lasts 4 days. Tracer investigations on the radionuclide retention of the anorganic separators HAP, TiP and ZP in 9N aqueous HNO 3 solution indicated that apart from Na-24, K-42 and P-32 the radionuclides Cs-134, Rb-86 and Se-75 are almost quantitatively adsorbed at the separators. For the remaining investigated radionuclides different but well-reproducible retention values resulted. The pH-value only slightly influences the extent of the radionuclide retention. Kinetic investigations on the radiochemical precipitation of some radionuclides on Cu and Cu(Hg)sub(x) were carried out. The depositing of the radionuclides Ag-110m, Hg-203 and Se-75 at 0 0 C and room temperature on Cu(Hg)sub(x) and Cu foil is a first order reaction. The half-life periods and the velocity constants of the depositing on Cu and Cu(Hg)sub(x) were determined for the investigated radionuclides in dependency of the temperature. The technique was examined by means of international biological multielement standards of known element combinations. The realisation of ring tests for the multielement determination in potatoe and milk powder showed that this method provides precise results. The applicability of the radiochemical method was confirmed by the simultaneous determination of 25 elements in overall nutrition samples. The instrumental technique was applied for the multielement determination in human hair (of the head) and in river water. (orig./MG) [de

  6. Determination of traces of silver in waters by anion exchange and atomic absorption spectrophotometry

    Science.gov (United States)

    Chao, T.T.; Fishman, M. J.; Ball, J.W.

    1969-01-01

    A method has been developed for the accurate determination of 0.1-1 ??g of silver per liter of water. The method permits stabilization of silver in water without loss to container walls. Optimum conditions have been established for the complete recovery of silver from water with an anion-exchange column, for quantitative elution of silver from the resin, and for measurement of silver by atomic absorption spectrophotometry after chelation with ammonium pyrrolidine dithiocarbamate and extraction of the chelate with MIBK. Silver in the 1-10 ??g 1 range can be determined by extraction without pre-concentration on an ion-exchange resin. ?? 1969.

  7. Determination of boron traces in water according to the Lucien Ducret method

    International Nuclear Information System (INIS)

    Isaurralde, Haydee.

    1975-11-01

    We present a method for the determination of borine in water from a nuclear reactor, based in the method of Lucien Ducret. The original procedure uses ammonium difluoride in acid medium to obtain the fluoborique anion, which reacts with methilene blue, giving a coloured compound. We propose to use sodium fluoride, instead of ammonium difluoride, to avoid the presence of free hydrofluoric acid, prooving that also in this medium we obtain the coloured compound blue methilene fluoborate. This method enables one to determine microquantities of borine. (author) [es

  8. Non-destructive determination of trace-element concentrations. Annual progress report, August 1979

    International Nuclear Information System (INIS)

    Gordon, G.E.; Zoller, W.H.; Walters, W.B.

    1979-08-01

    Development and testing of the neutron-capture prompt γ-ray activation analysis method continued. A wide range of NBS Standard Reference Materials, USGS Standard Rocks, and other materials have been analyzed in order to identify elements whose lines can be observed, to determine interferences and detection limits for each important γ ray of observable elements and to measure concentrations of observable elements for comparison with certified or other previous results. In most crustal samples, concentrations of 16 to 20 elements can be determined

  9. Determination of traces of iridium with thiodibenzoylmethane by substoichiometric isotope dilution analysis

    International Nuclear Information System (INIS)

    Roebisch, G.; Bansse, W.; Ludwig, E.

    1980-01-01

    Iridium(III or IV) reacts with thiodibenzoylmethane on heating at pH 6 to form a 1:3 complex, which can be concentrated by extraction into chloroform. Based on this reaction, a reproducible, selective determination of iridium is achieved by means of substoichiometric isotope dilution analysis, based on 192 Ir. The linear range is 1-11 nmol of iridium. (Auth.)

  10. Determination of trace amounts of hydroperoxides by column liquid chromatography and colorimetric detection

    NARCIS (Netherlands)

    Deelder, R.S.; Kroll, M.; van den Berg, J.H.M.

    1976-01-01

    The sensitive and selective determination of separated compounds in effluents from liquid chromatographic columns can be carried out by continuously adding a suitable colorimetric agent to the column effluent and continuously monitoring the absorbance of the reaction mixture. However, a considerable

  11. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  12. Monochloramine determination using NN diethyl-p-phenylene-diamine. Influence of iodide traces

    International Nuclear Information System (INIS)

    Fiquet, J.M.

    1980-09-01

    When determining ''D.P.D.'' free oxidizers, the monochloramine interfers in particular for iodide levels analogous to those likely to be found in sea water. This is not so for iodate. The zero time extrapolation of the change in colour curve is one method that enables the method to be made more selective [fr

  13. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Bentlin, Fabrina R.S.; Pozebon, Dirce; Mello, Paola A.; Flores, Erico M.M.

    2007-01-01

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO 3 ) 2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 μg g -1 of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  14. Determination of trace elements in fish by instrumental neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Awadallah, R.M.; Mohamed, A.E.; Gabr, S.A.

    1985-08-01

    INAA was utilized for the determination of Al, Au, Br, Ca, Cl, Co, Cr, Cu, Fe, I, K, Mg, Mn, Na, Rb, Sc, V and W in 12 Tilapia Nilotica samples collected from the Aswan High Dam Lake following destructive techniques. The results are tabulated.

  15. Solar UV-treatment of water samples for stripping-voltammetric determination of trace heavy metals in Awash river, Ethiopia

    Directory of Open Access Journals (Sweden)

    Gelaneh Woldemichael

    2016-03-01

    Full Text Available We report about testing a new mobile and sustainable water sample digestion method in a preliminary field trial in Ethiopia. In order to determine heavy metals at the ultra-trace level by stripping voltammetric techniques in water samples from Awash River, we applied our new method of solar UV-assisted sample pretreatment to destroy the relevant interfering dissolved organic matter. The field tests revealed that 24 h of solar UV irradiation were sufficient to achieve the same sample pretreatment results as with classic digestion method based on intense and hard UV. Analytical results of this study suggest that both a hydroelectric power station and agrichemical applications at Koka Lake have increased the levels of the investigated metals zinc, cadmium, lead, copper, cobalt, nickel, and uranium.

  16. Determination of the levels of trace elements in ten years old children from Antofagasta city, Chile by neutron activation analysis

    International Nuclear Information System (INIS)

    Gras, N.; Munoz, A.L.; Jamett J, A.; Pena C, L.; Santander M, M.

    1988-01-01

    The levels of trace elements in scalp hair of ten years old children of Antofagasta city were determined. For this study, the city was divided in convenient areas. Comparisons between levels of concentrations considering residential areas, sex, values obtained for children of Santiago, and the ranges given in the literature were established. Fifty samples of hair were analyzed by instrumental neutron activation analisis. The elements selected were: As, Br, Co, Cr, Cu, Fe, Hg, K, Na. Sb, and Zn. The effectiveness of wash procedure before irradiation was studied. Ten samples were taken with sufficient amount of hair and each was divided into two, only one of them was washed and both were analyzed. The levels of concentrations were compared. (author)

  17. Determination of trace thorium in water samples by flow injection fluorescence spectrophotometry with microcolumn on-line preconcentration

    International Nuclear Information System (INIS)

    Shen Zhuqin; Zhang Yanan; Guo Dongfa; Huang Yun

    1991-01-01

    An on-line preconcentration time resolved fluorimetric method was developed for the determination of trace thorium in water, based on luminescence of complex Th-morin-TOPO (or TRPO)-sodium lauryl sulfate in sulfuric acid medium. Interferences from companied cations, such as Al 3+ and Zr 4+ , which emit fluorescence with much slower rising rate at the same condition were effectively eliminated through optimization of the manifold parameters and precisely controlling of the elution flow rate. Effects of nearly 40 ions were also investigated. The detection limit, the liner range and relative standard deviation for 50 ng Th are 2.5 ng/L, 0∼80 ng and 3.6%, respectively. Sampling rate is 30 per hour

  18. Determination of lead element trace in some Syrian cigarettes and Its mixtures using voltammetric method on HMDE

    International Nuclear Information System (INIS)

    Nasser, H.; Kabass, H.

    2010-01-01

    This study aims for estimating of trace for these elements in various brands of Syrian Cigarettes and its mixtures, by using voltammetric method (HMDE) hanging mercury drop elec trod. This method is first used to determined Syrian Cigarettes brand and its mixtures, during this study it was found that we can use it easily with low commission, high sensitivity and accurate results comparing with others studies. We prepare the samples by using reference methods. The samples were collected during two times in one year from the same kinds of samples. We noticed that the high concentrations was (3.795μg/g) in Gitanes samples, and the low concentrations in shame samples was (0.37 μg/g). This study refers that there is different concentrations of lead element in this samples.(author)

  19. Determination of trace element level in different tissues of the leaping mullet (Liza saliens, Mugilidae) collected from Caspian Sea.

    Science.gov (United States)

    Ebrahimzadeh, Mohammad Ali; Eslami, Shahram; Nabavi, Seyed Fazel; Nabavi, Seyed Mohammad

    2011-12-01

    The concentrations of Cr, Cu, Fe, Mn, Ni, Pb, Cd, and Zn were determined in the brain, heart, liver, gill, gonad, spleen, kidney, and red and white muscles of Liza saliens (leaping mullet). Trace element levels in fish samples were analyzed by flame atomic absorption spectrometry. Among the non-essential metals, the levels of Ni and Pb in the tissues were higher than limits for fish proposed by FAO/WHO, EU, and TFC. Generally, the levels of the non-essential metals were much higher than those of manganese in the red and white muscles. Fe distribution pattern in tissues was in order of spleen > liver > heart > gill > brain > kidney > gonad > red muscle > white muscle. Red muscle was not within the safe limits for human consumption because non-essential metal (Ni, Pb) contents were higher than standard limits.

  20. Determination of trace elements in eyeshadow, face powder and rouge make-up cosmetics by neutron activation analysis

    International Nuclear Information System (INIS)

    Kanias, G.D.

    1985-01-01

    Some trace elements exist in cosmetics due to the mineral origin of their raw materials and there is no information about their concentration levels in these products. Instrumental neutron activation analysis was applied to determine the elements: cerium, cesium, europium, hafnium, lanthanum, lutetium, potassium, rubidium, samarium, scandium, sodium, tantalum, terbium, tungsten and ytterbium in eyeshadow, face powder and rouge make-up cosmetic products from the Greek market. According to the results, a wide range of values was found between the three examined cosmetics as well as between the different samples belonging to the same kind of cosmetics. This probably could be attributed to the various manufacturers of the analyzed samples. Moreover, the use of neutron activation analysis as a suitable routine method is discussed for the control of some elements which must not be contained in cosmetics. (author)

  1. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira Souza, Sidnei de [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Silvério Lopes da Costa, Silvânio [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Coordenação de Química, Universidade Federal de Alagoas (UFAL), Campus Arapiraca, 57309-005, Arapiraca, AL (Brazil); Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); and others

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg{sup −1} for Mn to 77.3 mg kg{sup −1} for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

  2. 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)

  3. Determination of Heavy and Toxic Trace Elements in Sediments of Qarun Lake Using Instrumental Neutron Activation Analysis Technique

    International Nuclear Information System (INIS)

    Hamed, A.; Abd EI-Samad, M.; Soliman, N.F.

    2011-01-01

    An investigation of certain heavy and toxic trace elements in 15 sediment samples from different areas at Qarun Lake was performed by a neutron activation technique using the neutron irradiation facilities of the Second Egyptian Research Reactor (ETRR-2). The samples together with two sets of gold foils (one bare and the other covered with cadmium) and two Standard Reference Materials IAEA (Soil-7) were irradiated at the core of the reactor in two capsules for 8520 seconds, another two capsules each has two sets of gold foils (one bare and the other covered with cadmium) are used to determine the neutron fluxes around the sediment samples. The gamma-rays of nuclides from the irradiated samples were carried out by means of a well calibrated high resolution HPGe detection system. The concentrations of product nuclides containing in the irradiated samples were determined from the peak counting-rates of the prominent gamma-ray lines for the corresponding nuclides using Single External Comparator Method (k 0 -Standardization Method) which called k 0 -NAA technique. The neutron flux ratios (f) in the same radiation sites of the sediment samples bottles were calculated as well as the cadmium ratios (R e d). MS Excel work books were constructed and used in our calculation. The total contents of As , Ba , Ca ,Co, Cr ,Cs, Eu ,Hf ,Hg,Na ,Ru ,Sc ,Se ,Sm ,Sn ,Sr ,Th ,Rb ,Zn ,and Zr in these samples were measured. The objectives .of this study were evaluated to identify the variations of concentration of some elements that have an impact on environmental pollutions. The results indicated that the concentrations of toxic trace elements of Ba, Cr, Se, Sn, Hg, Sin and Zn may represent pollutions problem

  4. Assessment and modifications of digestion procedures to determine trace elements in urine of hypertensive and diabetes mellitus patients

    Directory of Open Access Journals (Sweden)

    Awad Abdalla Momen

    2013-01-01

    Full Text Available Context: There is accumulating evidence that the metabolism of several trace elements like Cr, Cu, Pb, Cd, Co, Mn and Zn might have specific roles in the pathogenesis and progress of many diseases like hypertension (HTN and diabetes mellitus (DM. Objectives: To provide a fast, efficient, sensitive, and reliable analytical procedure for trace element determination in urine samples of HTN and DM patients using inductively coupled plasma optical emission spectrometry (ICP-OES. Setting and Design: The ICP-OES operating conditions were optimised and carefully selected in order to maximise the sensitivity, precision and accuracy. Factors affecting analytical and biological variability of the concentrations under study were discussed and carefully optimised. Materials and Methods: Different digestion procedures with acids and oxidising reagents were tested. The suitable procedure ICP-OES was selected, carefully modified and applied. The validity and accuracy of the different elements were determined by spiking of samples with known amounts of multi-element standard solution. Statistical Analysis: Student t-test and analysis of variance (ANOVA test were used for analysis. Microsoft Excel was used to assess the significance of the difference between variables. The concentrations obtained were expressed as mean value ± standard deviation (P = 0.05. Results: The results of this study showed that the mean concentrations of Cd, Zn, Pb, Cu, Cr and Mn in urine from both HTN (study group A and DM (study group B patients were higher than the corresponding values observed in the control group. However, while the mean value of Co was low as compared to the control group, the differences found were not significant (P = 0.05. Conclusion: The method used had excellent sensitivity, multi-element data could be obtained with very short acquisition time. The elements Cr, Cd, Pb and Zn might have specific roles in the pathogenesis and progress of HTN and DM. Further

  5. Determination of trace element and heavy metal in black tea and tea leaves using x-ray fluorescence

    International Nuclear Information System (INIS)

    Salih, Mohamed Abualgasim Abdalhakam

    2016-08-01

    The aim of this study was to provide information about the trace element and heavy metals concentrations in black tea and tea leaves. 23 different samples were collected from the Sudanese local market. The collected samples were characterized as the most common used items in Sudan. The concentration of trace and heavy elements were determined using x-ray fluorescence (X RF) technique. The standard reference materials (IAEA-V-10) and hay (powder) were used to evaluate the accuracy of the analytical result. The measured values were found in agreement with the certified values. The elements determined were K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Pb, Br, Rb, and Sr. The average concentration of the elements is black tea were 2277.43, 7245.71, 1.11, 1025.29, 334.29, 6.88, 11.24, 9.47, 1.02, 7.08, 97.4 and 63.21 respectively while the average concentration of the elements in leaves tea were 2644.44, 8805.56, 1.02, 571.81, 295.44, 6.19, 10.69, 9.26, 0.91, 13.42, 63.03 and 67.14 respectively. The results showed an increase in the concentration of some elements such as calcium, chromium, manganese, iron, nickel, copper, zinc, bromine, rubidium and strontium (22500, 6.75, 48.9, 194, 4.37, 9,77, 24.9, 8.23, 7.79, 40,9) ppm respectively compared to certified values. Correlation between concentration of certain element and cluster analysis were preformed and the results compared with values of literature and the concentrations of some elements found to be similar.(Author)

  6. [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.

  7. Enrichment method for trace amounts of rare earth elements using chemofiltration and XRF determination

    International Nuclear Information System (INIS)

    De Vito, I.E.; Olsina, R.A.; Masi, A.N.

    2000-01-01

    A preconcentration method for subsequent determination of rare earth elements (REE) by X-ray fluorescence (XRF) spectrometry was developed. The method is based on using (o-[3,6-disulfo-2-hydroxy-1-naphthylazo]-benzenearsonic acid) (Thorin) as a complexing agent which is retained on a polyamide membrane by a chemofiltration process. The pH dependence of the chemofiltration of these metal ions on the membrane and other variables, such as flow-rate, contact time, kinetic of complex formation, etc. were determined. The membrane containing the chemofiltrate formed a thin film, which eliminated the interelemental effects when measured by XRF. The detection limits were 23, 23 and 49 ng/mL for Sm(III), Eu(III) and Gd(III), respectively. High enrichment factors were obtained. The method was successfully applied to the preconcentration of Sm(III), Eu(III) and Gd(III) from different samples. (orig.)

  8. [Standard sample preparation method for quick determination of trace elements in plastic].

    Science.gov (United States)

    Yao, Wen-Qing; Zong, Rui-Long; Zhu, Yong-Fa

    2011-08-01

    Reference sample was prepared by masterbatch method, containing heavy metals with known concentration of electronic information products (plastic), the repeatability and precision were determined, and reference sample preparation procedures were established. X-Ray fluorescence spectroscopy (XRF) analysis method was used to determine the repeatability and uncertainty in the analysis of the sample of heavy metals and bromine element. The working curve and the metrical methods for the reference sample were carried out. The results showed that the use of the method in the 200-2000 mg x kg(-1) concentration range for Hg, Pb, Cr and Br elements, and in the 20-200 mg x kg(-1) range for Cd elements, exhibited a very good linear relationship, and the repeatability of analysis methods for six times is good. In testing the circuit board ICB288G and ICB288 from the Mitsubishi Heavy Industry Company, results agreed with the recommended values.

  9. Electroadsorption-assisted direct determination of trace arsenic without interference using transmission X-ray fluorescence spectroscopy.

    Science.gov (United States)

    Jiang, Tian-Jia; Guo, Zheng; Liu, Jin-Huai; Huang, Xing-Jiu

    2015-08-18

    An analytical technique based on electroadsorption and transmission X-ray fluorescence (XRF) for the quantitative determination of arsenic in aqueous solution with ppb-level limits of detection (LOD) is proposed. The approach uses electroadsorption to enhance the sensitivity and LOD of the arsenic XRF response. Amine-functionalized carbonaceous microspheres (NH2-CMSs) are found to be the ideal materials for both the quantitative adsorption of arsenic and XRF analysis due to the basic amine sites on the surface and their noninterference in the XRF spectrum. In electroadsorptive X-ray fluorescence (EA-XRF), arsenic is preconcentrated by a conventional three-electrode system with a positive electricity field around the adsorbents. Then, the quantification of arsenic on the adsorbents is achieved using XRF. The electroadsorption preconcentration can realize the fast transfer of arsenic from the solution to the adsorbents and improve the LOD of conventional XRF compared with directly determining arsenic solution by XRF alone. The sensitivity of 0.09 cnt ppb(-1) is obtained without the interferences from coexisted metal ions in the determination of arsenic, and the LOD is found to be 7 ppb, which is lower than the arsenic guideline value of 10 ppb given by the World Health Organization (WHO). These results demonstrated that XRF coupled with electroadsorption was able to determine trace arsenic in real water sample.

  10. Sensitive determination of trace mercury by UV-visible diffuse reflectance spectroscopy after complexation and membrane filtration-enrichment.

    Science.gov (United States)

    Yin, Changhai; Iqbal, Jibran; Hu, Huilian; Liu, Bingxiang; Zhang, Lei; Zhu, Bilin; Du, Yiping

    2012-09-30

    A simple, sensitive and selective solid phase reflectometry method is proposed for the determination of trace mercury in aqueous samples. The complexation reagent dithizone was firstly injected into the properly buffered solution with vigorous stirring, which started a simultaneous formation of nanoparticles suspension of dithizone and its complexation reaction with the mercury(II) ions to make Hg-dithizone nanoparticles. After a definite time, the mixture was filtered with membrane, and then quantified directly on the surface of the membrane by using integrating sphere accessory of the UV-visible spectrophotometer. The quantitative analysis was carried out at a wavelength of 485 nm since it yielded the largest difference in diffuse reflectance spectra before and after reaction with mercury(II).A good linear correlation in the range of 0.2-4.0 μg/L with a squared correlation coefficient (R(2)) of 0.9944 and a detection limit of 0.12 μg/L were obtained. The accuracy of the method was evaluated by the analysis of spiked mercury(II) concentrations determined using this method along with those determined by the atomic fluorescence mercury vapourmeter and the results obtained were in good agreement. The proposed method was applied to the determination of mercury in tap water and river water samples with the recovery in an acceptable range (95.7-105.3%). Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Spectrofluorimetric determination of trace amount of coenzyme II using ciprofloxacin-terbium complex as a fluorescent probe

    International Nuclear Information System (INIS)

    Bian Weiwei; Wang Yusheng; Zhu Xiaojing; Jiang Chongqiu

    2006-01-01

    A new spectrofluorimetric method was developed for the determination of trace amount of nicotinamide adenine dinucleotide phosphate (NADP). Using terbium ion (Tb 3+ )-ciprofloxacin (CIP) complex as a fluorescent probe, in the buffer solution of pH=9.00, NADP can remarkably enhance the fluorescence intensity of the Tb 3+ -CIP complex at λ=545nm and the enhanced fluorescence intensity of Tb 3+ ion is in proportion to the concentration of NADP. Optimum conditions for the determination of NADP were also investigated. The dynamic range for the determination of NADP is 4.9x10 -7 -3.7x10 -6 molL -1 with detection limit of 1.3x10 -7 molL -1 . This method is simple, practical and relatively free interference from coexisting substances and can be successfully applied to determination of NADP in synthetic water samples. Moreover, the enhancement mechanisms of the fluorescence intensity in the Tb 3+ -CIP system and the Tb 3+ -CIP-NADP system have been also discussed

  12. A critical review of nuclear activation techniques for the determination of trace elements in atmospheric aerosols, particulates and sludge samples

    International Nuclear Information System (INIS)

    Dams, R.

    1992-01-01

    Activation analysis is one of the major techniques for the determination of many minor and trace elements in a large variety of solid environmental and pollution samples, such as atmospheric aerosols, particulate emissions, fly ash, coal, incineration ash and sewage sludge, etc. Neutron activation analysis of total, inhalable or respirable airborne particulate matter collected on a filter or in a cascade impactor on some substrate, is very popular. By Instrumental Neutron Activation Analysis (INAA) up to 45 elements can be determined. The irradiation and counting procedures can be adapted to optimize the sensitivity for particular elements. The precision is largely governed by counting statistics and a high accuracy can be obtained after calibration with multi-elemental standards. Radiochemical Neutron Activation Analysis (RNAA) is applied only when extremely low limits of determination are required. Instrumental Photon Activation Analysis (IPAA) is complementary to INAA, since some elements of environmental interest can be determined which do not produce appropriate radionuclides by neutron irradiation. Charged Particle Activation Analysis (CPAA) is used in particular circumstances such as for certification purposes or coupled to radiochemical separations for extremely low concentrations. (author)

  13. Determination of volatile trace elements in terrestrial minerals and lunar soils by RNAA

    International Nuclear Information System (INIS)

    Kraehenbuehl, U.; Wegmueller, F.

    1978-01-01

    A procedure is reported for the simultaneous determination of Au, Cd, Ge, Hg, In, Sb, Te and Zn in 5-50 mg aliquots of minerals and lunar soils. After irradiation with thermal neutrons the samples are dissolved in digestion bombs by HF/HClO 4 . Sulfide precipitates provide the necessary group separations. The purified elements are measured on Ge(Li) detectors. Accuracy and precision are generally better than 10%. (author)

  14. Determination of traces of uranium in sea water after separation by froth flotation

    International Nuclear Information System (INIS)

    Sekine, K.

    1975-01-01

    Uranium in sea water is separated by froth flotation of the uranium (VI)-Arsenazo III-Zephiramine ion-adduct and then determined by neutron activation or spectrophotometric method using the uranium(IV)-Arsenazo III complex. Results of the analysis of Pacific coastal samples by the two methods are in good agreement; an average value of 3.0μg U/per liter was obtained. (author)

  15. Determination by INAA of trace elements in Fucus sample (IAEA-0140)

    International Nuclear Information System (INIS)

    Salagean, M.; Pantelica, A.; Rusu, C.; Scarlat, A.

    1998-01-01

    The concentration of 25 elements (Al, As, Ba, Br, Ca, Ce, Co, Cr, Cs, Fe, Hf, Hg, K, La, Mg, Mn, Na, Rb, Sb, Sc, Sm, Sr, Th, V, Zn) in the marine algae Fucus sp. was determined by instrumental neutron activation analysis. This paper presents our contribution to an intercomparison exercise organized by IAEA. The results obtained in our laboratory, excepting Hg, are in very good or in good agreement with the intercomparison values

  16. Determination of atmospheric trace elements by INAA: An application of receptor modelling

    International Nuclear Information System (INIS)

    Tuncel, G.; Aras, N.K.; Yatin, M.

    1992-01-01

    The concentrations of twenty-eight elements in samples of airborne particulates from Ankara or a nearby area were determined by neutron activation analysis. It is hoped to use the data to provide information on the sources of the pollution in the city and to test emission inventory and dispersion models that will be developed in the course of the study. 14 refs, 6 tabs, figs

  17. Determination of some trace elements in biological materials using the short living isotopes

    International Nuclear Information System (INIS)

    Taskaev, E.

    1985-01-01

    A method for determination of V, Cu, Rb, Mo and K in breast cancer tumors is described. Samples were irradiated with ICIS pneumatic irradiation system of University of London Reactor Centre for 5 min. with mixed neutron flux: 1,7.10 1 2 thermal neutrons.cm -2 .s -1 and 9.10 11 fast neutrons.cm -2 .s -1 . Wet ashing procedure of Byrne and Kosta was used for the dissolution. Consecutive separation procedures of V and Mo, Cu, Mn, K and Rb, followed by counting and activity measuring were carried out. In order to study the chemical yields for all the elements both animal and plant matrixes were used. The error of 3% ( 0.05 confidence level) for single determination of chemical yield was chosen as the highest value acceptable. The possibility of using 137-Cs tracer for K and Rb chemical yield determination was also checked. To check the whole procedure the standard reference materials SRM-1577 Bovine Liver, SRM-1571 Orchard Leaves and Bowen's Kale were analysed

  18. Laser ablation inductively coupled plasma mass spectrometry for the determination of trace elements in soil

    International Nuclear Information System (INIS)

    Lee Yiling; Chang Chaochiang; Jiang Shiuhjen

    2003-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been applied to the determination of Cr, Cu, Zn, Cd and Pb in soil samples. The dried soil powder was pressed into a pellet for LA-ICP-MS analysis. Triton X-100 was added to work as the modifier to enhance the ion signals. The influences of instrument operating conditions (LA and ICP-MS) and pellet preparation on the ion signals were reported. For Cr determination, the ICP-MS was operated under the dynamic reaction cell mode which alleviated the mass overlap interference. Standard addition method and isotope dilution method were used for the quantitation work. The powder sample was spiked with suitable amounts of element standards and/or enriched isotopes, well-mixed, dried and then pressed into a pellet for LA-ICP-MS analysis. This method has been applied to determine Cr, Cu, Zn, Cd and Pb in NIST SRM 2711 Montana soil and NIST SRM 2709 San Joaquin soil reference materials. The analysis results were in agreement with the certified values. The precision between sample replicates was better than 5% with LA-ICP-MS method. Detection limits estimated from standard addition curves were approximately 0.9, 2, 9, 0.7 and 0.3 ng g -1 for Cr, Cu, Zn, Cd and Pb, respectively

  19. Adsorptive Stripping Determination of Trace Nickel Using Bismuth Modified Mesoporous Carbon Composite Electrode

    Science.gov (United States)

    Ouyang, Ruizhuo; Feng, Kai; Su, Yongfu; Zong, Tianyu; Zhou, Xia; Lei, Tian; Jia, Pengpeng; Cao, Penghui; Zhao, Yuefeng; Guo, Ning; Chang, Haizhou; Miao, Yuqing; Zhou, Shuang

    Novel bismuth nanoparticle-modified mesoporous carbon (MPC) was successfully prepared on a glassy carbon electrode (Bi@MPC/GCE) for the adsorptive stripping voltammetric determination of nickel by complexing with dimethylglyoxime (DMG). The presence of MPC obviously improved the properties of Bi particles like the electron transfer ability, particle size and hydrophicility, important parameters to achieve preferable analytical performances of Bi@MPC/GCE toward Ni(II). The best electrochemical behaviors of Bi@MPC/GCE was obtained for the stripping determination of Ni(II), compared with electrodes individually modified with Bi and MPC. The synergic effect between metallic Bi and ordered MPC (forming a 3D array like Bi microelectrodes) made major contribution to such improved electrochemical properties of Bi@MPC/GCE for Ni(II) sensing. The good linear analytical curve was achieved in a Ni(II) concentration range from 0.1μM to 5.0μM with a correlation coefficient of 0.9995. The detection limit and sensitivity were calculated to be 1.2nM (S/N=3) and 1410μAmM-1cm-2, respectively. The new method was successfully applied to Ni(II) determination in soybean samples with recoveries higher than 99% and proved to be a simple, efficient alternative for Ni(II) monitoring in real samples.

  20. Determination of trace elements in uranium and aluminum by emission spectrographic methods

    Energy Technology Data Exchange (ETDEWEB)

    Chao, C N; Lee, S L; Tsai, H T

    1976-07-01

    Owing to its simplicity and sensitivity, emission spectrographic method is used to analyze the impurities in nuclear grade uranium rod and aluminum tubings for their strict specifications. With higher quantities of impurities, reactor fuel cladding, aluminum flow-tube, is analyzed by a.c. spark, point to plane method which is developed in quality control without damage for large scale samples. D.C. arc method, either carrier-distillation or without carrier, is developed to determine the limited impurities and it is especially good for analyzing irregular shaped samples. Both standard and sample are converted to oxide form and special standards matching sample matrix are not required. One of the requirements of good reactor fuel and sheathing materials is that, non-fission capture of neutrons by impurities should be held to a minimum. Some of the elements such as boron, cadmium, lithium and rare earths have very great absorption power. It has been shown by calculation that some of them should not exist more than a few parts per million or even a fraction of a part per million. Lithium seldom exists in uranium fuel rod and aluminum sheathing material and is not sought after; the determination of boron and cadmium are included in these reports. Among the carrier-distillation methods, mixture of 3 percent gallium oxide--graphite (2:1) carrier is used in uranium determination and 10 percent silver chloride--lithium fluoride (1:1) carrier is adoped in aluminum analysis. Analytical lines, concentration range and precision data are shown.

  1. Tracing the social gradient in the health of Canadians: primary and secondary determinants.

    Science.gov (United States)

    Kosteniuk, Julie G; Dickinson, Harley D

    2003-07-01

    The social gradient in heath refers to the fact that inequalities in population health status are related to inequalities in social status. This study advances and tests a model of the relationships between what we term primary and secondary determinants of the social gradient in health. The primary determinants of health include socioeconomic and demographic indicators. Secondary determinants include stressors, control, self-esteem, social support, and social involvement. Health status is indicated by measures of physical health, self-reported health status, and mental distress. Data are taken from the Canadian National Population Health (NPH) Survey (1994-1995). The study sample consists of 7720 men and 9269 women 15 to over 80 years of age. Using path analysis, we found that higher household income, being retired and growing older are significantly associated with lower stressor levels. Higher stressor levels are associated with lower levels of control, self-esteem, and social support. Higher income Canadians experience greater levels of control and social support, while older Canadians experience lower rates of social support but higher rates of social involvement. Being employed and caring for one's family are positively associated with better physical and self-reported health status. Higher household income, being retired, and aging are associated with better physical health and lower mental distress when accounting for their role in lowering stressor levels and bolstering control, self-esteem, social support, and social involvement. Replicating this study with future samples of the NPH Survey should be of benefit in ascertaining whether the social gradient in Canadians' health status shows signs of declining.

  2. Selective Rayleigh light scattering determination of trace quercetin with silver nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Usoltseva, Liliya O.; Samarina, Tatiana O. [Department of Chemistry, M.V.Lomonosov Moscow State University, 119991 GSP-1 Moscow (Russian Federation); Abramchuk, Sergei S. [Nesmeyanov Institute of Organoelement Compounds (INEOS), Russian Academy of Sciences, Vavilova 28, Moscow 119991 (Russian Federation); Prokhorova, Aleksandra F. [Department of Chemistry, M.V.Lomonosov Moscow State University, 119991 GSP-1 Moscow (Russian Federation); Beklemishev, Mikhail K., E-mail: mkb@analyt.chem.msu.ru [Department of Chemistry, M.V.Lomonosov Moscow State University, 119991 GSP-1 Moscow (Russian Federation)

    2016-11-15

    Rayleigh light scattering (RLS) is a simple technique with a high potential of sensitive determination of small organic molecules. We have found that ppb amounts of quercetin (Qu) greatly enhance the RLS of the solution of silver nanoparticles (AgNPs) stabilized with cetyltrimethylammonium bromide (CTAB) or sodium n-dodecyl sulfate (SDS). Enhancement of light scattering is observed only in the presence of an excess of AgNO{sub 3}, which implies that it is a result of nanoparticle growth; another reason for the enhanced scattering is the aggregation of AgNPs by the analyte that was confirmed by dynamic light scattering technique. The conditions were chosen for the determination of Qu in aqueous solution with the detection limits of 0.01 and 0.03 μmol L{sup −1} and linear ranges of 0.1–1.3 and 0.1–2.0 μmol L{sup −1} for SDS- and CTAB-stabilized AgNPs, respectively; the intra-day RSDs did not exceed 7%. Unexpectedly, other bioflavonoids (rutin, dihydroquercetin, and naringenin) did not change the signal of Qu and did not interfere with its determination in 1:1 M ratio (0.5 μmol L{sup −1} each). Other compounds (asparagin, uric acid, urea and some inorganic ions) were also tolerated in high amounts. - Highlights: • Low concentrations of quercetin enhance the light scattering by silver nanoparticles. • Main processes are aggregation, nanoparticle growth and formation of new particles. • Other compounds exert a weaker effect on the light scattering signal.

  3. Kinetic method of ruthenium ion traces determination, basing on the reaction of oxidation of direct blue 6B, by means of hydrogen peroxide

    International Nuclear Information System (INIS)

    Suwinska, T.; Gregorowicz, A.; Matysek-Majewska, D.

    1980-01-01

    A sensitive and selective method of determination of ruthenium ion traces (1.10 - 3 μg/cm 3 ) has been worked out. The method is based on oxidation of direct blue 6B by hydrogen peroxide under acidic conditions at pH = 0,8 - 1,2 in the presence of ruthenium ions as catalyst. The method has been applied for determination of ruthenium traces in Pt, PdCl 2 , PtCl 4 and RhCl 3 .n H 2 O. In these materials ruthenium has been determined within the range of 1,10 - 2 % - 5,10 - 4 %. (author)

  4. Determination of trace elements in cardiotonic drugs by neutron activation analysis

    International Nuclear Information System (INIS)

    Kanias, G.D.

    1980-01-01

    Potassium may be intimately involved in the action of cardiac glycosides. Chlorine and potassium also act as diuretics. The elements chlorine, manganese, potassium and sodium are determined by instrumental neutron activation analysis in the cardiotonic drugs (pills, injections, water solutions). It has been found that there is a wide variation among the different values for manganese, sodium and chlorine while for potassium values are relatively constant. Results are discussed from the pharmacological point of view. It is proposed to study the role of manganese in cardiotonic drugs as well as the effect of potassium addition in oral pharmaceutical form of cardiotonic drugs in decreasing the toxicity of cardiac glycosides. (author)

  5. Trace and essential elements determination in baby formulas milk by INAA and k0-INAA techniques

    International Nuclear Information System (INIS)

    Lylia Hamidatou; Hocine Slamene; Tarik Akhal; Alaa Boulegane

    2014-01-01

    As a part of the food analysis program executed at Es-Salam research reactor by neutron activation analysis laboratory, the concentration of As, Ba, Br, Ca, Fe, K, La, Rb and Zn in baby formulas milk have been determined by using INAA and k 0 -NAA techniques. It was found that the concentration of all elements obtained by both techniques was relatively identical for the three brands of the 0-6 and 6-12 months of analyzed samples. In addition, the analytical results have been compared with those given by producers. (author)

  6. Determination of traces of thorium in ammonium/sodium diuranate by ICP-AES method

    International Nuclear Information System (INIS)

    Nair, V.R.; Kartha, K.N.M.

    1999-01-01

    Full text: Indian Rare Earths Ltd., Alwaye, produces ammonium diuranate from the thorium concentrate, obtained during monazite processing. This process involves a series of steps. The final uranium product obtained always contains microgram amounts of thorium as impurity. An analytical procedure has been standardised for the estimation of microgram amounts of thorium in ammonium/sodium diuranate. The method involves solvent extraction of uranium by using a tertiary amine followed by the determination of thorium by ICP-AES method in the raffinate. The recoveries of thorium were checked by standard addition to the uranium matrix. Limit of detection is adequate for the analysis of nuclear grade material

  7. Grain tracing and strain determination in a Be compact tension specimen using synchrotron radiation

    International Nuclear Information System (INIS)

    Varma, R.; Green, R.; Garcia, M.D.; Satyam, P.V.; Yun, W.B.; Maser, J.; Kai, Z.; Lai, B.; Sinha, S.K.

    1999-01-01

    X-ray synchrotron radiation of high (11 KeV) energy and high flux (10 10 photons per square centimeter per second) has been used to measure strains and polycrystallinity in 6-mm thick polycrystalline beryllium compact tension (CT) specimens at and around the crack tip (for fatigue-precracked sample) or at chevron notch point under load or no-load conditions. The authors demonstrated the feasibility strain field mapping as well as determining the polycrystallinity at or near the points of maximum load in beryllium CT specimens. The experimental techniques and results will be discussed

  8. Spectrophotometric determination of uranium traces in zircaloy-4 and zirconium sponge

    International Nuclear Information System (INIS)

    Correia, R.J.; Weber de D'Alessio, Ana; Zucal, R.H.

    1980-01-01

    The uranium contents of the zircaloy-4 which is used for the fabrication of the fuel cans for the PHWR Atucha and Embalse nuclear power stations must not exceed 3.ppM. A method was developed for performing that control, involving the separation of the uranium from its matrix by partition chromatography and its determination by spectrophotometry with Arsenazo (III). This method is applied within the range of 0.2 to 10 ppM, obtaining a relative standard deviation of 6% for U contents of 3 ppm. (M.E.L.) [es

  9. Provenance determination of pottery by trace element analysis. Problems, solutions and applications

    International Nuclear Information System (INIS)

    Mommsen, H.

    2001-01-01

    Provenance determinations of pottery by chemical analysis is reviewed and shown to work well. Since pottery is produced from a well homogenized clay paste according to a certain recipe, sharp elemental patterns are expected for a series of products having the same origin. To obtain such patterns when forming compositional groups of pottery, a consideration of experimental errors, a correction for dilution and a choice of only stable elements is necessary. The patterns thus obtained will have low probability of overlap with groups of different origin. Examples for well defined groups of German stonewares and of Mycenaean wares from the Peloponnese are recorded. (author)

  10. Simultaneous determination of twelve trace elements in estuarine and sea water using pre-irradiation chromatography

    International Nuclear Information System (INIS)

    Greenberg, R.R.; Kingston, H.M.

    1982-01-01

    A procedure is described for the preconcentration of 100 m of estuarine and seawater into a solid sample using Chelex-100 resin. This solid sample weighs less than half a gram and contains the transition metals and many other elements of interest, but is essentially free from the alkali metals, the alkaline earth metals, and the halogens. The concentrations of Co, Cr, Cu, Fe, Mn, Mo, Ni, Sc, Th, U, V and Zn have been determined in seawater when this procedure was coupled to neutron activation analysis. (author)

  11. Determination of traces of lithium in biological, environmental and metal samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Yang, J.Y.; Tseng, C.L.; Lo, J.M.; Yang, M.H.

    1985-01-01

    Lithium in environmental, biological and metal samples was determined by neutron activation analysis via the 6 Li(n,α)T and 16 O(T,n) 18 F reactions. The samples were converted to aqueous solutions either by dissolution or by digestion and their aliquots were irradiated in a nuclear reactor for 2 h. The irradiated sample solution, was placed in a ZrO 2 column on which the 18 F nuclide was adsorbed. Most of the coexisting nuclides 24 Na, 82 Br, 38 Cl, 64 Cu, etc. were separated by elution with pH 1proportional3 solution. The column was subjected to a Ge(Li) detector for γ-ray spectrometry. The lithium content in the sample was estimated from the 18 F activity obtained. The matrix effect can be eliminated by either strong dilution of the samples in aqueous medium or by the method of standard addition. Lithium can be determined with high precision and accuracy in sub-ppm samples. (orig.) [de

  12. A new system for the spectrophotometric determination of trace amounts of nitrite in environmental samples

    Directory of Open Access Journals (Sweden)

    Cherian Tom

    2006-01-01

    Full Text Available A selective and rapid spectrophotometric method for the determination of nitrite is presented. It is based on the reaction of nitrite with p-nitroaniline in acid medium to form diazonium ion, which is coupled with ethoxyethylenemaleic ester or ethylcyanoacetate in basic medium to form azo dyes, showing absorption maxima at 439 and 465 nm respectively. The method obeys Beer's law in the concentration range of 0.5-16 µg mL-1 of nitrite with ethoxyethylenemaleic ester and 0.2-18 µg mL-1 of nitrite with ethylcyanoacetate. The molar absorptivity and Sandell's sensitivity of p-nitroaniline-ethoxyethylenemaleic ester and p-nitroaniline-ethylcyanoacetate azo dyes are 5.04 X 10(4 L mol-1cm-1, 0.98 X 10-2 µg cm-2 and 1.21 X 10(4 L mol-1 cm-1, 0.98 X 10-2 µg cm-2 respectively. The optimum reaction conditions and other analytical parameters were evaluated. The method was successfully applied to the determination of nitrite in various water samples and soil samples.

  13. Determination of trace elements in some Nigerian vegetable based oils by neutron activation analysis

    International Nuclear Information System (INIS)

    Obi, A.L.; Jonah, S.A.; Umar, I.

    2001-01-01

    The concentrations of some essential micronutrient elements leading to short-lived activation products in four Nigerian vegetable based oils (palm oil, palm kernel oil, sheabutter and groundnut oil) have been determined by neutron activation analysis using a small research reactor. One sample of each material was analysed and presented as an introduction for further investigations. Results indicate that the concentration range of the elements are 19.4-44.0 μg/g for Al; 30.0-81.0 μg/g for Ca; 11.9-60.4 μg/g for Cl; 1.43-5.96 μg/g for Cu; 7.3-28.1 μg/g for Mg; 0.47-1.69 μg/g for Mn; 17.5-72.8 μg/g for Na and 0.04-0.07 μg/g for V. The experimental procedure is suitable for routine determination of micronutrient element in foods for control and monitoring purposes. (author)

  14. Trace elements determination in silicon and ferrosilicon reference materials by instrumental neutron activation analysis method

    International Nuclear Information System (INIS)

    Moreira, Edson Goncalves; Vasconcellos, Marina Beatriz Agostini; Saiki, Mitiko; Iamashita, Celia Omine

    2002-01-01

    The use of certified reference materials, CRM, is of uppermost importance in the rastreability realization of the measurement process. At times, CRM use is restricted by the non existence of a suitable CRM with similarity to the sample in respect to matrix composition or with element levels in different orders of magnitude. IPT Chemical Division launched a project to prepare a metallic silicon CRM, due to the requirements of the industries in this field. To characterize this new CRM, IPEN Nuclear Reactor Center is able to perform instrumental neutron activation analysis, INAA, a very suitable method for silicon matrix samples because they produce basically the short lived radionuclide 3 1 Si under thermal neutrons flux, which after radioactive decay, does not interfere in the determination of other elements. In this paper, it is presented the determination of As, Br, Co, Cr, K, Eu, Fe, La, Mn, Na Nb, Sb, Sm, Sc, Th, Tb, U, V, W and Yb in silicon CRM NBS SRM 57; ferrosilicon CRM IPT 56; IPT 70; NBS SRM 58a; NBS SRM 59a and silicon RM under preparation IPT 132. From the results, the accuracy and the precision of the process were assessed. (author)

  15. Determination of 210Pb at ultra-trace levels in water by ICP-MS

    International Nuclear Information System (INIS)

    Lariviere, D.; Reiber, K.M.; Evans, R.D.; Cornett, R.J.

    2005-01-01

    210 Pb (t 1/2 = 22.26 years) is one of the most difficult naturally occurring radionuclides to analyze directly via radiometric measurement due to its low-energy radioactive decay. In this work, inductively coupled plasma mass spectrometry (ICP-MS) was investigated as a possible alternative to radiometric counting for the determination of 210 Pb. The formation of isobaric and polyatomic (molecular) interferences was studied and various strategies (i.e. co-precipitation, extraction chromatography, and derivatization) were tested to assess their usefulness in reducing these interferences. In addition, the potential of these strategies as pre-concentration methods was demonstrated. A 210 Pb pre-concentration of >300-fold and recoveries of 63-73% were obtained using a combined co-precipitation and extraction chromatography protocol followed by derivatization using an ethylating reagent. The abundance sensitivity at m/z = 210 in the presence of stable Pb was also investigated for three types of mass spectrometers (sector-field (ICP-SFMS), quadrupole-based (ICP-QMS), and quadrupole-based with a dynamic reaction cell (ICP-QMS (DRC))). Finally, the method was applied to determine 210 Pb in water samples and a detection limit of 90 mBq L -1 (10 pg L -1 ) was obtained

  16. Trace determination of Pu by LIF in an inductively coupled plasma

    International Nuclear Information System (INIS)

    Mauchien, P.; Briand, A.; Moulin, C.

    1989-01-01

    Inductively Coupled Plasma/Emission Spectrometry (ICP/ES) technique is largely used in the nuclear industry as an elementary analytical technique. Nevertheless, when the sample to analyse presents elements with a lot of emission spectral lines, spectral interferences lead to limited sensitivity. This is the case for Pu determination in presence of large U concentration. In pure aqueous solution, the limit of detection (LOD) for Pu is 10 μg/1. In presence of U, the LOD is determined by a ratio U/Pu = 1000. Pulsed Laser Induced Fluorescence (LIF) spectrometry is known to be a very selective technique when associated with an Inductively Coupled Plasma source. The absolute sensitivity is better by 2 or 3 orders of magnitude; its principle is based on selective excitation of the ionic species in the plasma followed by fluorescence radiation detection of these species; this radiation being practically free from spectral interferences, it is possible to improve the relative LOD. In this presentation, experimental results performed at Cogema/Marcoule laboratory are presented. After the experimental set-up description, first results of LIF are shown: - very good selectivity is effectively obtained, - a series of analytical results obtained with excitation scanning from the visible to the U.V. show that sensitivity of LIF technique is strictly related to the spectroscopic scheme

  17. Automated energy-dispersive x-ray determination of trace elements in stream sediments

    International Nuclear Information System (INIS)

    Hansel, J.M.; Martell, C.J.

    1977-01-01

    Nickel, copper, tungsten, lead, bismuth, niobium, silver, cadmium, and tin are determined in stream sediments using a computer-controlled energy-dispersive x-ray fluorescence system. The system consists of an automatic 20-position sample changer, a silicon lithium-drifted detector, a pulsed molybdenum transmission-target x-ray tube, a multichannel analyzer, and a minicomputer. Samples are analyzed as minus 325-mesh powders. A computer program positions the samples, unfolds overlapping peaks, determines peak intensities for each element, and calculates the ratio of the intensity of each peak to that of the molybdenum Kα Compton peak. Concentrations of each element are then calculated using equations obtained by analyzing prepared standards. Detection limits range from 5 ppM for silver, cadmium, lead, and bismuth to 20 ppM for niobium. The relative standard is 10 percent or less at the 100-ppM level and 20 percent at the 20-ppM level. Samples can be analyzed at the rate of sixty per day

  18. Fever of unknown origin

    International Nuclear Information System (INIS)

    Misaki, Takashi; Matsui, Akira; Tanaka, Fumiko; Okuno, Yoshishige; Mitsumori, Michihide; Torizuka, Tatsurou; Dokoh, Shigeharu; Hayakawa, Katsumi; Shimbo, Shin-ichirou

    1990-01-01

    Gallium-67 scintigraphy is a commonly performed imaging modality in deteting pyrogenic lesions in cases of long-standing inexplainable fever. To re-evaluate the significance of gallium imaging in such cases, a retrospective review was made of 56 scans performed in febrile patients in whom sufficient clinical and laboratory findings were obtained. Gallium scans were true positive in 30 patients, false positive in 3, true negative in 19, and false negative in 4. In the group of true positive, local inflammatory lesions were detected in 23 patients with a final diagnosis of lung tuberculosis, urinary tract infection, and inflammatory joint disease. Abnormal gallium accumulation, as shown in the other 7 patients, provided clues to the diagnosis of generalized disorders, such as hematological malignancies (n=3), systemic autoimmune diseases (n=3), and severe infectious mononucleosis (n=one). In the group of false positive, gallium imaging revealed intestinal excretion of gallium in 2 patients and physiological pulmonary hilar accumulation in one. In the true negative group of 19 patients, fever of unknown origin was resolved spontaneously in 12 patients, and with antibiotics and corticosteroids in 2 and 5 patients, respectively. Four patients having false negative scans were finally diagnosed as having urinary tract infection (n=2), bacterial meningitis (n=one), and polyarteritis (n=one). Gallium imaging would remain the technique of choice in searching for origin of unknown fever. It may also be useful for early diagnosis of systemic disease, as well as focal inflammation. (N.K.)

  19. Trace elements in Turkish tea leaves determined by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Demiralp, R.

    1985-01-01

    The concentrations of the elements As, Sb, Zn, Co, which are closely related to human health and disorder, was determined by means of INAA in seven of the most commonly used brands of tea. Samples and standards were irradiated 10 min and 2 hrs at pneumatic system and central thimble in the TRIGA MARK-11 research reactor. After irradiation the activities were measured with a coaxial Ge detector coupled to a spectroscopic amplifier. A Cambera 90 model multichannel analyser with an 8K memory was used for pulse hight analysis. The system has a resolution of 2,0 KeV for 1332,5 KeV gamma ray of 60 Co with peak to Compton ratio of 43:1 and efficiency of 18 relative to the 3'' x 3'' NaI(Tl) crystal. Results of the study were presented

  20. Trace elements determination in red and white wines using total-reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Anjos, M.J.; Lopes, R.T.; Jesus, E.F.O. de; Moreira, S.; Barroso, R.C.; Castro, C.R.F.

    2003-01-01

    Several wines produced in different regions from south of Brazil and available in markets in Rio de Janeiro were analyzed for their contents of elements such as: P, S, Cl, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Rb and Sr. Multi-element analysis was possible with simple sample preparation and subsequent analysis by total-reflection X-ray fluorescence using synchrotron radiation. The measurement was carried at the X-ray fluorescence beamline in the Synchrotron Light Source Laboratory in Campinas, Brazil. The levels of the various elements obtained were lower in the Brazilian wines than the values generally found in the literature. The present study indicates the capability of multi-element analysis for determining the contents of various elements present in wines coming from Brazil vineyards by using a simple, sensitive and precise method

  1. Determination of trace elements in Tillandsia usneoides by neutron activation analysis for environmental biomonitoring

    International Nuclear Information System (INIS)

    Figueiredo, A.M.G.; Saiki, M.; Ticianelli, R.B.; Domingos, M.; Alves, E.S.; Markert, B.

    2001-01-01

    Neutron activation analysis was applied to the determination of the elements Al, As, Ba, Br, Cl, Co, Cr, Fe, K, Mg, Mn, Mo, Na, Rb, Sb, Sc, Ti, Th, V, Zn and the rare earths La, Ce, Nd, Sm, Eu, Tb and Yb in the epiphytic bromeliad Tillandsia usneoides. The samples were collected at an unpolluted area and exposed in different sites of the city of Sao Paulo, Brazil, and in a control site outside Sao Paulo. The results obtained showed an accumulation of Al, As, Cr, Fe, Mo, Sb, Ti, V and Zn elements in Tillandsia usneoides exposed in polluted sites, indicating a promising potential of this species as a biomonitor of air pollution in Sao Paulo. (author)

  2. Determination of trace elements in aerosols from the antarctic peninsula by neutron activation analysis

    International Nuclear Information System (INIS)

    Loureiro, A.L.M.

    1989-01-01

    In this work the neutron activation method was applied to carry out multielemental analysis in aerosols collected in the Brazilian Station 'Comandante Ferraz', located on King George Island, at the Antarctic Peninsula, during 1986 and 1987. The aerosols were collected on 0.45 μum Millipore-MF filter paper, type HA. The analytical method was based on the simultaneous irradiations of filters and synthetic standards in the IEA-R1 nuclear reactor under a thermal neutron flux of about 10 12 n cm -2 s -1 . The induced radioactivity was measured in a gamma ray spectrometer after suitable cooling times. Samples were irradiated twice, with irradiation times varying from 5 minutes to 24 hours. The elements Na, Al, Cl, K, Ca, Sc, V, Mn, Fe, Zn, Br, Sb, La, Au and Th were determined with concentration levels from ng/m 3 to pg/m 3 [pt

  3. Non-destructive determination of trace-element concentrations. Annual progress report, September 1977

    International Nuclear Information System (INIS)

    Gordon, G.E.; Zoller, W.H.; Walters, W.B.

    1977-01-01

    Equipment has been assembled at the National Bureau of Standards (NBS) reactor by the University of Maryland group in cooperation with the NBS staff in order to initiate studies of a new analytical technique, neutron-capture prompt γ-ray activation analysis. According to this technique one observes prompt γ-rays while the sample is under neutron bombardment, rather than observing γ rays from decay of radioactive species produced. It is expected that this technique will make possible the non-destructive determination of a number of elements in several classes of samples that cannot be measured by present analytical methods. A beam thimble has been built for insertion into the reactor. A beam stop and target holder have been designed and are under construction. The detection system has been designed and is on order. The pulse-height analyzer system has been obtained and debugged and most of the software needed has been written

  4. Determination of trace metals in nuclear-grade uranium dioxide by X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Salvador, V.L.R.; Imakuma, K.

    1988-04-01

    A method is described for the simultaneous determination of low concentrations of Ca, Cr, Cu, Fe, Mn and Ni in nuclear-grade uranium dioxide by X-ray fluorescence spectrometry, without the use of chemical treatment. The lower limits of detection range from 2 μg g -1 for nickel and manganese to 5 μg g -1 for copper. Samples are prepared in the form of double-layer pellets with boric acid as a binding agent. Standards are prepared in a U 3 O 8 matrix, which is more chemically stable than UO 2 and has similar matrix behaviour. The correlation coefficients for calibration curves are better than 0.999. Erros range from 2.4 % for chromium to 6.8 % for nickel. (author) [pt

  5. Use of activation analysis method for determining trace elements in human nail clippings

    International Nuclear Information System (INIS)

    Aguiar, Amilton Reinaldo; Saiki, Mitiko

    1999-01-01

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

  6. Utilization of ICP/OES for the determination of trace metal binding to different humic fractions.

    Science.gov (United States)

    de la Rosa, G; Peralta-Videa, J R; Gardea-Torresdey, J L

    2003-02-28

    In this study, the use of inductively coupled plasma/optical emission spectrometry (ICP/OES) to determine multi-metal binding to three biomasses, Sphagnum peat moss, humin and humic acids is reported. All the investigations were performed under part per billion (ppb) concentrations. Batch pH profile experiments were performed using multi-metal solutions of Cd(II), Cu(II), Pb(II), Ni(II), Cr(III) and Cr(VI). The results showed that at pH 2 and 3, the metal affinity of the three biomasses exposed to the multi-metal solution that included Cr(III) presented the following order: Cu(II), Pb(II)>Ni(II)>Cr(III)>Cd(II). On the other hand, when Cr(VI) was in the heavy metal mixture, Sphagnum peat moss and humin showed the following affinity: Cu(II), Pb(II)>Ni(II)>Cr(VI)>Cd(II); however, the affinity of the humic acids was: Cu(II)>Pb(II), Cr(VI)>Ni(II)>Cd(II). The results demonstrated that pH values of 4 and 5 were the most favorable for the heavy metal binding process. At pH 5, all the metals, except for Cr(VI), were bound between 90 and 100% to the three biomasses. However, the binding capacity of humic acids decreased at pH 6 in the presence of Cr(VI). The results showed that the ICP/OES permits the determination of heavy metal binding to organic matter at ppb concentration. These results will be very useful in understanding the role of humic substances in the fate and transport of heavy metals, and thus could provide information to develop new methodologies for the removal of low concentrations of toxic heavy metals from contaminated waters.

  7. The determination of trace element changes in Downer Cow Syndrome by nuclear methods

    International Nuclear Information System (INIS)

    Popescu, Ion V.; Iordan, M.; Dima, Gabriel; Stihi, Claudia; Oros, C.; Badica, Teodor

    2000-01-01

    Various biomedical applications of nuclear methods (especially Particle Induced X-Ray Emission PIXE) were developed in an extensive study by Johansson and Campbell.The causes of Downer Cow Syndrome (DCS) are the metabolic and toxic perturbation. The DCS is included in the largest group of dismineralisations with some other diseases of cattle like hypomagnesaemia. It is precisely a disease generated by the superposition of some factors. One of them is the type and the chemical composition of soil and plants involved in nutrition. Other factors are the chemical processes used in food preparation as well as some technological factors like: the husbandry system and the characteristics of the locally habitation and individual factors (the species, the productive type and physiological state). The origin of this syndrome is uncertain but the clinical experience indicates that the DCS is enhanced by the hypocalcaemic paresis of parturition. The diminution of some nutritive elements from food can be a cause of DCS. The cattle are more sensitive to the diminution of P in food in comparison to the diminution of Ca. An increase of this ratio determines unfortunately the Ca absorption because of the deficit of vitamin D. In the present study the elemental and enzymatic content of blood serum samples collected from cattle that are interesting from medical reasons was determined. The results obtained in pathological animals are compared with the normal data and with literature data for similar samples obtained from healthy cattle. Blood samples are collected from jugular zone of 30 cattle. Each serum sample was divided into three samples in order to make analyses by three methods (PIXE, Inductively Coupled Plasma and spectrometry using Bessey-Lowry method). (authors)

  8. Potentiometric determination of trace amounts of volatile thiols in natural gas

    International Nuclear Information System (INIS)

    Farroha, S.M.; Habboush, A.E.; Kurthab, S.Y.

    1986-01-01

    A potentiometric titration method was developed for the determination of volatile thiols in natural gas. An apparatus was devised for the quantitative absorption of volatile thiols. The measurements were performed in an ethanolic ammonium buffer solution containing a known amount of silver nitrate as supporting electrolyte. The excess silver was precipitated by a known amount of potassium iodide. The excess of iodide was back titrated potentiometrically with a standard solution of silver nitrate. The direct titration of the excess silver ions with a standard solution of potassium iodide gave a poor accuracy compared with the back titration method. Iodide selective electrode was employed as an indicator electrode and a silver-silver chloride electrode as reference electrode. The accuracy and reproducibility of the method were established by preparing several synthetic samples in which ethanthiol containing from 346.61 to 12.11 μUg mercaptan sulfur was taken as standard nitrogen as carrier gas with an optimum flow rate of 31.5 L/hr. The results obtained expressed in the form of Grans plot showed an error ranging from 0.16 to 2.39% by weight and the relative standard deviation did not exceed 2.20%. The amount of mercaptan sulfur determined in Iraqi natural gas taken directly in a cylinder from Dora refinery, Baghdad, Iraq, and after six months of storage we 23.15 Ug/L and 21.25 Ug/L respectively with a relative standard deviation not exceeded 1%. The interferences of hydrogen sulfide could be eliminated by absorption in cadimium acetate containing solution. Other sulfur containing compounds e.g. disulfides, sulfoxides which may be present in natural gas do not interfere with the analysis

  9. TLC-spectrophometric separation and trace determination of monocrotophos and dichlorvos in enviromental and biological samples.

    Science.gov (United States)

    Janghel, Etesh K; Rai, J K; Khan, S; Rai, M K; Gupta, V K

    2007-04-01

    Organophosphorus insecticides, monocrotophos and dichlrovos are increasingly being used in agriculture to control insects on a wide range of crops. Their ready access has resulted in misuse in many instances of homicidal and suicidal poisoning cases. This paper describes about a chromogenic spray reagent for the detection/determination of monocrophos and dichlrovos in environmental and biological samples by TLC and spectrophotometric method. Monocrotophos and dichlorvos on alkaline hydrolysis yield N-methyl acetoacetamide and dichlroacetaldehyde respectively, which in turn react with diazotized p-amino acetophenone to give red-violet and red coloured compounds. Other organophosphorus insecticides do not give this reaction. Moreover, organochlorine and synthetic pyrethroid insecticides and constituents of viscera (amino acids, peptides, proteins etc), which are generally coextracted with the insecticides, do not interfere. However, phenolic compounds and hydrolysed product of carbamate insecticides may interfere and differentiate from monocrotophos and dichlrovos by Rf values. The lower limit of detection is 0.2 mg for monocrotophos and 0.1 mg for dichlorovos. The absorption maxima of the reddish-violet and red colour formed by monocrotophos and dichlrovos, are measured at 560 nm and 540 nm respectively. Beer's Law is obeyed over the concentration range of 1.2 to 6.8 mg and 6.2 to 35 mg in the final solution volume of 25 mL. The molar absorptivity and Sandell's sensitivity of monocrotophos and dichlrovos were found to be 7.1 x 10(5) (+100) 1 mole(-1) cm(-1) and 0.008 mg cm(-2), 1.2 x 10(5) 1 mole(-1) cm(-1) and 0.003 mg cm(-2) respectively. The standard deviation and relative standard deviation were found be +/- 0.005 and 2.05% +/- 0.007 and 2.02% respectively. The developed method has been successfully applied to the detection and determination of monocrotophos and dichlrovos in environmental and biological samples.

  10. Multi-actinide analysis with AMS for ultra-trace determination and small sample sizes: advantages and drawbacks

    Energy Technology Data Exchange (ETDEWEB)

    Quinto, Francesca; Lagos, Markus; Plaschke, Markus; Schaefer, Thorsten; Geckeis, Horst [Institute for Nuclear Waste Disposal, Karlsruhe Institute of Technology (Germany); Steier, Peter; Golser, Robin [VERA Laboratory, Faculty of Physics, University of Vienna (Austria)

    2016-07-01

    With the abundance sensitivities of AMS for U-236, Np-237 and Pu-239 relative to U-238 at levels lower than 1E-15, a simultaneous determination of several actinides without previous chemical separation from each other is possible. The actinides are extracted from the matrix elements via an iron hydroxide co-precipitation and the nuclides sequentially measured from the same sputter target. This simplified method allows for the use of non-isotopic tracers and consequently the determination of Np-237 and Am-243 for which isotopic tracers with the degree of purity required by ultra-trace mass-spectrometric analysis are not available. With detection limits of circa 1E+4 atoms in a sample, 1E+8 atoms are determined with circa 1 % relative uncertainty due to counting statistics. This allows for an unprecedented reduction of the sample size down to 100 ml of natural water. However, the use of non-isotopic tracers introduces a dominating uncertainty of up to 30 % related to the reproducibility of the results. The advantages and drawbacks of the novel method will be presented with the aid of recent results from the CFM Project at the Grimsel Test Site and from the investigation of global fallout in environmental samples.

  11. Spectrophotometric Determination of the Trace Amount of Thallium in Water and Urine Samples by Novel Oxidative Coupling Reaction

    Directory of Open Access Journals (Sweden)

    P. Nagaraja

    2009-01-01

    Full Text Available A novel, simple, rapid, sensitive and selective method has been proposed for the trace determination of thallium by spectrophotometric detection. This method is based on the oxidation of MBTH (3-methyl-2-benzothiazolinone hydrazone hydrochloride by thallium(III to form diazonium cation, which couples with IPH (Imipramine hydrochloride in phosphoric acid medium at room temperature giving a blue colored species having a maximum absorption at 635 nm. The reagents and manifold variables influences on the sensitivity were investigated and the optimum reaction conditions have been established. The calibration curve was found to be linear over the range 0.1-5 μg mL-1 with the molar absorptivity and Sandell’s sensitivity of 2.9x104 L mol-1 cm-1, 0.0071 μg cm-2 respectively. The tolerance limit of the method towards various ions usually associated with thallium has been detected. The relative standard deviation for five replicate determination of 2μg mL-1 thallium was 0.47%. The method has been successfully applied for the determination of thallium(ІΙΙ and thallium(I in synthetic, standard reference materials, water and urine samples with satisfactory results. The performance of the proposed method was evaluated in terms of student’s t-test and variance ratio F-test, to find out the significance of proposed method over the reported methods.

  12. Spectrophotometric determination of trace carbaryl in water and grain samples by inhibition of the rhodamine-B oxidation.

    Science.gov (United States)

    Gupta, Nirja; Pillai, Ajai Kumar; Parmar, Prachi

    2015-03-15

    A novel, sensitive, selective and simple kinetic spectrophotometric method has been developed for determination of trace levels of carbaryl based on its inhibitory effect on the oxidation of rhodamine-B by chlorine and bromine released from reaction of potassium bromate with hydrochloric acid in micellar medium. A linear relationship was observed between the inhibitory effect and the concentration of the compound. The absorbance was monitored at the maximum wavelength of 555 nm. The effect of different parameters such as pH, temperature and concentration of rhodamine-B, potassium bromate and surfactant on the reaction were investigated and optimum conditions were established. Under the selected experimental conditions, carbaryl was determined in the range of 0.04-0.4 μg mL(-1). Sandell's sensitivity and molar absorptivity were found to be 0.00055 μg cm(-2) and 3.658×10(5) L mol(-1) cm(-1) respectively. The proposed method was applied satisfactorily for the determination of carbaryl in water and different grain samples. The results were compared with those obtained by reference method and were found to be in agreement. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry.

    Science.gov (United States)

    Amin, Alaa S; El-Sharjawy, Abdel-Azeem M; Kassem, Mohammed A

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L(-1) of Tl(III) with relative standard deviation (RSD) of 1.40% (n=10). The detection and quantification limits are 150 and 495 ng L(-1) using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31×10(7) L mol(-1)cm(-1) and 0.00156 ng cm(-2), respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Determination of trace amounts of rare earth elements in various environmental samples by spark source mass spectrography

    International Nuclear Information System (INIS)

    Sugimae, Akiyoshi

    1978-01-01

    A chemical concentration-mass spectrographic procedure was described for the determination of trace amounts of rare earth elements in various environmental samples: airborne particulate matter, dustfall, soil and so forth. A 0.5 to 1 gram of sample material was decomposed by fusion with sodium carbonate. The silica dehydrated in the usual way was filtered off and the filtrate from the silica was then treated with ammonium hydroxide to precipitate the rare earth elements. After ignition of the precipitate, two ml of internal standard solution containing 20 μg/ml of silver were added and the mixture was then evaporated to dryness. The residue was mixed with an equal amount of graphite powder and then pressed into electrodes. Relative sensitivity coefficients (Ag=1.0) were determined by using Spex Mix and U. S. Geological Survey rock standard G-2. U. S. Geological Survey rock standard GSP-1 and N.B.S. coal fly ash SRM 1633 were analysed to evaluate the accuracy of the proposed method. Comparison of the mass spectral values with literature ones indicated a good agreement. The coefficient of variation obtained by replicate analysis of SRM 1633 was better than 25%. The proposed method was applied to the determination of rare earth elements in airborne particulate matter and dustfall collected on polystyrene filter and in dustjars, respectively. Results for the rare earth elements in the blank of glass fiber filter which was widely used for the collection of airborne particulate matter were also presented. (auth.)

  15. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry

    Science.gov (United States)

    Amin, Alaa S.; El-Sharjawy, Abdel-Azeem M.; Kassem, Mohammed A.

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L-1 of Tl(III) with relative standard deviation (RSD) of 1.40% (n = 10). The detection and quantification limits are 150 and 495 ng L-1 using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31 × 107 L mol-1 cm-1 and 0.00156 ng cm-2, respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples.

  16. Determination of trace platinum by supramolecular catalytic kinetic spectrofluorimetry of {beta}-cyclodextrin-platinum-KBrO{sub 3}-salicylaldehyde furfuralhydrazone

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Bo; Zhang, Ning; Chen, Zhen-Zhen; Kong, Qing-Cheng [Shandong Normal University, College of Chemistry, Chemical Engineering and Materials Science, Jinan (China)

    2006-02-01

    A supramolecular catalytic kinetic spectrofluorimetric method was developed for the determination of platinum(IV) and the possible mechanism of catalytic reaction was discussed. The method was based on the fluorescence-enhancing reaction of salicylaldehyde furfuralhydrazone (SAFH) with potassium bromate, which was catalysed by platinum(IV) in a water-ethanol medium. {beta}-Cyclodextrin ({beta}-CD) obviously sensitized the determination at pH 5.20 and 25 C. Under optimum conditions, the {beta}-CD-platinum-KBrO{sub 3}-SAFH supramolecular kinetic catalytic reaction system had excitation and emission maxima at 372 and 461 nm, respectively. The linear range of this method was 0.60-180 ng ml{sup -1} with a relative standard deviation of 1.2%, and the detection limit was 0.18 ng ml{sup -1}. Investigation of the mechanism and the effects of interferences is presented. The proposed method was applied successfully to determine trace platinum(IV) in the chemotherapeutic drug cisplatin and serum from patients with satisfactory results. (orig.)

  17. A molecularly imprinted electrochemiluminescence sensor based on the mimetic enzyme catalytic effect for ultra-trace Ni2+ determination.

    Science.gov (United States)

    Yang, Bin; Li, Jianping; Zhang, Lianming; Xu, Guobao

    2016-10-21

    A novel molecularly imprinted polymer (MIP) electrochemiluminescence (MIP-ECL) sensor was developed for the highly sensitive and selective determination of ultra-trace levels of Ni 2+ . The complex Ni 2+ -dimethylglyoxime (Ni-DMG) was chosen as the template molecule to construct the MIP and then acted as a mimetic enzyme to catalyse the oxidisation of luminol to enhance the ECL signal. When the imprinted cavities were occupied by Ni-DMG in the rebinding process, the ECL intensities produced by the luminol-H 2 O 2 ECL system on the MIP-modified electrode surface increased with increased concentration of the Ni-DMG complex. The highly sensitive determination of Ni 2+ was achieved through a catalytic reaction. This technique could be used for the quantitative analysis of Ni 2+ with concentrations from 3.0 × 10 -12 mol L -1 to 6.0 × 10 -9 mol L -1 . The detection limit was 1.01 × 10 -12 mol L -1 , which is much lower than that reported previously. In addition, the allowable amounts of interference ions in the MIP-ECL sensor were higher than that in other common molecularly imprinted sensors because of its excellent recognition of 3D cavity-to-complex molecules and ligand-to-metal ions. This method was successfully used to determine Ni 2+ in real samples, such as apples, carrots and grapes, and has been proven feasible for practical applications.

  18. Determination and correlation of spatial distribution of trace elements in normal and neoplastic breast tissues evaluated by μ-XRF

    International Nuclear Information System (INIS)

    Silva, M.P.; Oliveira, M.A.; Poletti, M.E.

    2012-01-01

    Full text: Some trace elements, naturally present in breast tissues, participate in a large number of biological processes, which include among others, activation or inhibition of enzymatic reactions and changes on cell membranes permeability, suggesting that these elements may influence carcinogenic processes. Thus, knowledge of the amounts of these elements and their spatial distribution in normal and neoplastic tissues may help in understanding the role of these elements in the carcinogenic process and tumor progression of breast cancers. Concentrations of trace elements like Ca, Fe, Cu and Zn, previously studied at LNLS using TXRF and conventional XRF, were elevated in neoplastic breast tissues compared to normal tissues. In this study we determined the spatial distribution of these elements in normal and neoplastic breast tissues using μ-XRF technique. We analyzed 22 samples of normal and neoplastic breast tissues (malignant and benign) obtained from paraffin blocks available for study at the Department of Pathology HC-FMRP/USP. From the blocks, a small fraction of material was removed and subjected to histological sections of 60 μm thick made with a microtome. The slices where placed in holder samples and covered with ultralen film. Tissue samples were irradiated with a white beam of synchrotron radiation. The samples were positioned at 45 degrees with respect to the incident beam on a table with 3 freedom degrees (x, y and z), allowing independent positioning of the sample in these directions. The white beam was collimated by a 20 μm microcapillary and samples were fully scanned. At each step, a spectrum was detected for 10 s. The fluorescence emitted by elements present in the sample was detected by a Si (Li) detector with 165 eV at 5.9 keV energy resolution, placed at 90 deg with respect to the incident beam. Results reveal that trace elements Ca-Zn and Fe-Cu could to be correlated in malignant breast tissues. Quantitative results, achieved by Spearman

  19. Studies on the determination of trace amounts of nitrogen along with alkali and alkaline earth elements in uranium based samples by ion-chromatography (IC)

    International Nuclear Information System (INIS)

    Verma, Poonam; Rastogi, R.K.; Ramakumar, K.L.

    2006-12-01

    Present report describes an ion chromatography (IC) method with suppressed conductivity detection for the determination of traces of nitrogen along with alkali and alkaline earth elements in uranium based nuclear fuels. Method was developed to determine nitrogen as NH 4 + along with alkali and alkaline earth cations by IC using a cation exchange column. (author)

  20. Closed vessel miniaturized microwave assisted chelating extraction for determination of trace metals in plant materials

    Science.gov (United States)

    Czarnecki, Sezin; Duering, Rolf-Alexander

    2013-04-01

    In recent years, the use of closed vessel microwave assisted extraction (MAE) for plant samples has shown increasing research interest which will probably substitute conventional procedures in the future due to their general disadvantages including consumption of time and solvents. The objective of this study was to demonstrate an innovative miniaturized closed vessel microwave assisted extraction (µMAE) method under the use of EDTA (µMAE-EDTA) to determine metal contents (Cd, Co, Cu, Mn, Ni, Pb, Zn) in plant samples (Lolio-Cynosuretum) by inductively coupled plasma-optical emission spectrometry (ICP-OES). Validation of the method was done by comparison of the results with another miniaturized closed vessel microwave HNO3 method (µMAE-H) and with two other macro scale MAE procedures (MAE-H and MAE-EDTA) which were applied by using a mixture of nitric acid (HNO3) and hydrogen peroxide (H2O2) (MAE-H) and EDTA (MAE-EDTA), respectively. The already established MAE-H method is taken into consideration as a reference validation MAE method for plant material. A conventional plant extraction (CE) method, based on dry ashing and dissolving of the plant material in HNO3, was used as a confidence comparative method. Certified plant reference materials (CRMs) were used for comparison of recovery rates from different extraction protocols. This allowed the validation of the applicability of the µMAE-EDTA procedure. For 36 real plant samples with triplicates each, µMAE-EDTA showed the same extraction yields as the MAE-H in the determination of Cd, Co, Cu, Mn, Ni, Pb, and Zn contents in plant samples. Analytical parameters in µMAE-EDTA should be further investigated and adapted for other metals of interest. By the reduction and elimination of the use of hazardous chemicals in environmental analysis and thus allowing a better understanding of metal distribution and accumulation process in plants and also the metal transfer from soil to plants and into the food chain, µ

  1. Cloud point extraction-fluorimetric combined methodology for the determination of trace warfarin based on the sensitization effect of supramolecule

    Energy Technology Data Exchange (ETDEWEB)

    Chang Zheng [Department of Applied Chemistry of College of Science, Xi' an University of Technology, Xi' an 710048 (China); College of Chemistry and Materials Science, Northwest University, 229 North Taibai Road, Xi' an 710069 (China); Yan Hongtao, E-mail: cz610@163.com [College of Chemistry and Materials Science, Northwest University, 229 North Taibai Road, Xi' an 710069 (China)

    2012-03-15

    Compared to the fluorescence spectra of warfarin in pure ethanol and in the presence of the nonionic surfactant Tergitol 15-S-7 after cloud point extraction (CPE), it can be seen that the fluorescence emission peak underwent an obvious red shift and the fluorescence intensity of warfarin was significantly increased in the presence of Tergitol 15-S-7. In order to confirm Tergitol 15-S-7-induced supramolecular effects, the investigations on the fluorescence quantum yields of warfarin in the micellar medium and pure ethanol were performed. The experimental results showed that the supramolecular interactions between Tergitol 15-S-7 and the warfarin excimers played a key role for improving the warfarin fluorescence properties. Based on these facts, a simple fluorometric method combined with CPE for the determination of trace warfarin was developed for the first time. Under optimized experimental conditions, the linear concentration range for warfarin was 3.0 Multiplication-Sign 1.0{sup -9}-1.0 Multiplication-Sign 10{sup -6} mol L{sup -1} and the detection limit was 3.3 Multiplication-Sign 10{sup -10} mol L{sup -1}. And, the proposed method was approved to be appropriate for monitoring warfarin in actual pharmaceutical formulations and biological fluid samples by recovery test, in comparison with other reported methods being satisfactory. - Highlights: Black-Right-Pointing-Pointer A CPE fluorescence method for trace warfarin was developed for the first time. Black-Right-Pointing-Pointer Supramolecule effects play a key role for improving the fluorescence property. Black-Right-Pointing-Pointer Notion presents an opportunity so far neglected area of CPE investigation. Black-Right-Pointing-Pointer Without previous treatment, urine species after CPE had no significant interference.

  2. Cloud point extraction-fluorimetric combined methodology for the determination of trace warfarin based on the sensitization effect of supramolecule

    International Nuclear Information System (INIS)

    Chang Zheng; Yan Hongtao

    2012-01-01

    Compared to the fluorescence spectra of warfarin in pure ethanol and in the presence of the nonionic surfactant Tergitol 15-S-7 after cloud point extraction (CPE), it can be seen that the fluorescence emission peak underwent an obvious red shift and the fluorescence intensity of warfarin was significantly increased in the presence of Tergitol 15-S-7. In order to confirm Tergitol 15-S-7-induced supramolecular effects, the investigations on the fluorescence quantum yields of warfarin in the micellar medium and pure ethanol were performed. The experimental results showed that the supramolecular interactions between Tergitol 15-S-7 and the warfarin excimers played a key role for improving the warfarin fluorescence properties. Based on these facts, a simple fluorometric method combined with CPE for the determination of trace warfarin was developed for the first time. Under optimized experimental conditions, the linear concentration range for warfarin was 3.0×1.0 −9 –1.0×10 −6 mol L −1 and the detection limit was 3.3×10 −10 mol L −1 . And, the proposed method was approved to be appropriate for monitoring warfarin in actual pharmaceutical formulations and biological fluid samples by recovery test, in comparison with other reported methods being satisfactory. - Highlights: ► A CPE fluorescence method for trace warfarin was developed for the first time. ► Supramolecule effects play a key role for improving the fluorescence property. ► Notion presents an opportunity so far neglected area of CPE investigation. ► Without previous treatment, urine species after CPE had no significant interference.

  3. Determination of Degradation Products of Cyclobenzaprine Hydrochloride, Lidocaine and Piroxicam in a Semi-Topical Formulation: MS-MS Confirmation of Unknown Impurities.

    Science.gov (United States)

    Cioroiu, Bogdan Ionel; Grigoriu, Ioana Cezara; Cioroiu, Mona Elisabeta; Niculaua, Marius; Lupuleasa, Roxana; Lazar, Mihai Ioan

    2016-07-01

    Association of cyclobenzaprine hydrochloride, piroxicam and lidocaine in a topical formulation is one of the newest innovations in the pharmaceutical formulary field. In this study, a reversed-phase liquid chromatographic method was developed for the establishment of the impurities of cyclobenzaprine hydrochloride, lidocaine and piroxicam in the semisolid topical formulation. In this study, we not only determined 2,6-dimethylaniline, 2-pyrydilamine but also specified impurities of cyclobenzaprine hydrochloride (dibenzosuberenone, amitriptyline, carbinole, cyclobenzaprine N-oxide and anthrachinone). The target compounds were determined using a mobile phase that consisted of a mixture of phosphate buffer (0.025 M; pH 6.2)-acetonitrile-methanol (60 : 13 : 27, v/v/v). A minimum of three supplementary possible degradation products were determined. Using mass spectrometry, the unspecified impurities were identified and the use of correlation matrices permitted the association with the possible source compounds. The chromatographic conditions were qualified and validated according to ICH guideline requirements to confirm specificity, linearity, accuracy and precision. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  4. Design of a novel optical sensor for determination of trace gadolinium

    International Nuclear Information System (INIS)

    Zare-Dorabei, R.; Norouzi, P.; Ganjali, M.R.

    2009-01-01

    In this work, a highly selective and sensitive gadolinium (Gd) optical sensor based on immobilization of bis(thiophenal) pyridine-2,6-diamine (BPD), on a triacetylcellulose membrane has been reported. This optode exhibits a linear range of the Gd(III) ion concentration of 2.5 x 10 -6 M with a detection limit of 0.93 x 10 -8 M. Response time of the newly designed optode was within 1-2 min, depending on the Gd(III) ion concentration. Response of the sensor is independent of solution pH in the range of 2.0-9.0. It manifests advantages of: low detection limit, fast response time, and most significantly, very good selectivity with respect to a number of lanthanide ions (La, Ce, Sm, Tm, Ho, and Eu ions). The sensor was successfully regenerated with thiourea solutions and its response was reversible and reproducible (R.S.D. less than 1.4%). This optode was applied to determine Gd(III) in synthetic and water samples, and validated with certified reference materials (CRMs).

  5. Tracing mercury pathways in Augusta Bay (southern Italy) by total concentration and isotope determination

    International Nuclear Information System (INIS)

    Bonsignore, M.; Tamburrino, S.; Oliveri, E.; Marchetti, A.; Durante, C.; Berni, A.; Quinci, E.; Sprovieri, M.

    2015-01-01

    The mercury (Hg) pollution of sediments is the main carrier of Hg for the biota and, subsequently, for the local fish consumers in Augusta Bay area (SE Sicily, Italy), a coastal marine system affected by relevant sewage from an important chlor-alkali factory. This relationship was revealed by the determination of Mass Dependent (MDF) and Mass Independent Fractionation (MIF) of Hg isotopes in sediment, fish and human hair samples. Sediments showed MDF but no MIF, while fish showed MIF, possibly due to photochemical reduction in the water column and depending on the feeding habitat of the species. Benthic and demersal fish exhibited MDF similar to that of sediments in which anthropogenic Hg was deposited, while pelagic organisms evidenced higher MDF and MIF due to photoreduction. Human hair showed high values of δ 202 Hg (offset of +2.2‰ with respect to the consumed fish) and Δ 199 Hg, both associated to fish consumption. - Highlights: • We report the Hg isotope ratios of sediments, fish and human hair in Augusta Bay. • Hg isotopes show mercury transfers from sediments to benthic and demersal fish. • MIF in fish appears to be driven by effect of photoreduction. • MIF in human hair is inherited by fish consumption. - The mercury (Hg) isotope composition of sediments, fish muscles and human hair has been investigated from the highly polluted Augusta Bay (SE Sicily, Italy)

  6. A multiresidue method for determination of trace levels of pesticides in air and water.

    Science.gov (United States)

    Millet, M; Wortham, H; Sanusi, A; Mirabel, P

    1996-11-01

    A multiresidue analytical method is described for the analysis of 13 pesticides in fogwater, rainwater, gas, and particles. This method is based upon solid-liquid extraction using Sep-Pak tC18 light cartridges for aqueous samples, soxhlet for gas (adsorbed on XAD-2) and particles (on glass fiber filters), HPLC-based fractionation of the extracted residues using a silica column, and a linear gradient of n-hexane/tert butyl methyl ether followed by GC-ECD and HPLC-UV analyses of each fraction. Prior to analysis with GC-ECD, a methylation procedure using BF3/methanol was developed for the analysis of the fraction which contains chlorophenoxy acid herbicides. The recoveries of the extraction procedure of liquid samples and of the methylation were greater than 92 and 97% with a standard deviation lower than 8 and 5%, respectively. The detection limits varied between 0.1 and 0.01 microgram.ml-1 for the 13 pesticides studied with a standard deviation less than 9%. This method was used for the determination of pesticides in 18 fogwater samples (soluble + insoluble), 31 rainwater samples, and 17 air (gas + particles) samples collected between 1991 and 1993 in Colmar (east of France).

  7. Determination of trace elements in GPC fractions of oil-sand asphaltenes by INAA

    International Nuclear Information System (INIS)

    Jacobs, F.S.; Bachelor, F.W.; Filby, R.H.

    1984-01-01

    Asphaltene samples precipitated from Athabasca and Cold Lake oil-sand bitumens were separated into 12 fractions of varying molecular weight by preparative gel permeation chromatography (GPC). Each fraction was then analyzed by analytical GPC and visible spectrometry. Concentrations of As, Ce, Co, Cr, Eu, Ga, Hf, Hg, La, Ni, Sb, Sc, Se, Sm, Tb, Th, U, V, Zn, and Zr in the fractions were determined by neutron activation analysis. Molecular weights of the Athabasca fractions are generally higher than the corresponding Cold Lake fractions. Between 58% and 90% of the metal contents occur in the high molecular weight fractions of both asphaltenes. Except for V and Cr, which show biomodel distributions, all the elements have decreasing concentrations as the molecular weight of the fraction decreases. High molecular weight fractions, constituting about 55% of the whole asphaltenes, contain nonporphyrin bound vanadium compounds. It is estimated that 27% and 31% of V present in Athabasca and Cold Lake asphaltenes respectively occur as porphyrin type compounds, including vanadyl prophyrins released from the asphaltene micelle during the separation and vanadyl porphyrins bearing high-molecular-weight substituents

  8. Determination of trace uranium in human hair by nuclear track detection technique

    International Nuclear Information System (INIS)

    Chung, Yong Sam; Moon, Jong Hwa; En, Zinaida; Cho, Seung Yeon; Kang, Sang Hoon; Lee, Jae Ki

    2001-01-01

    The aim of this study is to describe a usefulness of nuclear analytical technique in assessing and comparing the concentration levels through the analysis of uranium using human hair sample in the field of environment. A fission track detection technique was applied to determine the uranium concentration in human hair. Hair samples were collected from two groups of people - a) workers not dealing with uranium directly, and b) workers possibly contaminated with uranium. The concentration of 235 U for the first group varied from <1 to 39 ng/g and the second group can be estimated up to the level of μg/g. Radiographs of heavy-duty work samples contained high dense 'hot spots' along a single hair. After washing in acetone and distilled water, external contamination was not totally removed. Insoluble uranium compounds were not completely washed out. The (n, f)-radiography technique, having high sensitivity, and capable of getting information on uranium content at each point of a single hair, is an excellent tool for environmental monitoring

  9. [Badminton--unknown sport].

    Science.gov (United States)

    Zekan-Petrinović, Lidija

    2007-01-01

    For a long time, badminton was considered to be only a slow and light game for children, a game that is played outdoors and is structurally undemanding.Today, it is not an unknown and unrecognised sport, especially after it was included into the Olympics Games in 1992. Badminton is one of the oldest sports in the world. It is suitable for all ages (for children and elderly equally), women and men and even handicapped persons. Beginners can start playing badminton matches early because the basics are learned quickly. As a recreational activity, badminton is very popular in Zagreb. In the last 10 years, a number of halls specialized for badminton or offering badminton as one of available sports activities have been opened in Zagreb. At present, there are over 70 professional playgrounds for training of top contestants but also for the citizens who can play recreational badminton.

  10. Determination of trace elements in lichen samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Saiki, Mitiko; Coccaro, D.M.B.; Vasconcellos, M.B.A.; Marcelli, M.P.

    1999-01-01

    Epiphytic lichens have been used as bioindicators of environmental pollution studies because of their ability to accumulate metals present in the atmosphere at very low concentrations. In this work, experimental conditions for collection and preparation of the lichen samples as well as the experimental procedure for neutron activation analysis were established in order to obtain reliable and useful data for environmental monitoring purposes. Lichen samples were collected from the barks of trees. They were first examined in a stereo microscope, cleaned and then they were washed with water, freeze-dried and ground for analysis. Out of the five species Usnea sp, Parmotrena tinctorum, Canoparmelia caroliniana, Parmotrema sanctiangeli and Canoparmelia texana analysed, the latter was chosen for this work since this species is very abundant on the Brazilian territory except for the coast. The samples and synthetic standards of elements were irradiated at the IEA-R1 nuclear reactor and the concentrations of the elements Al, As, Br, Ca, Cd, Cl, Co, Cr, Cs, Fe, K, lanthanides, Mg, Mn, Na, Rb, Sb, Sc, Se, Th, U, V and Zn were determined by using short and long irradiations. Results obtained in the washed and unwashed lichen samples showed that the cleaning with water can be used in order to eliminate adhering materials. Indeed, most of elements of interest for the environmental contamination accumulated by the lichens were not removed. The study of the influence of the age of the lichen indicated that its elemental concentrations increase with its age or with the length of exposure. Results obtained for lichens collected from four different trees in the same sampling area varied from about 3.4 to 50%. The homogeneity of the sample was checked by analyzing replicates. The precision and the accuracy of the method were evaluated by analyzing IAEA 336 Lichen and NIST 1752 Citrus Leaves. (author)

  11. Determination of trace elements in lichen samples by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Saiki, Mitiko; Horimoto, Lidia K.; Vasconcellos, Marina B.A.; Marcelli, Marcelo P.; Sumita, Nairo M.; Saldiva, Paulo H.N.

    2001-01-01

    Samples of Canoparmelia texana lichen collected in different sites of Sao Paulo and Parana States, Brazil, were analysed by neutron activation analysis in order to obtain preliminary information on the air quality in these regions and also to select a region of interest for biomonitoring studies. Also Tadescantia pallida plant has been analysed in order to study the viability of using this specimen in environmental pollution monitoring. Lichens samples were collected from tree barks which were also collected to investigate the contribution of substrate derived elements to elements present in lichens. Young and old leaves of T. pallida were collected separately in order to study the leaf age effects on their elemental levels. The samples were cleaned, washed with distilled water, dried and ground for the analyses. Samples and standards were irradiated at the IEA-Rlm nuclear reactor for short and long periods and concentrations of the elements Al, As, Ca, Cd, Cl, Co, Cr, Cs, Fe, Hf, Mg, Mn, Rb, Sb, Sc, D, Th, U, V Zn and lanthanides were determined. Preliminary results obtained for T. texana lichen indicated that three sites (Ibiuna, Botanical Garden and Parque de Vila Velha) present low concentrations of the most elements analysed. Therefore lichens from these regions could be analysed to establish baseline levels of elements for monitoring purposes. Samples collected in open areas presented high concentrations of some elements probably due to the accumulation of elements originating from soil and from heavy vehicular traffic. Elemental concentrations obtained in outer barks were similar or smaller than those results obtained for lichens. Results obtained for T. pallida indicated that concentrations of elements in old leaves of this plant are of the same magnitude or slightly higher than those presented in young ones. (author)

  12. Cytochrome c biosensor for determination of trace levels of cyanide and arsenic compounds

    International Nuclear Information System (INIS)

    Fuku, Xolile; Iftikar, Faiza; Hess, Euodia; Iwuoha, Emmanuel; Baker, Priscilla

    2012-01-01

    Highlights: ► Cytochrome c biosensor for detection of KCN, As 2 O 3 and Fe 2 K (CN) was constructed. ► Detection limits in the range of 4.3–9.1 μM for the analytes were obtained using CV, SWV and EIS. ► The detection limits for the biosensor were significantly lower than current EPA and WHO guidelines. - Abstract: An electrochemical method based on a cytochrome c biosensor was developed, for the detection of selected arsenic and cyanide compounds. Boron doped diamond (BDD) electrode was used as a transducer, onto which cytochrome c was immobilised and used for direct determination of Prussian blue, potassium cyanide and arsenic trioxide. The sensitivity as calculated from cyclic voltammetry (CV) and square wave voltammetry (SWV), for each analyte in phosphate buffer (pH = 7) was found to be in the range of (1.1–4.5) × 10 −8 A μM −1 and the detection limits ranged from 4.3 to 9.1 μM. The biosensor is therefore able to measure significantly lower than current Environmental Protection Agency (EPA) and World Health Organisation (WHO) guidelines, for these types of analytes. The protein binding was monitored as a decrease in biosensor peak currents by SWV and as an increase in biosensor charge transfer resistance by electrochemical impedance spectroscopy (EIS). EIS provided evidence that the electrocatalytic advantage of BDD electrode was not lost upon immobilisation of cytochrome c. The interfacial kinetics of the biosensor was modelled as equivalent electrical circuit based on electrochemical impedance spectroscopy data. UV–vis spectroscopy was used to confirm the binding of the protein in solution by monitoring the intensity of the soret bands and the Q bands. FTIR was used to characterise the protein in the immobilised state and to confirm that the protein was not denatured upon binding to the pre-treated bare BDD electrode. SNFTIR of cyt c immobilised at platinum electrode, was used to study the effect of oxidation state on the surface bond

  13. Application of Spectroscopic Techniques for the Determination of Trace Element Concentrations in some Sudanese vegetables and fruits

    International Nuclear Information System (INIS)

    Ahmed, A. N.; Ali, A. H.; Eltayeb, M. A. H.; Othman, M. M.; Taha, K. K.

    2004-01-01

    The objectives of this study were to determine the levels of the mineral nutrients, especially of trace elements, in some food items commonly consumed in Sudan and to compare the results of this work with local and international data. Food samples of fruits and vegetables were collected from different localities in Sudan. The samples were then prepared and their Br, Ca, Co, Cu, Fe, Mg, Mn, P, Pb, Na, Rb, Sr, and Zn content were determined using Atomic absorption spectroscopy (AAS), X-ray fluorescence spectroscopy (XRF), flame photometry and colorimetry. Verified standards TDD-1D and Hay-9 (supplied by the IAEA) were measured using the techniques mentioned above for accuracy. The Sudanese food items analyzed were found to contain considerable ranges of nutrients as follows: - Concentration levels for some of these elements Ca, Cu and Fe show higher values in fruits (4709, 21, and 633 ppm, respectively), and lower in vegetables (4094, 13, and 255 ppm , respectively). Pb and Mn were higher in vegetables (2 and 32 ppm, respectively) and lower in fruits (1 and 18 ppm) respectively). Na and Zn were higher in vegetables (3149 and 26 ppm, respectively) and lower in fruits (269 and 13 ppm, respectively). The values obtained agree, in general, with data available from other countries. Variations were observed among certain varieties of food. (Authors)

  14. Determination of trace amounts of Brown HT as a food dye by a CPE-scanometry method

    Directory of Open Access Journals (Sweden)

    A. Shokrollahi

    2017-01-01

    Full Text Available In this study, trace amounts of Brown HT were extracted, pre-concentrated and determined by cloud point extraction-scanometry (CPE-scanometry as a simple, fast and inexpensive method. The procedure is based on CPE of Brown HT from an aqueous solution, diluting the extracted surfactant-rich phase with ethanol to 500 μL, transferring the appropriate volume to Plexiglas® cells and scanning the cells. Then, the colour of each cell was analyzed by software written in visual basic (VB 6 into red, green and blue values. Effective parameters for the extraction efficiency, such as the pH of the system, the concentration of surfactant, the equilibration temperature and equilibration time, were investigated and optimized. Under optimal conditions, the calibration curve was linear in the range of 0.06–2.60 mg L−1. The detection limit of the proposed method was 0.04 mg L−1. In addition, the effects of some foreign species, including cations, anions and dyes, were investigated. The method was applied successfully for the determination of Brown HT in some water samples.

  15. Utility of solid phase spectrophotometry for the modified determination of trace amounts of cadmium in food samples.

    Science.gov (United States)

    Amin, Alaa S; Gouda, Ayman A

    2012-05-01

    A modified selective, highly sensitive and accurate procedure for the determination of trace amounts of cadmium which reacts with 1-(2-benzothiazolylazo)-2-hydroxy-3-naphthoic acid (BTAHNA) to give a deep violet complex with high molar absorptivity (7.05×10(6)Lmol(-1) cm(-1), 3.92×10(7)Lmol(-1)cm(-1), 1.78×10(8)Lmol(-1)cm(-1), and 4.10×10(8)Lmol(-1)cm(-1)), fixed on a Dowex 1-X8 type anion-exchange resin for 10mL, 100mL, 500mL, and 1000mL, respectively. Calibration is linear over the range 0.2-3.5μgL(-1) with RSD of ⩽1.14% (n=10). The detection and quantification limits were calculated. Increasing the sample volume can enhance the sensitivity. The method has been successfully applied for the determination of Cd(II) in food samples, water samples and some salts samples without interfering effect of various cations and anions. Copyright © 2011 Elsevier Ltd. All rights reserved.

  16. Development of a procedure for the multi-element determination of trace elements in wine by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Castineira, M.M.; Brandt, R.; von Bohlen, A.; Jakubowski, N. [Institut fuer Spektrochemie und Angewandte Spektroskopie e.V., Dortmund (Germany)

    2001-07-01

    An inductively coupled plasma mass spectrometric (ICP-MS) procedure has been developed for the determination of trace elements in wine. The procedure consists in simple 1+1 dilution of the wine and semi-quantitative analysis (without external calibration) using In as internal standard. Thirty-one elements at concentrations ranging from 0.1 mg mL{sup -1} to 0.5 ng mL{sup -1} can be determined by ICP-MS analysis with and without digestion. It was investigated whether a matrix effect observed for EtOH in the wine matrix can be overcome by application of a micro-concentric nebulizer with a membrane desolvator (MCN 6000). The results obtained for the MCN 6000 are compared with those obtained by use of a conventional Meinhard nebulizer. It is shown that the observed matrix effect can only be compensated by use of an internal standard for the Meinhard nebulizer, but not for the MCN 6000. Results for ICP-MS are compared with those obtained by total reflection X-ray fluorescence spectrometry (TXRF). (orig.)

  17. A new method for the determination of NO2 traces using isotope dilution and mass spectrometry analysis

    International Nuclear Information System (INIS)

    Stevens, C.; Barat, F.; Nguyen Nghi, H.

    1975-01-01

    A new method for the determination of NO 2 traces, in the order of 1ppb (10 -9 ), in atmosphere and stratosphere is described. The method consists in an isotope dilution technique using 15 NO 2 , followed by the reduction of NO 2 to N 2 and a mass spectrometry analysis. A known amount of 15 NO 2 is added to the air samples. Then, NO 2 is separated from H 2 O, HNO 3 , CO 2 and N 2 O and transferred to a SiO 2 reactor by trapping at -196 deg C. In the reactor NO 2 is reduced to N 2 by reaction with electrolytic Cu heated at 580 deg C. The mass 29/mass 30 ratio corresponding to 15 N 14 N and 15 N 15 N is determined by mass spectrometry. The sensitivity of the method depends on the contamination introduced during the analysis of the sample (reagents, separation and measuring devices). The contamination is reproducible and in the order of 4.5+-0.5 10 -2 mm 3 N 2 [fr

  18. Highly sensitive sorption-luminescence determination of trace europium with preconcentration on silica chemically modified with iminodiacetic acid

    International Nuclear Information System (INIS)

    Voronina, R.D.; Zorov, N.B.

    2007-01-01

    Features of a sorption-luminescence method for the determination of trace europium were studied. The method includes the preliminary sorption of europium at pH 7.1 from solutions with silica chemically modified with iminodiacetic acid, the subsequent treatment of the sorbent with 2-thenoyltrifluoroacetone at pH 8.0, and the measurement of the intensity of luminescence of the surface three-component europium complex at 613 nm. The effect of moisture as the quencher of luminescence of the surface europium complex was studied, and techniques for its removal were proposed. Sorption in the static mode provides the detection limit of europium of 7 x 10 -5 g/ml. The calibration plot is linear in the range of two orders of magnitude of europium concentration in solutions. The relative standard deviation in the determination of 1.5 x 10 -2 μg/ml europium is 5%. In the dynamic mode of sorption from 1000 ml of an analyzed solution with the use of sorption-desorption, the detection limit of europium of 8 x 10 -7 μg/ml was attained [ru

  19. Trace determination of the flame retardant tetrabromobisphenol A in the atmosphere by gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Xie Zhiyong; Ebinghaus, Ralf; Lohmann, Rainer; Heemken, Olaf; Caba, Armando; Puettmann, Wilhelm

    2007-01-01

    A simple and effective method has been developed for analysis of the flame retardant tetrabromobisphenol A (TBBPA) in environmental samples by using modified soxhlet extraction in combination with silica gel clean-up, derivatization with silylation reagent and gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). Satisfactory recoveries were achieved for the large volume sampling, soxhlet extraction and silica gel clean-up. The overall recovery is 79 ± 1%. The derivatization procedure is simple and fast, and produces stable TBBPA derivative. GC-MS with electronic impact (EI) ionization mode shows better detection power than using negative chemical ionization (NCI) mode. EI gives a method detection limit of 0.04 pg m -3 and enables to determine trace TBBPA in ambient air in remote area. The method was successfully applied to the determination of TBBPA in atmospheric samples collected over land and coastal regions. The concentrations of TBBPA ranged from below the method detection limit (0.04 pg m -3 ) to 0.85 pg m -3 . A declining trend with increasing latitude was present from the Wadden Sea to the Arctic. The atmospheric occurrence of TBBPA in the Arctic is significant and might imply that TBBPA has long-range transport potential

  20. Determination of trace mercury in water based on N-octylpyridinium ionic liquids preconcentration and stripping voltammetry.

    Science.gov (United States)

    Li, Zhenhan; Xia, Shanhong; Wang, Jinfen; Bian, Chao; Tong, Jianhua

    2016-01-15

    A novel method for determination of trace mercury in water is developed. The method is performed by extracting mercury firstly with ionic liquids (ILs) and then detecting the concentration of mercury in organic media with anodic stripping voltammetry. Liquid-liquid extraction of mercury(II) ions by four ionic liquids with N-octylpyridinium cations ([OPy](+)) was studied. N-octylpyridinium tetrafluoroborate and N-octylpyridinium trifluoromethylsulfonate were found to be efficient and selective extractant for mercury. Temperature controlled dispersive liquid phase microextraction (TC-DLPME) technique was utilized to improve the performance of preconcentration. After extraction, precipitated IL was diluted by acetonitrile buffer and mercury was detected by differential pulse stripping voltammetry (DPSV) with gold disc electrode. Mercury was enriched by 17 times while interfering ions were reduced by two orders of magnitude in the organic media under optimum condition. Sensitivity and selectivity for electrochemical determination of mercury were improved by using the proposed method. Tap, pond and waste water samples were analyzed with recoveries ranging from 81% to 107% and detection limit of 0.05 μg/L. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Determination of trace concentrations of chlorine in aqueous solutions by high-resolution continuum source graphite furnace molecular absorption spectrometry

    Science.gov (United States)

    Machyňák, Ľubomír; Čacho, František; Němeček, Martin; Beinrohr, Ernest

    2016-11-01

    Trace concentrations of total chlorine were determined by means of molecular absorption of indium mono-chloride (InCl) at 267.217 nm using high-resolution continuum source graphite furnace molecular absorption spectrometry. The effects of chemical modifiers and the amount of In on the sensitivity and accuracy were investigated. The optimum pyrolysis and vaporization temperatures were 600 °C and 1400 °C, respectively. The limit of detection and characteristic mass were found to be 0.10 ng and 0.21 ng, respectively. Potential non-spectral and spectral interferences were tested for various metals and non-metals at concentrations up to 50 mg L- 1 and for phosphoric, sulphuric and nitric acids. No spectral interferences were observed. Significant non-spectral interferences were observed with F, Br, and I at concentrations higher than 1 mg L- 1, 5 mg L- 1 and 25 mg L- 1, respectively, which is probably caused by formation of competitive indium halogen molecules. Higher concentrations of mineral acids depressed the signal owing to the formation of volatile HCl. The calibration curve was linear in the range between 0.3 and 10 ng with a correlation coefficient of R = 0.993. The elaborated method was used for the chlorine determination in various waters and a drug sample.

  2. A simple and selective spectrophotometric flow injection determination of trace amounts of ruthenium by catalytic oxidation of safranin-O

    Energy Technology Data Exchange (ETDEWEB)

    Rezaei, Behzad [Department of Chemistry, Isfahan University of Technology, Isfahan 84156-84111 (Iran, Islamic Republic of)], E-mail: rezaei@cc.iut.ac.ir; Keyvanfard, Mohsen [Faculty of Science, Majlesi Campus, Islamic Azad University, Isfahan (Iran, Islamic Republic of)

    2008-03-01

    In this work, a simple, selective and rapid flow injection method has been developed for determination of ruthenium. The method is based on its catalytic effect on the oxidation of safranin-O by metaperiodate. The reaction was monitored spectrophotometrically by measuring safranin-O absorbance at {lambda}{sub max} = 521. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine ruthenium in the ranges of 0.4-20.0 ng/mL ({delta}A = 0.2819C{sub Ru} + 1.1840) and 20.0-100.0 ng/mL ({delta}A = 0.0984C{sub Ru} + 7.9391) with a detection limit of 0.095 ng/mL and a sample rate of 30 {+-} 5 samples/h. Relative standard deviation for the five replicate measurements was less than 1.84%. The proposed method has been successfully applied for analysis of ultra trace amounts of ruthenium in real samples.

  3. A simple and selective spectrophotometric flow injection determination of trace amounts of ruthenium by catalytic oxidation of safranin-O

    International Nuclear Information System (INIS)

    Rezaei, Behzad; Keyvanfard, Mohsen

    2008-01-01

    In this work, a simple, selective and rapid flow injection method has been developed for determination of ruthenium. The method is based on its catalytic effect on the oxidation of safranin-O by metaperiodate. The reaction was monitored spectrophotometrically by measuring safranin-O absorbance at λ max = 521. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine ruthenium in the ranges of 0.4-20.0 ng/mL (ΔA = 0.2819C Ru + 1.1840) and 20.0-100.0 ng/mL (ΔA = 0.0984C Ru + 7.9391) with a detection limit of 0.095 ng/mL and a sample rate of 30 ± 5 samples/h. Relative standard deviation for the five replicate measurements was less than 1.84%. The proposed method has been successfully applied for analysis of ultra trace amounts of ruthenium in real samples

  4. Multielement determination of trace elements in seawater by inductively coupled plasma mass spectrometry after tandem preconcentration with cooperation of chelating resin adsorption and lanthanum coprecipitation

    International Nuclear Information System (INIS)

    Yabutani, Tomoki; Chiba, Koichi; Haraguchi, Hiroki

    2001-01-01

    A tandem preconcentration method, in which chelating resin adsorption and La coprecipitation were cooperatively employed for preconcentration, was developed as a pretreatment method for simultaneous multielement determination of trace elements in seawater by ICP-MS. First, the seawater sample (250 ml) was treated with a chelating resin for preconcentration of trace elements, and then trace elements with good recoveries were determined by ICP-MS. Trace elements with the chemical properties of oxoanion- and hydride-formation, which were poorly recovered in the chelating resin preconcentration, were further subjected to preconcentration by La coprecipitation. As a result, more than 30 elements could be determined in the concentration range from 9.6 μg L -1 for Mo to 0.00018 μg L -1 for Tm, when the present tandem method was applied to the analysis of open seawater standard reference material (NASS-4). Furthermore, the analytical results for open seawater reference materials were compared with those for coastal seawater reference material as well as for coastal seawater collected in the Ise Bay. It was found that the multielement data for trace elements in these seawater samples clearly showed different elemental distributions, reflecting the different marine environments. (author)

  5. Utilization of thermoluminescent dosemeters for determination of exposure or absorbed dose in a radiation gamma or X radiation field with unknown spectral distribution

    International Nuclear Information System (INIS)

    Rosa, L.A.R. da.

    1981-06-01

    Having in view the choice of the best pair of dosemeters to be used in the 'Tandem' method, the main response characteristics of LiF:Mg, Ti, Li 2 B 4 O 7 :Mn, CaSO 4 Dy, CaF 2 :Mn and CaF 2 :Dy thermoluminescent dosemeters and also some critical parameters in their calibration and evaluation processes were studied. Three different physical forms of TLD's were investigated: hot pressed chips, disc teflon dosemeters and glass mini TLD's. Their calibration factors were obtained for the energy of Cobalt-60 gamma rays. Their energy dependences normalized to 60 Co radiation were determined using spectral width as parameter. 'Tandens' formed by all TLD's evaluated were compaired. (E.G.) [pt

  6. Determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by ICP-OES

    Science.gov (United States)

    Yong, Cheng

    2018-03-01

    The method that direct determination of 18 kinds of trace impurities in the vanadium battery grade vanadyl sulfate by inductively coupled plasma atomic emission spectrometry (ICP-OES) was established, and the detection range includes 0.001% ∼ 0.100% of Fe, Cr, Ni, Cu, Mn, Mo, Pb, As, Co, P, Ti, Zn and 0.005% ∼ 0.100% of K, Na, Ca, Mg, Si, Al. That the influence of the matrix effects, spectral interferences and background continuum superposition in the high concentrations of vanadium ions and sulfate coexistence system had been studied, and then the following conclusions were obtained: the sulfate at this concentration had no effect on the determination, but the matrix effects or continuous background superposition which were generated by high concentration of vanadium ions had negative interference on the determination of potassium and sodium, and it produced a positive interference on the determination of the iron and other impurity elements, so that the impacts of high vanadium matrix were eliminated by the matrix matching and combining synchronous background correction measures. Through the spectral interference test, the paper classification summarized the spectral interferences of vanadium matrix and between the impurity elements, and the analytical lines, the background correction regions and working parameters of the spectrometer were all optimized. The technical performance index of the analysis method is that the background equivalent concentration -0.0003%(Na)~0.0004%(Cu), the detection limit of the element is 0.0001%∼ 0.0003%, RSD<10% when the element content is in the range from 0.001% to 0.007%, RSD< 20% even if the element content is in the range from 0.0001% to 0.001% that is beyond the scope of the method of detection, recoveries is 91.0% ∼ 110.0%.

  7. Online preconcentration and determination of trace levels cadmium in water samples using flow injection systems coupled with flame AAS

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Songlin; Liang, Huading; Yan, Hua; Yan, Zhengzhong; Chen, Suqing; Zhu, Xiandi; Cheng, Miaoxian [School of Pharmaceutical and Chemical Engineering, Taizhou University (China)

    2010-02-15

    A rapid and sensitive method for the determination of trace levels cadmium in water samples by flame atomic absorption spectrometry was developed. It is based on the online sorption of Cd(II) ions on a microcolumn packed with HCl treated bamboo charcoal. In a pH range of 5.0-7.5, Cd(II) ions were effectively retained on the microcolumn, which exhibited fast kinetics, permitting the use of high sample flow rates up to at least 12.8 mL/min without the loss of retention efficiency. The retained Cd(II) ions were quantitatively eluted with HCl (2.0 mol/L) for an online determination. With a preconcentration time of 80 s at a sample loading flow rate of 8.6 mL/min, a sensitivity enhancement factor of 63 was obtained compared with the slope of the linear portion of the calibration curves before and after preconcentration. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9997, at levels from 1-40 ng/mL. The precision (RSD) for 11 replicate measurements were 3.2% for the determination of 5 ng/mL Cd(II) and 1.8% for 20 ng/mL Cd(II), respectively, and the detection limit (3s) was 0.36 ng/mL. The accuracy was assessed through the determination of a certified reference material, and also through recovery experiments. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  8. Application of neutron activation analysis to biological materials. Pt. 4. Approach to simultaneous determination of trace elements in human eye tissues with non-destructive neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Yamaguchi, T; Bando, M; Nakajima, A [Juntendo Univ., Tokyo (Japan). School of Medicine; Terai, M [Tokyo Metropolitan Univ. (Japan). Faculty of Science; Suzuki-Yasumoto, M [National Inst. of Radiological Sciences, Chiba (Japan)

    1980-01-01

    Fourteen trace elements (short-lived nuclides: Al, Br, Cu, Mn and V; long-lived nuclides: Ag, Au, Cd, Co, Cr, Fe, Sc, Se and Zn) in human eye tissues are determined simultaneously by non-destructive neutron activation analysis. The quantity of Al, Br, Fe, Se and Zn in the eye tissues (about 1 to more than 10 ..mu..g/g dry weight tissue) seems to be higher than that of other trace elements, although the content of each trace element in individual tissue is scattered in a wide range. Conjunctiva, iris (+ciliary body) and choroid (+pigment epithelium) seem to contain larger amount of various trace elements than other eye tissues. From correlation studies it is evident that the relative distribution of 14 trace elements in various eye tissues are similar, and furthermore the content of trace elements in the eye tissues may be correlated in each of the three groups (group A: Cd, Se and Zn; group B: Al, Cr, Fe, Se and V; group C: Al, Au, Fe and Se).

  9. A simple chemical method for the separation of phosphorus interfering the trace element determinations by neutron activation analysis in high doped silicon wafers

    International Nuclear Information System (INIS)

    Wagler, H.; Flachowsky, J.

    1986-01-01

    Neutron activation analysis is one of the most available method for the determination of trace elements, but in the case of P-doped silicon wafers the 32 P-activity interferes the gamma spectrometry. It is not possible to determine the trace elements without chemical manipulations. On the other hand, time consuming chemical separations should be avoided. Therefore, a simple and rapid P-separation method has to be developed, in which the following twelve trace elements should be taken into consideration: Ag, As, Au, Co, Cr, Cu, Fe, Mo, Na, Sb, W, and Zn. After acid oxidative dissolution of the activated sample, P is present as phosphate ion. The phosphate ion is removed by precipitation as BiPO 4 . (author)

  10. Application of spectroscopic Techniques for the determination of trace element concentrations in some Sudanese vegetables and fruits

    International Nuclear Information System (INIS)

    Ahmed, A. N.; Ali, A. H.; Eltayeb, M. A. H.; Osman, M. M.; Taha, K. K.

    2004-12-01

    The objective of this study were to determine the levels of the mineral nutrients, especially of trace elements, in some food items commonly consumed in Sudan and to compare the results of this work with local and international data. To achieve these objectives, food samples analyzed were collected from different localities in Sudan, and the samples were prepared for analysis by using dry ashing and wet digestion. Atomic absorption spectroscopy (AAS), x-ray fluorescence spectroscopy (XRF), flame photometry and colorimetry were used for the determination of the concentrations of elements in the samples, samples were ashed using muffle furnace at temperature 550 C. The quality of the data was verified by the analysis of standard reference materials TDD-ID and Hay-9. The levels of the elemental contents (Br, Ca, Co, Cu, Fe, Mg, Mn, P, Pb, Na, Rb, Sr, and Zn) were determined in legumes, cereals, oil seeds, flour and cereals products, vegetables, fruits, milk and milk products, egg, meats and fish, and oils and fats. The Sudanese food items analyzed were found to contain considerable ranges of nutrients as follows. Concentration levels for some of these elements Ca, Cu and Fe show values which were higher in fruits(4709, 21, and 633 ppm, respectively), and lower in vegetables (4094, 13, and 255 ppm, respectively). Pb and Mn were higher in vegetables (2 and 32 ppm, respectively) and lower in fruits (1 and 18 ppm) respectively). Na and Zn were higher in vegetables (3149 and 26 ppm, respectively) and lower fruits (269 and 13 ppm, respectively). The values obtained agree, in general, with data available from other countries. Variations were observed among certain varieties of food.(Author)

  11. Determination of trace uranium by resonance fluorescence method coupled with photo-catalytic technology and dual cloud point extraction.

    Science.gov (United States)

    Li, Jiekang; Li, Guirong; Han, Qian

    2016-12-05

    In this paper, two kinds of salophens (Sal) with different solubilities, Sal1 and Sal2, have been respectively synthesized, and they all can combine with uranyl to form stable complexes: [UO2(2+)-Sal1] and [UO2(2+)-Sal2]. Among them, [UO2(2+)-Sal1] was used as ligand to extract uranium in complex samples by dual cloud point extraction (dCPE), and [UO2(2+)-Sal2] was used as catalyst for the determination of uranium by photocatalytic resonance fluorescence (RF) method. The photocatalytic characteristic of [UO2(2+)-Sal2] on the oxidized pyronine Y (PRY) by potassium bromate which leads to the decrease of RF intensity of PRY were studied. The reduced value of RF intensity of reaction system (ΔF) is in proportional to the concentration of uranium (c), and a novel photo-catalytic RF method was developed for the determination of trace uranium (VI) after dCPE. The combination of photo-catalytic RF techniques and dCPE procedure endows the presented methods with enhanced sensitivity and selectivity. Under optimal conditions, the linear calibration curves range for 0.067 to 6.57ngmL(-1), the linear regression equation was ΔF=438.0 c (ngmL(-1))+175.6 with the correlation coefficient r=0.9981. The limit of detection was 0.066ngmL(-1). The proposed method was successfully applied for the separation and determination of uranium in real samples with the recoveries of 95.0-103.5%. The mechanisms of the indicator reaction and dCPE are discussed. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Application of spectroscopic techniques of analysis for the determination of trace elements concentrations in some sudanese food items

    International Nuclear Information System (INIS)

    Ahmed, A. N.; Ali, A.H.; Eltayeb, M. A.; Ahmed, M.M.O

    2004-01-01

    The objectives of this study were to determine the levels of the mineral nutrients, especially of trace elements, in some food items commonly consumed in sudan and to compare the results of this work with local and inter nation data. to achieve these objectives.Food samples were collected from different localities in sudan, and the samples were prepared for analysis using dry ashing and wet digestion. Atomic absorption spectroscopy (Aas), X-ray florescence spectroscopy (XRF), flame photometry and colorimetry were used for the determination of the concentrations of elements in the samples. Samples were ashed using muffle furnace at temperature 55 degree C. The quality of the data was verified by the analysis of standard reference materials TDD-Id and hay-9. The levels of the elemental contents (Br,Ca,Co,Cu,Fe,Mg,Mn,P,Pb,Na,Rb,Sr, and Zn) were determined in legumes, cereals, oil seeds, flour and cereal products, vegetables, fruits, milk and milk products, egg, meats and fish, and oils and fats. The sudanese food items analyzed were found to contain considerable ranges of nutrients as follows:-concentration levels for some of these elements Ca, Cu and Fe show values which were higher in fruits (4709,21, and 633 ppm, respectively), and lower in oils and fat s (25, 2, and 11 ppm, respectively). Pb and Mn were higher in flour and cereals products (4 and 34 ppm, respectively) and lower in fruits (1 ppm) and meats and fish (1 ppm and 4 ppm, respectively ). Na and Zn were higher in flour and cereals products and legumes (4970 and 39 ppm, respectively). The values obtained agree, in general, with data available from other countries. Variations were observed among certain varieties of food. (Author)

  13. Worldwide Open Proficiency Test for X ray Fluorescence Laboratories PTXRFIAEA08: Determination of Minor and Trace Elements in Natural Soil

    International Nuclear Information System (INIS)

    2014-01-01

    The IAEA assists Member State laboratories to maintain their readiness by producing reference materials, developing standardized analytical methods, and conducting interlaboratory comparisons and proficiency tests as tools for quality control. To ensure a reliable, worldwide, rapid and consistent response, the IAEA Nuclear Spectrometry and Applications Laboratory organizes tests for Member State laboratories. This publication presents the results of the worldwide proficiency test PTXRFIAEA08 on the determination of minor and trace elements in natural soil. Methodologies, a data evaluation approach, a summary evaluation of each element and individual evaluation reports for each laboratory are also described. The test was carried out within the IAEA project Nuclear Spectrometry for Analytical Applications, under the Nuclear Science Programme. The main objective of the project was to enhance the capability of interested Member States in effective utilization of nuclear spectrometries and analytical services in industry, human health and agriculture, and in monitoring and evaluating environmental pollution. This proficiency test was designed to identify analytical problems and to support Member State laboratories in improving the quality of their analytical results, maintaining their accreditation and providing a regular forum for discussion and technology transfer in this area. The type of sample and the concentration levels of the analytes were designed to enable the identification of potential analytical problems

  14. Worldwide Open Proficiency Test for X Ray Fluorescence Laboratories PTXRFIAEA/06: Determination of Minor and Trace Elements in Grass Mixture

    International Nuclear Information System (INIS)

    2011-01-01

    The IAEA assists its Member States laboratories to maintain their readiness by producing reference materials, by developing standardized analytical methods, and by conducting interlaboratory comparisons and proficiency tests as tools for quality control. To ensure a reliable worldwide, rapid and consistent response, the IAEA Nuclear Spectrometry and Applications Laboratory in Seibersdorf, Austria organises tests. This summary report presents the results of the worldwide proficiency test IAEA-PTXRF-06 on the determination of minor and trace elements in a grass mixture. Methodologies, data evaluation approach, summary evaluation of each element and individual evaluation reports for each laboratory are also described. The test was carried out under IAEA Project 1.4.3.4 (D.3.03), Nuclear Spectrometry for Analytical Applications, under the Nuclear Science Programme. The main objective of this project is to enhance the capability of interested Member States in effective utilization of nuclear spectrometries and analytical services in industry, human health, agriculture, and in monitoring and evaluation of environmental pollution. This proficiency test was designed to identify analytical problems, to support IAEA Member States laboratories to improve the quality of their analytical results, to maintain their accreditation and to provide a regular forum for discussion and technology transfer in this area. The type of sample and the concentration levels of the analytes were designed in a way to enable identification of potential analytical problems. The next proficiency test exercise is expected to be organized in 2010

  15. Determination of trace metals in non-conventional oilseeds and oil bearing resources by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Anwer, T.; Kazi, T.G.; Bhanger, M.I.; Iqbal, S.; Anwar, F.

    2003-01-01

    The presence of small amount of trace metals in oil and fats is well known to produce deleterious effect. Crude oils and fat of rice bran varieties (super, 86), mango kernel and muskmelon were evaluated for the determination of Ca, Mg, and Zn by using atomic absorption spectrometric technique. Both rice bran varieties (super, 86) were found to contain high calcium content 12.72, 12.11 micro g/g respectively. In case of Mg, highest content noted in mango kernel 9.91 micro g/g and lowest concentration was in rice bran (super) 2.23 micro g/g. The concentration of Zn was high in rice bran (86) 21.0 micro g/g followed by mango kernel 14.4 micro g/g, rice bran (super) 12.20 micro g/g and muskmelon 8.71 micro g/g. The information gained in present study provides baseline for the stability of these oils. (author)

  16. World-wide and regional intercomparison for the determination of trace elements in tuna fish homogenate sample IAEA-350

    Energy Technology Data Exchange (ETDEWEB)

    Mee, L D; Oregioni, B; Horvat, M [International Atomic Energy Agency, Marine Environment Laboratory, Monaco (Monaco)

    1992-12-01

    The accurate and precise determination of trace elements in marine biological samples is an important aspect of marine pollution studies, especially regarding studies of human exposure to toxic elements through sea food consumption. Past intercomparison studies conducted by the Marine Environment Laboratory of IAEA (formerly the International Laboratory of Marine Radioactivity) have focused upon various marine organisms including fish, bivalves and crustaceans. The present intercalibration exercise was designed in order to satisfy the increased demand for certified reference materials of various origins and the wide range of parameters that should be studied. Additionally, different instrumental techniques, both nuclear and non-nuclear, were compared, and evaluated. By statistically examining the data from this study, the material can be certified for future use as a reference material. The present report presents the entire experimental data set ana a statistical evaluation of the results for each parameter. It should enable individual participants to assess their performance and make appropriate modifications to their laboratory's analytical procedures where necessary. Additionally, a graphical evaluation is made of the data for parameters where a consensus value could not easily be achieved in order to examine the source of any systematic errors. The exercise was designed to satisfy the requirements of participants in IAEA's Analytical Quality Assurance Service as well as laboratories involved in UNEP's Regional Seas Programme and similar activities conducted within the auspices of GIPME (Global Investigations of Pollution in the Marine Environment)

  17. Determination of trace impurities of aluminium, cadmium, chromium, copper and nickel in indium phosphate by flameless atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Chruscinska, T.J.

    1990-01-01

    The sample (0.25 g) was treated with a nitric (0.9 ml) + hydrochloric (0.25 ml) acid mixture, heated to syrup under glass and then dissolved with 5 mol · 1 -1 HNO 3 (1 ml). The traces were determined in 0.2 mol · 1 -1 HNO 3 using Perkin-Elmer Model 430 Atomic Absorption Spectrometer equipped with a HGA 76B Graphite Furnace and an AS-1 Auto Sampling System. Pyrolytically coated and then tantalum treated tubes was employed. Additive errors due to contamination with, and loss of, the analyte element were controlled by estimation of the blank value and recovery. Background was corrected throughout. The background correction system efficiency was checked for the continuum background by two line method and for structured background by decreasing the slit or choosing different analytical lines. No other multiplicative (influencing the slope of the analytical curve) matrix interferences were found except for cadmium. (author). 12 refs, 4 tabs, 3 figs

  18. A multi-element solid-phase extraction method for trace metals determination in environmental samples on Amberlite XAD-2000

    International Nuclear Information System (INIS)

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

    2007-01-01

    A method for the preconcentration of some transition elements at trace level was proposed using a column filled with Amberlite XAD-2000 resin. Metal ions were adsorbed on XAD-2000 as their diethyldithiocarbamate chelates, then analytes retained on the resin were eluted by 1 mol L -1 nitric acid in acetone and determined by flame atomic absorption spectrometry (FAAS). The influences of some analytical parameters including pH of sample solution, ligand amount, the type, concentration and volume of elution solution, flow rates of the sample and eluent solutions, adsorption capacity of the resin and sample volume on the preconcentration efficiency have been investigated. The influences of some matrix elements were also examined. The detection limit (N = 20, 3 sigma) for Mn(II), Fe(II), Co(II), Cu(II), Cd(II), Zn(II), Pb(II) and Ni(II) were found as 0.20, 0.35, 0.25, 0.20, 0.20, 0.15, 0.45 and 0.25 μg L -1 , respectively. The validation of the procedure was carried out by analysis of certified reference materials. The proposed method was applied to natural waters and kale vegetable (Brassica oleracea var. acephala)

  19. Trace determination of 10 beta-lactam antibiotics in environmental and food samples by capillary liquid chromatography.

    Science.gov (United States)

    Bailón-Pérez, M I; García-Campaña, A M; del Olmo-Iruela, M; Gámiz-Gracia, L; Cruces-Blanco, C

    2009-11-20

    A sensitive and reliable method using capillary HPLC with UV-diode array detection (DAD) has been developed and validated for the trace determination of residues of 10 beta-lactam antibiotics of human and veterinary use, in milk, chicken meat and environmental water samples. The analytes included ampicillin, amoxicillin, penicillin V, penicillin G, cloxacillin, oxacillin, dicloxacillin, nafcillin, piperacillin and clavulanic acid. Legal levels are regulated by the EU Council regulation 2377/90 in animal edible tissues for these compounds. For food analysis, a solid-phase extraction (SPE) procedure consisting in a tandem of Oasis HLB and Alumina N cartridges was applied for off-line preconcentration and cleanup. For water analysis, the first step was only necessary. The limits of detection for the studied compounds were between 0.04-0.06 microg l(-1) for water samples and 0.80-1.40 microg l(-1) (or microg kg(-1)) in the case of foods derived from animals. Average recoveries for fortified samples at different concentration levels ranged between 82.9% and 98.2%, with relative standard deviations (RSDs) lower than 9%. The method showed the advantages of capillary HPLC for the detection of these widely applied antibiotics in different samples at very low concentration levels.

  20. A nanosized cadmium(II)-imprinted polymer for use in selective trace determination of cadmium in complex matrices

    International Nuclear Information System (INIS)

    Behbahani, Mohammad; Bagheri, Akbar; Barati, Mozhgan; Pourali, Ali Reza; Tapeh, Nasim Akbari Ghareh; Bojdi, Majid Kalate

    2013-01-01

    We describe a nanosized Cd(II)-imprinted polymer that was prepared from 4-vinyl pyridine (the functional monomer), ethyleneglycol dimethacrylate (the cross-linker), 2,2′-azobisisobutyronitrile (the radical initiator), neocuproine (the ligand), and Cd(II) (the template ion) by precipitation polymerization in acetonitrile as the solvent. The imprinted polymer was characterized by X-ray diffraction, thermogravimetric analysis, differential thermal analysis, and scanning electron microscopy. The maximum adsorption capacity of the nanosized sorbent was calculated to be 64 mg g −1 . Cadmium(II) was then quantified by FAAS. The relative standard deviation and limit of detection are 4.2 % and 0.2 μg L −1 , respectively. The imprinted polymer displays improve selectivity for Cd(II) ions over a range of competing metal ions with the same charge and similar ionic radius. This nanosized sorbent is an efficient solid phase for selective extraction and preconcentration of Cd(II) in complex matrices. The method was successfully applied to the trace determination of Cd(II) in food and water samples. (author)