WorldWideScience

Sample records for absorption sample consistent

  1. Absorption factor for cylindrical samples

    International Nuclear Information System (INIS)

    Sears, V.F.

    1984-01-01

    The absorption factor for the scattering of X-rays or neutrons in cylindrical samples is calculated by numerical integration for the case in which the absorption coefficients of the incident and scattered beams are not equal. An extensive table of values having an absolute accuracy of 10 -4 is given in a companion report [Sears (1983). Atomic Energy of Canada Limited, Report No. AECL-8176]. In the present paper an asymptotic expression is derived for the absorption factor which can be used with an error of less than 10 -3 for most cases of interest in both neutron inelastic scattering and neutron diffraction in crystals. (Auth.)

  2. A Consistent System for Coding Laboratory Samples

    Science.gov (United States)

    Sih, John C.

    1996-07-01

    A formal laboratory coding system is presented to keep track of laboratory samples. Preliminary useful information regarding the sample (origin and history) is gained without consulting a research notebook. Since this system uses and retains the same research notebook page number for each new experiment (reaction), finding and distinguishing products (samples) of the same or different reactions becomes an easy task. Using this system multiple products generated from a single reaction can be identified and classified in a uniform fashion. Samples can be stored and filed according to stage and degree of purification, e.g. crude reaction mixtures, recrystallized samples, chromatographed or distilled products.

  3. Validation of consistency of Mendelian sampling variance.

    Science.gov (United States)

    Tyrisevä, A-M; Fikse, W F; Mäntysaari, E A; Jakobsen, J; Aamand, G P; Dürr, J; Lidauer, M H

    2018-03-01

    Experiences from international sire evaluation indicate that the multiple-trait across-country evaluation method is sensitive to changes in genetic variance over time. Top bulls from birth year classes with inflated genetic variance will benefit, hampering reliable ranking of bulls. However, none of the methods available today enable countries to validate their national evaluation models for heterogeneity of genetic variance. We describe a new validation method to fill this gap comprising the following steps: estimating within-year genetic variances using Mendelian sampling and its prediction error variance, fitting a weighted linear regression between the estimates and the years under study, identifying possible outliers, and defining a 95% empirical confidence interval for a possible trend in the estimates. We tested the specificity and sensitivity of the proposed validation method with simulated data using a real data structure. Moderate (M) and small (S) size populations were simulated under 3 scenarios: a control with homogeneous variance and 2 scenarios with yearly increases in phenotypic variance of 2 and 10%, respectively. Results showed that the new method was able to estimate genetic variance accurately enough to detect bias in genetic variance. Under the control scenario, the trend in genetic variance was practically zero in setting M. Testing cows with an average birth year class size of more than 43,000 in setting M showed that tolerance values are needed for both the trend and the outlier tests to detect only cases with a practical effect in larger data sets. Regardless of the magnitude (yearly increases in phenotypic variance of 2 or 10%) of the generated trend, it deviated statistically significantly from zero in all data replicates for both cows and bulls in setting M. In setting S with a mean of 27 bulls in a year class, the sampling error and thus the probability of a false-positive result clearly increased. Still, overall estimated genetic

  4. Are most samples of animals systematically biased? Consistent individual trait differences bias samples despite random sampling.

    Science.gov (United States)

    Biro, Peter A

    2013-02-01

    Sampling animals from the wild for study is something nearly every biologist has done, but despite our best efforts to obtain random samples of animals, 'hidden' trait biases may still exist. For example, consistent behavioral traits can affect trappability/catchability, independent of obvious factors such as size and gender, and these traits are often correlated with other repeatable physiological and/or life history traits. If so, systematic sampling bias may exist for any of these traits. The extent to which this is a problem, of course, depends on the magnitude of bias, which is presently unknown because the underlying trait distributions in populations are usually unknown, or unknowable. Indeed, our present knowledge about sampling bias comes from samples (not complete population censuses), which can possess bias to begin with. I had the unique opportunity to create naturalized populations of fish by seeding each of four small fishless lakes with equal densities of slow-, intermediate-, and fast-growing fish. Using sampling methods that are not size-selective, I observed that fast-growing fish were up to two-times more likely to be sampled than slower-growing fish. This indicates substantial and systematic bias with respect to an important life history trait (growth rate). If correlations between behavioral, physiological and life-history traits are as widespread as the literature suggests, then many animal samples may be systematically biased with respect to these traits (e.g., when collecting animals for laboratory use), and affect our inferences about population structure and abundance. I conclude with a discussion on ways to minimize sampling bias for particular physiological/behavioral/life-history types within animal populations.

  5. CONSISTENCY UNDER SAMPLING OF EXPONENTIAL RANDOM GRAPH MODELS.

    Science.gov (United States)

    Shalizi, Cosma Rohilla; Rinaldo, Alessandro

    2013-04-01

    The growing availability of network data and of scientific interest in distributed systems has led to the rapid development of statistical models of network structure. Typically, however, these are models for the entire network, while the data consists only of a sampled sub-network. Parameters for the whole network, which is what is of interest, are estimated by applying the model to the sub-network. This assumes that the model is consistent under sampling , or, in terms of the theory of stochastic processes, that it defines a projective family. Focusing on the popular class of exponential random graph models (ERGMs), we show that this apparently trivial condition is in fact violated by many popular and scientifically appealing models, and that satisfying it drastically limits ERGM's expressive power. These results are actually special cases of more general results about exponential families of dependent random variables, which we also prove. Using such results, we offer easily checked conditions for the consistency of maximum likelihood estimation in ERGMs, and discuss some possible constructive responses.

  6. Effect of ladder diagrams on optical absorption spectra in a quasiparticle self-consistent GW framework

    Science.gov (United States)

    Cunningham, Brian; Grüning, Myrta; Azarhoosh, Pooya; Pashov, Dimitar; van Schilfgaarde, Mark

    2018-03-01

    We present an approach to calculate the optical absorption spectra that combines the quasiparticle self-consistent GW method [Phys. Rev. B 76, 165106 (2007), 10.1103/PhysRevB.76.165106] for the electronic structure with the solution of the ladder approximation to the Bethe-Salpeter equation for the macroscopic dielectric function. The solution of the Bethe-Salpeter equation has been implemented within an all-electron framework, using a linear muffin-tin orbital basis set, with the contribution from the nonlocal self-energy to the transition dipole moments (in the optical limit) evaluated explicitly. This approach addresses those systems whose electronic structure is poorly described within the standard perturbative GW approaches with density-functional theory calculations as a starting point. The merits of this approach have been exemplified by calculating optical absorption spectra of a strongly correlated transition metal oxide, NiO, and a narrow gap semiconductor, Ge. In both cases, the calculated spectrum is in good agreement with the experiment. It is also shown that for systems whose electronic structure is well-described within the standard perturbative GW , such as Si, LiF, and h -BN , the performance of the present approach is in general comparable to the standard GW plus Bethe-Salpeter equation. It is argued that both vertex corrections to the electronic screening and the electron-phonon interaction are responsible for the observed systematic overestimation of the fundamental band gap and spectrum onset.

  7. Near-resonant absorption in the time-dependent self-consistent field and multiconfigurational self-consistent field approximations

    DEFF Research Database (Denmark)

    Norman, Patrick; Bishop, David M.; Jensen, Hans Jørgen Aa

    2001-01-01

    Computationally tractable expressions for the evaluation of the linear response function in the multiconfigurational self-consistent field approximation were derived and implemented. The finite lifetime of the electronically excited states was considered and the linear response function was shown...... to be convergent in the whole frequency region. This was achieved through the incorporation of phenomenological damping factors that lead to complex response function values....

  8. Determining photon energy absorption parameters for different soil samples

    International Nuclear Information System (INIS)

    Kucuk, Nil; Cakir, Merve; Tumsavas, Zeynal

    2013-01-01

    The mass attenuation coefficients (μ s ) for five different soil samples were measured at 661.6, 1173.2 and 1332.5 keV photon energies. The soil samples were separately irradiated with 137 Cs and 60 Co (370 kBq) radioactive point gamma sources. The measurements were made by performing transmission experiments with a 2″ x 2″ NaI(Tl) scintillation detector, which had an energy resolution of 7% at 0.662 MeV for the gamma-rays from the decay of 137 Cs. The effective atomic numbers (Z eff ) and the effective electron densities (N eff ) were determined experimentally and theoretically using the obtained μ s values for the soil samples. Furthermore, the Z eff and N eff values of the soil samples were computed for the total photon interaction cross-sections using theoretical data over a wide energy region ranging from 1 keV to 15 MeV. The experimental values of the soils were found to be in good agreement with the theoretical values. Sandy loam and sandy clay loam soils demonstrated poor photon energy absorption characteristics. However, clay loam and clay soils had good photon energy absorption characteristics. (author)

  9. Thermal neutron absorption cross section of small samples

    International Nuclear Information System (INIS)

    Nghiep, T.D.; Vinh, T.T.; Son, N.N.; Vuong, T.V.; Hung, N.T.

    1989-01-01

    A modified steady method for determining the macroscopic thermal neutron absorption cross section of small samples 500 cm 3 in volume is described. The method uses a moderating block of paraffin, Pu-Be neutron source emitting 1.1x10 6 n.s. -1 , SNM-14 counter and ordinary counting equipment. The interval of cross section from 2.6 to 1.3x10 4 (10 -3 cm 2 g -1 ) was measured. The experimental data are described by calculation formulae. 7 refs.; 4 figs

  10. Correction for sample self-absorption in activity determination by gamma spectrometry

    International Nuclear Information System (INIS)

    Galloway, R.B.

    1991-01-01

    Gamma ray spectrometry is a convenient method of determining the activity of the radioactive components in environmental samples. Commonly samples vary in gamma absorption or differ in absorption from the calibration standards available, so that accurate correction for self-absorption in the sample is essential. A versatile correction procedure is described. (orig.)

  11. Absorption corrections for x-ray fluorescence analysis of environmental samples

    International Nuclear Information System (INIS)

    Bazan, F.; Bonner, N.A.

    1975-01-01

    The discovery of a very simple and useful relationship between the absorption coefficient of a particular element and the ratio of incoherent to coherent scattering by the sample containing the element is discussed. By measuring the absorption coefficients for a few elements in a few samples, absorption coefficients for many elements in an entire set of similar samples can be obtained. (auth)

  12. Absorption corrections for x-ray fluorescence analysis of environmental samples

    International Nuclear Information System (INIS)

    Bazan, F.; Bonner, N.A.

    1976-01-01

    The discovery of a very simple and useful relationship between the absorption coefficient of a particular element and the ratio of incoherent to coherent scattering by the sample containing the element is discussed. By measuring the absorption coefficients for a few elements in a few samples, absorption coefficients for many elements in an entire set of similar samples can be obtained

  13. Enhanced microwave absorption properties of MnO{sub 2} hollow microspheres consisted of MnO{sub 2} nanoribbons synthesized by a facile hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yan; Han, Bingqian; Chen, Nan; Deng, Dongyang; Guan, Hongtao [Department of Materials Science and Engineering, Yunnan University, 650091, Kunming (China); Wang, Yude, E-mail: ydwang@ynu.edu.cn [Department of Materials Science and Engineering, Yunnan University, 650091, Kunming (China); Yunnan Province Key Lab of Micro-Nano Materials and Technology, Yunnan University, 650091, Kunming (China)

    2016-08-15

    MnO{sub 2} hollow microspheres consisted of nanoribbons were successfully fabricated via a facile hydrothermal method with SiO{sub 2} sphere templates. The crystal structure, morphology and microwave absorption properties in X and Ku band of the as-synthesized samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and a vector network analyzer. The results show that the three-dimensional (3D) hollow microspheres are assembled by ultra thin and narrow one-dimensional (1D) nanoribbons. A rational process for the formation of hollow microspheres is proposed. The 3D MnO{sub 2} hollow microspheres possess improved dielectric and magnetic properties than the 1D nanoribbons prepared by the same procedures with the absence of SiO{sub 2} hard templates, which are closely related to their special nanostructures. The MnO{sub 2} microspheres also show much better microwave absorption properties in X (8–12 GHz) and Ku (12–18 GHz) microwave band compared with 1D MnO{sub 2} nanoribbons. The minimum reflection loss of −40 dB for hollow microsphere can be observed at 14.2 GHz and reflection loss below −10 dB is 3.5 GHz with a thickness of only 4 mm. The possible mechanism for the enhanced microwave absorption properties is also discussed. - Graphical abstract: MnO{sub 2} hollow microspheres composed of nanoribbons show the excellent microwave absorption properties in X and Ku band. - Highlights: • MnO{sub 2} hollow microspheres consisted of MnO{sub 2} nanoribbons were successfully prepared. • MnO{sub 2} hollow microspheres possess good microwave absorption performances. • The excellent microwave absorption properties are in X and Ku microwave band. • Electromagnetic impedance matching is great contribution to absorption properties.

  14. Research on self-absorption corrections for laboratory γ spectral analysis of soil samples

    International Nuclear Information System (INIS)

    Tian Zining; Jia Mingyan; Li Huibin; Cheng Ziwei; Ju Lingjun; Shen Maoquan; Yang Xiaoyan; Yan Ling; Fen Tiancheng

    2010-01-01

    Based on the calibration results of the point sources,dimensions of HPGe crystal were characterized.Linear attenuation coefficients and detection efficiencies of all kinds of samples were calculated,and the function F(μ) of φ75 mm x 25 mm sample was established. Standard surface source was used to simulate the source of different heights in the soil sample. And the function ε(h) which reflect the relationship between detection efficiencies and heights of the surface sources was determined. The detection efficiency of calibration source can be obtained by integration, F(μ) functions of soil samples established is consistent with the result of MCNP calculation code. Several φ75 mm x 25 mm soil samples were measured by the HPGe spectrometer,and the function F(μ) was used to correct the self absorption. F(μ) functions of soil samples of various dimensions can be calculated by MCNP calculation code established, and self absorption correction can be done. To verify the efficiency of calculation results, φ75 mm x 75 mm soil samples were measured. Several φ75 mm x 25 mm soil samples from aerosphere nuclear testing field was measured by the HPGe spectrometer,and the function F(μ) was used to correct the self absorption. The function F(m) was established, and the technical method which is used to correct the soil samples of unknown area is also given. The correction method of surface source greatly improves the gamma spectrum's metrical accuracy, and it will be widely applied to environmental radioactive investigation. (authors)

  15. Phosphate absorption and distribution in flue-cured tobacco under different ozone consistency by using 32P

    International Nuclear Information System (INIS)

    Qiang Jiye

    2004-01-01

    The absorption and distribution of phosphate in flue-cured tobacco under different ozone consistencies was studied by using 32 P. The results showed that the percentage of root of whole tobacco plant assimilating 32 p reduced as growing, but in stem it increased as growing in the sand culture. Root and stem of flue-cured tobacco assimilating 32 P varied little in the whole growing period in the solution culture. Distribution situation in leaf with two consistencies was in the order of lower leaf>cutters leaf>upper leaf, and the ratio of radioactivity showed root>stem>lower leaf>cutters leaf>upper leaf. However, flue-cured tobacco assimilating phosphate in the two consistencies showed significantly positive correlation with length of growth period. Assimilating phosphate in the solution culture was more and faster than in the low ozone consistency culture

  16. Random Sampling of Correlated Parameters – a Consistent Solution for Unfavourable Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Žerovnik, G., E-mail: gasper.zerovnik@ijs.si [Jožef Stefan Institute, Jamova cesta 39, SI-1000 Ljubljana (Slovenia); Trkov, A. [Jožef Stefan Institute, Jamova cesta 39, SI-1000 Ljubljana (Slovenia); International Atomic Energy Agency, PO Box 100, A-1400 Vienna (Austria); Kodeli, I.A. [Jožef Stefan Institute, Jamova cesta 39, SI-1000 Ljubljana (Slovenia); Capote, R. [International Atomic Energy Agency, PO Box 100, A-1400 Vienna (Austria); Smith, D.L. [Argonne National Laboratory, 1710 Avenida del Mundo, Coronado, CA 92118-3073 (United States)

    2015-01-15

    Two methods for random sampling according to a multivariate lognormal distribution – the correlated sampling method and the method of transformation of correlation coefficients – are briefly presented. The methods are mathematically exact and enable consistent sampling of correlated inherently positive parameters with given information on the first two distribution moments. Furthermore, a weighted sampling method to accelerate the convergence of parameters with extremely large relative uncertainties is described. However, the method is efficient only for a limited number of correlated parameters.

  17. Determination of copper in powdered chocolate samples by slurry-sampling flame atomic-absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Walter N.L. dos; Silva, Erik G.P. da; Fernandes, Marcelo S.; Araujo, Rennan G.O.; Costa, Anto' ' enio C.S.; Ferreira, Sergio L.C. [Nucleo de Excelencia em Quimica Analitica da Bahia, Universidade Federal da Bahia, Instituto de Quimica, Salvador, Bahia (Brazil); Vale, M.G.R. [Instituto de Quimica, Universidade Federal da Bahia do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul (Brazil)

    2005-06-01

    Chocolate is a complex sample with a high content of organic compounds and its analysis generally involves digestion procedures that might include the risk of losses and/or contamination. The determination of copper in chocolate is important because copper compounds are extensively used as fungicides in the farming of cocoa. In this paper, a slurry-sampling flame atomic-absorption spectrometric method is proposed for determination of copper in powdered chocolate samples. Optimization was carried out using univariate methodology involving the variables nature and concentration of the acid solution for slurry preparation, sonication time, and sample mass. The recommended conditions include a sample mass of 0.2 g, 2.0 mol L{sup -1} hydrochloric acid solution, and a sonication time of 15 min. The calibration curve was prepared using aqueous copper standards in 2.0 mol L{sup -1} hydrochloric acid. This method allowed determination of copper in chocolate with a detection limit of 0.4 {mu}g g{sup -1} and precision, expressed as relative standard deviation (RSD), of 2.5% (n=10) for a copper content of approximately 30 {mu}g g{sup -1}, using a chocolate mass of 0.2 g. The accuracy was confirmed by analyzing the certified reference materials NIST SRM 1568a rice flour and NIES CRM 10-b rice flour. The proposed method was used for determination of copper in three powdered chocolate samples, the copper content of which varied between 26.6 and 31.5 {mu}g g{sup -1}. The results showed no significant differences with those obtained after complete digestion, using a t-test for comparison. (orig.)

  18. Self-absorption corrections for gamma ray spectral measurements of 210Pb in environmental samples

    International Nuclear Information System (INIS)

    Miller, K.M.

    1987-01-01

    Theoretical considerations and experimental data are used to demonstrate the basic behaviour of the self-absorption effect of a sample matrix in gamma ray spectrometry, particularly as it relates to the analysis of 210 Pb in environmental media. The results indicate that it may not be appropriate to apply the commonly used self-absorption function in all cases. (orig.)

  19. Optical absorption study of radiation and thermal effects in Brazilian samples of spodumene

    International Nuclear Information System (INIS)

    Isotani, S.; Fujii, A.T.; Antonini, R.; Furtado, W.

    1988-03-01

    A detailed analysis of the optical absorption spectra of five varieties of Brazilian spodumene is presented. The samples were submitted to heat treatments and irradiated with gamma rays, x radiation, electrons and ultraviolet light. (M.C.K.) [pt

  20. Effect of density increase on self-absorption property of bulk samples

    International Nuclear Information System (INIS)

    Dao Anh Minh; Tran Duc Thiep

    1990-01-01

    Asymptotic behaviour due to self-absorption of photon attenuation function in terms of material density for bulk samples has been considered. Some practical applications have also been presented. (author). 9 refs., 4 figs., 2 tabs

  1. Range-efficient consistent sampling and locality-sensitive hashing for polygons

    DEFF Research Database (Denmark)

    Gudmundsson, Joachim; Pagh, Rasmus

    2017-01-01

    Locality-sensitive hashing (LSH) is a fundamental technique for similarity search and similarity estimation in high-dimensional spaces. The basic idea is that similar objects should produce hash collisions with probability significantly larger than objects with low similarity. We consider LSH for...... or union of a set of preprocessed polygons. Curiously, our consistent sampling method uses transformation to a geometric problem....

  2. High-throughput liquid-absorption preconcentrator sampling methods

    Science.gov (United States)

    Zaromb, Solomon

    1994-01-01

    A system for detecting trace concentrations of an analyte in air includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container comprising a wettable material. The wettable material is continuously wetted with an analyte-sorbing liquid which flows from one part of the container to a lower end. Sampled air flows through the container in contact with the wetted material with a swirling motion which results in efficient transfer of analyte vapors or aerosol particles to the sorbing liquid and preconcentration of traces of analyte in the liquid. The preconcentrated traces of analyte may be either detected within the container or removed therefrom for injection into a separate detection means or for subsequent analysis.

  3. Direct analysis of 210Pb in sediment samples: Self-absorption corrections

    International Nuclear Information System (INIS)

    Cutshall, N.H.; Larsen, I.L.; Olsen, C.R.

    1983-01-01

    A procedure for the direct #betta#-ray instrumental analysis of 210 Pb in sediment samples is presented. The problem of dependence of self-absorption on sample composition is solved by making a direct transmission measurement on each sample. The procedure has been verified by intercalibrations and other tests. (orig.)

  4. Capillary absorption spectrometer and process for isotopic analysis of small samples

    Energy Technology Data Exchange (ETDEWEB)

    Alexander, M. Lizabeth; Kelly, James F.; Sams, Robert L.; Moran, James J.; Newburn, Matthew K.; Blake, Thomas A.

    2018-04-24

    A capillary absorption spectrometer and process are described that provide highly sensitive and accurate stable absorption measurements of analytes in a sample gas that may include isotopologues of carbon and oxygen obtained from gas and biological samples. It further provides isotopic images of microbial communities that allow tracking of nutrients at the single cell level. It further targets naturally occurring variations in carbon and oxygen isotopes that avoids need for expensive isotopically labeled mixtures which allows study of samples taken from the field without modification. The process also permits sampling in vivo permitting real-time ambient studies of microbial communities.

  5. Capillary absorption spectrometer and process for isotopic analysis of small samples

    Energy Technology Data Exchange (ETDEWEB)

    Alexander, M. Lizabeth; Kelly, James F.; Sams, Robert L.; Moran, James J.; Newburn, Matthew K.; Blake, Thomas A.

    2016-03-29

    A capillary absorption spectrometer and process are described that provide highly sensitive and accurate stable absorption measurements of analytes in a sample gas that may include isotopologues of carbon and oxygen obtained from gas and biological samples. It further provides isotopic images of microbial communities that allow tracking of nutrients at the single cell level. It further targets naturally occurring variations in carbon and oxygen isotopes that avoids need for expensive isotopically labeled mixtures which allows study of samples taken from the field without modification. The method also permits sampling in vivo permitting real-time ambient studies of microbial communities.

  6. Self-absorption corrections of various sample-detector geometries in gamma-ray spectrometry using sample Monte Carlo Simulations

    International Nuclear Information System (INIS)

    Ahmad Saat; Appleby, P.G.; Nolan, P.J.

    1997-01-01

    Corrections for self-absorption in gamma-ray spectrometry have been developed using a simple Monte Carlo simulation technique. The simulation enables the calculation of gamma-ray path lengths in the sample which, using available data, can be used to calculate self-absorption correction factors. The simulation was carried out on three sample geometries: disk, Marinelli beaker, and cylinder (for well-type detectors). Mathematical models and experimental measurements are used to evaluate the simulations. A good agreement of within a few percents was observed. The simulation results are also in good agreement with those reported in the literature. The simulation code was carried out in FORTRAN 90,

  7. Factor Structure, Internal Consistency, and Screening Sensitivity of the GARS-2 in a Developmental Disabilities Sample

    OpenAIRE

    Martin A. Volker; Elissa H. Dua; Christopher Lopata; Marcus L. Thomeer; Jennifer A. Toomey; Audrey M. Smerbeck; Jonathan D. Rodgers; Joshua R. Popkin; Andrew T. Nelson; Gloria K. Lee

    2016-01-01

    The Gilliam Autism Rating Scale-Second Edition (GARS-2) is a widely used screening instrument that assists in the identification and diagnosis of autism. The purpose of this study was to examine the factor structure, internal consistency, and screening sensitivity of the GARS-2 using ratings from special education teaching staff for a sample of 240 individuals with autism or other significant developmental disabilities. Exploratory factor analysis yielded a correlated three-factor solution si...

  8. Anomalous non-resonant microwave absorption in SmFeAs(O,F) polycrystalline sample

    Energy Technology Data Exchange (ETDEWEB)

    Onyancha, R.B., E-mail: 08muma@gmail.com [Department of Physics, College of Science, Engineering and Technology, University of South Africa, Johannesburg, 1710 (South Africa); Shimoyama, J. [Department of Applied Chemistry, University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo (Japan); Singh, S.J. [Leibniz-Institute for Solid State and Materials Research, IFW-Dresden, D-01171 Dresden (Germany); Hayashi, K.; Ogino, H. [Department of Applied Chemistry, University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo (Japan); Srinivasu, V.V. [Department of Physics, College of Science, Engineering and Technology, University of South Africa, Johannesburg, 1710 (South Africa)

    2017-02-15

    Highlights: • The non-resonant microwave absorption (NRMA) line shape in evolved with microwave power. • Observed a cross over from ‘normal’ absorption to ‘anomalous’ absorption as a function of microwave power. • The anomalous absorption has been explained in the context of non-hysteretic Josephson junction. - Abstract: Here we present the non-resonant microwave absorption (NRMA) studies on SmFeAsO{sub 0.88}F{sub 0.12} polycrystalline sample measured at 6.06 K with the magnetic field swept from −250 G to +250 G at a frequency of 9.45 GHz. It was observed that the (NRMA) line shape evolves as a function of microwave power. Again, the signal intensity increases from 22.83 µW to 0.710 mW where it reaches a maximum and quite remarkably it changed from ‘normal’ absorption to ‘anomalous’ absorption at 2.247 mW, then the intensity decreases with further increase of microwave power. The crossover from ‘normal’ to ‘anomalous’ NRMA absorption and its dependence on microwave power is a new phenomenon in iron pnictides superconductors and we have attributed this anomaly to come from non-hysteretic Josephson junction.

  9. Results of Self-Absorption Study on the Versapor 3000 Filters for Radioactive Particulate Air Sampling

    International Nuclear Information System (INIS)

    Barnett, J.M.

    2008-01-01

    Since the mid-1980s the Pacific Northwest National Laboratory (PNNL) has used a value of 0.85 as a correction factor for the self absorption of activity of particulate radioactive air samples. More recently, an effort was made to evaluate the current particulate radioactive air sample filters (Versapor(reg s ign) 3000) used at PNNL for self absorption effects. There were two methods used in the study, (1) to compare the radioactivity concentration by direct gas-flow proportional counting of the filter to the results obtained after acid digestion of the filter and counting again by gas-flow proportional detection and (2) to evaluate sample filters by high resolution visual/infrared microscopy to determine the depth of material loading on or in the filter fiber material. Sixty samples were selected from the archive for acid digestion in the first method and about 30 samples were selected for high resolution visual/infrared microscopy. Mass loading effects were also considered. From the sample filter analysis, large error is associated with the average self absorption factor, however, when the data is compared directly one-to-one, statistically, there appears to be good correlation between the two analytical methods. The mass loading of filters evaluated was <0.2 mg cm-2 and was also compared against other published results. The microscopy analysis shows the sample material remains on the top of the filter paper and does not imbed into the filter media. Results of the microscopy evaluation lead to the conclusion that there is not a mechanism for significant self absorption. The overall conclusion is that self-absorption is not a significant factor in the analysis of filters used at PNNL for radioactive air stack sampling of radionuclide particulates and that an applied correction factor is conservative in determining overall sample activity. A new self absorption factor of 1.0 is recommended

  10. Mass Absorption Coefficients At 661,6 keV Energy In Various Samples

    International Nuclear Information System (INIS)

    Suhariyono, Gatot; Bunawas

    2000-01-01

    Determination mass absorption coefficients (mum) at 661.6 keV energy in the samples various, such as lysine, coffee, chocolate, nutrisari, coconut oil, monosodium glutamate (MSG), tea, tin fish and the soil with experiment method has been carried out. The mum research was carried out in effort to give the measurement result of Cs-137 concentration that more accurate to the samples, because the sample density increases, mass absorption coefficients (mum) decreases. The mum correction on measurement of Cs-137 concentration in the samples various around between 0 and 13%, the highest is on the chocolate sample and the lowest is on the tin fish sample. Density of the samples decreases, the mum influence increases on the counting of Cs-137 concentration in the sample (Bq/kg)

  11. Preparation of rock samples for measurement of the thermal neutron macroscopic absorption cross-section

    International Nuclear Information System (INIS)

    Czubek, J.A.; Burda, J.; Drozdowicz, K.; Igielski, A.; Kowalik, W.; Krynicka-Drozdowicz, E.; Woznicka, U.

    1986-03-01

    Preparation of rock samples for the measurement of the thermal neutron macroscopic absorption cross-section in small cylindrical two-region systems by a pulsed technique is presented. Requirements which should be fulfilled during the preparation of the samples due to physical assumptions of the method are given. A cylindrical vessel is filled with crushed rock and saturated with a medium strongly absorbing thermal neutrons. Water solutions of boric acid of well-known macroscopic absorption cross-section are used. Mass contributions of the components in the sample are specified. This is necessary for the calculation of the thermal neutron macroscopic absorption cross-section of the rock matrix. The conditions necessary for assuring the required accuracy of the measurement are given and the detailed procedure of preparation of the rock sample is described. (author)

  12. Device to investigate samples by means of flameless atomic absorption measurement

    International Nuclear Information System (INIS)

    Sperling, K.R.

    1977-01-01

    An improvement on a device to investigate samples by means of flameless atomic absorption measurement is suggested in which one aims to produce a most complete possible atomic clond from the sample to be investigated within the sample space defined by the beam bundle, through which the measuring beam bundle is passed. According to the invention, the tubular sample space should be closed by an optically penetrable window on one side. (RW) [de

  13. Absorption and enhancement corrections using XRF analysis of some chemical samples

    International Nuclear Information System (INIS)

    Falih, Arwa Gaddal

    1996-06-01

    In this work samples containing Cr, Fe and Ni salts invarying ratios were prepared so as to represent approximately the concentrations of these elements in naturally occurring ore samples. These samples were then analyzed by EDXRF spectrometer system and the inter element effects (absorption and enhancement) were evaluated by means of two method: by using AXIL-QXAS software to calculate the effects and by the emission-transmission method to experimentally determine the same effects. The results obtained were compared and a discrepancy in the absorption results was observed. The discrepancy was attributed to the fact that the absorption in the two methods was calculated in different manners, i.e. in the emission-transmission method the absorption factor was calculated by adding different absorption terms by what is known as the additive law, but in the software program it was calculated from the scattered peaks method which does not obey this law. It was concluded that the program should be modified by inserting the emission-transmission method in the software program to calculate the absorption. Quality assurance of the data was performed though the analysis of the standard alloys obtained from the International Atomic Energy Agency (IAEA). (Author)

  14. Absolute activity determinations on large volume geological samples independent of self-absorption effects

    International Nuclear Information System (INIS)

    Wilson, W.E.

    1980-01-01

    This paper describes a method for measuring the absolute activity of large volume samples by γ-spectroscopy independent of self-absorption effects using Ge detectors. The method yields accurate matrix independent results at the expense of replicative counting of the unknown sample. (orig./HP)

  15. Mg II ABSORPTION CHARACTERISTICS OF A VOLUME-LIMITED SAMPLE OF GALAXIES AT z ∼ 0.1

    International Nuclear Information System (INIS)

    Barton, Elizabeth J.; Cooke, Jeff

    2009-01-01

    We present an initial survey of Mg II absorption characteristics in the halos of a carefully constructed, volume-limited subsample of galaxies embedded in the spectroscopic part of the Sloan Digital Sky Survey (SDSS). We observed quasars near sightlines to 20 low-redshift (z ∼ 0.1), luminous (M r + 5log h ≤-20.5) galaxies in SDSS DR4 and DR6 with the LRIS-B spectrograph on the Keck I telescope. The primary systematic criteria for the targeted galaxies are a redshift z ∼> 0.1 and the presence of an appropriate bright background quasar within a projected 75 h -1 kpc of its center, although we preferentially sample galaxies with lower impact parameters and slightly more star formation within this range. Of the observed systems, six exhibit strong (W eq (2796) ≥ 0.3 A) Mg II absorption at the galaxy's redshift, six systems have upper limits which preclude strong Mg II absorption, while the remaining observations rule out very strong (W eq (2796) ≥ 1-2 A) absorption. The absorbers fall at higher impact parameters than many non-absorber sightlines, indicating a covering fraction f c ∼ -1 kpc (f c ∼ 0.25). The data are consistent with a possible dependence of covering fraction and/or absorption halo size on the environment or star-forming properties of the central galaxy.

  16. Reliability and consistency of a validated sun exposure questionnaire in a population-based Danish sample.

    Science.gov (United States)

    Køster, B; Søndergaard, J; Nielsen, J B; Olsen, A; Bentzen, J

    2018-06-01

    An important feature of questionnaire validation is reliability. To be able to measure a given concept by questionnaire validly, the reliability needs to be high. The objectives of this study were to examine reliability of attitude and knowledge and behavioral consistency of sunburn in a developed questionnaire for monitoring and evaluating population sun-related behavior. Sun related behavior, attitude and knowledge was measured weekly by a questionnaire in the summer of 2013 among 664 Danes. Reliability was tested in a test-retest design. Consistency of behavioral information was tested similarly in a questionnaire adapted to measure behavior throughout the summer. The response rates for questionnaire 1, 2 and 3 were high and the drop out was not dependent on demographic characteristic. There was at least 73% agreement between sunburns in the measurement week and the entire summer, and a possible sunburn underestimation in questionnaires summarizing the entire summer. The participants underestimated their outdoor exposure in the evaluation covering the entire summer as compared to the measurement week. The reliability of scales measuring attitude and knowledge was high for majority of scales, while consistency in protection behavior was low. To our knowledge, this is the first study to report reliability for a completely validated questionnaire on sun-related behavior in a national random population based sample. Further, we show that attitude and knowledge questions confirmed their validity with good reliability, while consistency of protection behavior in general and in a week's measurement was low.

  17. [Extracting THz absorption coefficient spectrum based on accurate determination of sample thickness].

    Science.gov (United States)

    Li, Zhi; Zhang, Zhao-hui; Zhao, Xiao-yan; Su, Hai-xia; Yan, Fang

    2012-04-01

    Extracting absorption spectrum in THz band is one of the important aspects in THz applications. Sample's absorption coefficient has a complex nonlinear relationship with its thickness. However, as it is not convenient to measure the thickness directly, absorption spectrum is usually determined incorrectly. Based on the method proposed by Duvillaret which was used to precisely determine the thickness of LiNbO3, the approach to measuring the absorption coefficient spectra of glutamine and histidine in frequency range from 0.3 to 2.6 THz(1 THz = 10(12) Hz) was improved in this paper. In order to validate the correctness of this absorption spectrum, we designed a series of experiments to compare the linearity of absorption coefficient belonging to one kind amino acid in different concentrations. The results indicate that as agreed by Lambert-Beer's Law, absorption coefficient spectrum of amino acid from the improved algorithm performs better linearity with its concentration than that from the common algorithm, which can be the basis of quantitative analysis in further researches.

  18. A general framework for thermodynamically consistent parameterization and efficient sampling of enzymatic reactions.

    Directory of Open Access Journals (Sweden)

    Pedro Saa

    2015-04-01

    Full Text Available Kinetic models provide the means to understand and predict the dynamic behaviour of enzymes upon different perturbations. Despite their obvious advantages, classical parameterizations require large amounts of data to fit their parameters. Particularly, enzymes displaying complex reaction and regulatory (allosteric mechanisms require a great number of parameters and are therefore often represented by approximate formulae, thereby facilitating the fitting but ignoring many real kinetic behaviours. Here, we show that full exploration of the plausible kinetic space for any enzyme can be achieved using sampling strategies provided a thermodynamically feasible parameterization is used. To this end, we developed a General Reaction Assembly and Sampling Platform (GRASP capable of consistently parameterizing and sampling accurate kinetic models using minimal reference data. The former integrates the generalized MWC model and the elementary reaction formalism. By formulating the appropriate thermodynamic constraints, our framework enables parameterization of any oligomeric enzyme kinetics without sacrificing complexity or using simplifying assumptions. This thermodynamically safe parameterization relies on the definition of a reference state upon which feasible parameter sets can be efficiently sampled. Uniform sampling of the kinetics space enabled dissecting enzyme catalysis and revealing the impact of thermodynamics on reaction kinetics. Our analysis distinguished three reaction elasticity regions for common biochemical reactions: a steep linear region (0> ΔGr >-2 kJ/mol, a transition region (-2> ΔGr >-20 kJ/mol and a constant elasticity region (ΔGr <-20 kJ/mol. We also applied this framework to model more complex kinetic behaviours such as the monomeric cooperativity of the mammalian glucokinase and the ultrasensitive response of the phosphoenolpyruvate carboxylase of Escherichia coli. In both cases, our approach described appropriately not only

  19. Factor Structure, Internal Consistency, and Screening Sensitivity of the GARS-2 in a Developmental Disabilities Sample

    Directory of Open Access Journals (Sweden)

    Martin A. Volker

    2016-01-01

    Full Text Available The Gilliam Autism Rating Scale-Second Edition (GARS-2 is a widely used screening instrument that assists in the identification and diagnosis of autism. The purpose of this study was to examine the factor structure, internal consistency, and screening sensitivity of the GARS-2 using ratings from special education teaching staff for a sample of 240 individuals with autism or other significant developmental disabilities. Exploratory factor analysis yielded a correlated three-factor solution similar to that found in 2005 by Lecavalier for the original GARS. Though the three factors appeared to be reasonably consistent with the intended constructs of the three GARS-2 subscales, the analysis indicated that more than a third of the GARS-2 items were assigned to the wrong subscale. Internal consistency estimates met or exceeded standards for screening and were generally higher than those in previous studies. Screening sensitivity was .65 and specificity was .81 for the Autism Index using a cut score of 85. Based on these findings, recommendations are made for instrument revision.

  20. Reliability and consistency of a validated sun exposure questionnaire in a population-based Danish sample

    Directory of Open Access Journals (Sweden)

    B. Køster

    2018-06-01

    Full Text Available An important feature of questionnaire validation is reliability. To be able to measure a given concept by questionnaire validly, the reliability needs to be high.The objectives of this study were to examine reliability of attitude and knowledge and behavioral consistency of sunburn in a developed questionnaire for monitoring and evaluating population sun-related behavior.Sun related behavior, attitude and knowledge was measured weekly by a questionnaire in the summer of 2013 among 664 Danes. Reliability was tested in a test-retest design. Consistency of behavioral information was tested similarly in a questionnaire adapted to measure behavior throughout the summer.The response rates for questionnaire 1, 2 and 3 were high and the drop out was not dependent on demographic characteristic. There was at least 73% agreement between sunburns in the measurement week and the entire summer, and a possible sunburn underestimation in questionnaires summarizing the entire summer. The participants underestimated their outdoor exposure in the evaluation covering the entire summer as compared to the measurement week. The reliability of scales measuring attitude and knowledge was high for majority of scales, while consistency in protection behavior was low.To our knowledge, this is the first study to report reliability for a completely validated questionnaire on sun-related behavior in a national random population based sample. Further, we show that attitude and knowledge questions confirmed their validity with good reliability, while consistency of protection behavior in general and in a week's measurement was low. Keywords: Questionnaire, Validation, Reliability, Skin cancer, Prevention, Ultraviolet radiation

  1. The Consistency of Isotopologues of Ambient Atmospheric Nitric Acid in Passively Collected Samples

    Science.gov (United States)

    Bell, M. D.; Sickman, J. O.; Bytnerowicz, A.; Padgett, P.; Allen, E. B.

    2012-12-01

    Anthropogenic sources of nitrogen oxides have previously been shown to have distinctive isotopic signatures of oxygen and nitrogen. Nylon filters are currently used in passive sampling arrays to measure ambient atmospheric nitric acid concentrations and estimate deposition rates. This experiment measured the ability of nylon filters to consistently collect isotopologues of atmospheric nitric acid in the same ratios as they are present in the atmosphere. Samplers were deployed in continuous stirred tank reactors (CSTR) and at field sites across a nitrogen deposition gradient in Southern California. Filters were exposed over a four week period with individual filters being subjected to 1-4 week exposure times. Extracted nitric acid were measured for δ18O and δ15N ratios and compared for consistency based on length of exposure and amount of HNO3 collected. Filters within the CSTRs collected HNO3 at a consistent rate in both high and low concentration chambers. After two weeks of exposure, the mean δ18O values were within 0.5‰ of the δ18O of the source HNO3 solution. The mean of all weekly exposures were within 0.5‰ of the δ15N of the source solution, but after three weeks, the mean δ15N of adsorbed HNO3 was within 0.2‰. As the length of the exposure increased, the variability of measured delta values decreased for both elements. The field samplers collected HNO3 consistent with previously measured values along a deposition gradient. The mean δ18O at high deposition sites was 52.2‰ compared to 35.7‰ at the low deposition sites. Mean δ15N values were similar at all sites across the deposition gradient. Due to precipitation events occurring during the exposure period, the δ15N and δ18O of nitric acid were highly variable at all field sites. At single sites, changes in δ15N and δ18O were negatively correlated, consistent with two-sourcing mixing dynamics, but the slope of the regressions differed between high and low deposition sites. Anthropogenic

  2. 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

  3. Simulating systematic errors in X-ray absorption spectroscopy experiments: Sample and beam effects

    Energy Technology Data Exchange (ETDEWEB)

    Curis, Emmanuel [Laboratoire de Biomathematiques, Faculte de Pharmacie, Universite Rene, Descartes (Paris V)-4, Avenue de l' Observatoire, 75006 Paris (France)]. E-mail: emmanuel.curis@univ-paris5.fr; Osan, Janos [KFKI Atomic Energy Research Institute (AEKI)-P.O. Box 49, H-1525 Budapest (Hungary); Falkenberg, Gerald [Hamburger Synchrotronstrahlungslabor (HASYLAB), Deutsches Elektronen-Synchrotron (DESY)-Notkestrasse 85, 22607 Hamburg (Germany); Benazeth, Simone [Laboratoire de Biomathematiques, Faculte de Pharmacie, Universite Rene, Descartes (Paris V)-4, Avenue de l' Observatoire, 75006 Paris (France); Laboratoire d' Utilisation du Rayonnement Electromagnetique (LURE)-Ba-hat timent 209D, Campus d' Orsay, 91406 Orsay (France); Toeroek, Szabina [KFKI Atomic Energy Research Institute (AEKI)-P.O. Box 49, H-1525 Budapest (Hungary)

    2005-07-15

    The article presents an analytical model to simulate experimental imperfections in the realization of an X-ray absorption spectroscopy experiment, performed in transmission or fluorescence mode. Distinction is made between sources of systematic errors on a time-scale basis, to select the more appropriate model for their handling. For short time-scale, statistical models are the most suited. For large time-scale, the model is developed for sample and beam imperfections: mainly sample inhomogeneity, sample self-absorption, beam achromaticity. The ability of this model to reproduce the effects of these imperfections is exemplified, and the model is validated on real samples. Various potential application fields of the model are then presented.

  4. Simulating systematic errors in X-ray absorption spectroscopy experiments: Sample and beam effects

    International Nuclear Information System (INIS)

    Curis, Emmanuel; Osan, Janos; Falkenberg, Gerald; Benazeth, Simone; Toeroek, Szabina

    2005-01-01

    The article presents an analytical model to simulate experimental imperfections in the realization of an X-ray absorption spectroscopy experiment, performed in transmission or fluorescence mode. Distinction is made between sources of systematic errors on a time-scale basis, to select the more appropriate model for their handling. For short time-scale, statistical models are the most suited. For large time-scale, the model is developed for sample and beam imperfections: mainly sample inhomogeneity, sample self-absorption, beam achromaticity. The ability of this model to reproduce the effects of these imperfections is exemplified, and the model is validated on real samples. Various potential application fields of the model are then presented

  5. Thermal neutron absorption cross-section for small samples (experiments in cylindrical geometry)

    International Nuclear Information System (INIS)

    Czubek, J.A.; Drozdowicz, K.; Igielski, A.; Krynicka-Drozdowicz, E.; Woznicka, U.

    1982-01-01

    Measurement results for thermal neutron macroscopic absorption cross-sections Σsub(a)1 when applying the cylindrical sample-moderator system are presented. Experiments for liquid (water solutions of H 3 BO 3 ) and solid (crushed basalts) samples are reported. Solid samples have been saturated with the H 3 BO 3 ''poisoning'' solution. The accuracy obtained for the determination of the absorption cross-section of the solid material was σ(Σsub(ma))=(1.2+2.2) c.u. in the case when porosity was measured with the accuracy of σ(phi)=0.001+0.002. The dispersion of the Σsub(ma) data obtained for basalts (taken from different quarries) was higher than the accuracy of the measurement. All experimental data for the fundamental decay constants lambda 0 together with the whole information about the samples are given. (author)

  6. Procedure for intercomparison study for trace elements determination in soil samples by absorption spectroscopy

    International Nuclear Information System (INIS)

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

    1996-01-01

    In the environmental sampling analysis there is very important to establish an adequate methodologies on the laboratories for improvement the quality of the results obtained, so the establishment of a qualified laboratories network for environmental analysis. The objective of this work is to show the working plan for the analysis of eight elements on a Russian soil sample for an interlaboratory comparison with IAEA, by the Absorption spectroscopy technique using flame. (Author)

  7. Determination Of Activity Of Radionuclides In Moss-Soil Sample With Self-Absorption Correction

    International Nuclear Information System (INIS)

    Tran Thien Thanh; Chau Van Tao; Truong Thi Hong Loan; Hoang Duc Tam

    2011-01-01

    Hyper Pure Germanium (HPGe) spectrometer system is a very powerful tool for radioactivity measurements. The systematic uncertainty in the full energy peak efficiency is due to the differences between the matrix (density and chemical composition) of the reference and the other bulk samples. For getting precision from the gamma spectrum analysis, the absorbed correction in the sample should be considered. For gamma spectral analysis, a correction for absorption effects in sample should be considered, especially for bulk samples. The results were presented and discussed in this paper. (author)

  8. White light photothermal lens spectrophotometer for the determination of absorption in scattering samples.

    Science.gov (United States)

    Marcano, Aristides; Alvarado, Salvador; Meng, Junwei; Caballero, Daniel; Moares, Ernesto Marín; Edziah, Raymond

    2014-01-01

    We developed a pump-probe photothermal lens spectrophotometer that uses a broadband arc-lamp and a set of interference filters to provide tunable, nearly monochromatic radiation between 370 and 730 nm as the pump light source. This light is focused onto an absorbing sample, generating a photothermal lens of millimeter dimensions. A highly collimated monochromatic probe light from a low-power He-Ne laser interrogates the generated lens, yielding a photothermal signal proportional to the absorption of light. We measure the absorption spectra of scattering dye solutions using the device. We show that the spectra are not affected by the presence of scattering, confirming that the method only measures the absorption of light that results in generation of heat. By comparing the photothermal spectra with the usual absorption spectra determined using commercial transmission spectrophotometers, we estimate the quantum yield of scattering of the sample. We discuss applications of the device for spectroscopic characterization of samples such as blood and gold nanoparticles that exhibit a complex behavior upon interaction with light.

  9. X-ray speckle contrast variation at a sample-specific absorption edges

    International Nuclear Information System (INIS)

    Retsch, C. C.; Wang, Y.; Frigo, S. P.; Stephenson, G. B.; McNulty, I.

    2000-01-01

    The authors measured static x-ray speckle contrast variation with the incident photon energy across sample-specific absorption edges. They propose that the variation depends strongly on the spectral response function of the monochromator. Speckle techniques have been introduced to the x-ray regime during recent years. Most of these experiments, however, were done at photon energies above 5 keV. They are working on this technique in the 1 to 4 keV range, an energy range that includes many important x-ray absorption edges, e.g., in Al, Si, P, S, the rare-earths, and others. To their knowledge, the effect of absorption edges on speckle contrast has not yet been studied. In this paper, they present their initial measurements and understanding of the observed phenomena

  10. Secondary electron emission and self-consistent charge transport in semi-insulating samples

    Energy Technology Data Exchange (ETDEWEB)

    Fitting, H.-J. [Institute of Physics, University of Rostock, Universitaetsplatz 3, D-18051 Rostock (Germany); Touzin, M. [Unite Materiaux et Transformations, UMR CNRS 8207, Universite de Lille 1, F-59655 Villeneuve d' Ascq (France)

    2011-08-15

    Electron beam induced self-consistent charge transport and secondary electron emission (SEE) in insulators are described by means of an electron-hole flight-drift model (FDM) now extended by a certain intrinsic conductivity (c) and are implemented by an iterative computer simulation. Ballistic secondary electrons (SE) and holes, their attenuation to drifting charge carriers, and their recombination, trapping, and field- and temperature-dependent detrapping are included. As a main result the time dependent ''true'' secondary electron emission rate {delta}(t) released from the target material and based on ballistic electrons and the spatial distributions of currents j(x,t), charges {rho}(x,t), field F(x,t), and potential V(x,t) are obtained where V{sub 0} = V(0,t) presents the surface potential. The intrinsic electronic conductivity limits the charging process and leads to a conduction sample current to the support. In that case the steady-state total SE yield will be fixed below the unit: i.e., {sigma} {eta} + {delta} < 1.

  11. Atomic absorption determination of ultratrace tellurium in rocks utilizing high sensitivity sampling systems

    International Nuclear Information System (INIS)

    Beaty, R.D.

    1973-01-01

    The sampling boat and the graphite furnace were shown to possess the required sensitivity to detect tellurium at ultratrace levels, in a variety of sample types, by atomic absorption. In the sampling boat approach, tellurium in sample solutions is chemically separated and concentrated by extraction into methyl isobutyl ketone before measurement. For samples exhibiting extraction interferences or excessively high background absorption, a preliminary separation of tellurium by coprecipitation with selenium is described. Using this technique, tellurium can be quantitatively detected down to 5 nanograms and linear response is observed to 100 nanograms. Relative standard deviations of better than 7 percent are achieved for 50 nanograms of tellurium. For samples that have a tellurium content below the detection limits of the sampling boat, the graphite furnace is used for atomization. By this method, as little as 0.07 nanograms of tellurium can be detected, and a precision of 1 percent relative standard deviation is achievable at the 5 nanogram level. A routinely applicable procedure was developed for determining tellurium in rocks, using the graphite furnace, after a hydrofluoric acid decomposition of the sample. Using this procedure, tellurium data were obtained on 20 different rocks, and the significance of this new information is discussed. (Diss. Abstr. Int., B)

  12. Correction for the absorption of plutonium alpha particles in filter paper used for dust sampling

    Energy Technology Data Exchange (ETDEWEB)

    Simons, J G

    1956-01-01

    This sample of air-borne dust collected on a filter paper when laboratory air is monitored for plutonium with the 1195 portable dust sampling unit may be regarded, for counting purposes, as a thick source with a non-uniform distribution of alpha-active plutonium. Experiments have been carried out to determine a correction factor to be applied to the observed count on the filter paper sample to correct for internal absorption in the paper and on the dust layer. From the results obtained it is recommended that a correction factor of 2 be used.

  13. On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yebra, M.C.; Moreno-Cid, A.

    2003-01-01

    Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g -1 manganese (dry mass). The detection limit is 0.4 μg g -1 (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples

  14. Introduction of Flame Atomic Absorption Spectrometry (FAAS) For River Water Samples Analysis

    International Nuclear Information System (INIS)

    Shakirah Abd Shukor; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman

    2015-01-01

    Metal contamination in water is a major component in the determination of water quality monitoring. In spite of the viability of several other metal ion analysis techniques for river water, atomic absorption spectroscopy (AAS) method is most commonly used due to the reproducibility results, short analysis time, cost effective, lower level detection and robust. Therefore, this article gives an overview on the principles, instrumentation techniques, sample preparations, instrument calibration and data analysis in a simple manner for beginner. (author)

  15. Matrix modifiers application during microimpurities determination in complex samples by electrothermal atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Bejzel', N.F.; Daaman, F.I.; Fuks-Pol', G.R.; Yudelevich, I.G.

    1993-01-01

    The review covers publications of primarily last 5 years and is devoted to the use of matrix modifiers (MM) for the determinations of trace impurities in complex samples by electrothermal atomic-absorption analysis. The role of MM in analytical process has been discussed as well as MM influence on all the elements of analytical system; factors, determining the effectiveness of MM action, the basis types of MM have been described. A great body of information is tabulated on the use of different MM for the determination of particular analysis in geological, medicobiological, technological, ecological samples and in pure materials and chemicals

  16. Matrix modification for determination of microimpurities in complex samples by electrothermal atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Bejzel', N.F.; Daaman, F.I.; Fuks-Pol', G.R.; Yudelevich, I.G.

    1993-01-01

    The review covers publications of primarily last 5 years and is devoted to the use of matrix modifiers (MM) for the determinations of trace impurities in complex samples by electrothermal atomic-absorption analysis. The role of MM in analytical process has been discussed as well as MM influence on all the elements of analytical system; factors, determining the effectiveness of MM action, the basis types of MM have been described. A great body of information is tabulated on the use of different MM for the determination of particular analysis in geological, medicobiological, technological, ecological samples and in pure materials and chemicals

  17. Mercury speciation in environmental solid samples using thermal release technique with atomic absorption detection

    Energy Technology Data Exchange (ETDEWEB)

    Shuvaeva, Olga V. [Institute of Inorganic Chemistry, Academician Lavrent' ev Prospect 3, 630090 Novosbirsk (Russian Federation)], E-mail: olga@che.nsk.su; Gustaytis, Maria A.; Anoshin, Gennadii N. [Institute of Geology and Mineralogy, Siberian Branch of Russian Academy of Sciences, Koptyug Prospect 3, 630090 Novosibirsk (Russian Federation)

    2008-07-28

    A sensitive and very simple method for determination of mercury species in solid samples has been developed involving thermal release analysis in combination with atomic absorption (AAS) detection. The method allows determination of mercury(II) chloride, methylmercury and mercury sulfide at the level of 0.70, 0.35 and 0.20 ng with a reproducibility of the results of 14, 25 and 18%, respectively. The accuracy of the developed assay has been estimated using certified reference materials and by comparison of the results with those of an independent method. The method has been applied for Hg species determination in original samples of lake sediments and plankton.

  18. Results of Self-Absorption Study on the Versapor 3000 Filters for Radioactive Particulate Air Sampling

    International Nuclear Information System (INIS)

    Barnett, J.M.; Cullinan, Valerie I.; Barnett, Debra S.; Trang-Le, Truc LT; Bliss, Mary; Greenwood, Lawrence R.; Ballinger, Marcel Y.

    2009-01-01

    Since the mid-1980s, Pacific Northwest National Laboratory (PNNL) has used a value of 0.85 as the correction factor for self absorption of activity for particulate radioactive air samples collected from building exhaust for environmental monitoring. This value accounts for activity that cannot be detected by direct counting of alpha and beta particles. Emissions can be degraded or blocked by filter fibers for particles buried in the filter material or by inactive dust particles collected with the radioactive particles. These filters are used for monitoring air emissions from PNNL stacks for radioactive particles. This paper describes an effort to re-evaluate self-absorption effects in particulate radioactive air sample filters (Versapor(reg s ign) 3000, 47 mm diameter) used at PNNL. There were two methods used to characterize the samples. Sixty samples were selected from the archive for acid digestion to compare the radioactivity measured by direct gas-flow proportional counting of filters to the results obtained after acid digestion of the filter and counting again by gas-flow proportional detection. Thirty different sample filters were selected for visible light microscopy to evaluate filter loading and particulate characteristics. Mass-loading effects were also considered. Filter ratios were calculated by dividing the initial counts by the post-digestion counts with the expectation that post-digestion counts would be higher because digestion would expose radioactivity embedded in the filter in addition to that on top of the filter. Contrary to expectations, the post digestion readings were almost always lower than initial readings and averaged approximately half the initial readings for both alpha and beta activity. Before and after digestion readings appeared to be related to each other, but with a low coefficient of determination (R 2 ) value. The ratios had a wide range of values indicating that this method did not provide sufficient precision to quantify

  19. Low-energy absorption and luminescence of higher plant photosystem II core samples

    International Nuclear Information System (INIS)

    Hughes, Joseph L.; Smith, Paul J.; Pace, Ron J.; Krausz, Elmars

    2007-01-01

    The charge-separating state of PSII has been recently assigned as a homogeneously broadened band peaking at 705 nm. The possibility of observing emission due to luminescence from the charge-separating state was investigated. Emission from the charge-separating state is predicted to be both broad and substantially Stokes shifted. Our PSII cores show an easily observable and broad emission peaking near 735 nm when excited at 707 nm and beyond for temperatures below 100 K as well as the well-known F685 and F695 nm emission when excited at 633 nm. However, the 735 nm emission bears a close correspondence to that previously reported for the light harvesting pigment of photosystem I (PSI), LHCI-730, and we attribute our observed emission to a minor contamination of our sample with this protein. High sensitivity circular dichroism (CD) spectra establish that LHCI and/or PSI contamination of our samples does not contribute significantly to the absorption seen in the 700-730 nm region. Furthermore, systematic illumination-induced absorption changes seen in this region are shown to quantitatively track with charge separation and the subsequent secondary acceptor plastoquinone (Q A ) acceptor anion formation. These results confirm that absorption in the 700-730 nm region is associated with the reaction centre of active PSII

  20. 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)

  1. 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)

  2. The influence of the self-absorption on the measure of the total alpha activity in water samples

    International Nuclear Information System (INIS)

    Acena, M.L.; Gonzalez, J.A.; De Pablo, A.

    1981-01-01

    The self-absorption is an important difficulty in measuring α-activities in river water samples. A semiempirical equation for calculating the self-absorption versus sample thickness has been obtained. This equation is valid for the regular saline residues in spanish rivers and for thicknesses lower than 2 mg x cm -2 . This figure sets a limit for the amount of water to be evaporated from the sample. (author)

  3. Atomic absorption determination of metals in soils using ultrasonic sample preparation

    International Nuclear Information System (INIS)

    Chmilenko, F.A.; Smityuk, N.M.; Baklanov, A.N.

    2002-01-01

    It was shown that ultrasonic treatment accelerates sample preparation of soil extracts from chernozem into different solvents by a factor of 6 to 60. These extracts are used for the atomic absorption determination of soluble species of Cd, Co, Cr, Cu, Ni, Pb, and Zn. The optimum ultrasound parameters (frequency, intensity, and treatment time) were found for preparing soil extracts containing analytes in concentrations required in agrochemical procedures. Different extractants used to extract soluble heavy metals from soils of an ordinary chernozem type in agrochemical procedures using ultrasonic treatment were classified in accordance with the element nature [ru

  4. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

    1995-12-01

    Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

  5. Consistent Estimation of Continuous-Time Signals from Nonlinear Transformations of Noisy Samples,

    Science.gov (United States)

    1980-03-10

    t, then hn is given by (5) (with W = n) and represents the Szasz operator. Theorem 3.0, while guaranteeing mean-square consistency of the estimate Sw...t), provides no bounds on the rate of convergence. We shall derive such bounds for linear systems hW corresponding to the class of generalized Szasz ...operators [6] (see below) and to the Bernstein operator. While the Szasz operator (5) can be generated as in Proposition 3.0, the class of generalized

  6. The use of slurry sampling for the determination of manganese and copper in various samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tokman, Nilgun

    2007-01-01

    Manganese and copper in multivitamin-mineral supplements and standard reference materials were determined by slurry sampling electrothermal atomic absorption spectrometry. Slurries were prepared in an aqueous solution containing Triton X-100. The effects of different parameters such as ratio of solid to liquid phase volume, total slurry volume and addition of Triton X-100 as a dispersant on the analytical results were investigated. The graphite furnace programs were optimized for slurry sampling depending on the analytes and their concentrations in the samples. The linear calibration method with aqueous standard solutions was used for the quantification. At optimum experimental conditions, R.S.D. values were below 5%. The analytes were determined in the limits of 95% confidence level with respect to certified values in coal and soil standard reference materials and to those found by wet-digestion in multivitamin-mineral supplements. Detection limits (3δ) for Mn and Cu were 0.10 μg L -1 and 1.82 μg L -1 for 10 μL coal standard reference material slurry, respectively

  7. Wet sample digestion for quantification of vanadium(V) in serum by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Heinemann, G.; Vogt, W.; Jacob, K.

    1999-01-01

    Three types of pressure digestion systems used prior to the determination of the ultratrace element vanadium by electrothermal atomic absorption spectrometry were evaluated: The high-pressure ashing (HPA) system, the DAB III pressure digestion system and the pressurized microwave digestion (PMD) system. Complete sample digestion and no loss of graphite tube sensitivity as well as reliable vanadium values could only be achieved with HPA digests of freeze-dried serum. The mean recovery rate was 98% and no loss of tube sensitivity could be observed. Using non-lyophilized serum the mean recovery rate was 70%. The DAB III digestion system, vicarious for closed pressure digestion in steel bombs with an allowable temperature up to about 200C, cannot be recommended to mineralize human biological material for vanadium determinations, because the remaining not completely decomposed organic compounds extracted together with the vanadium-cupferron complex caused a marked carbon-buildup and formation of carbides in the graphite tube were found to change the shape of the absorption signals distinctly, and to decline the tube sensitivity strongly (about 25%) so that reliable results cannot be achieved. The recovery rate was too low in general (about 50%). In addition, a subsequent treatment of the DAB III digests with perchloric acid was unsuccessful. The PMD system proved to be not suited, because the samples became highly contaminated by vanadium possibly from the titan seal. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  8. Total CMB analysis of streaker aerosol samples by PIXE, PIGE, beta- and optical-absorption analyses

    International Nuclear Information System (INIS)

    Annegarn, H.J.; Przybylowicz, W.J.

    1993-01-01

    Multielemental analyses of aerosol samples are widely used in air pollution receptor modelling. Specifically, the chemical mass balance (CMB) model has become a powerful tool in urban air quality studies. Input data required for the CMB includes not only the traditional X-ray fluorescence (and hence PIXE) detected elements, but also total mass, organic and inorganic carbon, and other light elements including Mg, Na and F. The circular streaker sampler, in combination with PIXE analysis, has developed into a powerful tool for obtaining time-resolved, multielemental aerosol data. However, application in CMB modelling has been limited by the absence of total mass and complementary light element data. This study reports on progress in using techniques complementary to PIXE to obtain additional data from circular streaker samples, maintaining the nondestructive, instrumental approach inherent in PIXE: Beta-gauging using a 147 Pm source for total mass; optical absorption for inorganic carbon; and PIGE to measure the lighter elements. (orig.)

  9. [Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

    Science.gov (United States)

    Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

    2015-11-01

    To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

  10. Does volumetric absorptive microsampling eliminate the hematocrit bias for caffeine and paraxanthine in dried blood samples? A comparative study.

    Science.gov (United States)

    De Kesel, Pieter M M; Lambert, Willy E; Stove, Christophe P

    2015-06-30

    Volumetric absorptive microsampling (VAMS) is a novel sampling technique that allows the straightforward collection of an accurate volume of blood (approximately 10μL) from a drop or pool of blood by dipping an absorbent polymeric tip into it. The resulting blood microsample is dried and analyzed as a whole. The aim of this study was to evaluate the potential of VAMS to overcome the hematocrit bias, an important issue in the analysis of dried blood microsamples. An LC-MS/MS method for analysis of the model compounds caffeine and paraxanthine in VAMS samples was fully validated and fulfilled all pre-established criteria. In conjunction with previously validated procedures for dried blood spots (DBS) and blood, this allowed us to set up a meticulous comparative study in which both compounds were determined in over 80 corresponding VAMS, DBS and liquid whole blood samples. These originated from authentic human patient samples, covering a wide hematocrit range (0.21-0.50). By calculating the differences with reference whole blood concentrations, we found that analyte concentrations in VAMS samples were not affected by a bias that changed over the evaluated hematocrit range, in contrast to DBS results. However, VAMS concentrations tend to overestimate whole blood concentrations, as a consistent positive bias was observed. A different behavior of VAMS samples prepared from incurred and spiked blood, combined with a somewhat reduced recovery of caffeine and paraxanthine from VAMS tips at high hematocrit values, an effect that was not observed for DBS using a very similar extraction procedure, was found to be at the basis of the observed VAMS-whole blood deviations. Based on this study, being the first in which the validity and robustness of VAMS is evaluated by analyzing incurred human samples, it can be concluded that VAMS effectively assists in eliminating the effect of hematocrit. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

  11. Self-absorption of neutron capture gamma-rays in gold samples

    International Nuclear Information System (INIS)

    Wisshak, K.; Walter, G.; Kaeppeler, F.

    1983-06-01

    The self absorption of neutron capture gamma rays in gold samples has been determined experimentally for two standard setups used in measurements of neutron capture cross sections. One makes use of an artificially collimated neutron beam and two C 6 D 6 detectors, the other of kinematically collimated neutrons and three Moxon-Rae detectors. Correction factors for an actual measurement of a neutron capture cross section using a gold standard of 1 mm thickness up to 12% were found for the first setup while they are only 4% for the second setup. The present data allow to determine the correction in an actual measurement with an accuracy of 0.5-1%. (orig.) [de

  12. Sensitivity and accuracy of atomic absorption spectrophotometry for trace elements in marine biological samples

    International Nuclear Information System (INIS)

    Fukai, R.; Oregioni, B.

    1976-01-01

    During the course of 1974-75 atomic absorption spectrophotometry (AAS) has been used extensively in our laboratory for measuring various trace elements in marine biological materials in order to conduct homogeneity tests on the intercalibration samples for trace metal analysis as well as to obtain baseline data for trace elements in various kinds of marine organisms collected from different locations in the Mediterranean Sea. Several series of test experiments have been conducted on the current methodology in use in our laboratory to ensure satisfactory analytical performance in measuring a number of trace elements for which analytical problems have not completely been solved. Sensitivities of the techniques used were repeatedly checked for various elements and the accuracy of the analyses were always critically evaluated by analyzing standard reference materials. The results of these test experiments have uncovered critical points relevant to the application of the AAS to routine analysis

  13. Evaluation of metal ion absorptive characteristics of three types of plastic sample bags used for pecipitation sampling

    Science.gov (United States)

    Good, A.B.; Schroder, L.J.

    1984-01-01

    Simulated precipitation samples containing 16 metal ions were prepared at 4 pH values. Absorptive characteristics of polypropylene, polyethylene, and polyester/polyolefin sacks were evaluated at pH 3.5, 4.0, 4.5, and 5.0. Simulated precipitation was in contact with the sacks for 17 days, and subsamples were removed for chemical analysis at 3, 7, 10, 14, and 17 days after initial contact. All three types of plastic sacks absorbed Fe throughout the entire pH range. Polypropylene and polyethylene absorbed Pb throughout the entire pH range; polyester/polyolefin sacks absorbed Pb at pH 4.0 or greater. All plastic sacks also absorbed Cu, Mo, and V at pH 4.5 and 5.0. Leaching the plastic sacks with 0.7 percent HNO3 did not result in 100 percent of Cu, Fe, Pb, and V. These sacks would be suitable collection vessels for Ba, Be, Ca, Cd, Co, Li, Mg, Mn, Na Sr and Zn in precipitation through the pH range of 3.5 to 5.0.

  14. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    International Nuclear Information System (INIS)

    Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; Furtado da Silva, Alessandra; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson Jose

    2005-01-01

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1

  15. Rare earth analysis in human biological samples by atomic absorption using electrothermal atomization

    International Nuclear Information System (INIS)

    Citron, I.M.; Holtzman, R.B.; Leiman, J.

    1982-01-01

    The determination of Sc and seven rare earth elements, Nd, Sm, Dy, Ho, Eu, Tm, and Yb, in biological samplesby atomic absorption spectrophotometric analysis (AAS) using electrothermal atomization in a pyrolytic graphite tube is shown to be rapid, precise and accurate. The technique utilizes the method of standard additions and linear regression analysis to determine results from peak area data. Inter-elemental interferences are negligible. The elements found sensitive enough for this type of analysis are, in order of decreasing sensitivity, Yb, Eu, Tm, Dy, Sc, Ho, Sm and Nd. The determination in these types of materials of Gd and elements less sensitive to AAS detection than Gd does not appear to be feasible. Results are presented on the concentrations of these elements in 41 samples from human subjects, cows and vegetables with normal environmental exposure to the rare earth elements. The composite percent mean deviation in peak-area readings for all samples and all elements examined was 4%. The mean standard error in the results among samples was about 6.5%

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

    Science.gov (United States)

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

    2015-12-01

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

  17. A sample design for globally consistent biomass estimation using lidar data from the Geoscience Laser Altimeter System (GLAS)

    Science.gov (United States)

    Sean P. Healey; Paul L. Patterson; Sassan S. Saatchi; Michael A. Lefsky; Andrew J. Lister; Elizabeth A. Freeman

    2012-01-01

    Lidar height data collected by the Geosciences Laser Altimeter System (GLAS) from 2002 to 2008 has the potential to form the basis of a globally consistent sample-based inventory of forest biomass. GLAS lidar return data were collected globally in spatially discrete full waveform "shots," which have been shown to be strongly correlated with aboveground forest...

  18. BROAD ABSORPTION LINE VARIABILITY ON MULTI-YEAR TIMESCALES IN A LARGE QUASAR SAMPLE

    Energy Technology Data Exchange (ETDEWEB)

    Filiz Ak, N.; Brandt, W. N.; Schneider, D. P. [Department of Astronomy and Astrophysics, Pennsylvania State University, University Park, PA 16802 (United States); Hall, P. B. [Department of Physics and Astronomy, York University, 4700 Keele St., Toronto, Ontario, M3J 1P3 (Canada); Anderson, S. F. [Astronomy Department, University of Washington, Seattle, WA 98195 (United States); Hamann, F. [Department of Astronomy, University of Florida, Gainesville, FL 32611-2055 (United States); Lundgren, B. F. [Department of Astronomy, University of Wisconsin, Madison, WI 53706 (United States); Myers, Adam D. [Department of Physics and Astronomy, University of Wyoming, Laramie, WY 82071 (United States); Pâris, I. [Departamento de Astronomía, Universidad de Chile, Casilla 36-D, Santiago (Chile); Petitjean, P. [Universite Paris 6, Institut d' Astrophysique de Paris, 75014, Paris (France); Ross, Nicholas P. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 92420 (United States); Shen, Yue [Harvard-Smithsonian Center for Astrophysics, 60 Garden St., MS-51, Cambridge, MA 02138 (United States); York, Don, E-mail: nfilizak@astro.psu.edu [The University of Chicago, Department of Astronomy and Astrophysics, Chicago, IL 60637 (United States)

    2013-11-10

    We present a detailed investigation of the variability of 428 C IV and 235 Si IV broad absorption line (BAL) troughs identified in multi-epoch observations of 291 quasars by the Sloan Digital Sky Survey-I/II/III. These observations primarily sample rest-frame timescales of 1-3.7 yr over which significant rearrangement of the BAL wind is expected. We derive a number of observational results on, e.g., the frequency of BAL variability, the velocity range over which BAL variability occurs, the primary observed form of BAL-trough variability, the dependence of BAL variability upon timescale, the frequency of BAL strengthening versus weakening, correlations between BAL variability and BAL-trough profiles, relations between C IV and Si IV BAL variability, coordinated multi-trough variability, and BAL variations as a function of quasar properties. We assess implications of these observational results for quasar winds. Our results support models where most BAL absorption is formed within an order-of-magnitude of the wind-launching radius, although a significant minority of BAL troughs may arise on larger scales. We estimate an average lifetime for a BAL trough along our line-of-sight of a few thousand years. BAL disappearance and emergence events appear to be extremes of general BAL variability, rather than being qualitatively distinct phenomena. We derive the parameters of a random-walk model for BAL EW variability, finding that this model can acceptably describe some key aspects of EW variability. The coordinated trough variability of BAL quasars with multiple troughs suggests that changes in 'shielding gas' may play a significant role in driving general BAL variability.

  19. Effects of sampling methods on the quantity and quality of dissolved organic matter in sediment pore waters as revealed by absorption and fluorescence spectroscopy.

    Science.gov (United States)

    Chen, Meilian; Lee, Jong-Hyeon; Hur, Jin

    2015-10-01

    Despite literature evidence suggesting the importance of sampling methods on the properties of sediment pore waters, their effects on the dissolved organic matter (PW-DOM) have been unexplored to date. Here, we compared the effects of two commonly used sampling methods (i.e., centrifuge and Rhizon sampler) on the characteristics of PW-DOM for the first time. The bulk dissolved organic carbon (DOC), ultraviolet-visible (UV-Vis) absorption, and excitation-emission matrixes coupled with parallel factor analysis (EEM-PARAFAC) of the PW-DOM samples were compared for the two sampling methods with the sediments from minimal to severely contaminated sites. The centrifuged samples were found to have higher average values of DOC, UV absorption, and protein-like EEM-PARAFAC components. The samples collected with the Rhizon sampler, however, exhibited generally more humified characteristics than the centrifuged ones, implying a preferential collection of PW-DOM with respect to the sampling methods. Furthermore, the differences between the two sampling methods seem more pronounced in relatively more polluted sites. Our observations were possibly explained by either the filtration effect resulting from the smaller pore size of the Rhizon sampler or the desorption of DOM molecules loosely bound to minerals during centrifugation, or both. Our study suggests that consistent use of one sampling method is crucial for PW-DOM studies and also that caution should be taken in the comparison of data collected with different sampling methods.

  20. A comparison of the modulated microwave absorption spectra of ceramic and powdered YBa2Cu3O7-δ samples

    International Nuclear Information System (INIS)

    Rubins, R.S.; Hutton, S.L.; Drumheller, J.E.; Jeong, D.Y.; Black, T.D.

    1990-01-01

    Flux trapping in the 9.3 GHz modulated microwave absorption spectra observed near 4 K from ceramic and powdered ceramic specimens of two separately prepared YBa 2 Cu 3 O 7-δ samples has been used to separate the intergranular and intragranular contributions to the spectra. In the denser, glassy sample, a broad absorption with a peak near 400 Oe for forward sweeps was observed with appreciable intensity after the maximum flux was trapped. This spectrum is attributed to intergranular junctions, since its relative intensity was reduced on powdering and suspending in wax. In the less dense, more uniform sample, the latter spectrum was appreciably weaker in both ceramic and powder. Both types of junction appear to contribute to the narrow low-field absorption which was observed after zero field cooling in all the samples

  1. Random Photon Absorption Model Elucidates How Early Gain Control in Fly Photoreceptors Arises from Quantal Sampling

    Science.gov (United States)

    Song, Zhuoyi; Zhou, Yu; Juusola, Mikko

    2016-01-01

    Many diurnal photoreceptors encode vast real-world light changes effectively, but how this performance originates from photon sampling is unclear. A 4-module biophysically-realistic fly photoreceptor model, in which information capture is limited by the number of its sampling units (microvilli) and their photon-hit recovery time (refractoriness), can accurately simulate real recordings and their information content. However, sublinear summation in quantum bump production (quantum-gain-nonlinearity) may also cause adaptation by reducing the bump/photon gain when multiple photons hit the same microvillus simultaneously. Here, we use a Random Photon Absorption Model (RandPAM), which is the 1st module of the 4-module fly photoreceptor model, to quantify the contribution of quantum-gain-nonlinearity in light adaptation. We show how quantum-gain-nonlinearity already results from photon sampling alone. In the extreme case, when two or more simultaneous photon-hits reduce to a single sublinear value, quantum-gain-nonlinearity is preset before the phototransduction reactions adapt the quantum bump waveform. However, the contribution of quantum-gain-nonlinearity in light adaptation depends upon the likelihood of multi-photon-hits, which is strictly determined by the number of microvilli and light intensity. Specifically, its contribution to light-adaptation is marginal (≤ 1%) in fly photoreceptors with many thousands of microvilli, because the probability of simultaneous multi-photon-hits on any one microvillus is low even during daylight conditions. However, in cells with fewer sampling units, the impact of quantum-gain-nonlinearity increases with brightening light. PMID:27445779

  2. Environmental samples analysis by Atomic Absorption Spectrophotometry and Inductively Coupled Plasma-Optical Emission Spectroscopy

    International Nuclear Information System (INIS)

    Popescu, I.V.; Iordan, M.; Stihi, C.; Bancuta, A.; Busuioc, G.; Dima, G.; Ciupina, V.; Belc, M.; Vlaicu, Gh.; Marian, R.

    2002-01-01

    Biological samples are interesting from many aspects of environmental monitoring. By analyzing tree leaves conclusions can be drown regarding the metal loading in the growth medium. So that, starting from assumption that the pollution factors from environmental medium can modify the normal concentration of elements, we decided to control the presence of toxic elements and the deviation from normal state of elements in leaves of different trees from areas situated at different distances of pollution source. The aim of this work is to determine the elemental composition of tree leaves using Atomic Absorption Spectrophotometry (AAS) method and Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) method. Using AAS spectrophotometer SHIMADZU we identified and determined the concentration of: Cd, Co, Cu, Zn, Mn, Cr, Fe, Se, Pb with an instrumental error less than 1% for most of the elements analyzed. The same samples were analyzed by ICP-OES spectrometer, BAIRD ICP2070-Sequential Plasma spectrometer. We identified and determined in leaves of different trees the concentration of Mg, Ca, and Sr with a precision less than 6%. (authors)

  3. Overcoming Matrix Effects in a Complex Sample: Analysis of Multiple Elements in Multivitamins by Atomic Absorption Spectroscopy

    Science.gov (United States)

    Arnold, Randy J.; Arndt, Brett; Blaser, Emilia; Blosser, Chris; Caulton, Dana; Chung, Won Sog; Fiorenza, Garrett; Heath, Wyatt; Jacobs, Alex; Kahng, Eunice; Koh, Eun; Le, Thao; Mandla, Kyle; McCory, Chelsey; Newman, Laura; Pithadia, Amit; Reckelhoff, Anna; Rheinhardt, Joseph; Skljarevski, Sonja; Stuart, Jordyn; Taylor, Cassie; Thomas, Scott; Tse, Kyle; Wall, Rachel; Warkentien, Chad

    2011-01-01

    A multivitamin tablet and liquid are analyzed for the elements calcium, magnesium, iron, zinc, copper, and manganese using atomic absorption spectrometry. Linear calibration and standard addition are used for all elements except calcium, allowing for an estimate of the matrix effects encountered for this complex sample. Sample preparation using…

  4. {sup 137}Cs Absorption factors (Afs) some vegetable and protein samples in cooking

    Energy Technology Data Exchange (ETDEWEB)

    Malek, M A [Bangladesh Atomic Energy Commission, Dhaka (Bangladesh); Nakahara, M [National Institute of Radiological Sciences, Hitachinaka City (Japan)

    2004-07-01

    Full text: The human race uses fresh water for cooking, drinking and washing purposes. The source of fresh water may be radioactively contaminated by various sources of contaminants. With the increased use of radioisotopes, nuclear testing, possible nuclear warfare and terror activities, the apprehension of widespread contamination of the surface and ground water is increasing day by day. In the case of widespread contamination of freshwater sources, people may be compelled to use the contaminated water. The radionuclides in fresh water may enter the human body through two major routes: drinking and cooking food with the water. During cooking, the radionuclide present in the water may be transferred to the various ingredients of the cooked dish. The degree of contamination in the ingredients during the cooking depends on the absorption power of the individual ingredients and on the level of radionuclide present in the water. The ratio of the concentration of the radionuclide absorbed in the ingredients to the concentration in the water can be designated as the 'Absorption factor' (Af). A consumer always has the choice of eating either the whole dish or a part of the dish. The Af of every consumed ingredient can be used to predict the radionuclide absorbed by the individual ingredients cooked with contaminated water, and as such to predict the dose to the consumer. The factor can also be used to assess the dispersion of radionuclide from the water used in cooking to the ingredients in the cooked dish. A better understanding of variables in the cooking that affect the Af in various ingredients is central to deriving the contamination level of the ingredients. To the best of our knowledge, no investigation on this topic has been conducted before. In order to assess this topic and for obtaining base line data, a research project was undertaken to determine the Afs of some vegetable and protein samples, and to investigate the effects of salinity and cooling on Af

  5. An approach based on HPLC-fingerprint and chemometrics to quality consistency evaluation of Matricaria chamomilla L. commercial samples

    Directory of Open Access Journals (Sweden)

    Agnieszka Viapiana

    2016-10-01

    Full Text Available Chamomile has been used as an herbal medication since ancient times and is still popular because it contains various bioactive phytochemicals that could provide therapeutic effects. In this study, a simple and reliable HPLC method was developed to evaluate the quality consistency of nineteen chamomile samples through establishing a chromatographic fingerprint, quantification of phenolic compounds and determination of antioxidant activity. For fingerprint analysis, 12 peaks were selected as the common peaks to evaluate the similarities of commercial samples of chamomile obtained from different manufacturers. A similarity analysis was performed to assess the similarity/dissimilarity of chamomile samples where values varied from 0.868 to 0.990 what indicating that samples from different manufacturers were consistent. Additionally, simultaneous quantification of five phenolic acids (gallic, caffeic, syringic, p-coumaric, ferulic and four flavonoids (rutin, myricetin, quercetin and keampferol was performed to interpret the quality consistency. In quantitative analysis, the nine individual phenolic compounds showed good regression (r > 0.9975. Inter- and intra-day precisions for all analysed compounds expressed as relative standard deviation (CV ranged from 0.05% to 3.12%. Since flavonoids and other polyphenols are commonly recognised as natural antioxidants, the antioxidant activity of chamomile samples was evaluated using 1,1-diphenyl-2-picrylhydrazyl (DPPH radical scavenging activity and ferric reducing/antioxidant power (FRAP assay. Correlation analysis was used to assess the relationship between antioxidant activity and phenolic composition, and multivariate analysis (PCA and HCA were applied to distinguish chamomile samples. Results shown in the study indicate high similarity of chamomile samples among them, widely spread in the market and commonly used by people as infusions or teas, as well as that there were no statistically significant

  6. An Approach Based on HPLC-Fingerprint and Chemometrics to Quality Consistency Evaluation of Matricaria chamomilla L. Commercial Samples

    Science.gov (United States)

    Viapiana, Agnieszka; Struck-Lewicka, Wiktoria; Konieczynski, Pawel; Wesolowski, Marek; Kaliszan, Roman

    2016-01-01

    Chamomile has been used as an herbal medication since ancient times and is still popular because it contains various bioactive phytochemicals that could provide therapeutic effects. In this study, a simple and reliable HPLC method was developed to evaluate the quality consistency of nineteen chamomile samples through establishing a chromatographic fingerprint, quantification of phenolic compounds and determination of antioxidant activity. For fingerprint analysis, 12 peaks were selected as the common peaks to evaluate the similarities of commercial samples of chamomile obtained from different manufacturers. A similarity analysis was performed to assess the similarity/dissimilarity of chamomile samples where values varied from 0.868 to 0.990 what indicating that samples from different manufacturers were consistent. Additionally, simultaneous quantification of five phenolic acids (gallic, caffeic, syringic, p-coumaric, ferulic) and four flavonoids (rutin, myricetin, quercetin and keampferol) was performed to interpret the quality consistency. In quantitative analysis, the nine individual phenolic compounds showed good regression (r > 0.9975). Inter- and intra-day precisions for all analyzed compounds expressed as relative standard deviation (CV) ranged from 0.05% to 3.12%. Since flavonoids and other polyphenols are commonly recognized as natural antioxidants, the antioxidant activity of chamomile samples was evaluated using 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging activity and ferric reducing/antioxidant power (FRAP) assay. Correlation analysis was used to assess the relationship between antioxidant activity and phenolic composition, and multivariate analysis (PCA and HCA) were applied to distinguish chamomile samples. Results shown in the study indicate high similarity of chamomile samples among them, widely spread in the market and commonly used by people as infusions or teas, as well as that there were no statistically significant differences among

  7. Discussion of parameters associated with the determination of arsenic by electrothermal atomic absorption spectrometry in slurried environmental samples.

    Science.gov (United States)

    Vassileva, E; Baeten, H; Hoenig, M

    2001-01-02

    A slurry sampling-fast program procedure has been developed for the determination of arsenic in plants, soils and sediments by electrothermal atomic absorption spectrometry. Efficiencies of various single and mixed modifiers for thermal stabilization of arsenic and for a better removal of the matrix during pyrolysis step were compared. The influence of the slurry concentration, amounts of modifier and parameters of the pyrolysis step on the As integrated absorbance signals have been studied and a comparison between fast and conventional furnace programs was also made. The ultrasonic agitation of the slurry followed by a fast electrothermal program using an Ir/Mg modifier provides the most consistent performance in terms of precision and accuracy. The reliability of the whole procedure has been compared with results obtained after application of a wet digestion method with an HF step and validated by analyzing eleven certified reference materials. Arsenic detection and quantitation limits expressed on dry sample matter were about 30 and 100 micrograms kg-1, respectively.

  8. An Approach Based on HPLC-Fingerprint and Chemometrics to Quality Consistency Evaluation of Matricaria chamomilla L. Commercial Samples

    OpenAIRE

    Viapiana, Agnieszka; Struck-Lewicka, Wiktoria; Konieczynski, Pawel; Wesolowski, Marek; Kaliszan, Roman

    2016-01-01

    Chamomile has been used as an herbal medication since ancient times and is still popular because it contains various bioactive phytochemicals that could provide therapeutic effects. In this study, a simple and reliable HPLC method was developed to evaluate the quality consistency of nineteen chamomile samples through establishing a chromatographic fingerprint, quantification of phenolic compounds and determination of antioxidant activity. For fingerprint analysis, 12 peaks were selected as th...

  9. Determination of cadmium in real water samples by flame atomic absorption spectrometry after cloud point extraction

    International Nuclear Information System (INIS)

    Naeemullah, A.; Kazi, T.G.

    2011-01-01

    Water pollution is a global threat and it is the leading world wide cause of death and diseases. The awareness of the potential danger posed by heavy metals to the ecosystems and in particular to human health has grown tremendously in the past decades. Separation and preconcentration procedures are considered of great importance in analytical and environmental chemistry. Cloud point is one of the most reliable and sophisticated separation methods for determination of traces quantities of heavy metals. Cloud point methodology was successfully employed for preconcentration of trace quantities of cadmium prior to their determination by flame atomic absorption spectrometry (FAAS). The metals react with 8-hydroxquinoline in a surfactant Triton X-114 medium. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation and the cadmium content was measured by FAAS. The validation of the procedure was carried out by spiking addition methods. The method was applied for determination of Cd in water samples of different ecosystems (lake and river). (author)

  10. BROAD ABSORPTION LINE DISAPPEARANCE ON MULTI-YEAR TIMESCALES IN A LARGE QUASAR SAMPLE

    Energy Technology Data Exchange (ETDEWEB)

    Filiz Ak, N.; Brandt, W. N.; Schneider, D. P. [Department of Astronomy and Astrophysics, Pennsylvania State University, University Park, PA 16802 (United States); Hall, P. B. [Department of Physics and Astronomy, York University, 4700 Keele St., Toronto, Ontario M3J 1P3 (Canada); Anderson, S. F.; Gibson, R. R. [Astronomy Department, University of Washington, Seattle, WA 98195 (United States); Lundgren, B. F. [Department of Physics, Yale University, New Haven, CT 06511 (United States); Myers, A. D. [Department of Physics and Astronomy, University of Wyoming, Laramie, WY 82071 (United States); Petitjean, P. [Institut d' Astrophysique de Paris, Universite Paris 6, F-75014, Paris (France); Ross, Nicholas P. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 92420 (United States); Shen Yue [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, MS-51, Cambridge, MA 02138 (United States); York, D. G. [Department of Astronomy and Astrophysics, and Enrico Fermi Institute, University of Chicago, 5640 S. Ellis Ave., Chicago, IL 60637 (United States); Bizyaev, D.; Brinkmann, J.; Malanushenko, E.; Oravetz, D. J.; Pan, K.; Simmons, A. E. [Apache Point Observatory, P.O. Box 59, Sunspot, NM 88349-0059 (United States); Weaver, B. A., E-mail: nfilizak@astro.psu.edu [Center for Cosmology and Particle Physics, New York University, New York, NY 10003 (United States)

    2012-10-01

    We present 21 examples of C IV broad absorption line (BAL) trough disappearance in 19 quasars selected from systematic multi-epoch observations of 582 bright BAL quasars (1.9 < z < 4.5) by the Sloan Digital Sky Survey-I/II (SDSS-I/II) and SDSS-III. The observations span 1.1-3.9 yr rest-frame timescales, longer than have been sampled in many previous BAL variability studies. On these timescales, Almost-Equal-To 2.3% of C IV BAL troughs disappear and Almost-Equal-To 3.3% of BAL quasars show a disappearing trough. These observed frequencies suggest that many C IV BAL absorbers spend on average at most a century along our line of sight to their quasar. Ten of the 19 BAL quasars showing C IV BAL disappearance have apparently transformed from BAL to non-BAL quasars; these are the first reported examples of such transformations. The BAL troughs that disappear tend to be those with small-to-moderate equivalent widths, relatively shallow depths, and high outflow velocities. Other non-disappearing C IV BALs in those nine objects having multiple troughs tend to weaken when one of them disappears, indicating a connection between the disappearing and non-disappearing troughs, even for velocity separations as large as 10,000-15,000 km s{sup -1}. We discuss possible origins of this connection including disk-wind rotation and changes in shielding gas.

  11. High-throughput liquid-absorption air-sampling apparatus and methods

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2000-07-11

    A portable high-throughput liquid-absorption air sampler [PHTLAAS] has an asymmetric air inlet through which air is drawn upward by a small and light-weight centrifugal fan driven by a direct current motor that can be powered by a battery. The air inlet is so configured as to impart both rotational and downward components of motion to the sampled air near said inlet. The PHTLAAS comprises a glass tube of relatively small size through which air passes at a high rate in a swirling, highly turbulent motion, which facilitates rapid transfer of vapors and particulates to a liquid film covering the inner walls of the tube. The pressure drop through the glass tube is < 10 cm of water, usually < 5 cm of water. The sampler's collection efficiency is usually > 20% for vapors or airborne particulates in the 2--3 microns range and > 50% for particles larger than 4 microns. In conjunction with various analyzers, the PHTLAAS can serve to monitor a variety of hazardous or illicit airborne substances, such as lead-containing particulates, tritiated water vapor, biological aerosols, or traces of concealed drugs or explosives.

  12. High-throughput liquid-absorption air-sampling apparatus and methods

    Science.gov (United States)

    Zaromb, Solomon

    2000-01-01

    A portable high-throughput liquid-absorption air sampler [PHTLAAS] has an asymmetric air inlet through which air is drawn upward by a small and light-weight centrifugal fan driven by a direct current motor that can be powered by a battery. The air inlet is so configured as to impart both rotational and downward components of motion to the sampled air near said inlet. The PHTLAAS comprises a glass tube of relatively small size through which air passes at a high rate in a swirling, highly turbulent motion, which facilitates rapid transfer of vapors and particulates to a liquid film covering the inner walls of the tube. The pressure drop through the glass tube is 20% for vapors or airborne particulates in the 2-3.mu. range and >50% for particles larger than 4.mu.. In conjunction with various analyzers, the PHTLAAS can serve to monitor a variety of hazardous or illicit airborne substances, such as lead-containing particulates, tritiated water vapor, biological aerosols, or traces of concealed drugs or explosives.

  13. High-throughput liquid-absorption air-sampling apparatus and methods

    International Nuclear Information System (INIS)

    2000-01-01

    A portable high-throughput liquid-absorption air sampler [PHTLAAS] has an asymmetric air inlet through which air is drawn upward by a small and light-weight centrifugal fan driven by a direct current motor that can be powered by a battery. The air inlet is so configured as to impart both rotational and downward components of motion to the sampled air near said inlet. The PHTLAAS comprises a glass tube of relatively small size through which air passes at a high rate in a swirling, highly turbulent motion, which facilitates rapid transfer of vapors and particulates to a liquid film covering the inner walls of the tube. The pressure drop through the glass tube is 20% for vapors or airborne particulates in the 2--3 microns range and > 50% for particles larger than 4 microns. In conjunction with various analyzers, the PHTLAAS can serve to monitor a variety of hazardous or illicit airborne substances, such as lead-containing particulates, tritiated water vapor, biological aerosols, or traces of concealed drugs or explosives

  14. Comparison of conventional and total reflection excitation geometry for fluorescence X-ray absorption spectroscopy on droplet samples

    International Nuclear Information System (INIS)

    Falkenberg, G.; Pepponi, G.; Streli, C.; Wobrauschek, P.

    2003-01-01

    X-ray absorption fine structure (XAFS) experiments in fluorescence mode have been performed in total reflection excitation geometry and conventional 45 deg. /45 deg. excitation/detection geometry for comparison. The experimental results have shown that XAFS measurements are feasible under normal total reflection X-ray fluorescence (TXRF) conditions, i.e. on droplet samples, with excitation in grazing incidence and using a TXRF experimental chamber. The application of the total reflection excitation geometry for XAFS measurements increases the sensitivity compared to the conventional geometry leading to lower accessible concentration ranges. However, XAFS under total reflection excitation condition fails for highly concentrated samples because of the self-absorption effect

  15. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Yanlin [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia); Adeloju, Samuel B., E-mail: Sam.Adeloju@monash.edu [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia)

    2012-04-06

    Highlights: Black-Right-Pointing-Pointer Successful speciation of inorganic and organic Hg with Fe{sup 3+}, Cu{sup 2+} and thiourea as catalysts. Black-Right-Pointing-Pointer Best sensitivity enhancement and similar sensitivity for MeHg and Hg{sup 2+} with Fe{sup 3+}. Black-Right-Pointing-Pointer Successful use of Hg{sup 2+} as the primary standard for quantification of inorganic and total-Hg. Black-Right-Pointing-Pointer Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. Black-Right-Pointing-Pointer Integration with FIA for rapid analysis with a sample throughput of 180 h{sup -1}. - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH{sub 4} were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe{sup 3+}, Cu{sup 2+} and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu{sup 2+} and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe{sup 3+} gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg{sup 2+}. Due to similarity of resulting sensitivity, Hg{sup 2+} was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury

  16. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Zhang Yanlin; Adeloju, Samuel B.

    2012-01-01

    Highlights: ► Successful speciation of inorganic and organic Hg with Fe 3+ , Cu 2+ and thiourea as catalysts. ► Best sensitivity enhancement and similar sensitivity for MeHg and Hg 2+ with Fe 3+ . ► Successful use of Hg 2+ as the primary standard for quantification of inorganic and total-Hg. ► Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. ► Integration with FIA for rapid analysis with a sample throughput of 180 h −1 . - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH 4 were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe 3+ , Cu 2+ and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu 2+ and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe 3+ gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg 2+ . Due to similarity of resulting sensitivity, Hg 2+ was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury, respectively. The use of flow injection enabled rapid analysis with a sample throughput of 180 h −1 .

  17. Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.; Herrero Latorre, C., E-mail: carlos.herrero@usc.es

    2015-04-01

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L{sup −1}, respectively, and for Pb these limits were 0.13 and 0.43 μg L{sup −1}. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. - Highlights: • Cd and Pb determination based on the combination of DSP, SS and ETAAS • Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes. • Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.

  18. Isotope Enrichment Detection by Laser Ablation - Laser Absorption Spectrometry: Automated Environmental Sampling and Laser-Based Analysis for HEU Detection

    International Nuclear Information System (INIS)

    Anheier, Norman C.; Bushaw, Bruce A.

    2010-01-01

    The global expansion of nuclear power, and consequently the uranium enrichment industry, requires the development of new safeguards technology to mitigate proliferation risks. Current enrichment monitoring instruments exist that provide only yes/no detection of highly enriched uranium (HEU) production. More accurate accountancy measurements are typically restricted to gamma-ray and weight measurements taken in cylinder storage yards. Analysis of environmental and cylinder content samples have much higher effectiveness, but this approach requires onsite sampling, shipping, and time-consuming laboratory analysis and reporting. Given that large modern gaseous centrifuge enrichment plants (GCEPs) can quickly produce a significant quantity (SQ ) of HEU, these limitations in verification suggest the need for more timely detection of potential facility misuse. The Pacific Northwest National Laboratory (PNNL) is developing an unattended safeguards instrument concept, combining continuous aerosol particulate collection with uranium isotope assay, to provide timely analysis of enrichment levels within low enriched uranium facilities. This approach is based on laser vaporization of aerosol particulate samples, followed by wavelength tuned laser diode spectroscopy to characterize the uranium isotopic ratio through subtle differences in atomic absorption wavelengths. Environmental sampling (ES) media from an integrated aerosol collector is introduced into a small, reduced pressure chamber, where a focused pulsed laser vaporizes material from a 10 to 20-(micro)m diameter spot of the surface of the sampling media. The plume of ejected material begins as high-temperature plasma that yields ions and atoms, as well as molecules and molecular ions. We concentrate on the plume of atomic vapor that remains after the plasma has expanded and then cooled by the surrounding cover gas. Tunable diode lasers are directed through this plume and each isotope is detected by monitoring absorbance

  19. VLE measurements using a static cell vapor phase manual sampling method accompanied with an empirical data consistency test

    International Nuclear Information System (INIS)

    Freitag, Joerg; Kosuge, Hitoshi; Schmelzer, Juergen P.; Kato, Satoru

    2015-01-01

    Highlights: • We use a new, simple static cell vapor phase manual sampling method (SCVMS) for VLE (x, y, T) measurement. • The method is applied to non-azeotropic, asymmetric and two-liquid phase forming azeotropic binaries. • The method is approved by a data consistency test, i.e., a plot of the polarity exclusion factor vs. pressure. • The consistency test reveals that with the new SCVMS method accurate VLE near ambient temperature can be measured. • Moreover, the consistency test approves that the effect of air in the SCVMS system is negligible. - Abstract: A new static cell vapor phase manual sampling (SCVMS) method is used for the simple measurement of constant temperature x, y (vapor + liquid) equilibria (VLE). The method was applied to the VLE measurements of the (methanol + water) binary at T/K = (283.2, 298.2, 308.2 and 322.9), asymmetric (acetone + 1-butanol) binary at T/K = (283.2, 295.2, 308.2 and 324.2) and two-liquid phase forming azeotropic (water + 1-butanol) binary at T/K = (283.2 and 298.2). The accuracy of the experimental data was approved by a data consistency test, that is, an empirical plot of the polarity exclusion factor, β, vs. the system pressure, P. The SCVMS data are accurate, because the VLE data converge to the same lnβ vs. lnP straight line determined from conventional distillation-still method and a headspace gas chromatography method

  20. Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection

    Czech Academy of Sciences Publication Activity Database

    Huber, C. S.; Vale, M. G. R.; Dessuy, M. B.; Svoboda, Milan; Musil, Stanislav; Dědina, Jiří

    2017-01-01

    Roč. 175, DEC (2017), s. 406 -412 ISSN 0039-9140 R&D Projects: GA MŠk(CZ) LH15174 Institutional support: RVO:68081715 Keywords : slurry sampling * methyl-substituted arsenic species * hydride generation-cryotrapping-atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.162, year: 2016

  1. Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection

    Czech Academy of Sciences Publication Activity Database

    Huber, C. S.; Vale, M. G. R.; Dessuy, M. B.; Svoboda, Milan; Musil, Stanislav; Dědina, Jiří

    2017-01-01

    Roč. 175, DEC (2017), s. 406-412 ISSN 0039-9140 R&D Projects: GA MŠk(CZ) LH15174 Institutional support: RVO:68081715 Keywords : slurry sampling * methyl-substituted arsenic species * hydride generation-cryotrapping-atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.162, year: 2016

  2. Consistently low prevalence of syphilis among female sex workers in Jinan, China: findings from two consecutive respondent driven sampling surveys.

    Directory of Open Access Journals (Sweden)

    Meizhen Liao

    Full Text Available BACKGROUND: Routine surveillance using convenient sampling found low prevalence of HIV and syphilis among female sex workers in China. Two consecutive surveys using respondent driven sampling were conducted in 2008 and 2009 to examine the prevalence of HIV and syphilis among female sex workers in Jinan, China. METHODS: A face-to-face interview was conducted to collect demographic, behavioral and service utilization information using a structured questionnaire. Blood samples were drawn for serological tests of HIV-1 antibody and syphilis antibody. Respondent Driven Sampling Analysis Tool was used to generate population level estimates. RESULTS: In 2008 and in 2009, 363 and 432 subjects were recruited and surveyed respectively. Prevalence of syphilis was 2.8% in 2008 and 2.2% in 2009, while no HIV case was found in both years. Results are comparable to those from routine sentinel surveillance system in the city. Only 60.8% subjects in 2008 and 48.3% in 2009 reported a consistent condom use with clients during the past month. Over 50% subjects had not been covered by any HIV-related services in the past year, with only 15.6% subjects in 2008 and 13.1% in 2009 ever tested for HIV. CONCLUSIONS: Despite the low prevalence of syphilis and HIV, risk behaviors are common. Targeted interventions to promote the safe sex and utilization of existing intervention services are still needed to keep the epidemic from growing.

  3. On the Influence of the Sample Absorptivity when Studying the Thermal Degradation of Materials

    Directory of Open Access Journals (Sweden)

    Pascal Boulet

    2015-08-01

    Full Text Available The change in absorptivity during the degradation process of materials is discussed, and its influence as one of the involved parameters in the degradation models is studied. Three materials with very different behaviors are used for the demonstration of its role: a carbon composite material, which is opaque, almost grey, a plywood slab, which is opaque and spectral-dependent and a clear PMMA slab, which is semitransparent. Data are analyzed for virgin and degraded materials at different steps of thermal degradation. It is seen that absorptivity and emissivity often reach high values in the range of 0.90–0.95 with a near-grey behavior after significant thermal aggression, but depending on the materials of interest, some significant evolution may be first observed, especially during the early stages of the degradation. Supplementary inaccuracy can come from the heterogeneity of the incident flux on the slab. As a whole, discrepancies up to 20% can be observed on the absorbed flux depending on the degradation time, mainly because of the spectral variations of the absorption and up to 10% more, depending on the position on the slab. Simple models with a constant and unique value of absorptivity may then lead to inaccuracies in the evaluation of the radiative flux absorption, with possible consequences on the pyrolysis analysis, especially for properties related to the early step of the degradation process, like the time to ignition, for example.

  4. On the Influence of the Sample Absorptivity when Studying the Thermal Degradation of Materials.

    Science.gov (United States)

    Boulet, Pascal; Brissinger, Damien; Collin, Anthony; Acem, Zoubir; Parent, Gilles

    2015-08-21

    The change in absorptivity during the degradation process of materials is discussed, and its influence as one of the involved parameters in the degradation models is studied. Three materials with very different behaviors are used for the demonstration of its role: a carbon composite material, which is opaque, almost grey, a plywood slab, which is opaque and spectral-dependent and a clear PMMA slab, which is semitransparent. Data are analyzed for virgin and degraded materials at different steps of thermal degradation. It is seen that absorptivity and emissivity often reach high values in the range of 0.90-0.95 with a near-grey behavior after significant thermal aggression, but depending on the materials of interest, some significant evolution may be first observed, especially during the early stages of the degradation. Supplementary inaccuracy can come from the heterogeneity of the incident flux on the slab. As a whole, discrepancies up to 20% can be observed on the absorbed flux depending on the degradation time, mainly because of the spectral variations of the absorption and up to 10% more, depending on the position on the slab. Simple models with a constant and unique value of absorptivity may then lead to inaccuracies in the evaluation of the radiative flux absorption, with possible consequences on the pyrolysis analysis, especially for properties related to the early step of the degradation process, like the time to ignition, for example.

  5. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

  6. Efficiency calibration and measurement of self-absorption correction of environmental gamma spectroscopy of soils samples using Marinelli beaker

    International Nuclear Information System (INIS)

    Abdi, M. R.; Mostajaboddavati, M.; Hassanzadeh, S.; Faghihian, H.; Rezaee, Kh.; Kamali, M.

    2006-01-01

    A nonlinear function in combination with the method of mixing activity calibrated is applied for fitting the experimental peak efficiency of HPGe spectrometers in 59-2614 keV energy range. The preparation of Marinelli beaker standards of mixed gamma and RG-set at secular equilibrium with its daughter radionuclides was studied. Standards were prepared by mixing of known amounts of 13B a, 241 Am, 152 Eu, 207 Bi, 24 Na, Al 2 O 3 powder and soil. The validity of these standards was checked by comparison with certified standard reference material RG-set and IAEA-Soil-6 Self-absorption was measured for the activity calculation of the gamma-ray lines about series of 238 U daughter, 232 Th series, 137 Cs and 40 K in soil samples. Self-absorption in the sample will depend on a number of factor including sample composition, density, sample size and gamma-ray energy. Seven Marinelli beaker standards were prepared in different degrees of compaction with bulk density ( ρ) of 1.000 to 1.600 g cm -3 . The detection efficiency versus density was obtained and the equation of self-absorption correction factors calculated for soil samples

  7. Diameter grouping in bulk samples of single-walled carbon nanotubes from optical absorption spectroscopy

    NARCIS (Netherlands)

    Golden, M.S.; Fink, J.; Dunsch, L.; Bauer, H.-D.; Reibold, M.; Knupfer, M.; Friedlein, R.; Pichler, T.; Jost, O.

    1999-01-01

    The influence of the synthesis parameters on the mean characteristics of single-wall carbon nanotubes in soot produced by the laser vaporization of graphite has been analyzed using optical absorption spectroscopy. The abundance and mean diameter of the nanotubes were found to be most influenced by

  8. Portable sample preparation and analysis system for micron and sub-micron particle characterization using light scattering and absorption spectroscopy

    Science.gov (United States)

    Stark, Peter C [Los Alamos, NM; Zurek, Eduardo [Barranquilla, CO; Wheat, Jeffrey V [Fort Walton Beach, FL; Dunbar, John M [Santa Fe, NM; Olivares, Jose A [Los Alamos, NM; Garcia-Rubio, Luis H [Temple Terrace, FL; Ward, Michael D [Los Alamos, NM

    2011-07-26

    There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.

  9. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Sardans, Jordi; Montes, Fernando; Penuelas, Josep

    2010-01-01

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at μg L -1 levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages of

  10. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at mug L{sup -1} levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages

  11. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

    OpenAIRE

    Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria das Graças Andrade; Bezerra, Marcos de Almeida

    2009-01-01

    Texto completo: acesso restrito. p. 1041-1045 A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L−1 nitric acid solution, the analytes are determinate employing fla...

  12. Anomalous optical surface absorption in nominally pure silicon samples at 1550 nm

    Science.gov (United States)

    Bell, Angus S.; Steinlechner, Jessica; Martin, Iain W.; Craig, Kieran; Cunningham, William; Rowan, Sheila; Hough, Jim; Schnabel, Roman; Khalaidovski, Alexander

    2017-10-01

    The announcement of the direct detection of gravitational waves (GW) by the LIGO and Virgo collaboration in February 2016 has removed any uncertainty around the possibility of GW astronomy. It has demonstrated that future detectors with sensitivities ten times greater than the Advanced LIGO detectors would see thousands of events per year. Many proposals for such future interferometric GW detectors assume the use of silicon test masses. Silicon has low mechanical loss at low temperatures, which leads to low displacement noise for a suspended interferometer mirror. In addition to the low mechanical loss, it is a requirement that the test masses have a low optical loss. Measurements at 1550 nm have indicated that material with a low enough bulk absorption is available; however there have been suggestions that this low absorption material has a surface absorption of  >100 ppm which could preclude its use in future cryogenic detectors. We show in this paper that this surface loss is not intrinsic but is likely to be a result of particular polishing techniques and can be removed or avoided by the correct polishing procedure. This is an important step towards high gravitational wave detection rates in silicon based instruments.

  13. Anomalous optical surface absorption in nominally pure silicon samples at 1550 nm

    International Nuclear Information System (INIS)

    Bell, Angus S; Steinlechner, Jessica; Martin, Iain W; Craig, Kieran; Cunningham, William; Rowan, Sheila; Hough, Jim; Schnabel, Roman; Khalaidovski, Alexander

    2017-01-01

    The announcement of the direct detection of gravitational waves (GW) by the LIGO and Virgo collaboration in February 2016 has removed any uncertainty around the possibility of GW astronomy. It has demonstrated that future detectors with sensitivities ten times greater than the Advanced LIGO detectors would see thousands of events per year. Many proposals for such future interferometric GW detectors assume the use of silicon test masses. Silicon has low mechanical loss at low temperatures, which leads to low displacement noise for a suspended interferometer mirror. In addition to the low mechanical loss, it is a requirement that the test masses have a low optical loss. Measurements at 1550 nm have indicated that material with a low enough bulk absorption is available; however there have been suggestions that this low absorption material has a surface absorption of  >100 ppm which could preclude its use in future cryogenic detectors. We show in this paper that this surface loss is not intrinsic but is likely to be a result of particular polishing techniques and can be removed or avoided by the correct polishing procedure. This is an important step towards high gravitational wave detection rates in silicon based instruments. (paper)

  14. Determination of the thermal neutron absorption cross section for rock samples by a single measurement of the time decay constant

    International Nuclear Information System (INIS)

    Krynicka, E.

    1993-01-01

    A calibration method for the determination of the thermal neutron macroscopic mass absorption cross section for rock samples is presented. The standard deviation of the final results is discussed in detail. A big advantage of the presented method is that the calibration curves have been found using the results obtained for a variety of natural rock samples of different stratigraphies and lithologies measured by Czubek's methods. An important part of the paper is a through analysis of the standard deviation of the final result. (author). 13 refs, 11 figs, 5 tabs

  15. Lead preconcentration in synthetic samples with triton x-114 in the cloud point extraction and analysis by atomic absorption (EAAF)

    International Nuclear Information System (INIS)

    Zegarra Pisconti, Marixa; Cjuno Huanca, Jesus

    2015-01-01

    A methodology was developed about lead preconcentration in water samples that were added dithizone as complexing agent, previously dissolved in the nonionic surfactant Triton X-114, until the formation of the critical micelle concentration and the cloud point temperature. The centrifuged system gave a precipitate with high concentrations of Pb (II) that was measured by atomic absorption spectroscopy with flame (EAAF). The method has proved feasible to be implemented as a method of preconcentration and analysis of Pb in aqueous samples with concentrations less than 1 ppm. Several parameters were evaluated to obtain a percentage recovery of 89.8%. (author)

  16. 137Cs absorption factors (AFs) from contaminated cooking water to some vegetable and protein samples

    International Nuclear Information System (INIS)

    Malek, M.A.

    2006-01-01

    The radionuclide in contaminated freshwater may directly gain access to the human body through two major routes: drinking and cooking food with fresh water. During cooking, the radionuclide present in the water may be transferred to the various ingredients of the cooked food. The degree of contamination of food during cooking depends both on absorption power of the individual ingredients and the level of radionuclide present in the water. The ratio of the concentration of the radionuclide absorbed in the individual ingredients to the concentration in the cooking water can be designated as 'Absorption factor' (AF). AF can be used to predict the radionuclide absorbed by the ingredients cooked with contaminated water, to assess the internal radiation dose to the consumer and radionuclide transfer from the cooking water to the ingredients. A better understanding of the variables that affect the AF in various ingredients during cooking is central to deriving the contamination level of the ingredients. 10 kinds of greens and vegetable and 3 kinds of animal protein were boiled with 37 Cs contaminated freshwater and corresponding AFs were determined in both hot and cooled condition

  17. Atomic absorption instrument functional description

    International Nuclear Information System (INIS)

    Bystroff, R.I.; Boyle, W.G. Jr.; Barton, G.W. Jr.

    1976-01-01

    This report describes a proposed system for automating atomic absorption analysis. The system consists of two atomic absorption instruments and an automatic sampler that can be attached to either instrument. A computer program controls the sampling and gathers data. The program then uses the data to perform bookkeeping, data processing, and report writing

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  19. Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

    International Nuclear Information System (INIS)

    Andrada, Daniel; Pinto, Frederico G.; Magalhaes, Cristina Goncalves; Nunes, Berta R.; Silva, Jose Bento Borba da; Franco, Milton B.

    2006-01-01

    The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ETAAS). Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 μL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO 3 1% v/v and 0.02% v/v of cetyl trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 μL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 μg), the best pyrolysis and atomization temperatures were 900 and 1600 deg C, respectively, with a characteristic mass of 12 pg (recommended of 10 pg), with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence) for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh) and between 93.9 and 105.2% (Zr+Rh). In both recovery studies, the relative standard deviation (n=3) was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r 2 higher than 0.99. The limits of detection were 0.7 μg L -1 for serum samples, with Zr+Rh permanent, and 1.0 μg L -1 for urine with iridium permanent. (author)

  20. Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

    Directory of Open Access Journals (Sweden)

    Andrada Daniel

    2006-01-01

    Full Text Available The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ET AAS. Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 µL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO3 1% v/v and 0.02% v/v of cetil trimethyl ammonium chloride (CTAC were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 µL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 µg, the best pyrolysis and atomization temperatures were 900 and 1600 ºC, respectively, with a characteristic mass of 12 pg (recommended of 10 pg, with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh and between 93.9 and 105.2% (Zr+Rh. In both recovery studies, the relative standard deviation (n=3 was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r² higher than 0.99. The limits of detection were 0.7 µg L-1 for serum samples, with Zr+Rh permanent, and 1.0 µg L-1 for urine with iridium permanent.

  1. Determination of self absorption correction factor (SAF) for gross alpha measurement in water samples by BIS method

    International Nuclear Information System (INIS)

    Raveendran, Nanda; Baburajan, A.; Ravi, P.M.

    2018-01-01

    The laboratories accredited by AERB undertake the measurement of gross alpha and gross beta in packaged drinking water from manufactures across the country and analyze as per the procedure of Bureau of Indian standards. The accurate measurements of gross alpha in the drinking water sample is a challenge due to the self absorption of alpha particle from varying precipitate (Fe(OH) 3 +BaSO 4 ) thickness and total dissolved solids (TDS). This paper deals with a study on tracer recovery generation and self absorption correction factor (SAF). ESL, Tarapur has participated in an inter-laboratory comparison exercise conducted by IDS, RSSD, BARC as per the recommendation of AERB for the accredited laboratories. The thickness of the precipitate is an important aspect which affected the counting process. The activity was reported after conducting multiple experiments with uranium tracer recovery and precipitate thickness. Later on to make our efforts simplified, an average tracer recovery and Self Absorption correction Factor (SAF) was derived by the present experiment and the same was used for the re-calculation of activity from the count rate reported earlier

  2. Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

    Energy Technology Data Exchange (ETDEWEB)

    Giang, Nguyen; Tam, Nguyen Thanh; Ngoc Trinh, Le Thi; Mai, Truong Phuong; Minh, Nguyen Van [Nuclear Research Institute, Dalat (Viet Nam)

    2004-08-01

    Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

  3. Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

    International Nuclear Information System (INIS)

    Nguyen Giang; Nguyen Thanh Tam; Le Thi Ngoc Trinh; Truong Phuong Mai; Nguyen Van Minh

    2004-01-01

    Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

  4. An analysis of lead (Pb) from human hair samples (20-40 years of age) by atomic absorption spectrophotometry

    Energy Technology Data Exchange (ETDEWEB)

    Gelsano, Flordeliza K; Timing, Laurie D

    2003-02-17

    This analysis of lead from human hair samples in five different groups namely scavengers from Payatas Quezon City, tricycle drivers, car shop workers, paint factory workers, and students from Polytechnic University of the Philippines. The people from Nagcarlan, Laguna represented as a ''base-line value'' or as a control group. The method applied was acid digestion using HNO{sub 3} and HClO{sub 4} then the samples were subjected to atomic absorption spectrophotometer. In terms of lead found from hair, the scavengers from Payatas Q.C. obtained high exposure of lead among the samples that were tested. The result of the analysis of concentration of lead was expressed in mg/L. (Authors)

  5. An analysis of lead (Pb) from human hair samples (20-40 years of age) by atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Gelsano, Flordeliza K.; Timing, Laurie D.

    2003-01-01

    This analysis of lead from human hair samples in five different groups namely scavengers from Payatas Quezon City, tricycle drivers, car shop workers, paint factory workers, and students from Polytechnic University of the Philippines. The people from Nagcarlan, Laguna represented as a ''base-line value'' or as a control group. The method applied was acid digestion using HNO 3 and HClO 4 then the samples were subjected to atomic absorption spectrophotometer. In terms of lead found from hair, the scavengers from Payatas Q.C. obtained high exposure of lead among the samples that were tested. The result of the analysis of concentration of lead was expressed in mg/L. (Authors)

  6. Proton Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrometry (AAS) applied in the environmental sample analysis

    International Nuclear Information System (INIS)

    Popescu, Ion V.; Iordan, M.; Stihi, C.; Bancuta, A.; Dima, G.; Busuioc, G.; Ciupina, V.; Belc, M.; Badica, T.

    2003-01-01

    The aim of this work is to determine the elemental composition of tree leaves using Proton-Induced X-Rays Emission (PIXE) and Atomic Absorption Spectrophotometry (AAS) methods. By PIXE Spectrometry we identified and determined the concentration of S, Cl, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu Zn, As, Br, Sr and by AAS method the concentration of elements: Cr, Mn, Fe, Co, Cu, Zn, Se, Cd. Pb was identified in only 2 samples from 29. For tree leave samples collected at a large distance to the polluting source the Sr concentration decreased and the Mg, Ca, Se, Zn and Fe concentrations increased. Also, we can observe a small affinity of these leaves for the environmental Pb which was detected for two samples at a small distance to polluting source. (authors)

  7. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

    2013-01-01

    A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

  8. A reaction cell with sample laser heating for in situ soft X-ray absorption spectroscopy studies under environmental conditions.

    Science.gov (United States)

    Escudero, Carlos; Jiang, Peng; Pach, Elzbieta; Borondics, Ferenc; West, Mark W; Tuxen, Anders; Chintapalli, Mahati; Carenco, Sophie; Guo, Jinghua; Salmeron, Miquel

    2013-05-01

    A miniature (1 ml volume) reaction cell with transparent X-ray windows and laser heating of the sample has been designed to conduct X-ray absorption spectroscopy studies of materials in the presence of gases at atmospheric pressures. Heating by laser solves the problems associated with the presence of reactive gases interacting with hot filaments used in resistive heating methods. It also facilitates collection of a small total electron yield signal by eliminating interference with heating current leakage and ground loops. The excellent operation of the cell is demonstrated with examples of CO and H2 Fischer-Tropsch reactions on Co nanoparticles.

  9. Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Feichtmeier, Nadine S; Leopold, Kerstin

    2014-06-01

    In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples.

  10. Thermal neutron absorption cross-section measured on rock samples and brines in the Institute of Nuclear Physics

    International Nuclear Information System (INIS)

    Czubek, J.A.; Drozdowicz, K.; Krynicka-Drozdowicz, E.; Igielski, A.; Woznicka, U.

    1983-01-01

    In consecutive measurements the rock sample (having a fixed and well known shape -in our case it is a sphere or a cylinder and the sample is powdered or liquid) is enveloped in shells of a plexiglass moderator (the neutron parameters of which are known) of variable thickness and irradiated with the pulsed beam of fast neutrons. The die-away rate of thermal neutrons escaping from the whole system is measured. The absorption cross-section of the sample is found as the intersection of the experimental curve (i.e. die -away rate vs thickness of the moderator) with the theoretical one. The theoretical curve is calculated for a given moderator under the assumption of a constant value of the neutron flux inside the sample. This method is independent of the value of the transport cross-section of the sample. It has been checked on artificial materials with a well known elemental composition (liquid or solid) and on the natural brines and rock samples (basalts and dolomite). A special method of calculation of the variance of the measurement has been established. It is based on the multiple computer simulations of all experimental data used in the computation. The one standard deviation of our methods is of the order of 1 up to 3 capture units (1 c.u. = 10 -3 cm -1 ). The volume of the sample needed is of the order of 500ccm. (author)

  11. Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Nomura, Cassiana S.; Silva, Cintia S.; Nogueira, Ana R.A.; Oliveira, Pedro V.

    2005-01-01

    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 deg. C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg - 1 and 128 mg kg - 1 , respectively. The relative standard deviations were lower than 6% (n = 5). The

  12. The correlations between natural elements (K, U, Th) concentrations and thermal neutron absorption cross-section value (Σa) for rock samples of Carpatia area

    International Nuclear Information System (INIS)

    Swakon, J.; Cywicka-Jakiel, T.; Drozdowicz, E.; Gabanska, B.; Loskiewicz, J.; Woznicka, U.

    1991-01-01

    The paper presents a study of correlations between concentrations of potassium, uranium and thorium and thermal neutron absorption cross section in rock samples. This knowledge of correlation should help in recognizing the expansion ways and accumulation places of the elements responsible of high thermal neutron absorption cross section in some geological environments. The correlations show the existence of connections between the thermal neutron absorption cross section value and natural radioactivity elements concentration in rocks. The results confirm the existence of correlations between natural radioactive elements concentrations (particularly thorium) and thermal neutron absorption cross - section value in some rocks. (author). 12 refs, 23 figs, 6 tabs

  13. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  14. Solid sample atomic absorption spectroscopy in a chemical contaminant monitoring pilot project

    Energy Technology Data Exchange (ETDEWEB)

    Klein, J.; Schmidt, H.; Dirscherl, C.; Muntau, H.

    1987-09-01

    The Institute for Technology and Hygiene of Food of Animal Origin is developing a practible system of monitoring the distribution of toxic substances in the environment, using the dairy cows as bioindicators. A pilot project has been established to solve basic problems as sampling strategy, sample preparation, analysis and data handling. In the preliminary stage of this study the new technique of SS-AAS turned out to be a useful tool. In order to test overall analytical reliability of the data obtained all analytical procedures applied for the different matrices are controlled by the use of reference material of similar matrix compositions. Results of studies on the distribution of admium and lead are reported; the representativity of small sample amounts of cortical tissue (50-60 mg and 1-2 mg dry mass) has additionally been investigated. Direct analysis of wet tissue aliquots (5-10 mg) was not feasible. A possible method of sample preparation of wet tissue is presented which yields reliable results within 10 min of operation time.

  15. Direct analysis of Antarctic krill by slurry sampling: determination of copper, iron, manganese and zinc by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Alves Flávia L.

    2000-01-01

    Full Text Available Slurry sampling in combination with flame atomic absorption spectrometry was employed for the direct determination of four essential trace elements, namely Cu, Fe, Mn and Zn in Antarctic krill. The effect of instrumental operating conditions and slurry sampling preparation on the analytical signal was investigated. For the determination of Cu, Fe and Zn, samples were suspended in a solution containing 2 mol L-1 HNO3. In the case of Mn, 4 mol L-1 HNO3 was necessary for the preparation of the slurry. The precision between sample replicates was better than 5%. The method was applied to the direct determination of Cu, Fe, Mn and Zn in Antarctic krill samples using aqueous reference solutions to prepare the calibration curves. The results obtained were in good agreement with those achieved by FAAS and ICP-AES after microwave-assisted wet digestion of the krill samples. The detection limits were 4.5, 1.0, 4.9 and 8.4 mug L-1 for Cu, Zn, Mn and Fe, respectively.

  16. Development of a methodology for low-energy X-ray absorption correction in biological samples using radiation scattering techniques

    International Nuclear Information System (INIS)

    Pereira, Marcelo O.; Anjos, Marcelino J.; Lopes, Ricardo T.

    2009-01-01

    Non-destructive techniques with X-ray, such as tomography, radiography and X-ray fluorescence are sensitive to the attenuation coefficient and have a large field of applications in medical as well as industrial area. In the case of X-ray fluorescence analysis the knowledge of photon X-ray attenuation coefficients provides important information to obtain the elemental concentration. On the other hand, the mass attenuation coefficient values are determined by transmission methods. So, the use of X-ray scattering can be considered as an alternative to transmission methods. This work proposes a new method for obtain the X-ray absorption curve through superposition peak Rayleigh and Compton scattering of the lines L a e L β of Tungsten (Tungsten L lines of an X-ray tube with W anode). The absorption curve was obtained using standard samples with effective atomic number in the range from 6 to 16. The method were applied in certified samples of bovine liver (NIST 1577B) , milk powder and V-10. The experimental measurements were obtained using the portable system EDXRF of the Nuclear Instrumentation Laboratory (LIN-COPPE/UFRJ) with Tungsten (W) anode. (author)

  17. Determination of total sulfur in agricultural samples by high-resolution continuum source flame molecular absorption spectrometry.

    Science.gov (United States)

    Virgilio, Alex; Raposo, Jorge L; Cardoso, Arnaldo A; Nóbrega, Joaquim A; Gomes Neto, José A

    2011-03-23

    The usefulness of molecular absorption was investigated for the determination of total sulfur (S) in agricultural samples by high-resolution continuum source flame molecular absorption spectrometry. The lines for CS at 257.595, 257.958, and 258.056 nm and for SH at 323.658, 324.064, and 327.990 nm were evaluated. Figures of merit, such as linear dynamic range, sensitivity, linear correlation, characteristic concentration, limit of detection, and precision, were established. For selected CS lines, wavelength-integrated absorbance equivalent to 3 pixels, analytical curves in the 100-2500 mg L(-1) (257.595 nm), 250-2000 mg L(-1) (257.958 nm), and 250-5000 mg L(-1) (258.056 nm) ranges with a linear correlation coefficient better than 0.9980 were obtained. Results were in agreement at a 95% confidence level (paired t test) with those obtained by gravimetry. Recoveries of S in fungicide and fertilizer samples were within the 84-109% range, and the relative standard deviation (n=12) was typically <5%.

  18. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry.

    Science.gov (United States)

    Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S; Korn, Maria G A; Bezerra, Marcos A

    2009-03-15

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

  19. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria G.A.; Bezerra, Marcos A.

    2009-01-01

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L -1 nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 μg L -1 , respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 μg L -1 . The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish

  20. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Citak, Demirhan [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Ferreira, Hadla S.; Korn, Maria G.A. [Universidade Federal da Bahia, Instituto de Quimica, 40170-290 Salvador (Brazil); Bezerra, Marcos A. [Universidade Estadual do Sudoeste da Bahia, 45200-190 Jequie (Brazil)

    2009-03-15

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L{sup -1} nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 {mu}g L{sup -1}, respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 {mu}g L{sup -1}. The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

  1. The effect of pathological processes on absorption and scattering spectra of samples of bile and pancreatic juice

    Science.gov (United States)

    Giraev, K. M.; Ashurbekov, N. A.; Magomedov, M. A.; Murtazaeva, A. A.; Medzhidov, R. T.

    2015-07-01

    Spectra of optical transmission coefficients and optical reflectance for bile and pancreatic juice samples were measured experimentally for different forms of pathologies of the pancreas within the range of 250-2500 nm. The absorption and scattering spectra, as well as the spectrum of the anisotropy factor of scattering, were determined based on the results obtained using the reverse Monte Carlo method. The surface morphology for the corresponding samples of the biological media was studied employing electron microscopy. The dynamics of the optical properties of the biological media was determined depending on the stage of the pathology. It has been demonstrated that the results of the study presented are in a good agreement with pathophysiological data and could supplement and broaden the results of conventional methods for diagnostics of the pancreas.

  2. Tritium absorption and desorption in ITER relevant materials: comparative study of tungsten dust and massive samples

    Energy Technology Data Exchange (ETDEWEB)

    Grisolia, C., E-mail: christian.grisolia@cea.fr [CEA, IRFM, F-13108 Saint Paul lez Durance (France); Hodille, E. [CEA, IRFM, F-13108 Saint Paul lez Durance (France); Chene, J.; Garcia-Argote, S.; Pieters, G.; El-Kharbachi, A. [CEA Saclay, SCBM, iBiTec-S, PC n° 108, 91191 Gifsur-Yvette (France); Marchetti, L.; Martin, F.; Miserque, F. [CEA Saclay, DEN/DPC/SCCME/LECA, F-91191 Gif-sur-Yvette (France); Vrel, D.; Redolfi, M. [LSPM, Université Paris 13, Sorbonne Paris Cité, UPR 3407 CNRS, 93430 Villetaneuse (France); Malard, V. [CEA, DSV, IBEB, Lab Biochim System Perturb, Bagnols-sur-Cèze F-30207 (France); Dinescu, G.; Acsente, T. [NILPRP, 409 Atomistilor Street, 77125 Magurele, Bucharest (Romania); Gensdarmes, F.; Peillon, S. [IRSN, PSN-RES/SCA/LPMA, Saclay, Gif-sur-Yvette, 91192 (France); Pegourié, B. [CEA, IRFM, F-13108 Saint Paul lez Durance (France); Rousseau, B. [CEA Saclay, SCBM, iBiTec-S, PC n° 108, 91191 Gifsur-Yvette (France)

    2015-08-15

    Tritium adsorption and desorption from well characterized tungsten dust are presented. The dust used are of different types prepared by planetary milling and by aggregation technique in plasma. For the milled powder, the surface specific area (SSA) is 15.5 m{sup 2}/g. The particles are poly-disperse with a maximum size of 200 nm for the milled powder and 100 nm for the aggregation one. Prior to tritiation the particles are carefully de-oxidized. Both samples are experiencing a high tritium inventory from 5 GBq/g to 35 GBq/g. From comparison with massive samples and considering that tritium inventory increases with SSA, it is shown that surface effects are predominant in the tritium trapping process. Extrapolation to the ITER environment is undertaken with the help of a Macroscopic Rate Equation model. It is shown that, during the life time of ITER, these particles can exceed rapidly 1 GBq/g.

  3. Two-Sample Two-Stage Least Squares (TSTSLS estimates of earnings mobility: how consistent are they?

    Directory of Open Access Journals (Sweden)

    John Jerrim

    2016-08-01

    Full Text Available Academics and policymakers have shown great interest in cross-national comparisons of intergenerational earnings mobility. However, producing consistent and comparable estimates of earnings mobility is not a trivial task. In most countries researchers are unable to observe earnings information for two generations. They are thus forced to rely upon imputed data from different surveys instead. This paper builds upon previous work by considering the consistency of the intergenerational correlation (ρ as well as the elasticity (β, how this changes when using a range of different instrumental (imputer variables, and highlighting an important but infrequently discussed measurement issue. Our key finding is that, while TSTSLS estimates of β and ρ are both likely to be inconsistent, the magnitude of this problem is much greater for the former than it is for the latter. We conclude by offering advice on estimating earnings mobility using this methodology.

  4. Factorial Validity and Internal Consistency of Malaysian Adapted Depression Anxiety Stress Scale - 21 in an Adolescent Sample

    OpenAIRE

    Hairul Anuar Hashim; Freddy Golok; Rosmatunisah Ali

    2011-01-01

    Background: Psychometrically sound measurement instrument is a fundamental requirement across broad range of research areas. In negative affect research, Depression Anxiety Stress Scale (DASS) has been identified as a psychometrically sound instrument to measure depression, anxiety and stress, especially the 21-item version. However, its psychometric properties in adolescents have been less consistent. Objectives: Thus, the present study sought to examine the factorial validity and internal c...

  5. The Work Role Functioning Questionnaire v2.0 Showed Consistent Factor Structure Across Six Working Samples

    NARCIS (Netherlands)

    Abma, F.I.; Bultmann, U.; Amick III, B.C.; Arends, I.; Dorland, P.A.; Flach, P.A.; Klink, J.J.L van der; Ven H.A., van de; Bjørner, J.B.

    2017-01-01

    Objective The Work Role Functioning Questionnaire v2.0 (WRFQ) is an outcome measure linking a persons’ health to the ability to meet work demands in the twenty-first century. We aimed to examine the construct validity of the WRFQ in a heterogeneous set of working samples in the Netherlands with

  6. An historically consistent and broadly applicable MRV system based on LiDAR sampling and Landsat time-series

    Science.gov (United States)

    W. Cohen; H. Andersen; S. Healey; G. Moisen; T. Schroeder; C. Woodall; G. Domke; Z. Yang; S. Stehman; R. Kennedy; C. Woodcock; Z. Zhu; J. Vogelmann; D. Steinwand; C. Huang

    2014-01-01

    The authors are developing a REDD+ MRV system that tests different biomass estimation frameworks and components. Design-based inference from a costly fi eld plot network was compared to sampling with LiDAR strips and a smaller set of plots in combination with Landsat for disturbance monitoring. Biomass estimation uncertainties associated with these different data sets...

  7. The Work Role Functioning Questionnaire v2.0 Showed Consistent Factor Structure Across Six Working Samples

    DEFF Research Database (Denmark)

    Abma, Femke I.; Bültmann, Ute; Amick, Benjamin C.

    2017-01-01

    Objective: The Work Role Functioning Questionnaire v2.0 (WRFQ) is an outcome measure linking a persons’ health to the ability to meet work demands in the twenty-first century. We aimed to examine the construct validity of the WRFQ in a heterogeneous set of working samples in the Netherlands...

  8. In vitro assessment of potential intestinal absorption of some phenolic families and carboxylic acids from commercial instant coffee samples.

    Science.gov (United States)

    López-Froilán, R; Ramírez-Moreno, E; Podio, N S; Pérez-Rodríguez, M L; Cámara, M; Baroni, M V; Wunderlin, D A; Sánchez-Mata, M C

    2016-06-15

    Coffee is one of the most consumed beverages in the world, being a source of bioactive compounds as well as flavors. Hydroxycinnamic acids, flavonols, and carboxylic acids have been studied in the samples of instant coffee commercialized in Spain. The studies about contents of food components should be complemented with either in vitro or in vivo bioaccessibility studies to know the amount of food components effectively available for functions in the human body. In this sense, a widely used in vitro model has been applied to assess the potential intestinal absorption of phenolic compounds and organic acids. The contents of hydroxycinnamic acids and flavonols were higher in instant regular coffee samples than in the decaffeinated ones. Bioaccessible phenolic compounds in most analyzed samples account for 20-25% of hydroxycinnamic acids and 17-26% of flavonols. This could mean that a great part of them can remain in the gut, acting as potential in situ antioxidants. Quinic, acetic, pyroglutamic, citric and fumaric acids were identified in commercial instant coffee samples. Succinic acid was found in the coffee blend containing chicory. All carboxylic acids showed a very high bioaccessibility. Particularly, acetic acid and quinic acid were found in higher contents in the samples treated with the in vitro simulation of gastrointestinal processes, compared to the original ones, which can be explained by their cleavage from chlorogenic acid during digestion. This is considered as a positive effect, since quinic acid is considered as an antioxidant inducer.

  9. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Science.gov (United States)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

  10. Arsenic speciation in environmental samples by hydride generation and electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Anawar, Hossain Md

    2012-01-15

    For the past few years many studies have been performed to determine arsenic (As) speciation in drinking water, food chain and other environmental samples due to its well-recognized carcinogenic and toxic effects relating to its chemical forms and oxidation states. This review provides an overview of analytical methods, preconcentration and separation techniques, developed up to now, using HGAAS and ETAAS for the determination of inorganic As and organoarsenic species in environmental samples. Specific advantages, disadvantages, selectivity, sensitivity, efficiency, rapidity, detection limit (DL), and some aspects of recent improvements and modifications for different analytical and separation techniques, that can define their application for a particular sample analysis, are highlighted. HG-AAS has high sensitivity, selectivity and low DL using suitable separation techniques; and it is a more suitable, affordable and much less expensive technique than other detectors. The concentrations of HCl and NaBH(4) have a critical effect on the HG response of As species. Use of l-cysteine as pre-reductant is advantageous over KI to obtain the same signal response for different As species under the same, optimum and mild acid concentration, and to reduce the interference of transition metals on the arsine generation. Use of different pretreatment, digestion, separation techniques and surfactants can determine As species with DL from ngL(-1) to μgL(-1). Out of all the chromatographic techniques coupled with HGAAS/ETAAS, ion-pair reversed-phase chromatography (IP-RP) is the most popular due to its higher separation efficiency, resolution selectivity, simplicity, and ability to separate up to seven As species for both non-ionic and ionic compounds in a signal run using the same column and short time. However, a combination of anion- and cation-exchange chromatography seems the most promising for complete resolution up to eight As species. The ETAAS method using different

  11. Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of boron in plant tissues

    International Nuclear Information System (INIS)

    Resano, M.; Briceno, J.; Aramendia, M.; Belarra, M.A.

    2007-01-01

    In this work, the potential of graphite furnace atomic absorption spectrometry for the direct determination of B in plant tissues has been investigated. Three certified reference materials (NIST SRM 1570a spinach leaves, NIST SRM 1573a tomato leaves and BCR CRM 679 white cabbage) were selected for this study, the goal always being to develop a fast procedure that could be robust enough to provide a satisfactory performance for all of them, without any modifications in the conditions applied. The use of a suitable chemical modifier was found to be essential for obtaining a reproducible and sufficiently sensitive signal for boron solutions. In this regard, the performance of the combination of citric acid plus W (added as a permanent modifier) was noteworthy, resulting in well-defined signal profiles, a remarkable analyte stabilization during the pyrolysis step (up to 2100 deg. C) and minimal memory effects. This mixture of modifiers provided a good performance for the direct analysis of solid samples as well, but only if a suitable temperature program, favoring the interaction between the analyte and the modifiers, was used. Thus, such a temperature program, with two pyrolysis steps and the addition of NH 4 NO 3 in order to carry out the in situ sample microdigestion, was optimized. Under these conditions, the peak areas obtained for both solid samples and aqueous standards were comparable. Finally, the analysis of the samples was carried out. In all cases, a good agreement with the certified values was obtained, while R.S.D. values ranged between 6 and 10%. It can be concluded that the method proposed shows significant advantages for the determination of this complicated element in solid samples such as the use of aqueous standards for calibration, a high sample throughput (20 min per sample), a suitable limit of detection (0.3 μg g -1 ) and reduced risk of analyte losses and contamination

  12. Flame Atomic Absorption Determination of Gold Ion in Aqueous Samples after Preconcentration Using 9-Acridinylamine Functionalized γ-Alumina Nanoparticles

    Directory of Open Access Journals (Sweden)

    Mohammad Karimi

    2013-01-01

    Full Text Available A simple and sensitive solid phase extraction utilizing 9-acridinylamine functionalized alumina nanoparticles was developed, and their potential use for preconcentration and subsequent determination of gold by flame atomic absorption spectrometry (FAAS was investigated. A number of parameters, namely, type, concentration, and volume of eluent, pH of the sample solution, flow rate of extraction, and volume of the sample, were evaluated. The effect of a variety of ions on preconcentration and recovery was also investigated. Gold ions were found to be recovered quantitatively at pH 3.0, with 0.1 mol L−1 thiourea in 2 mol L−1 H2SO4 as eluent. The limit of detection (LOD, defined as five times the standard deviation of the blank, was determined to be lower than 13.0 ppb. Under optimum conditions, the accuracy and precision (RSD% of the method were >98.0 and <1.5%, respectively. To gauge its ability in terms of application to real samples, the proposed method was successfully applied for determination of gold concentration in waste water samples and one soil standard material, and satisfactory results were obtained.

  13. In-situ suspended aggregate microextraction of gold nanoparticles from water samples and determination by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Choleva, Tatiana G; Kappi, Foteini A; Tsogas, George Z; Vlessidis, Athanasios G; Giokas, Dimosthenis L

    2016-05-01

    This work describes a new method for the extraction and determination of gold nanoparticles in environmental samples by means of in-situ suspended aggregate microextraction and electrothermal atomic absorption spectrometry. The method relies on the in-situ formation of a supramolecular aggregate phase through ion-association between a cationic surfactant and a benzene sulfonic acid derivative. Gold nanoparticles are physically entrapped into the aggregate phase which is separated from the bulk aqueous solution by vacuum filtration on the surface of a cellulose filter in the form of a thin film. The film is removed from the filter surface and is dissociated into an acidified methanolic solution which is used for analysis. Under the optimized experimental conditions, gold nanoparticles can be efficiently extracted from water samples with recovery rates between 81.0-93.3%, precision 5.4-12.0% and detection limits as low as 75femtomolL(-1) using only 20mL of sample volume. The satisfactory analytical features of the method along with the simplicity indicate the efficiency of this new approach to adequately collect and extract gold nanoparticle species from water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. On-line preconcentration and determination of mercury in biological and environmental samples by cold vapor-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ferrua, N.; Cerutti, S.; Salonia, J.A.; Olsina, R.A.; Martinez, L.D.

    2007-01-01

    An on-line procedure for the determination of traces of total mercury in environmental and biological samples is described. The present methodology combines cold vapor generation associated to atomic absorption spectrometry (CV-AAS) with preconcentration of the analyte on a minicolumn packed with activated carbon. The retained analyte was quantitatively eluted from the minicolumn with nitric acid. After that, volatile specie of mercury was generated by merging the acidified sample and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the atomizer device. Optimizations of both, preconcentration and mercury volatile specie generation variables were carried out using two level full factorial design (2 3 ) with 3 replicates of the central point. Considering a sample consumption of 25 mL, an enrichment factor of 13-fold was obtained. The detection limit (3σ) was 10 ng L -1 and the precision (relative standard deviation) was 3.1% (n = 10) at the 5 μg L -1 level. The calibration curve using the preconcentration system for mercury was linear with a correlation coefficient of 0.9995 at levels near the detection limit up to at least 1000 μg L -1 . Satisfactory results were obtained for the analysis of mercury in tap water and hair samples

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-22

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

  16. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  17. 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.

  18. Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

    Science.gov (United States)

    Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

    2015-01-01

    A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

  19. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Vilar Farinas, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Barciela Garcia, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Garcia Martin, S. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena Crecente, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Herrero Latorre, C. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)]. E-mail: cherrero@lugo.usc.es

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO{sub 3}){sub 2} and (NH{sub 4})H{sub 2}PO{sub 4}-Mg(NO{sub 3}){sub 2}] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 {mu}g L{sup -1}), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

  20. Radiocarbon dating of archaeological samples (sambaqui) using CO(2) absorption and liquid scintillation spectrometry of low background radiation.

    Science.gov (United States)

    Mendonça, Maria Lúcia T G; Godoy, José M; da Cruz, Rosana P; Perez, Rhoneds A R

    2006-01-01

    Sambaqui means, in the Tupi language, a hill of shells. The sambaquis are archaeological sites with remains of pre-historical Brazilian occupation. Since the sambaqui sites in the Rio de Janeiro state region are older than 10,000 years, the applicability of CO(2) absorption on Carbo-sorb and (14)C determination by counting on a low background liquid scintillation counter was tested. In the present work, sambaqui shells were treated with H(3)PO(4) in a closed vessel in order to generate CO(2). The produced CO(2) was absorbed on Carbo-sorb. On saturation about 0.6g of carbon, as CO(2), was mixed with commercial liquid scintillation cocktail (Permafluor), and the (14)C activity determined by counting on a low background counter, Packard Tricarb 3170 TR/SL, for a period of 1000 mins to enable detection of a radiocarbon age of 22,400 BP. But only samples with ages up to 3500 BP were submitted to the method because the samples had been collected in the municipality of Guapimirim, in archaeological sambaqui-type sites belonging to this age range. The same samples were sent to the (14)C Laboratory of the Centro de Energia Nuclear na Agricultura (CENA/USP) where similar results were obtained.

  1. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    International Nuclear Information System (INIS)

    Vilar Farinas, M.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.; Herrero Latorre, C.

    2007-01-01

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO 3 ) 2 and (NH 4 )H 2 PO 4 -Mg(NO 3 ) 2 ] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 μg L -1 ), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged -1

  2. The use of atomic absorption spectroscopy to measure arsenic, selenium, molybdenum, and vanadium in water and soil samples from uranium mill tailings sites

    International Nuclear Information System (INIS)

    Hollenbach, M.H.

    1988-01-01

    The Technical Measurements Center (TMC) was established to support the environmental measurement needs of the various DOE remedial action programs. A laboratory intercomparison study conducted by the TMC, using soil and water samples from sites contaminated by uranium mill tailings, indicated large discrepancies in analytical results reported by participating laboratories for arsenic, selenium, molybdenum, and vanadium. The present study was undertaken to investigate the most commonly used analytical techniques for measuring these four elements, ascertain routine and reliable quantification, and assess problems and successes of analysts. Based on a survey of the technical literature, the analytical technique of atomic absorption spectroscopy was selected for detailed study. The application of flame atomic absorption, graphite furnace atomic absorption, and hydride generation atomic absorption to the analysis of tailings-contaminated samples is discussed. Additionally, laboratory sample preparation methods for atomic absorption spectroscopy are presented. The conclusion of this report is that atomic absorption can be used effectively for the determination of arsenic, selenium, molybdenum, and vanadium in water and soil samples if the analyst understands the measurement process and is aware of potential problems. The problem of accurate quantification of arsenic, selenium, molybdenum, and vanadium in water and soil contaminated by waste products from uranium milling operations affects all DOE remedial action programs [Surplus Facilities Management Program (SFMP), Formerly Utilized Site Remedial Action Program (FUSRAP), and Uranium Mill Tailings Remedial Action Program (UMTRAP)], since all include sites where uranium was processed. 96 refs., 9 figs

  3. Restricted access carbon nanotubes for direct extraction of cadmium from human serum samples followed by atomic absorption spectrometry analysis.

    Science.gov (United States)

    Barbosa, Adriano F; Barbosa, Valéria M P; Bettini, Jefferson; Luccas, Pedro O; Figueiredo, Eduardo C

    2015-01-01

    In this paper, we propose a new sorbent that is able to extract metal ions directly from untreated biological fluids, simultaneously excluding all proteins from these samples. The sorbent was obtained through the modification of carbon nanotubes (CNTs) with an external bovine serum albumin (BSA) layer, resulting in restricted access carbon nanotubes (RACNTs). The BSA layer was fixed through the interconnection between the amine groups of the BSA using glutaraldehyde as cross-linker. When a protein sample is percolated through a cartridge containing RACNTs and the sample pH is higher than the isoelectric point of the proteins, both proteins from the sample and the BSA layer are negatively ionized. Thus, an electrostatic repulsion prevents the interaction between the proteins from the sample on the RACNTs surface. At the same time, metal ions are adsorbed in the CNTs (core) after their passage through the chains of proteins. The Cd(2+) ion was selected for a proof-of-principle case to test the suitability of the RACNTs due to its toxicological relevance. RACNTs were able to extract Cd(2+) and exclude almost 100% of the proteins from the human serum samples in an online solid-phase extraction system coupled with thermospray flame furnace atomic absorption spectrometry. The limits of detection and quantification were 0.24 and 0.80 μg L(-1), respectively. The sampling frequency was 8.6h(-1), and the intra- and inter-day precisions at the 0.80, 15.0, and 30.0 μg L(-1) Cd(2+) levels were all lower than 10.1% (RSD). The recoveries obtained for human blood serum samples fortified with Cd(2+) ranged from 85.0% to 112.0%. The method was successfully applied to analyze Cd(2+) directly from six human blood serum samples without any pretreatment, and the observed concentrations ranged from

  4. Preconcentration of gold ions from water samples by modified organo-nanoclay sorbent prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mirzaei, Mohammad [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2010-09-15

    In this work, the applicability of modified organo nanoclay as a new and easy prepared solid sorbent for the preconcentration of trace amounts of Au(III) ion from water samples is studied. The organo nanoclay was modified with 5-(4'-dimethylamino benzyliden)-rhodanine and used as a sorbent for separation of Au(III) ions. The sorption of gold ions was quantitative in the pH range of 2.0-6.0. Quantitative desorption occurred with 6.0 mL of 1.0 mol L{sup -1} Na{sub 2}S{sub 2}O{sub 3}. The amount of eluted Au(III) was measured using flame atomic absorption spectrometry. In the initial solution the linear dynamic range was in the range of 0.45 ng mL{sup -1} to 10.0 {mu}g mL{sup -1}, the detection limit was 0.1 ng mL{sup -1} and the preconcentration factor was 105. Also, the relative standard deviation was {+-}2.3% (n = 8 and C = 2.0 {mu}g mL{sup -1}) and the maximum capacity of the sorbent was 3.9 mg of Au(III) per gram of modified organo nanoclay. The influences of the experimental parameters including sample pH, eluent volume and eluent type, sample volume, and interference of some ions on the recoveries of the gold ion were investigated. The proposed method was applied for preconcentration and determination of gold in different samples.

  5. Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection.

    Science.gov (United States)

    Huber, Charles S; Vale, Maria Goreti R; Dessuy, Morgana B; Svoboda, Milan; Musil, Stanislav; Dědina, Jiři

    2017-12-01

    A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO 3 , HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL -1 HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg -1 for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg -1 which were below the limits of 300, 200 and 100µgkg -1 set by the Brazilian, Chinese and European legislation, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Investigation of the levels of some element in edible oil samples produced in Turkey by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Mendil, Durali; Uluoezlue, Ozguer Dogan; Tuezen, Mustafa; Soylak, Mustafa

    2009-01-01

    The element contents (Fe, Mn, Zn, Cu, Pb, Co, Cd, Na, K, Ca and Mg) in edible oils (olive oil, hazelnut oil, sunflower oil, margarine, butter and corn oil) from Turkey were determined using atomic absorption spectrometry after microwave digestion. The concentrations of trace element in the samples were found to be 291.0-52.0, 1.64-0.04, 3.08-1.03, 0.71-0.05, 0.03-0.01, 1.30-0.50, 84.0-0.90, 50.1-1.30, 174.2-20.8 and 20.8-0.60 μg/g for iron, manganese, zinc, copper, lead, cobalt, sodium, potassium, calcium, and magnesium, respectively. Cadmium was found to be 4.57-0.09 μg/kg. The high heavy metal and minerals accumulation levels in the samples were found in olive oil for Cu, Pb, Co, margarine for Fe, K, corn oil for Zn, Mn, butter for Na, Mg, sunflower oil for Ca and hazelnut oil for Cd, respectively.

  7. Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

    Science.gov (United States)

    Cizdziel, James V.

    2011-01-01

    In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

  8. Determination of antimony by electrochemical hydride generation atomic absorption spectrometry in samples with high iron content using chelating resins as on-line removal system

    International Nuclear Information System (INIS)

    Bolea, E.; Arroyo, D.; Laborda, F.; Castillo, J.R.

    2006-01-01

    A method for the removal of the interference caused by iron on electrochemical generation of stibine is proposed. It consists of a chelating resin Chelex 100 column integrated into a flow injection system and coupled to the electrochemical hydride generator quartz tube atomic absorption spectrometer (EcHG-QT-AAS). Iron, as Fe(II), is retained in the column with high efficiency, close to 99.9% under optimal conditions. No significant retention was observed for Sb(III) under same conditions and a 97 ± 5% signal recovery was achieved. An electrochemical hydride generator with a concentric configuration and a reticulated vitreous carbon cathode was employed. The system is able to determine antimony concentrations in the range of ng ml -1 in presence of iron concentrations up to 400 mg l -1 . The procedure was validated by analyzing PACS-2 marine sediments reference material with a 4% (w/w) iron content and a [Fe]:[Sb] ratio of 4000:1, which caused total antimony signal suppression on the electrochemical hydride generation system. A compost sample with high iron content (0.7%, w/w), was also analyzed. A good agreement was found on both samples with the certified value and the antimony concentration determined by ICP-MS, respectively

  9. Method Comparison of Neutron Activation Analysis and Atomic Absorption Spectrometry for Determination of Zinc in Food Samples

    International Nuclear Information System (INIS)

    Endah Damastuti; Syukria Kurniawati; Natalia Adventini

    2009-01-01

    Zinc as a micro nutrient, has important roles in human metabolism system. It is required by the body in appropriate amount from food intake. Due to the very low concentration of Zinc in food, high selectivity and sensitivity analysis technique is required for the determination, such as Neutron Activation Analysis (NAA) and Atomic Absorption Spectrometry (AAS). In this experiment, both methods were compared in zinc analysis of food samples. The subject of this experiment is to examine of those methods conformity and improving the technique capability in zinc analysis in food sample. Those methods were validated by analyzing zinc in SRM NIST 1548a Typical Diet and were tested its accuracy and precision. The results of Zn concentration were 25.1 ± 2.14 mg/kg by NAA and 24.1 ± 1.40 mg/kg by AAS while the certificate value was 24.6 ± 1.80 mg/kg. Percentage of relative bias, %CV, μ-test score and HORRAT(Horwitz ratio) value given by NAA were 2%, 8.5%, 0.18 and 0.9 respectively, while %relative bias, %CV, μ-test score and HORRAT value given by AAS were 2%, 5.8 %, 0.20 and 0.6 respectively. The result obtained for Zn concentration in various food samples by NAA and AAS were varied from 13.7 – 29.3 mg/kg with mean value 19.8 mg/kg and 11.2 – 26.0 mg/kg with mean value 17.3 mg/kg (author)

  10. Determination of palladium in various samples by atomic absorption spectrometry after preconcentration with dimethylglyoxime on silica gel

    International Nuclear Information System (INIS)

    Tokalioglu, Serife; Oymak, Tuelay; Kartal, Senol

    2004-01-01

    A preconcentration method based on the adsorption of palladium-dimethylglyoxime (DMG) complex on silica gel for the determination of palladium at trace levels by atomic absorption spectrometry (AAS) has been developed. The retained palladium as Pd(DMG) 2 complex was eluted with 1 mol l -1 HCl in acetone. The effect of some analytical parameters such as pH, amount of reagent and the sample volume on the recovery of palladium was examined in synthetic solutions containing street dust matrix. The influence of some matrix ions on the recovery of palladium was investigated by using the developed method when the elements were present both individually and together. The results showed that 2500 μg ml -1 Na + , K + , Mg 2+ , Al 3+ and Fe 3+ ; 5000 μg ml -1 Ca 2+ ; 500 μg ml -1 Pb 2+ ; 125 μg ml -1 Zn 2+ ; 50 μg ml -1 Cu 2+ and 25 μg ml -1 Ni 2+ did not interfere with the palladium signal. At the optimum conditions determined experimentally, the recovery for palladium was found to be 95.3±1.2% at the 95% confidence level. The relative standard deviation and limit of detection (3s/b) of the method were found to be 1.7% and 1.2 μg l -1 , respectively. In order to determine the adsorption behaviour of silica gel, the adsorption isotherm of palladium was studied and the binding equilibrium constant and adsorption capacity were calculated to be 0.38 l mg -1 and 4.06 mg g -1 , respectively. The determination of palladium in various samples was performed by using both flame AAS and graphite furnace AAS. The proposed method was successfully applied for the determination of palladium in the street dust, anode slime, rock and catalytic converter samples

  11. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Cortez Diaz, Mirella del Carmen

    2002-01-01

    Heavy metals are a big source of environmental contamination and are also highly toxic to humans. Since shellfish are bio-accumulators of these metals, proper techniques for quantifying them should be available. This work aims to develop an analytical method for the quantitative determination of heavy metals in biological materials (shellfish), specifically arsenic and cadmium at the trace level, using graphite furnace atomic absorption spectrometry, for which nickel and phosphate solutions were used to modify the modifiers. Prior to the analysis, the sample was diluted with nitric acid in a DAB II pressure digestion system order to destroy the organic matter. The instrument conditions were initially set (wavelength, slit, integration peaks, graphite tube, etc.), then the work range was defined for each element and the most appropriate operational parameters were studied, such as: temperature, ramp times, hold times and internal gas flow, in the different stage of the electrothermal treatment (drying, calcination, atomization) for the furnace program. Once the above mentioned conditions were set and since this was a biological sample, a matrix chemical modifier had to be used, in order to make the elements that accompany the element being studied more volatile. In this way the chemical and spectral interferences decrease together with the high background absorption of the matrix. Therefore, different matrix modifiers were studied for the definition of each analyte. The method validation was done using Certified Oyster Tissue Reference Material N o 1566a from the National Institute of Standards and Technology applying different tests in order to eliminate outliers. Repeatability, uncertainty, sensitivity, lineal range, working range, detection limit and quantification limit were evaluated for each element, and the results were compared with the values for the certified material. The Fisher and Student tests were the statistical tools used. The experimental values

  12. Sixteen-item Anxiety Sensitivity Index: Confirmatory factor analytic evidence, internal consistency, and construct validity in a young adult sample from the Netherlands

    NARCIS (Netherlands)

    Vujanovic, Anka A.; Arrindell, Willem A.; Bernstein, Amit; Norton, Peter J.; Zvolensky, Michael J.

    The present investigation examined the factor structure, internal consistency, and construct validity of the 16-item Anxiety Sensitivity Index (ASI; Reiss Peterson, Gursky, & McNally 1986) in a young adult sample (n = 420)from the Netherlands. Confirmatory factor analysis was used to comparatively

  13. Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sigrist, Mirna, E-mail: msigrist@fiq.unl.edu.ar [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Albertengo, Antonela; Beldomenico, Horacio [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Tudino, Mabel [Laboratorio de Analisis de Trazas, Departamento de Quimica Inorganica, Analitica y Quimica Fisica/INQUIMAE, Facultad de Ciencias Exactas y Naturales, Pabellon II, Ciudad Universitaria (1428), Buenos Aires (Argentina)

    2011-04-15

    A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH{sub 3} generation using 3.5 mol L{sup -1} HCl as carrier solution and 0.35% (m/v) NaBH{sub 4} in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl{sup -}, SO{sub 4}{sup 2-}, NO{sub 3}{sup -}, HPO{sub 4}{sup 2-}, HCO{sub 3}{sup -} on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C{sub 6}H{sub 8}O{sub 6} solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 {mu}g L{sup -1} and 0.6 {mu}g L{sup -1} for As(III) and inorganic total As, respectively, were obtained for a 500 {mu}L sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h{sup -1}. The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species

  14. Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Sigrist, Mirna; Albertengo, Antonela; Beldomenico, Horacio; Tudino, Mabel

    2011-01-01

    A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH 3 generation using 3.5 mol L -1 HCl as carrier solution and 0.35% (m/v) NaBH 4 in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl - , SO 4 2- , NO 3 - , HPO 4 2- , HCO 3 - on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C 6 H 8 O 6 solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 μg L -1 and 0.6 μg L -1 for As(III) and inorganic total As, respectively, were obtained for a 500 μL sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h -1 . The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species separation was performed through the employ of a serial connection of membrane filters and

  15. Graphene for separation and preconcentration of trace amounts of cobalt in water samples prior to flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Yukun Wang

    2016-09-01

    Full Text Available A new sensitive and simple method was developed for the preconcentration of trace amounts of cobalt (Co using 1-(2-pyridylazo-2-naphthol (PAN as chelating reagent prior to its determination by flame atomic absorption spectrometry. The proposed method is based on the utilization of a column packed with graphene as sorbent. Several effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 5.0–240.0 μg L−1 with a detection limit of 0.36 μg L−1. The relative standard deviation for ten replicate measurements of 20.0 and 100.0 μg L−1 of Co were 3.45 and 3.18%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Co. The proposed method was successfully applied in the analysis of four real environmental water samples. Good spiked recoveries over the range of 95.8–102.6% were obtained.

  16. Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

    2013-12-01

    A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

  17. Evaluation of the self-absorption of 14C beta-rays in gel-suspension samples by Monte Carlo simulation

    International Nuclear Information System (INIS)

    Wakabayashi, G.; Nagao, K.; Okai, T.; Matoba, M.

    2003-01-01

    In order to investigate the self-absorption of the β-rays from 14 C in a gel-suspension sample, the Monte Carlo code, simulating the sequence of stages occurring in the sample, has been developed. The trajectory of the electron was calculated by the continuous slowing down approximation and the multiple Coulomb scattering theory. The effects of the self-absorption, strong quenching and particle size distribution of calcium carbonate on the output counting efficiency and the shape of the energy spectrum were evaluated. (author)

  18. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Villalobos Aranda, Juan; Cortez Diaz, Mirella

    2003-01-01

    Serious problems of environmental contamination due to the activity of the man exist at the present time. Where the greater impact is the produced one by heavy metals that go to the sea. Where the shellfish can collect some of them, the highly toxic ones, since these are bioaccumulation of these metals. Therefore one becomes necessary to count with the reliable analytical procedures to determine these elements. The purpose of this work is to present the determination of arsenic and cadmium in shellfish, by spectroscopy of atomic absorption with graphite furnace. For each determined element, solutions of nickel and phosphate like matrix modifiers were used respectively The validation was made using a Reference Certified Material, Oyster ' Tissue 156 (National Institute of Standards and Technology). The sample previously was digested in triplicate by two consecutive days, with nitric acid in a pressure digestion system DAB 11. For each element it was evaluated: limit of detection and quantification, sensitivity, repeatability, linear, slope rank and uncertainty. In addition, the obtained results were compared with the certified values of the certified material of reference using like statistical tools the tests of Student and Fisher. In both tests the calculated values were smaller to the shown ones in table, for degrees of freedom with 95% of confidence. Thus it was verified that it does not exist significant differences between the precision and the average values of the results obtained with respect to the values of the certified material. In addition, the obtained parameters are appropriate for the determination of these trace elements in this type of environmental sample (author)

  19. Daily Elevations in Dissociative Absorption and Depersonalization in a Nonclinical Sample Are Related to Daily Stress and Psychopathological Symptoms.

    Science.gov (United States)

    Soffer-Dudek, Nirit

    2017-01-01

    Dissociative experiences are associated with several psychopathological symptoms and are a hindrance to therapeutic gain. Depersonalization-derealization (DEP-DER) is positively associated with stress and anxiety, while absorption and imaginative involvement (ABS), a tendency for total, immersed attention, is commonly referred to as nonpathological dissociation, although it is positively associated with obsessive-compulsive (OC) symptoms. Previous studies in the field have been mainly cross-sectional. The present study aimed to examine these associations rigorously and attempted to determine directionality between dissociation and distress. The current study employed both variable-centered (cross-sectional) and person-centered (longitudinal, within-subjects) analyses of the associations of DEP-DER and ABS with distress. Undergraduate students (N = 184) completed trait questionnaires on dissociation, stress, anxiety, depression, and OC symptoms, and n = 78 also completed questionnaires assessing the same constructs daily for 14 days. Multiple regression and multilevel modeling analyses were conducted. In the cross-sectional phase, DEP-DER was uniquely positively related to anxiety and OC symptoms, and ABS was uniquely positively related to OC symptoms. In the daily diary phase, increases in DEP-DER were related to increases in anxiety, depression, OC symptoms, and stress, while increases in ABS were related to increases in OC symptoms and stress. In addition, time-lag analysis showed that ABS tended to temporally precede OC. ABS foretold increases in OC symptoms, at least in this nonclinical sample. Future studies on clinical samples should explore whether ABS should be referred to as "nonpathological" and its possible role in the development or maintenance of clinical-level OCD.

  20. Comparison of different sample preparation methods for platinum determination in cultured cells by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Man Xiao

    2017-01-01

    Full Text Available Background Platinum-based agents are widely used in chemotherapy against solid tumors and insufficient intracellular drug accumulation is one of the leading causes of platinum resistance which is associated with poor survival of tumor patients. Thus, the detection of intracellular platinum is pivotal for studies aiming to overcome platinum resistance. In the present study, we aimed to establish a reliable graphite furnace atomic absorption spectrometry (GFAAS-based assay to quantify the intracellular platinum content for cultured cells. Methods Several most commonly applied cell preparation methods, including 0.2% HNO3, 0.2% Triton X-100, concentrated nitric acid, RIPA combined with concentrated nitric acid and hydroxide, followed by GFAAS for platinum detection were compared in ovarian, cervical and liver cancer cell lines to obtain the optimal one, and parameters regarding linearity, accuracy, precision and sensitivity were evaluated. Influence of other metals on platinum detection and the storage conditions of samples were also determined. Results The treatment of cells with 0.2% HNO3 was superior to other approaches with fewer platinum loss and better repeatability. The recovery rate and precision of this method were 97.3%–103.0% and 1.4%–3.8%, respectively. The average recoveries in the presence of other metals were 95.1%–103.1%. The detection limit was 13.23 ug/L. The recovery rate of platinum remained acceptable even in cell samples stored in −20 °C or −80 °C for two months. Discussion After comparison, we found that 0.2% HNO3 was optimal for intracellular platinum quantification based on GFAAS, which presented values compatible with that of inductively-coupled plasma mass-spectrometry (ICP-MS, and this is partially attributed to the simplicity of this method. Moreover, the assay was proved to be accurate, sensitive, cost-effective and suitable for the research of platinum-based antitumor therapy.

  1. Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Satrústegui, Jorgina; Procopio, Jesús R

    2017-08-01

    A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL -1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL -1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Reliability of attitude and knowledge items and behavioral consistency in the validated sun exposure questionnaire in a Danish population based sample

    DEFF Research Database (Denmark)

    Køster, Brian; Søndergaard, Jens; Nielsen, Jesper Bo

    2018-01-01

    in protection behavior was low. To our knowledge, this is the first study to report reliability for a completely validated questionnaire on sun-related behavior in a national random population based sample. Further, we show that attitude and knowledge questions confirmed their validity with good reliability......An important feature of questionnaire validation is reliability. To be able to measure a given concept by questionnaire validly, the reliability needs to be high. The objectives of this study were to examine reliability of attitude and knowledge and behavioral consistency of sunburn in a developed...... questionnaire for monitoring and evaluating population sun-related behavior. Sun related behavior, attitude and knowledge was measured weekly by a questionnaire in the summer of 2013 among 664 Danes. Reliability was tested in a test-retest design. Consistency of behavioral information was tested similarly...

  3. Effective absorption correction for energy dispersive X-ray mapping in a scanning transmission electron microscope: analysing the local indium distribution in rough samples of InGaN alloy layers.

    Science.gov (United States)

    Wang, X; Chauvat, M-P; Ruterana, P; Walther, T

    2017-12-01

    We have applied our previous method of self-consistent k*-factors for absorption correction in energy-dispersive X-ray spectroscopy to quantify the indium content in X-ray maps of thick compound InGaN layers. The method allows us to quantify the indium concentration without measuring the sample thickness, density or beam current, and works even if there is a drastic local thickness change due to sample roughness or preferential thinning. The method is shown to select, point-by-point in a two-dimensional spectrum image or map, the k*-factor from the local Ga K/L intensity ratio that is most appropriate for the corresponding sample geometry, demonstrating it is not the sample thickness measured along the electron beam direction but the optical path length the X-rays have to travel through the sample that is relevant for the absorption correction. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

  4. Portable ultrahigh-vacuum sample storage system for polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, Yoshihide, E-mail: e0827@mosk.tytlabs.co.jp; Nishimura, Yusaku F.; Suzuki, Ryo; Beniya, Atsushi; Isomura, Noritake [Toyota Central R& D Labs., Inc., Yokomichi 41-1, Nagakute, Aichi 480-1192 (Japan); Uehara, Hiromitsu; Asakura, Kiyotaka; Takakusagi, Satoru [Catalysis Research Center, Hokkaido University, Kita 21-10, Sapporo, Hokkaido 001-0021 (Japan); Nimura, Tomoyuki [AVC Co., Ltd., Inada 1450-6, Hitachinaka, Ibaraki 312-0061 (Japan)

    2016-03-15

    A portable ultrahigh-vacuum sample storage system was designed and built to investigate the detailed geometric structures of mass-selected metal clusters on oxide substrates by polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy (PTRF-XAFS). This ultrahigh-vacuum (UHV) sample storage system provides the handover of samples between two different sample manipulating systems. The sample storage system is adaptable for public transportation, facilitating experiments using air-sensitive samples in synchrotron radiation or other quantum beam facilities. The samples were transferred by the developed portable UHV transfer system via a public transportation at a distance over 400 km. The performance of the transfer system was demonstrated by a successful PTRF-XAFS study of Pt{sub 4} clusters deposited on a TiO{sub 2}(110) surface.

  5. Internal consistency, test-retest reliability and measurement error of the self-report version of the social skills rating system in a sample of Australian adolescents.

    Directory of Open Access Journals (Sweden)

    Sharmila Vaz

    Full Text Available The social skills rating system (SSRS is used to assess social skills and competence in children and adolescents. While its characteristics based on United States samples (US are published, corresponding Australian figures are unavailable. Using a 4-week retest design, we examined the internal consistency, retest reliability and measurement error (ME of the SSRS secondary student form (SSF in a sample of Year 7 students (N = 187, from five randomly selected public schools in Perth, western Australia. Internal consistency (IC of the total scale and most subscale scores (except empathy on the frequency rating scale was adequate to permit independent use. On the importance rating scale, most IC estimates for girls fell below the benchmark. Test-retest estimates of the total scale and subscales were insufficient to permit reliable use. ME of the total scale score (frequency rating for boys was equivalent to the US estimate, while that for girls was lower than the US error. ME of the total scale score (importance rating was larger than the error using the frequency rating scale. The study finding supports the idea of using multiple informants (e.g. teacher and parent reports, not just student as recommended in the manual. Future research needs to substantiate the clinical meaningfulness of the MEs calculated in this study by corroborating them against the respective Minimum Clinically Important Difference (MCID.

  6. Internal consistency, test-retest reliability and measurement error of the self-report version of the social skills rating system in a sample of Australian adolescents.

    Science.gov (United States)

    Vaz, Sharmila; Parsons, Richard; Passmore, Anne Elizabeth; Andreou, Pantelis; Falkmer, Torbjörn

    2013-01-01

    The social skills rating system (SSRS) is used to assess social skills and competence in children and adolescents. While its characteristics based on United States samples (US) are published, corresponding Australian figures are unavailable. Using a 4-week retest design, we examined the internal consistency, retest reliability and measurement error (ME) of the SSRS secondary student form (SSF) in a sample of Year 7 students (N = 187), from five randomly selected public schools in Perth, western Australia. Internal consistency (IC) of the total scale and most subscale scores (except empathy) on the frequency rating scale was adequate to permit independent use. On the importance rating scale, most IC estimates for girls fell below the benchmark. Test-retest estimates of the total scale and subscales were insufficient to permit reliable use. ME of the total scale score (frequency rating) for boys was equivalent to the US estimate, while that for girls was lower than the US error. ME of the total scale score (importance rating) was larger than the error using the frequency rating scale. The study finding supports the idea of using multiple informants (e.g. teacher and parent reports), not just student as recommended in the manual. Future research needs to substantiate the clinical meaningfulness of the MEs calculated in this study by corroborating them against the respective Minimum Clinically Important Difference (MCID).

  7. Study on the application of electrothermal atomization atomic absorption spectrometry for the determination of metallic Cu, Pb, Zn, Cd traces in sea water samples

    International Nuclear Information System (INIS)

    Nguyen Thi Kim Dung; Doan Thanh Son; Tran Thi Ngoc Diep

    2004-01-01

    The trace amount of some heavy metallic elements (Cu, Zn, Pb, Cd) in sea water samples were determined directly (without separation) and quantitatively by using Electro-Thermal Atomization Atomic Absorption Spectrometry (ETA-AAS). The effect of mainly major constituents such as Na, Mg, Ca, K, and the mutual effect of the trace elements, which were present in the matrix on the absorption intensity of each analyzed element was studied. The adding of a certain chemical modification for each trace element was also investigated in order to eliminate the overall effect of the background during the pyrolysis and atomization. The sea water sample after fitrating through a membrane with 0.45 μm-hole size was injected in to the graphite tube via an autosampler (MPE50). The absorption intensity of each element was then measured on the VARIO-6 under the optimum parameters for spectrometer such as: maximum wavelength, current of hollow cathode lamp, and that for graphite furnace such as dry temperature, pyrolysis temperature, atomization temperature, ect. The analytical procedures were set-up and applied for the determination of these above mentioned elements in the synthesized sea water sample and in the real sea water samples with high precision and accuracy. (author)

  8. Towards the harmonization between National Forest Inventory and Forest Condition Monitoring. Consistency of plot allocation and effect of tree selection methods on sample statistics in Italy.

    Science.gov (United States)

    Gasparini, Patrizia; Di Cosmo, Lucio; Cenni, Enrico; Pompei, Enrico; Ferretti, Marco

    2013-07-01

    In the frame of a process aiming at harmonizing National Forest Inventory (NFI) and ICP Forests Level I Forest Condition Monitoring (FCM) in Italy, we investigated (a) the long-term consistency between FCM sample points (a subsample of the first NFI, 1985, NFI_1) and recent forest area estimates (after the second NFI, 2005, NFI_2) and (b) the effect of tree selection method (tree-based or plot-based) on sample composition and defoliation statistics. The two investigations were carried out on 261 and 252 FCM sites, respectively. Results show that some individual forest categories (larch and stone pine, Norway spruce, other coniferous, beech, temperate oaks and cork oak forests) are over-represented and others (hornbeam and hophornbeam, other deciduous broadleaved and holm oak forests) are under-represented in the FCM sample. This is probably due to a change in forest cover, which has increased by 1,559,200 ha from 1985 to 2005. In case of shift from a tree-based to a plot-based selection method, 3,130 (46.7%) of the original 6,703 sample trees will be abandoned, and 1,473 new trees will be selected. The balance between exclusion of former sample trees and inclusion of new ones will be particularly unfavourable for conifers (with only 16.4% of excluded trees replaced by new ones) and less for deciduous broadleaves (with 63.5% of excluded trees replaced). The total number of tree species surveyed will not be impacted, while the number of trees per species will, and the resulting (plot-based) sample composition will have a much larger frequency of deciduous broadleaved trees. The newly selected trees have-in general-smaller diameter at breast height (DBH) and defoliation scores. Given the larger rate of turnover, the deciduous broadleaved part of the sample will be more impacted. Our results suggest that both a revision of FCM network to account for forest area change and a plot-based approach to permit statistical inference and avoid bias in the tree sample

  9. Determination of gold, indium, tellurium and thallium in the same sample digest of geological materials by atomic-absorption spectroscopy and two-step solvent extraction

    Science.gov (United States)

    Hubert, A.E.; Chao, T.T.

    1985-01-01

    A rock, soil, or stream-sediment sample is decomposed with hydrofluoric acid, aqua regia, and hydrobromic acid-bromine solution. Gold, thallium, indium and tellurium are separated and concentrated from the sample digest by a two-step MIBK extraction at two concentrations of hydrobromic add. Gold and thallium are first extracted from 0.1M hydrobromic acid medium, then indium and tellurium are extracted from 3M hydrobromic acid in the presence of ascorbic acid to eliminate iron interference. The elements are then determined by flame atomic-absorption spectrophotometry. The two-step solvent extraction can also be used in conjunction with electrothermal atomic-absorption methods to lower the detection limits for all four metals in geological materials. ?? 1985.

  10. Hair MDMA samples are consistent with reported ecstasy use: findings from a study investigating effects of ecstasy on mood and memory.

    Science.gov (United States)

    Scholey, A B; Owen, L; Gates, J; Rodgers, J; Buchanan, T; Ling, J; Heffernan, T; Swan, P; Stough, C; Parrott, A C

    2011-01-01

    Our group has conducted several Internet investigations into the biobehavioural effects of self-reported recreational use of MDMA (3,4-methylenedioxymethamphetamine or Ecstasy) and other psychosocial drugs. Here we report a new study examining the relationship between self-reported Ecstasy use and traces of MDMA found in hair samples. In a laboratory setting, 49 undergraduate volunteers performed an Internet-based assessment which included mood scales and the University of East London Drug Use Questionnaire, which asks for history and current drug use. They also provided a hair sample for determination of exposure to MDMA over the previous month. Self-report of Ecstasy use and presence in hair samples were consistent (p happiness and higher self-reported stress. Self-reported Ecstasy use, but not presence in hair, was also associated with decreased tension. Different psychoactive drugs can influence long-term mood and cognition in complex and dynamically interactive ways. Here we have shown a good correspondence between self-report and objective assessment of exposure to MDMA. These data suggest that the Internet has potentially high utility as a useful medium to complement traditional laboratory studies into the sequelae of recreational drug use. Copyright © 2010 S. Karger AG, Basel.

  11. A nanocomposite consisting of graphene oxide and Fe3O4 magnetic nanoparticles for the extraction of flavonoids from tea, wine and urine samples

    International Nuclear Information System (INIS)

    Wu, Jianrong; Xiao, Deli; Peng, Jun; Wang, Cuixia; Zhang, Chan; He, Jia; Zhao, Hongyan; He, Hua

    2015-01-01

    We describe a single-step solvothermal method for the preparation of nanocomposites consisting of graphene oxide and Fe 3 O 4 nanoparticles (GO/Fe 3 O 4 ). This material is shown to be useful as a magnetic sorbent for the extraction of flavonoids from green tea, red wine, and urine samples. The nanocomposite is taking advantage of the high surface area of GO and the magnetic phase separation feature of the magnetic sorbent. The nanocomposite is recyclable and was applied to the extraction of flavonoids prior to their determination by HPLC. The effects of amount of surfactant, pH value of the sample solution, extraction time, and desorption condition on the extraction efficiency, and the regeneration conditions were optimized. The limits of detection for luteolin, quercetin and kaempferol range from 0.2 to 0.5 ng∙ mL −1 in urine, from 3.0 to 6.0 ng∙mL −1 in green tea, and from 1.0 to 2.5 ng∙mL −1 in red wine. The recoveries are between 82.0 and 101.4 %, with relative standard deviations of <9.3 %. (author)

  12. Interface Consistency

    DEFF Research Database (Denmark)

    Staunstrup, Jørgen

    1998-01-01

    This paper proposes that Interface Consistency is an important issue for the development of modular designs. Byproviding a precise specification of component interfaces it becomes possible to check that separately developedcomponents use a common interface in a coherent matter thus avoiding a very...... significant source of design errors. Awide range of interface specifications are possible, the simplest form is a syntactical check of parameter types.However, today it is possible to do more sophisticated forms involving semantic checks....

  13. Determination of self-absorption coefficient in measurement of solid sample activity using 4π ionization chamber

    International Nuclear Information System (INIS)

    Dryak, P.

    1982-01-01

    Computation based on the Monte Carlo method was tested for a 4π cylindrical ionization chamber with a detection volume of 7 litres, filled with argon. The sources are placed in the geometrical centre. The correction coefficient for self-absorption was determined as being the ratio of ionization currents induced by a source of finite size and by a massless point source. A flowchart of the program is given. The computations were experimentally tested for cylindrical sources of aqueous 137 Cs and 57 Co solutions. (M.D.)

  14. CHANG-ES. IX. Radio scale heights and scale lengths of a consistent sample of 13 spiral galaxies seen edge-on and their correlations

    Science.gov (United States)

    Krause, Marita; Irwin, Judith; Wiegert, Theresa; Miskolczi, Arpad; Damas-Segovia, Ancor; Beck, Rainer; Li, Jiang-Tao; Heald, George; Müller, Peter; Stein, Yelena; Rand, Richard J.; Heesen, Volker; Walterbos, Rene A. M.; Dettmar, Ralf-Jürgen; Vargas, Carlos J.; English, Jayanne; Murphy, Eric J.

    2018-03-01

    Aim. The vertical halo scale height is a crucial parameter to understand the transport of cosmic-ray electrons (CRE) and their energy loss mechanisms in spiral galaxies. Until now, the radio scale height could only be determined for a few edge-on galaxies because of missing sensitivity at high resolution. Methods: We developed a sophisticated method for the scale height determination of edge-on galaxies. With this we determined the scale heights and radial scale lengths for a sample of 13 galaxies from the CHANG-ES radio continuum survey in two frequency bands. Results: The sample average values for the radio scale heights of the halo are 1.1 ± 0.3 kpc in C-band and 1.4 ± 0.7 kpc in L-band. From the frequency dependence analysis of the halo scale heights we found that the wind velocities (estimated using the adiabatic loss time) are above the escape velocity. We found that the halo scale heights increase linearly with the radio diameters. In order to exclude the diameter dependence, we defined a normalized scale height h˜ which is quite similar for all sample galaxies at both frequency bands and does not depend on the star formation rate or the magnetic field strength. However, h˜ shows a tight anticorrelation with the mass surface density. Conclusions: The sample galaxies with smaller scale lengths are more spherical in the radio emission, while those with larger scale lengths are flatter. The radio scale height depends mainly on the radio diameter of the galaxy. The sample galaxies are consistent with an escape-dominated radio halo with convective cosmic ray propagation, indicating that galactic winds are a widespread phenomenon in spiral galaxies. While a higher star formation rate or star formation surface density does not lead to a higher wind velocity, we found for the first time observational evidence of a gravitational deceleration of CRE outflow, e.g. a lowering of the wind velocity from the galactic disk.

  15. Coupling continuous ultrasound-assisted extraction, preconcentration and flame atomic absorption spectrometric detection for the determination of cadmium and lead in mussel samples

    International Nuclear Information System (INIS)

    Yebra-Biurrun, M.C.; Cancela-Perez, S.; Moreno-Cid-Barinaga, A.

    2005-01-01

    Continuous ultrasound-assisted extraction has been coupled with preconcentration and flame atomic absorption spectrometry for the determination of cadmium and lead in mussel samples. Experimental designs were used for the optimisation of the leaching and preconcentration steps. The use of diluted nitric acid as extractant in the continuous mode at a flow rate of 3.5 ml min -1 and room temperature was sufficient for quantitative extraction of these trace metals. A minicolumn containing a chelating resin (Chelite P, with aminomethylphosphoric acid groups) was proved as an excellent material for the quantitative preconcentration of cadmium and lead prior to their flame atomic absorption detection. A flow injection manifold was used as interface for coupling the three analytical steps, which allowed the automation of the whole analytical process. A good precision of the whole procedure (2.0 and 2.3%), high enrichment factors (20.5 and 11.8) and a detection limit of 0.011 and 0.25 μg g -1 for cadmium and lead, respectively, were obtained for 80 mg of sample. The sample throughputs were ca. 16 and 14 samples h -1 for cadmium and lead, respectively. The accuracy of the analytical procedures was verified by using a standard reference material (BCR 278-R, mussel tissue) and the results were in good agreement with the certified values. The method was successfully applied to the determination of trace amounts of cadmium and lead in mussel samples from the coast of Galicia (NW, Spain)

  16. Determination of phospholipids in soybean lecithin samples via the phosphorus monoxide molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    Science.gov (United States)

    Pires, Laís N; Brandão, Geovani C; Teixeira, Leonardo S G

    2017-06-15

    This paper presents a method for determining phospholipids in soybean lecithin samples by phosphorus determination using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) via molecular absorption of phosphorus monoxide. Samples were diluted in methyl isobutyl ketone. The best conditions were found to be 213.561nm with a pyrolysis temperature of 1300°C, a volatilization temperature of 2300°C and Mg as a chemical modifier. To increase the analytical sensitivity, measurement of the absorbance signal was obtained by summing molecular transition lines for PO surrounding 213nm: 213.561, 213.526, 213.617 and 213.637nm. The limit of detection was 2.35mgg -1 and the precision, evaluated as relative standard deviation (RSD), was 2.47% (n=10) for a sample containing 2.2% (w/v) phosphorus. The developed method was applied for the analysis of commercial samples of soybean lecithin. The determined concentrations of phospholipids in the samples varied between 38.1 and 45% (w/v). Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Measurement of electron-spin transports in GaAs quantum wells using a transmission-grating-sampled circular dichroism absorption spectroscopy

    International Nuclear Information System (INIS)

    Yu, Hua-Liang; Fang, Shaoyin; Wen, Jinhui; Lai, Tianshu

    2014-01-01

    A transmission-grating-sampled circular dichroism absorption spectroscopy (TGS-CDAS) and its theoretical model are developed sensitively to measure decay dynamics of a transient spin grating (TSG). A binary transmission grating with the same period as TSG is set behind TSG. It allows only a same small part of each period in TSG measured by circular dichroism absorption effect of a probe. In this way, the zero average of spin-dependent effects measured over a whole period in TSG is avoided so that TGS-CDAS has a high sensitivity to spin evolution in TSG. Spin transport experiments are performed on GaAs/AlGaAs quantum wells. Experimental results prove the feasibility and reliability of TGS-CDAS

  18. Robust and economical multi-sample, multi-wavelength UV/vis absorption and fluorescence detector for biological and chemical contamination

    Science.gov (United States)

    Lu, Peter J.; Hoehl, Melanie M.; Macarthur, James B.; Sims, Peter A.; Ma, Hongshen; Slocum, Alexander H.

    2012-09-01

    We present a portable multi-channel, multi-sample UV/vis absorption and fluorescence detection device, which has no moving parts, can operate wirelessly and on batteries, interfaces with smart mobile phones or tablets, and has the sensitivity of commercial instruments costing an order of magnitude more. We use UV absorption to measure the concentration of ethylene glycol in water solutions at all levels above those deemed unsafe by the United States Food and Drug Administration; in addition we use fluorescence to measure the concentration of d-glucose. Both wavelengths can be used concurrently to increase measurement robustness and increase detection sensitivity. Our small robust economical device can be deployed in the absence of laboratory infrastructure, and therefore may find applications immediately following natural disasters, and in more general deployment for much broader-based testing of food, agricultural and household products to prevent outbreaks of poisoning and disease.

  19. Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Ma Jesús; Sevilla, Ma Teresa; Procopio, Jesús R

    2015-01-07

    The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Selective reduction of arsenic species by hydride generation - atomic absorption spectrometry. Part 2 - sample storage and arsenic determination in natural waters

    Directory of Open Access Journals (Sweden)

    Quináia Sueli P.

    2001-01-01

    Full Text Available Total arsenic, arsenite, arsinate and dimethylarsinic acid (DMA were selectively determined in natural waters by hydride generation - atomic absorption spectrometry, using sodium tetrahydroborate(III as reductant but in different reduction media. River water samples from the north region of Paraná State, Brazil, were analysed and showed arsenate as the principal arsenical form. Detection limits found for As(III (citrate buffer, As(III + DMA (acetic acid and As(III + As(V (hydrochloric acid were 0.6, 1.1 and 0.5 mg As L-1, respectively. Sample storage on the proper reaction media revealed to be a useful way to preserve the water sample.

  1. Optimization of microwave assisted digestion procedure for the determination of zinc, copper and nickel in tea samples employing flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Soylak, Mustafa; Tuzen, Mustafa; Souza, Anderson Santos; Korn, Maria das Gracas Andrade; Ferreira, Sergio Luis Costa

    2007-01-01

    The present paper describes the development of a microwave assisted digestion procedure for the determination of zinc, copper and nickel in tea samples employing flame atomic absorption spectrometry (FAAS). The optimization step was performed using a full factorial design (2 3 ) involving the factors: composition of the acid mixture (CMA), microwave power (MP) and radiation time (RT). The experiments of this factorial were carried out using a certified reference material of tea GBW 07605 furnished by National Research Centre for Certified Reference Materials, China, being the metal recoveries considered as response. The relative standard deviations of the method were found below 8% for the three elements. The procedure proposed was used for the determination of copper, zinc and nickel in several samples of tea from Turkey. For 10 tea samples analyzed, the concentration achieved for copper, zinc and nickel varied at 6.4-13.1, 7.0-16.5 and 3.1-5.7 (μg g -1 ), respectively

  2. Multi-edge X-ray absorption spectroscopy study of road dust samples from a traffic area of Venice using stoichiometric and environmental references

    Science.gov (United States)

    Valotto, Gabrio; Cattaruzza, Elti; Bardelli, Fabrizio

    2017-02-01

    The appropriate selection of representative pure compounds to be used as reference is a crucial step for successful analysis of X-ray absorption near edge spectroscopy (XANES) data, and it is often not a trivial task. This is particularly true when complex environmental matrices are investigated, being their elemental speciation a priori unknown. In this paper, an investigation on the speciation of Cu, Zn, and Sb based on the use of conventional (stoichiometric compounds) and non-conventional (environmental samples or relevant certified materials) references is explored. This method can be useful in when the effectiveness of XANES analysis is limited because of the difficulty in obtaining a set of references sufficiently representative of the investigated samples. Road dust samples collected along the bridge connecting Venice to the mainland were used to show the potentialities and the limits of this approach.

  3. Investigating effects of sample pretreatment on protein stability using size-exclusion chromatography and high-resolution continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Rakow, Tobias; El Deeb, Sami; Hahne, Thomas; El-Hady, Deia Abd; AlBishri, Hassan M; Wätzig, Hermann

    2014-09-01

    In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Influence of citric acid as chemical modifier for lead determination in dietary calcium supplement samples by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Cezar Paz de Mattos, Julio; Medeiros Nunes, Adriane; Figueiredo Martins, Ayrton; Luiz Dressler, Valderi; Marlon de Moraes Flores, Erico

    2005-01-01

    Citric acid was used as a chemical modifier for Pb determination by graphite furnace atomic absorption spectrometry in dietary supplement samples (calcium carbonate, dolomite and oyster shell samples) and its efficiency was compared to the use of palladium. Pyrolysis and atomization curves were established without use of chemical modifier, with the addition of 20, 100 and 200 μg of citric acid, and with 3 μg of palladium. The citric acid modifier made possible the interference-free Pb determination in the presence of high concentrations of Ca and Mg nitrates. Acid sample digestion involving closed vessels (microwave-assisted and conventional heating) and acid attack using polypropylene vessels at room temperature were compared. All digestion procedures presented similar results for calcium carbonate and dolomite samples. However, for oyster shell samples accurate results were obtained only with the use of closed vessel systems. Analyte addition and matrix-matched standards were used for calibration. The characteristic mass for Pb using citric acid and palladium were 16 and 25 pg, respectively. The relative standard deviation (RSD) was always less than 5% when citric acid was used. The relative and absolute limits of detection were 0.02 μg g -1 and 8 pg with citric acid and 0.1 μg g -1 and 44 pg with the Pd modifier, respectively (n = 10, 3σ). The recovery of Pb in spiked calcium supplement samples (10 μg l -1 ) was between 98% and 105%. With the use of 100 μg of citric acid as chemical modifier, problems such as high background absorption and high RSD values were minimized in comparison to the addition of 3 μg of palladium

  5. Buffer choice and effects of sample composition examined by experiment planning methods for determination of molybdenum by atomic absorption with a flame atomizer

    International Nuclear Information System (INIS)

    Zav'yalkov, P.I.; Danishehvskii, A.L.; Rakita, R.A.; Yakshinskii, A.I.

    1986-01-01

    The authors use orthogonal experiment planning to define the optimum form of buffer and to establish the effects of sample composition since there are high levels of cation and anion interference in the atomic-absorption determination of molybdenum. A spectroscopic buffer has been identified (HCLO 4 + NH 4 Cl mixture), which eliminates the interference from the elements tested and improves the analytical characteristics in determining molybdenum. A model has been formulated enabling one to estimate the buffer performance and the effects of the components on the determination of molybdenum. The model enables one to forecast the expected order of the effect without performing additional experiments

  6. A new approach for the determination of sulphur in food samples by high-resolution continuum source flame atomic absorption spectrometer.

    Science.gov (United States)

    Ozbek, N; Baysal, A

    2015-02-01

    The new approach for the determination of sulphur in foods was developed, and the sulphur concentrations of various fresh and dried food samples determined using a high-resolution continuum source flame atomic absorption spectrometer with an air/acetylene flame. The proposed method was optimised and the validated using standard reference materials, and certified values were found to be within the 95% confidence interval. The sulphur content of foods ranged from less than the LOD to 1.5mgg(-1). The method is accurate, fast, simple and sensitive. Copyright © 2014 Elsevier Ltd. All rights reserved.

  7. Cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry after ultrasound-assisted sample preparation

    International Nuclear Information System (INIS)

    Aleixo, Poliana Carolina; Junior, Dario Santos; Tomazelli, Andrea Cristina; Rufini, Iolanda A.; Berndt, Harald; Krug, Francisco Jose

    2004-01-01

    A simple method for cadmium and lead determination in foods by beam injection flame furnace atomic absorption spectrometry (BIFF-AAS) was proposed. Food slurries were prepared by transferring an exact amount of cryogenic-ground homogenized material (50-100 mg) to centrifuge tubes, followed by addition of 5 ml (up to 2.8 mol l -1 ) nitric acid solution and sonication in an ultrasonic bath during 5-10 min. Thereafter, slurries were diluted with water to 10 ml, centrifuged during 5 min at 5400 rpm and 400 μl aliquot of the supernatant was analyzed by BIFF-AAS. The detection limits based on peak height measurements were 0.03 μg g -1 Cd and 1.6 μg g -1 Pb for 2% (m/v) slurry (200 mg/10 ml). For method validation, the certified reference materials Pig Kidney (BCR 186) and Rice Flour (NIES 10) were used. Quantitative cadmium and lead recoveries were obtained and no statistical differences were found at 95% level by applying the t-test

  8. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    International Nuclear Information System (INIS)

    Matos Reyes, Mariela N.; Campos, Reinaldo C.

    2005-01-01

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO 3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation (n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits (k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l -1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples

  9. Strontium mono-chloride — A new molecule for the determination of chlorine using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Lopez, Alfredo H.D.; Gois, Jefferson S. de; Caramori, Giovanni F. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Borges, Daniel L.G.; Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2014-12-01

    A new method has been developed for the determination of chlorine in biological reference materials using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) of the strontium mono-chloride (SrCl) molecule and direct solid sample analysis. The use of the SrCl molecule for high-temperature MAS was not described up to now in the literature. Preliminary time-dependent density functional theory calculations of the SrCl structure were carried out in order to obtain reasonable estimates of the absorption spectrum of the target molecule. The calculations, which were carried out at BHandHLyp/def2-QZVP level of theory, proved a very accurate and inexpensive way to get information about the spectrum of the SrCl molecule, which enabled us to perform the Cl determination with good sensitivity and specificity. The molecular absorption of the SrCl molecule has been measured using the wavelength at 635.862 nm, and zirconium and palladium have been evaluated as the chemical modifiers in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Accuracy and precision of the method have been evaluated using biological certified reference materials of both animal and plant origins, showing good agreement with the informed and certified values. Limit of detection and characteristic mass were 1.0 and 2.2 ng, respectively. The results found using HR-CS GF MAS were in agreement (95% confidence level) compared to those obtained by electrothermal vaporization-inductively coupled plasma mass spectrometry. - Highlights: • The spectrum of the SrCl molecule was calculated on a theoretical basis and found very close to the predicted wavelength. • It is the first time that the spectrum of the SrCl molecule is described and used analytically for the determination of Cl. • No spectral interferences were observed as the

  10. Preconcentration of trace amounts of lead in water samples with cetyltrimethylammonium bromide coated magnetite nanoparticles and its determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Faraji

    2016-11-01

    Full Text Available A sensitive and simple magnetic solid phase extraction procedure was presented for the preconcentration of lead ions in environmental water samples. In the present study, lead ions form complexes with 1-(2-pyridilazo-2-naphthol reagent (PAN in basic medium, and then are quantitatively extracted to the surface of cetyltrimethylammonium bromide (CTAB-coated magnetite nanoparticles (Fe3O4 NPs. After magnetic separation of adsorbent, the adsorbent was eluted with 0.5% (v/v HCl in methanol prior to its analysis by flame atomic absorption spectrometry (FAAS. The pH of sample, concentrations of PAN, amounts of CTAB and Fe3O4 NPs, sample volume and desorption conditions were optimized. Under optimum conditions, the calibration curve was linear in the range of 0.05–100 ng mL−1 with R2 = 0.9996. Detection and quantification limits of the proposed method were 0.005 and 0.05 ng mL−1, respectively. Enhancement factor of 1050 was achieved using this method to extract 1000 mL of different environmental water samples. Compared with conventional solid phase extraction methods, the advantages of this method still include easy preparation of sorbents, short times of sample pre-treatment, high extraction yield, and high breakthrough volume. It shows great analytical potential in preconcentration of lead from large volume water samples.

  11. In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

    2018-03-01

    In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

  12. Investigation of spectral interferences in the determination of lead in fertilizers and limestone samples using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; François, Luciane L.; Jesus, Alexandre de [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2014-11-01

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH{sub 4}H{sub 2}PO{sub 4} at 217.001 nm, and a mixture of H{sub 2}SO{sub 4} + Ca and HNO{sub 3} + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part. - Highlights: • Spectral interferences on the determination of lead in fertilizers and limestone. • The analytical lines at 217.001 nm and 283.306 nm using HR-CS GF AAS. • Various combinations of compounds were used to create reference spectra. • LSBC

  13. Application of cloud point preconcentration and flame atomic absorption spectrometry for the determination of cadmium and zinc ions in urine, blood serum and water samples

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2013-01-01

    Full Text Available A simple, sensitive and selective cloud point extraction procedure is described for the preconcentration and atomic absorption spectrometric determination of Zn2+ and Cd2+ ions in water and biological samples, after complexation with 3,3',3",3'"-tetraindolyl (terephthaloyl dimethane (TTDM in basic medium, using Triton X-114 as nonionic surfactant. Detection limits of 3.0 and 2.0 µg L-1 and quantification limits 10.0 and 7.0 µg L-1were obtained for Zn2+ and Cd2+ ions, respectively. Relative standard deviation was 2.9 and 3.3, and enrichment factors 23.9 and 25.6, for Zn2+ and Cd2+ ions, respectively. The method enabled determination of low levels of Zn2+ and Cd2+ ions in urine, blood serum and water samples.

  14. Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

    2018-02-01

    A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

  15. Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

    Science.gov (United States)

    Goudarzi, Nasser

    2009-02-11

    A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples.

  16. [Determination of Al, Be, Cd, Co, Cr, Mn, Ni, Pb, Se and Tl in whole blood by atomic absorption spectrometry without preliminary sample digestion].

    Science.gov (United States)

    Ivanenko, N B; Ivanenko, A A; Solov'ev, N D; Navolotskiĭ, D V; Pavlova, O V; Ganeev, A A

    2014-01-01

    Methods of whole blood trace element determination by Graphite furnace atomic absorption spectrometry (in the variant of Zeeman's modulation polarization spectrometry) have been proposed. They do not require preliminary sample digestion. Furnace programs, modifiers and blood dilution factors were optimized. Seronorm™ human whole blood reference materials were used for validation. Dynamic ranges (for undiluted blood samples) were: Al 8 ¸ 210 мg/L; Be 0.3 ¸ 50 мg/L; Cd 0.2 ¸ 75 мg/L; Сo 5 ¸ 350 мg/L; Cr 10 ¸ 100 мg/L; Mn 6 ¸ 250 мg/L; Ni 10 ¸ 350 мg/L; Pb 3 ¸ 240 мg/L; Se 10 ¸ 500 мg/L; Tl 2 ¸ 600 мg/L. Precision (RSD) for the middle of dynamic range ranged from 5% for Mn to 11 for Se.

  17. A rapid method for determining tin and molybdenum in geological samples by flame atomic-absorption spectroscopy

    Science.gov (United States)

    Welsch, E.P.

    1985-01-01

    The proposed method uses a lithium metaborate fusion, dissolution of the fusion bead in 15% v v hydrochloric acid, extraction into a 4% solution of trioctylphosphine oxide in methyl isobutyl ketone, and aspiration into a nitrous oxide-acetylene flame. The limits of detection for tin and molybdenum are 1.0 and 0.5 ppm, respectively. Approximately 50 samples can be analysed per day. ?? 1985.

  18. Use of slurry sampling for the direct determination of zinc in yogurt by high resolution-continuum source flame atomic absorption spectrometry.

    Science.gov (United States)

    Brandao, Geovani C; de Jesus, Raildo M; da Silva, Erik G P; Ferreira, Sergio L C

    2010-06-15

    This paper presents an analytical procedure for the direct determination of zinc in yogurt employing sampling slurry and high resolution-continuum source flame atomic absorption spectrometry (HR-CS FAAS). The step optimization established the experimental conditions of: 2.0molL(-1) hydrochloric acid, a sonication time of 20min and a sample mass of 1.0g for a slurry volume of 25mL. This method allows the determination of zinc with a limit of quantification of 0.32microgg(-1). The precision expressed as relative standard deviation (RSD) were 0.82 and 2.08% for yogurt samples containing zinc concentrations of 4.85 and 2.49microgg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of non-fat milk powder furnished by the National Institute of Standard and Technology. The proposed method was applied for the determination of zinc in seven yogurt samples. The zinc content was varied from 2.19 to 4.85microgg(-1). These results agreed with those reported in the literature. The samples were also analyzed after acid digestion and zinc determination by FAAS. No statistical difference was observed between the results obtained by both of the procedures performed.

  19. Investigation of chemical modifiers for sulfur determination in diesel fuel samples by high-resolution continuum source graphite furnace molecular absorption spectrometry using direct analysis

    Energy Technology Data Exchange (ETDEWEB)

    Huber, Charles S. [Instituto Federal Sul-rio-grandense, Câmpus Pelotas, Pelotas, RS (Brazil); Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Universidade Federal de Santa Catarina, Departamento de Química, Florianópolis, SC (Brazil); Andrade, Jailson B. [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2015-06-01

    High-resolution continuum source graphite furnace molecular absorption spectrometry has been applied for sulfur determination in diesel fuel. The sharp rotational lines of the carbon monosulfide molecule (formed during the vaporization step) were used to measure the absorbance. The analytical line at 258.056 nm was monitored using the sum of three pixels. Different chemical modifiers were investigated and the mixture of palladium and magnesium was used as chemical modifier in combination with iridium as permanent modifier. L-Cysteine was chosen as sulfur standard and the calibration was done against aqueous standard solutions. The proposed method was applied for the analyses of four diesel samples: two S10 samples and two S500 samples. The trueness of the method was checked with a certified reference material (CRM) of sulfur in diesel fuel (NIST 2724b). Accurate results, for samples and CRM, were achieved after a dilution with propan-1-ol. The following figures of merit were obtained: characteristic mass of 17 ± 3 ng, limit of detection and limit of quantification of 1.4 mg kg{sup −1} and 4.7 mg kg{sup −1}, respectively. - Highlights: • Ir, Ru and Zr were investigated as permanent modifiers. • Ca, Mg, Pd and Pd/Mg were investigated as modifiers in solution. • Indirect determination of sulfur monitoring the molecular absorbance of the CS • Direct analysis of diesel samples using a dilution in propan-1-ol.

  20. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    International Nuclear Information System (INIS)

    Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

    2012-01-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 °C and 2400 °C, respectively. Slopes of calibration curves (50–750 pg Cr, R 2 > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3–17.7 μg g −1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g −1 Cr. The limit of detection was 3.3 ng g −1 Cr. - Highlights: ► Direct solid sampling is first time employed for Cr in plant materials. ► Calibration curves with liquids and solids are coincident. ► Microanalysis of plants for Cr is validated by reference materials. ► The proposed HR-CS GF AAS method is environmental friendly.

  1. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    Energy Technology Data Exchange (ETDEWEB)

    Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

  2. Automatic flow-batch system for cold vapor atomic absorption spectroscopy determination of mercury in honey from Argentina using online sample treatment.

    Science.gov (United States)

    Domínguez, Marina A; Grünhut, Marcos; Pistonesi, Marcelo F; Di Nezio, María S; Centurión, María E

    2012-05-16

    An automatic flow-batch system that includes two borosilicate glass chambers to perform sample digestion and cold vapor atomic absorption spectroscopy determination of mercury in honey samples was designed. The sample digestion was performed by using a low-cost halogen lamp to obtain the optimum temperature. Optimization of the digestion procedure was done using a Box-Behnken experimental design. A linear response was observed from 2.30 to 11.20 μg Hg L(-1). The relative standard deviation was 3.20% (n = 11, 6.81 μg Hg L(-1)), the sample throughput was 4 sample h(-1), and the detection limit was 0.68 μg Hg L(-1). The obtained results with the flow-batch method are in good agreement with those obtained with the reference method. The flow-batch system is simple, allows the use of both chambers simultaneously, is seen as a promising methodology for achieving green chemistry goals, and is a good proposal to improving the quality control of honey.

  3. Determination of mercury in airborne particulate matter collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling

    Energy Technology Data Exchange (ETDEWEB)

    Araujo, Rennan G.O., E-mail: rgoa01@terra.com.br [Laboratorio de Quimica Analitica Ambiental, Departamento de Quimica, Universidade Federal de Sergipe, Campus Sao Cristovao, 49.100-000, Sao Cristovao, SE (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Vignola, Fabiola; Castilho, Ivan N.B. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borges, Daniel L.G.; Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti R. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal do Rio Grande do Sul, 91501-970 Porto Alegre, RS (Brazil); Smichowski, Patricia [Comision Nacional de Energia Atomica (CNEA) and Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Buenos Aires (Argentina); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, 40170-290, Salvador, BA (Brazil); Becker-Ross, Helmut [Leibniz-Institut fuer Analytische Wissenschaften-ISAS-e.V., Department Berlin, 12489 Berlin (Germany)

    2011-05-15

    A study has been undertaken to assess the capability of high-resolution continuum source graphite furnace atomic absorption spectrometry for the determination of mercury in airborne particulate matter (APM) collected on glass fiber filters using direct solid sampling. The main Hg absorption line at 253.652 nm was used for all determinations. The certified reference material NIST SRM 1648 (Urban Particulate Matter) was used to check the accuracy of the method, and good agreement was obtained between published and determined values. The characteristic mass was 22 pg Hg. The limit of detection (3{sigma}), based on ten atomizations of an unexposed filter, was 40 ng g{sup -1}, corresponding to 0.12 ng m{sup -3} in the air for a typical air volume of 1440 m{sup 3} collected within 24 h. The limit of quantification was 150 ng g{sup -1}, equivalent to 0.41 ng m{sup -3} in the air. The repeatability of measurements was better than 17% RSD (n = 5). Mercury concentrations found in filter samples loaded with APM collected in Buenos Aires, Argentina, were between < 40 ng g{sup -1} and 381 {+-} 24 ng g{sup -1}. These values correspond to a mercury concentration in the air between < 0.12 ng m{sup -3} and 1.47 {+-} 0.09 ng m{sup -3}. The proposed procedure was found to be simple, fast and reliable, and suitable as a screening procedure for the determination of mercury in APM samples.

  4. Determination of lead and nickel in environmental samples by flame atomic absorption spectrometry after column solid-phase extraction on Ambersorb-572 with EDTA

    Energy Technology Data Exchange (ETDEWEB)

    Baytak, Sitki [Department of Chemistry, Faculty of Science and Arts, Harran University, 63100 Sanliurfa (Turkey); Tuerker, A. Rehber [Department of Chemistry, Faculty of Science and Arts, Gazi University, 06500 Ankara (Turkey)]. E-mail: aturker@gazi.edu.tr

    2006-02-28

    Lead and nickel were preconcentrated as their ethylenediaminetetraacedic acid (EDTA) complexes from aqueous sample solutions using a column containing Ambersorb-572 and determined by flame atomic absorption spectrometry (FAAS). pH values, amount of solid phase, elution solution and flow rate of sample solution have been optimized in order to obtain quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of Pb and Ni under the optimum conditions were 99 {+-} 2 and 97 {+-} 3%, respectively, at 95% confidence level. Seventy-five-fold (using 750 mL of sample solution and 10 mL of eluent) and 50-fold (using 500 mL of sample solution and 10 mL of eluent) preconcentration was obtained for Pb and Ni, respectively. Time of analysis is about 4.5 h (for obtaining enrichment factor of 75). By applying these enrichment factors, the analytical detection limits of Pb and Ni were found as 3.65 and 1.42 ng mL{sup -1}, respectively. The capacity of the sorbent was found as 0.17 and 0.21 mmol g{sup -1} for Pb and Ni, respectively. The interferences of some cations, such as Mn{sup 2+}, Co{sup 2+}, Fe{sup 3+}, Al{sup 3+}, Zn{sup 2+}, Cd{sup 2+}, Ca{sup 2+}, Mg{sup 2+}, K{sup +} and Na{sup +} usually present in water samples were also studied. This procedure was applied to the determination of lead and nickel in parsley, green onion, sea water and waste water samples. The accuracy of the procedure was checked by determining Pb and Ni in standard reference tea leaves sample (GBW-07605). The results demonstrated good agreement with the certified values.

  5. Determination of tellurium in coal samples by means of graphite furnace atomic absorption spectrometry after coprecipitation with iron(III) hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Oda, S.; Arikawa, Y. [Japan Womens University, Tokyo (Japan)

    2005-11-01

    A simple and accurate method for the determination of tellurium in coal samples was investigated by the combustion of samples under a high pressure of oxygen and coprecipitation with Fe(OH){sub 3}, followed by a measurement by graphite furnace atomic absorption spectrometry (GF-AAS). About 0.5 g of an accurately weighed ground coal sample and 0.5 g of starch were combusted in an oxygen combustion bomb filled with oxygen to 3 MPa and added with 3 ml of water as an absorbing solution. The formed tellurium trioxide TeOs dissolved in water as TeO{sub 4}{sup 2-}, which was in turn reduced to TeO{sub 3}{sup 2-} by heating. After diluting the above-mentioned solution up to about 50 ml with water, Fe(OH){sub 3} is formed upon adding Fe(NO{sub 3}){sub 3} and sodium hydroxide solutions at pH 8-9 and left standing overnight. After dissolving the precipitate by HCl, the solution was diluted to 10 ml with water and the concentration of tellurium was measured by GF-AAS at a wavelength of 214.3 nm. The standard addition method was employed for the determination of tellurium in real coal samples, because those processes for the formation of tellurium(VI) oxide and coprecipitation with Fe(OH)3 were interfered by matrices. For NIST SRM 1632c, the standard coal sample tellurium content of 0.057 {+-} 0.004 mg kg{sup -1} was in good agreement with the information value of 0.05 mg kg{sup -1} with 7% of RSD in five replicate analyses. The tellurium contents in 20 real coal samples given by Center for Coal Utilization, Japan were also determined. The tellurium contents in these samples were scattered over the narrow range between 0.032 and 0.100 mg kg{sup -1}.

  6. Determination of Cu, Cd, Pb and Cr in yogurt by slurry sampling electrothermal atomic absorption spectrometry: A case study for Brazilian yogurt.

    Science.gov (United States)

    de Andrade, Camila Kulek; de Brito, Patrícia Micaella Klack; Dos Anjos, Vanessa Egéa; Quináia, Sueli Pércio

    2018-02-01

    A slurry sampling electrothermal atomic absorption spectrometric method is proposed for the determination of trace elements such as Cu, Cr, Cd and Pb in yogurt. The main factors affecting the slurry preparation were optimized: nature and concentration of acid solution and sonication time. The analytical method was validated in-house by calibration, linearity, limits of detection and quantification, precision and accuracy test obtaining satisfactory results in all cases. The proposed method was applied for the determination of Cd, Cr, Cu and Pb in some Brazilian yogurt samples. For these samples, the concentrations ranged from 2.5±0.2 to 12.4±0.2ngg -1 ; 34±3 to 899±7ngg -1 ; <8.3 to 12±1ngg -1 ; and <35.4 to 210±16ngg -1 for Cd, Cu, Cr and Pb, respectively. The daily intake of Cd, Cu, Cr and Pb via consumption of these samples was estimated. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Separation and Enrichment of Gold in Water, Geological and Environmental Samples by Solid Phase Extraction on Multiwalled Carbon Nanotubes Prior to its Determination by Flame Atomic Absorption Spectrometry.

    Science.gov (United States)

    Duran, Ali; Tuzen, Mustafa; Soylak, Mustafa

    2015-01-01

    This study proposes the application of multi-walled carbon nanotubes as a solid sorbent for the preconcentration of gold prior to its flame atomic absorption spectrometry determination. Extraction was achieved by using a glass column (15.0 cm in length and 1.0 cm in diameter). Quantitative recoveries were obtained in the pH range of 2.5-4.0; the elution step was carried out with 5.0 ml of 1.0 mol/L HNO3 in acetone. In the ligand-free study, variables such as pH, eluent type, sample volume, flow rates, and matrix effect were examined for the optimum recovery of gold ions. The gold ions were able to be pre-concentrated by a factor of 150 and their LOD was determined to be 1.71 μg/L. In order to evaluate the accuracy of the developed method, addition-recovery tests were applied for the tap water, mineral water, and sea water samples. Gold recovery studies were implemented using a wet digestion technique for mine and soil samples taken from various media, and this method was also applied for anodic slime samples taken from the factories located in the Kayseri Industrial Zone of Turkey.

  8. A pre-concentration procedure using coprecipitation for determination of lead and iron in several samples using flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Saracoglu, S.; Soylak, M.; Peker, D.S. Kacar; Elci, L.; Santos, W.N.L. dos; Lemos, V.A.; Ferreira, S.L.C.

    2006-01-01

    The present paper proposes a pre-concentration procedure for determination of lead and iron in several samples by flame atomic absorption spectrometry. In it, lead(II) and iron(III) ions are coprecipitated using the violuric acid-copper(II) system as collector. Afterwards, the precipitate is dissolved with 1 M HNO 3 solution and the metal ions are determined. The optimization step was performed using factorial design involving the variables: pH, violuric acid mass (VA) and copper concentration (Cu). Using the optimized experimental conditions, the proposed procedure allows the determination these metals with detection limits of 0.18 μg L -1 for iron and 0.16 μg L -1 for lead. The effects of foreign ions on the pre-concentration procedure were also evaluated and the results demonstrated that this method could be applied for determination of iron and lead in several real samples. The proposed method was successfully applied to the analysis of seawater, urine, mineral water, soil and physiological solution samples. The concentrations of lead and iron achieved in these samples agree well with others data reported in the literature

  9. A Green Preconcentration Method for Determination of Cobalt and Lead in Fresh Surface and Waste Water Samples Prior to Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Naeemullah

    2012-01-01

    Full Text Available Cloud point extraction (CPE has been used for the preconcentration and simultaneous determination of cobalt (Co and lead (Pb in fresh and wastewater samples. The extraction of analytes from aqueous samples was performed in the presence of 8-hydroxyquinoline (oxine as a chelating agent and Triton X-114 as a nonionic surfactant. Experiments were conducted to assess the effect of different chemical variables such as pH, amounts of reagents (oxine and Triton X-114, temperature, incubation time, and sample volume. After phase separation, based on the cloud point, the surfactant-rich phase was diluted with acidic ethanol prior to its analysis by the flame atomic absorption spectrometry (FAAS. The enhancement factors 70 and 50 with detection limits of 0.26 μg L−1 and 0.44 μg L−1 were obtained for Co and Pb, respectively. In order to validate the developed method, a certified reference material (SRM 1643e was analyzed and the determined values obtained were in a good agreement with the certified values. The proposed method was applied successfully to the determination of Co and Pb in a fresh surface and waste water sample.

  10. Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

    2015-04-01

    A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be <5.0%. This method was successfully applied to real water and acid digested food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Feasibility of using in situ fusion for the determination of Co, Cr and Mn in Portland cement by direct solid sampling graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Intima, Danielle Polidorio; de Oliveira, Elisabeth; Oliveira, Pedro Vitoriano

    2009-01-01

    In situ fusion on the boat-type graphite platform has been used as a sample pretreatment for the direct determination of Co, Cr and Mn in Portland cement by solid sampling graphite furnace atomic absorption spectrometry (SS-GF AAS). The 3-field Zeeman technique was adopted for background correction to decrease the sensitivity during measurements. This strategy allowed working with up to 200 μg of sample. The in situ fusion was accomplished using 10 μL of a flux mixture 4.0% m/v Na 2 CO 3 + 4.0% m/v ZnO + 0.1% m/v Triton (registered) X-100 added over the cement sample and heated at 800 deg. C for 20 s. The resulting mould was completely dissolved with 10 μL of 0.1% m/v HNO 3 . Limits of detection were 0.11 μg g - 1 for Co, 1.1 μg g - 1 for Cr and 1.9 μg g - 1 for Mn. The accuracy of the proposed method has been evaluated by the analysis of certified reference materials. The values found presented no statistically significant differences compared to the certified values (Student's t-test, p < 0.05). In general, the relative standard deviation was lower than 12% (n = 5).

  12. Determination of fluorine in copper concentrate via high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis - Comparison of three target molecules.

    Science.gov (United States)

    Cadorim, Heloisa R; de Gois, Jefferson S; Borges, Aline R; Vale, Maria Goreti R; Welz, Bernhard; Gleisner, Heike; Ott, Christina

    2018-01-01

    The chemical composition of complex inorganic materials, such as copper concentrate, may influence the economics of their further processing because most smelters, and particularly the producers of high-purity electrolyte copper, have strict limitations for the permissible concentration of impurities. These components might be harmful to the quality of the products, impair the production process and be hazardous to the environment. The goal of the present work is the development of a method for the determination of fluorine in copper concentrate using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis. The molecular absorption of the diatomic molecule CaF was measured at 606.440nm. The molecule CaF was generated by the addition of 200µg Ca as the molecule-forming reagent; the optimized pyrolysis and vaporization temperatures were 900°C and 2400°C, respectively. The characteristic mass and limit of detection were 0.5ng and 3ng, respectively. Calibration curves were established using aqueous standard solutions containing the major components Cu, Fe, S and the minor component Ag in optimized concentrations. The accuracy of the method was verified using certified reference materials. Fourteen copper concentrate samples from Chile and Australia were analyzed to confirm the applicability of the method to real samples; the concentration of fluorine ranged from 34 to 5676mgkg -1 . The samples were also analyzed independently at Analytik Jena by different operators, using the same equipment, but different target molecules, InF and GaF, and different operating conditions; but with a few exceptions, the results agreed quite well. The results obtained at Analytik Jena using the GaF molecule and our results obtained with CaF, with one exception, were also in agreement with the values informed by the supplier of the samples, which were obtained using ion selective electrode potentiometry after alkaline fusion. A comparison will

  13. Parameters Influencing Sulfur Speciation in Environmental Samples Using Sulfur K-Edge X-Ray Absorption Near-Edge Structure

    Directory of Open Access Journals (Sweden)

    Siwatt Pongpiachan

    2012-01-01

    Full Text Available This paper aims to enhance the credibility of applying the sulfur K-edge XANES spectroscopy as an innovative “fingerprint” for characterizing environmental samples. The sensitivities of sulfur K-edge XANES spectra of ten sulfur compound standards detected by two different detectors, namely, Lytle detector (LyD and Germanium detector (GeD, were studied and compared. Further investigation on “self-absorption” effect revealed that the maximum sensitivities of sulfur K-edge XANES spectra were achieved when diluting sulfur compound standards with boron nitride (BN at the mixing ratio of 0.1%. The “particle-size” effect on sulfur K-edge XANES spectrum sensitivities was examined by comparing signal-to-noise ratios of total suspended particles (TSP and particulate matter of less than 10 millionths of a meter (PM10 collected at three major cities of Thailand. The analytical results have demonstrated that the signal-to-noise ratios of sulfur K-edge XANES spectra were positively correlated with sulfate content in aerosols and negatively connected with particle sizes. The combination of hierarchical cluster analysis (HCA and principal component analysis (PCA has proved that sulfur K-edge XANES spectrum can be used to characterize German terrestrial soils and Andaman coastal sediments. In addition, this study highlighted the capability of sulfur K-edge XANES spectra as an innovative “fingerprint” to distinguish tsunami backwash deposits (TBD from typical marine sediments (TMS.

  14. Separation/preconcentration of silver(I) and lead(II) in environmental samples on cellulose nitrate membrane filter prior to their flame atomic absorption spectrometric determinations

    International Nuclear Information System (INIS)

    Soylak, Mustafa; Cay, Rukiye Sungur

    2007-01-01

    An enrichment method for trace amounts of Ag(I) and Pb(II) has been established prior to their flame atomic absorption spectrometric determinations. The preconcentration/separation procedure is based on chelate formation of Ag(I) and Pb(II) with ammonium pyrrolidine dithiocarbamate (APDC) and on retention of the chelates on cellulose nitrate membrane filter. The influences of some analytical parameters including pH and amounts of reagent, etc. on the recoveries of analytes were investigated. The effects of interferic ions on the quantitative recoveries of analytes were also examined. The detection limits (k = 3, N = 11) were 4.6 μg L -1 for silver(I) and 15.3 μg L -1 for lead(II). The relative standard deviations (R.S.D.) of the determinations for analyte ions were below 3%. The method was applied to environmental samples for the determination of analyte ions with satisfactory results (recoveries >95%)

  15. Flame atomic absorption spectrometric determination of trace quantities of cadmium in water samples after cloud point extraction in Triton X-114 without added chelating agents

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Madrakian, Tayyebeh; Siampour, Hajar

    2006-01-01

    A new micell-mediated phase separation method for preconcentration of ultra-trace quantities of cadmium as a prior step to its determination by flame atomic absorption spectrometry has been developed. The method is based on the cloud point extraction (CPE) of cadmium in iodide media with Triton X-114 in the absence of any chelating agent. The optimal extraction and reaction conditions (e.g., acid concentration, iodide concentration, effect of time) were studied, and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and improvement factors) were obtained. Linearity was obeyed in the range of 3-300 ng mL -1 of cadmium. The detection limit of the method is 1.0 ng mL -1 of cadmium. The interference effect of some anions and cations was also tested. The method was applied to the determination of cadmium in tap water, waste water, and sea water samples

  16. Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres

    KAUST Repository

    Hoffman, A. S.; Debefve, L. M.; Bendjeriou-Sedjerari, Anissa; Ould-Chikh, Samy; Bare, Simon R.; Basset, Jean-Marie; Gates, B. C.

    2016-01-01

    X-ray absorption spectroscopy is an element-specific technique for probing the local atomic-scale environment around an absorber atom. It is widely used to investigate the structures of liquids and solids, being especially valuable for characterization of solid-supported catalysts. Reported cell designs are limited in capabilities—to fluorescence or transmission and to static or flowing atmospheres, or to vacuum. Our goal was to design a robust and widely applicable cell for catalyst characterizations under all these conditions—to allow tracking of changes during genesis and during operation, both under vacuum and in reactive atmospheres. Herein, we report the design of such a cell and a demonstration of its operation both with a sample under dynamic vacuum and in the presence of gases flowing at temperatures up to 300 °C, showing data obtained with both fluorescence and transmission detection. The cell allows more flexibility in catalyst characterization than any reported.

  17. Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres

    KAUST Repository

    Hoffman, A. S.

    2016-07-26

    X-ray absorption spectroscopy is an element-specific technique for probing the local atomic-scale environment around an absorber atom. It is widely used to investigate the structures of liquids and solids, being especially valuable for characterization of solid-supported catalysts. Reported cell designs are limited in capabilities—to fluorescence or transmission and to static or flowing atmospheres, or to vacuum. Our goal was to design a robust and widely applicable cell for catalyst characterizations under all these conditions—to allow tracking of changes during genesis and during operation, both under vacuum and in reactive atmospheres. Herein, we report the design of such a cell and a demonstration of its operation both with a sample under dynamic vacuum and in the presence of gases flowing at temperatures up to 300 °C, showing data obtained with both fluorescence and transmission detection. The cell allows more flexibility in catalyst characterization than any reported.

  18. Method Performance of Total Mercury (Hg) Testing in the Biological Samples by Using Cold Vapour Atomic Absorption Spectrophotometer (CV-AAS)

    International Nuclear Information System (INIS)

    Susanna TS; Samin

    2007-01-01

    Method performance (validation) of total mercury (Hg) testing in the biological samples by using cold vapour atomic absorption spectrophotometer (CV-AAS) has been done. The objective of this research is to know the method performance of CV-AAS as one of points for the accreditation testing of laboratory according IS0/IEC 17025-2005. The method performance covering limit of detection (LOD), accuracy, precision and bias. As a standard material used SRM Oyster Tissue 15660 from Winopal Forshung Germany, whereas the biological samples were human hair. In principle of mercury testing for solid samples using CV-AAS is dissolving this sample and standard with 10 mL HNO 3 supra pure into a closed quartz tube and heating at 150 °C for 4 hours. The concentration of mercury in each samples was determined at the condition of operation were stirring time (T 1 ) 70 seconds, delay time (T 2 ) 15 seconds, heating time (T 3 ) 13 seconds and cooling time (T 4 ) of 25 seconds. Mercury ion in samples are reduced with SnCl 2 10 % in H 2 SO 4 20 %, and then the vapour of mercury from reduction is passed in NaOH 20 % solution and aquatridest. The result of method performance were: limit of detection (LOD) = 0.085 ng, accuracy 99.70 %, precision (RSD) = 1.64 % and bias = 0.30 %. From the validation result showed that the content of mercury total was in the range of certified values. The total mercury content (Hg) in human hair were varied from 406.93 - 699.07 ppb. (author)

  19. Monitoring and Method development of Hg in Istanbul Airborne Particulates by Solid Sampling Continuum Source-High Resolution Electrothermal Atomic Absorption Spectromerty

    Directory of Open Access Journals (Sweden)

    Soydemir E.

    2014-07-01

    Full Text Available In this work, a method has been developed and monitoring for the determination of mercury in PM2.5 airborne particulates by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. The PM2.5 airborne particulates were collected on quartz filters using high volume samplers (500 L/min in Istanbul (Turkey for 96 hours every month in one year. At first, experimental conditions as well as the validation tests were optimized using collected filter. For this purpose, the effects of atomization temperature, amount of sample intoduced in to the furnace, addition of acids and/or KMnO4 on the sample, covering of graphite tube and platform or using of Ag nanoparticulates, Au nanoparticulates, and Pd solutions on the accuracy and precision were investigated. After optimization of the experimental conditions, the mercury concentrations were determined in the collected filter. The filters with PM2.5 airborne particulates were dried, divided into small fine particles and then Hg concentrations were determined directly. In order to eliminate any error due to the sensitivity difference between aqueous standards and solid samples, the quantification was performed using solid calibrants. The limit of detection, based on three times the standard deviations for ten atomizations of an unused filter, was 30 ng/g. The Hg content was dependent on the sampling site, season etc, ranging from samples, addition of AuNPs, AgNPs and Pd solution for amalgamation effects on the recoveries were investigated. The results were compared using statistical tests.

  20. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

  1. In situ emulsification microextraction using a dicationic ionic liquid followed by magnetic assisted physisorption for determination of lead prior to micro-sampling flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Shokri, Masood; Beiraghi, Asadollah; Seidi, Shahram

    2015-01-01

    For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L −1 lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf 2 ], was added into the sample solution containing 100 μL of 1.0 mol L −1 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl 2 , to form a water immiscible ionic liquid, [pbmim][NTf 2 ] 2 . This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe 3 O 4 magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf 2 ] 2 , physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L −1 . Good linearity was obtained in the range of 2.5–150 μg L −1 with determination coefficient (r 2 ) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L −1 was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples. - Highlights: • A dicationic ionic liquid was used as the extraction solvent, for the first time. • A simple and efficient in situ emulsification microextraction

  2. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    Martinis, Estefanía M; Bertón, Paula; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

    2009-08-15

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 microl of 9.0 mol L(-1) hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3ngL(-1) and the relative standard deviation (RSD) for 10 replicates at 1 microg L(-1) Hg(2+) was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  3. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Martinis, Estefania M.; Berton, Paula; Olsina, Roberto A.; Altamirano, Jorgelina C.; Wuilloud, Rodolfo G.

    2009-01-01

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 mim][PF 6 ]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 μl of 9.0 mol L -1 hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3 ng L -1 and the relative standard deviation (RSD) for 10 replicates at 1 μg L -1 Hg 2+ was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  4. Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

    Science.gov (United States)

    de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

    2017-08-15

    Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl -1 , respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction followed by atomic absorption spectrometry for trace determination of zinc in water and food samples

    International Nuclear Information System (INIS)

    Zeeb, M.; Sadeghi, M.

    2011-01-01

    We report on a new method for the microextraction and determination of zinc (II). The ion is accumulated via ionic-liquid cold-induced aggregation dispersive liquid-liquid microextraction (IL-CIA-DLLME) followed by flame atomic absorption spectrometry (FAAS). The ionic liquid (IL) 1-hexyl-3-methylimidazolium hexafluorophosphate is dispersed into a heated sample solution containing sodium hexafluorophosphate as a common ion source. The solution is then placed in an ice-water bath upon which a cloudy solution forms due to the decrease of the solubility of the IL. Zinc is complexed with 8-hydroxyquinoline and extracted into the IL. The enriched phase is dissolved in a diluting agent and introduced to the FAAS. The method is not influenced by variations in the ionic strength of the sample solution. Factors affecting the performance were evaluated and optimized. At optimum conditions, the limit of detection is 0.18 μg L -1 , and the relative standard deviation is 3.0% (at n=5). The method was validated by recovery experiments and by analyzing a certified reference material and successfully applied to the determination of Zn (II) in water and food samples. (author)

  6. Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L.; Gil, F.

    2010-01-01

    For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

  7. Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L. [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain); Gil, F., E-mail: fgil@ugr.es [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain)

    2010-02-05

    For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

  8. Cloud point extraction of palladium in water samples and alloy mixtures using new synthesized reagent with flame atomic absorption spectrometry (FAAS)

    International Nuclear Information System (INIS)

    Priya, B. Krishna; Subrahmanayam, P.; Suvardhan, K.; Kumar, K. Suresh; Rekha, D.; Rao, A. Venkata; Rao, G.C.; Chiranjeevi, P.

    2007-01-01

    The present paper outlines novel, simple and sensitive method for the determination of palladium by flame atomic absorption spectrometry (FAAS) after separation and preconcentration by cloud point extraction (CPE). The cloud point methodology was successfully applied for palladium determination by using new reagent 4-(2-naphthalenyl)thiozol-2yl azo chromotropic acid (NTACA) and hydrophobic ligand Triton X-114 as chelating agent and nonionic surfactant respectively in the water samples and alloys. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. The preconcentration factor was found to be (50-fold) for 250 ml of water sample. Under optimum condition the detection limit was found as 0.067 ng ml -1 for palladium in various environmental matrices. The present method was applied for the determination of palladium in various water samples, alloys and the result shows good agreement with reported method and the recoveries are in the range of 96.7-99.4%

  9. One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Mo, Yajun

    2016-01-01

    A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Cloud point extraction for determination of lead in blood samples of children, using different ligands prior to analysis by flame atomic absorption spectrometry: A multivariate study

    Energy Technology Data Exchange (ETDEWEB)

    Shah, Faheem, E-mail: shah_ceac@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Kazi, Tasneem Gul, E-mail: tgkazi@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Afridi, Hassan Imran, E-mail: hassanimranafridi@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Naeemullah, E-mail: khannaeemullah@ymail.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Arain, Muhammad Balal, E-mail: bilal_ku2004@yahoo.com [Department of Chemistry, University of Science and Technology, Bannu, KPK (Pakistan); Baig, Jameel Ahmed, E-mail: jab_mughal@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)

    2011-09-15

    Highlights: {yields} Trace levels of lead in blood samples of healthy children and with different kidney disorders {yields} Pre-concentration of Pb{sup +2} in acid digested blood samples after chelating with two complexing reagents. {yields} Multivariate technique was used for screening of significant factors that influence the CPE of Pb{sup +2} {yields} The level of Pb{sup +2} in diseased children was significantly higher than referents of same age group. - Abstract: The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of lead (Pb{sup 2+}) from digested blood samples after simultaneous complexation with ammonium pyrrolidinedithiocarbamate (APDC) and diethyldithiocarbamate (DDTC) separately. The complexed analyte was quantitatively extracted with octylphenoxypolyethoxyethanol (Triton X-114). The multivariate strategy was applied to estimate the optimum values of experimental factors. Acidic ethanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometer (FAAS). The detection limit value of Pb{sup 2+} for the preconcentration of 10 mL of acid digested blood sample was 1.14 {mu}g L{sup -1}. The accuracy of the proposed methods was assessed by analyzing certified reference material (whole blood). Under the optimized conditions of both CPE methods, 10 mL of Pb{sup 2+} standards (10 {mu}g L{sup -1}) complexed with APDC and DDTC, permitted the enhancement factors of 56 and 42, respectively. The proposed method was used for determination of Pb{sup 2+} in blood samples of children with kidney disorders and healthy controls.

  11. Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

    2015-12-01

    The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

  12. Determination of cadmium in whole blood and scalp hair samples of Pakistani male lung cancer patients by electrothermal atomic absorption spectrometer

    International Nuclear Information System (INIS)

    Kazi, T.G.; Memon, A.R.; Afridi, H.I.; Jamali, M.K.; Arain, M.B.; Jalbani, N.; Sarfraz, R.A.

    2008-01-01

    A large number of epidemiologic studies have been undertaken to identify potential risk factors for cancer, amongst which the association with cadmium has received considerable attention. There is compelling evidence in support of positive associations between cadmium and risk of lung cancer. In present study we measured the concentration of Cd in whole blood and scalp hair samples of 120 male lung cancer patients (smokers) and 150 controls or referents (smokers and nonsmokers) from different cities of Pakistan. Both referents and patients were of same age group (ranged 40-70 years), socio-economic status, localities and dietary habits. The scalp hair and whole blood samples were oxidized by 65% nitric acid: 30% hydrogen peroxide (2:1) ratio in microwave oven. To check the validity of the proposed method, a conventional wet acid digestion method was used to obtain total Cd concentration in certified samples of human hair BCR 397 and Clincheck control-lyophilized human whole blood. All digests were analyzed for Cd concentration by electrothermal atomic absorption spectrometer (ETAAS). The results of this study showed that the average Cd concentration was higher in the blood and scalp hair of lung cancer patients at different stages as compared to controls (p < 001). The smoker referents have high level of Cd in both biological samples as compared to nonsmoker subjects. These results illustrate that the patients who continued smoking after confirmed diagnosis of lung cancer have 34.2-67.26 and 22.4-57.3% more Cd in blood samples and scalp hair than lung cancer patients who cease smoking. This study is compelling evidence in support of positive associations between cadmium, cigarette smoking and lung cancer risk

  13. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  14. Determination of chlorine in food samples via the AlCl molecule using high-resolution continuum source molecular absorption spectrometry in a graphite furnace

    Energy Technology Data Exchange (ETDEWEB)

    Fechetia, Miriam; Tognon, Andre Luiz; Veiga, Marcia A.M.S. da, E-mail: mamsveiga@ffclrp.usp.br

    2012-05-15

    Determination of chlorine using the molecular absorption of aluminum mono-chloride (AlCl) at the 261.418 nm wavelength was accomplished by high-resolution continuum source molecular absorption spectrometry using a transversely heated graphite tube furnace with an integrated platform. For the analysis, 10 {mu}L of the sample followed by 10 {mu}L of a solution containing Al-Ag-Sr modifier, (1 g L{sup -1} each), were directly injected onto the platform. A spectral interference due to the use of Al-Ag-Sr as mixed modifier was easily corrected by the least-squares algorithm present in the spectrometer software. The pyrolysis and vaporization temperatures were 500 Degree-Sign C and 2200 Degree-Sign C, respectively. To evaluate the feasibility of a simple procedure for the determination of chlorine in food samples present in our daily lives, two different digestion methods were applied, namely (A) an acid digestion method using HNO{sub 3} only at room temperature, and (B) a digestion method with Ag, HNO{sub 3} and H{sub 2}O{sub 2}, where chlorine is precipitated as a low-solubility salt (AgCl), which is then dissolved with ammonia solution. The experimental results obtained with method B were in good agreement with the certified values and demonstrated that the proposed method is more accurate than method A. This is because the formation of silver chloride prevented analyte losses by volatilization. The limit of detection (LOD, 3{sigma}/s) for Cl in methods A and B was 18 {mu}g g{sup -1} and 9 {mu}g g{sup -1}, respectively, 1.7 and 3.3 times lower compared to published work using inductively coupled plasma optical emission spectrometry, and absolute LODs were 2.4 and 1.2 ng, respectively. - Highlights: Black-Right-Pointing-Pointer HR-CS MAS as technique for Cl determination via AlCl molecule Black-Right-Pointing-Pointer Spectral interference was corrected by the least-squares algorithm. Black-Right-Pointing-Pointer Chorine precipitation as AgCl prevents Cl losses during

  15. Method development for the determination of fluorine in water samples via the molecular absorption of strontium monofluoride formed in an electrothermal atomizer

    Energy Technology Data Exchange (ETDEWEB)

    Ozbek, Nil, E-mail: nil.ozbek@itu.edu.tr; Akman, Suleyman, E-mail: akmans@itu.edu.tr

    2012-03-15

    The presence of fluorine (F) was detected via the rotational molecular absorption line of diatomic strontium-monofluoride (SrF) generated in the gas phase at 651.187 nm using high-resolution continuum source electrothermal atomic absorption spectrometry. Upon the addition of excess strontium (Sr) as the nitrate, the fluorine in the sample was converted to SrF in the gas phase of a graphite furnace. The effects on the accuracy, precision and sensitivity of variables such as the SrF wavelength, graphite furnace program, amount of Sr, coating of the graphite tube and platform with Zr and Ir and the use of a modifier were investigated and optimized. It was determined that there was no need to use a modifier or to cover the platform/tubes with Zr or Ir. Fluorine concentrations in various water samples (certified waste water, tap water, drinking water and mineral water) were determined using 20 {mu}g of Sr as the molecule-forming reagent and applying a maximum pyrolysis temperature of 800 Degree-Sign C and a molecule-forming temperature of 2200 Degree-Sign C with a heating rate of 2000 Degree-Sign C s{sup -1}. Good linearity was maintained up to 0.1 {mu}g of F. The accuracy and precision of the method were tested by analyzing certified reference wastewater. The results were in good agreement with certified values, and the precision was satisfactory (RSD < 10%). The limit of detection and the characteristic mass for the method were 0.36 ng and 0.55 ng, respectively. Finally, the fluorine concentrations in several drinking water and mineral water samples taken from the market were determined. The results were in good agreement with the values supplied by the producers. No significant differences were found between the results from the linear calibration and standard addition techniques. The method was determined to be simple, fast, accurate and sensitive. - Highlights: Black-Right-Pointing-Pointer F is determined via MAS of SrF at 651.187 nm using HR-CS-ET AAS. Black

  16. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    International Nuclear Information System (INIS)

    Brum, Daniel M.; Lima, Claudio F.; Robaina, Nicolle F.; Fonseca, Teresa Cristina O.; Cassella, Ricardo J.

    2011-01-01

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO 3 , the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO 3 medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  17. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    Energy Technology Data Exchange (ETDEWEB)

    Brum, Daniel M.; Lima, Claudio F. [Departamento de Quimica, Universidade Federal de Vicosa, A. Peter Henry Rolfs s/n, Vicosa/MG, 36570-000 (Brazil); Robaina, Nicolle F. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil); Fonseca, Teresa Cristina O. [Petrobras, Cenpes/PDEDS/QM, Av. Horacio Macedo 950, Ilha do Fundao, Rio de Janeiro/RJ, 21941-915 (Brazil); Cassella, Ricardo J., E-mail: cassella@vm.uff.br [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de S.J. Batista s/n, Centro, Niteroi/RJ, 24020-141 (Brazil)

    2011-05-15

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO{sub 3}, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO{sub 3} medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  18. Graphene-based solid-phase extraction combined with flame atomic absorption spectrometry for a sensitive determination of trace amounts of lead in environmental water and vegetable samples

    International Nuclear Information System (INIS)

    Wang Yukun; Gao Shutao; Zang Xiaohuan; Li Jingci; Ma Jingjun

    2012-01-01

    Highlights: ► Graphene as a novel sorbent material in a column for solid-phase extraction (SPE). ► SPE for the determination of lead (Pb) in environment water samples and vegetable samples. ► The system can be reused for many times. ► The adsorption capacity of graphene over many other adsorbents. ► Graphene has great potentials as an excellent sorbent material. - Abstract: Graphene, a novel class of carbon nanostructures, has great promise for use as sorbent materials because of its ultrahigh specific surface area. A new method using a column packed with graphene as sorbent was developed for the preconcentration of trace amounts of lead (Pb) using dithizone as chelating reagent prior to its determination by flame atomic absorption spectrometry. Some effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 10.0–600.0 μg L −1 with a detection limit of 0.61 μg L −1 . The relative standard deviation for ten replicate measurements of 20.0 and 400.0 μg L −1 of Pb were 3.56 and 3.25%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Pb. The proposed method was successfully applied in the analysis of environmental water and vegetable samples. Good spiked recoveries over the range of 95.3–100.4% were obtained. This work not only proposes a useful method for sample preconcentration, but also reveals the great potential of graphene as an excellent sorbent material in analytical processes.

  19. Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples

    International Nuclear Information System (INIS)

    Li Shengqing; Cai Shun; Hu Wei; Chen Hao; Liu Hanlan

    2009-01-01

    A new method was developed for the determination of cadmium in water samples using ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-based USA-DLLME) followed by electrothermal atomic absorption spectrometry (ETAAS). The IL-based USA-DLLME procedure is free of volatile organic solvents, and there is no need for a dispersive solvent, in contrast to conventional DLLME. The ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF 6 ), was quickly disrupted by an ultrasonic probe for 1 min and dispersed in water samples like a cloud. At this stage, a hydrophobic cadmium-DDTC complex was formed and extracted into the fine droplets of HMIMPF 6 . After centrifugation, the concentration of the enriched cadmium in the sedimented phase was determined by ETAAS. Some effective parameters of the complex formation and microextraction, such as the concentration of the chelating agent, the pH, the volume of the extraction solvent, the extraction time, and the salt effect, have been optimized. Under optimal conditions, a high extraction efficiency and selectivity were reached for the extraction of 1.0 ng of cadmium in 10.0 mL of water solution employing 73 μL of HMIMPF 6 as the extraction solvent. The enrichment factor of the method is 67. The detection limit was 7.4 ng L - 1 , and the characteristic mass (m 0 , 0.0044 absorbance) of the proposed method was 0.02 pg for cadmium (Cd). The relative standard deviation (RSD) for 11 replicates of 50 ng L - 1 Cd was 3.3%. The method was applied to the analysis of tap, well, river, and lake water samples and the Environmental Water Reference Material GSBZ 50009-88 (200921). The recoveries of spiked samples were in the range of 87.2-106%.

  20. Combination of flame atomic absorption spectrometry with ligandless-dispersive liquid- liquid microextraction for preconcentration and determination of trace amount of lead in water samples

    Directory of Open Access Journals (Sweden)

    Y.M. Baghelani

    2013-05-01

    Full Text Available A new ligandless-dispersive liquid–liquid microextraction method has been developed for the separation and flame atomic absorption spectrometry determination of trace amount of lead(II ion. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents. Factors influencing the extraction efficiency of lead, including the extraction and dispersive solvent type and volume, pH of sample solution, concentration of chloride and extraction time were studied. Under the optimal conditions, the calibration curve was linear in the range of 7.0–6000 ng mL−1 of lead with R2 = 0.9992 (n = 10 and detection limit based on three times the standard deviation of the blank (3Sb was 0.5 ng mL−1 in original solution. The relative standard deviation for eight replicate determinations of 1.0 mg mL-1 lead was ±1.6%. The high efficiency of dispersive liquid-liquid microextraction to carry out the determination of trace amounts of lead in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in water samples and satisfactory results were obtained. The accuracy was checked by analyzing a certified reference material from the National Institute of Standard and Technology, Trace elements in water (NIST CRM 1643e.

  1. Separation and Preconcentration of Ag(1) in Aqueous Samples by Flotation as an Ion-Associate Using Iodide and Ferroin Followed the Determination by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Hosseini, M.S.; Kardan-Moghaddam, G.; Hashemi-Moghaddam, M.

    2007-01-01

    A simple method for separation/preconcentration and determination of Ag (1) in aqueous samples is described. The method is based on formation of an ion-associate between Ag (1)-iodide complex and ferroin, which can be floated at the interface of the aqueous/n-heptane phases. The flotation process was carried out using 500-ml aliquot of the aqueous solution and the floated layer was dissolved in 5 ml of 1 M HNO 3 containing methanol (50% v/v) as the solvent. The Ag (1) content was then determined by flame atomic absorption spectrometry (FAAS). The method so could be considered as an enrichment process, was achieved to a quantitative feature, when the pH of the solution was adjusted to 4 and the concentrations of iodide and ferroin were about 3.2x10 -4 M and 6.25x10 -5 M, respectively. The LOD and RSD (n=7) were obtained 1.0x10 -8 M and 2.4%, respectively. It was found that a large number of cations and anions even at high considerably foreign ion/Ag(1) ratios were not interfered. The method was applied satisfactorily to recovery of Ag(I) from different aqueous samples

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

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, Mehrorang, E-mail: m_ghaedi@mail.yu.ac.ir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Shokrollahi, Ardeshir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Niknam, Khodabakhsh [Chemistry Department, Persian Gulf University, Bushehr (Iran, Islamic Republic of); Niknam, Ebrahim; Najibi, Asma [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2009-09-15

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  4. On-line preconcentration of ultra-trace thallium(I in water samples with titanium dioxide nanoparticles and determination by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Saeid Asadpour

    2016-11-01

    Full Text Available A new method has been developed for the determination of Tl(I based on simultaneous sorption and preconcentration with a microcolumn packed with TiO2 nanoparticle with a high specific surface area prepared by Sonochemical synthesis prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS. The optimum experimental parameters for preconcentration of thallium, such as elution condition, pH, and sample volume and flow rate have been investigated. Tl(I can be quantitatively retained by TiO2 nanoparticles at pH 9.0, then eluted completely with 1.0 mol L−1 HCl. The adsorption capacity of TiO2 nanoparticles for Tl(I was found to be 25 mg g−1. Also detection limit, precision (RSD, n = 8 and enrichment factor for Tl(I were 87 ng L−1, 6.4% and 100, respectively. The method has been applied for the determination of trace amounts of Tl(I in some environmental water samples with satisfactory results.

  5. A new cloud point extraction procedure for determination of inorganic antimony species in beverages and biological samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan

    2015-05-15

    A new cloud-point extraction (CPE) for the determination of antimony species in biological and beverages samples has been established with flame atomic absorption spectrometry (FAAS). The method is based on the fact that formation of the competitive ion-pairing complex of Sb(III) and Sb(V) with Victoria Pure Blue BO (VPB(+)) at pH 10. The antimony species were individually detected by FAAS. Under the optimized conditions, the calibration range for Sb(V) is 1-250 μg L(-1) with a detection limit of 0.25 μg L(-1) and sensitive enhancement factor of 76.3 while the calibration range for Sb(III) is 10-400 μg L(-1) with a detection limit of 5.15 μg L(-1) and sensitive enhancement factor of 48.3. The precision as a relative standard deviation is in range of 0.24-2.35%. The method was successfully applied to the speciative determination of antimony species in the samples. The validation was verified by analysis of certified reference materials (CRMs). Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

    2013-01-01

    A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

  7. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry in water samples

    Directory of Open Access Journals (Sweden)

    Arpa Şahin Ç.

    2013-04-01

    Full Text Available A simple, rapid and inexpensive solidified floating organic drop microextraction (SFODME and flow injection flame atomic absorption spectrometric determination (FI-FAAS method for copper was developed. 3-amino-7-dimethylamino-2-methylphenazine (Neutral red, NR was used as the complexing agent. Several factors affecting the microextraction efficiency, such as, pH, NR and sodium dodecylbenzenesulfonate (SDBS concentration, extraction time, stirring rate, and temperature were investigated and optimized. Under optimized experimental conditions an enrichment factor of 541 was obtained for 100 mL of sample solution. The calibration graph was linear in the range of 0.5 – 20.0 ng mL–1 and the limit of detection (3s was 0.18 ng mL–1, the limit of quantification (10s was 0.58 ng mL–1. The relative standard deviation (RSD for 10 replicate measurements of 10 ng mL–1 copper was 2.7%. The developed method was successfully applied to the extraction and determination of copper in different certified reference materials (Estuarine water, Slew 3 and fortified water, TM 23.2 and real water samples and satisfactory results were obtained.

  8. Validation of methods of atomic absorption with flame for the analysis of potasium, zinc and manganese, and a spectrophotometer for the analysis of phosphorus in samples of fertilizers

    International Nuclear Information System (INIS)

    Pineda Castro, L. E.

    1998-01-01

    This study validated the spectrophotometric method by atomic absorption for the analysis of potassium, manganese and zinc in samples of fertilizers. Likewise, it validated the spectrophotometric method for the analysis of phosphorus by generation of the fosfomolibdovanadate. species The limits of detection and quantification obtained to a level of confidence of the 95% were: 0,6 ppm and 1,1 ppm for the potassium, 1,1 ppm, and 2,2 ppm for the phosphorus, 0,3 ppm and 0,5 ppm for the zinc and 0,6 ppm and 1,1 ppm for the manganese respectively. It established the repetibility and reproducible of the method to a level of the 95% of confidence and it determined that the fertilizers tolerance norm is complied with adequately for the potassium and the manganese. On the other hand, for the concentrations of phosphorus higher than 20%, it presented smaller reproducibility. For the zinc, it presented problems of precision of the method, in the two samples analyzed. The accuracy of the methodologies were the adequate. In the case of the phosphorus, it recommended the employment of a composed digestive mixture of nitric and perchloric acid when be a matter of materials that possess organic matter. (S. Grainger) [es

  9. Speciation of Mn(II), Mn(VII) and total manganese in water and food samples by coprecipitation-atomic absorption spectrometry combination

    International Nuclear Information System (INIS)

    Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

    2010-01-01

    A speciation procedure based on the coprecipitation of manganese(II) with zirconium(IV) hydroxide has been developed for the investigation of levels of manganese species. The determination of manganese levels was performed by flame atomic absorption spectrometry (FAAS). Total manganese was determined after the reduction of Mn(VII) to Mn(II) by ascorbic acid. The analytical parameters including pH, amount of zirconium(IV), sample volume, etc., were investigated for the quantitative recoveries of manganese(II). The effects of matrix ions were also examined. The recoveries for manganese(II) were in the range of 95-98%. Preconcentration factor was calculated as 50. The detection limit for the analyte ions based on 3 sigma (n = 21) was 0.75 μg L -1 for Mn(II). The relative standard deviation was found to be lower than 7%. The validation of the presented procedure was performed by analysis of certified reference material having different matrices, NIST SRM 1515 (Apple Leaves) and NIST SRM 1568a (Rice Flour). The procedure was successfully applied to natural waters and food samples.

  10. Consistency of genetic inheritance mode and heritability patterns of triglyceride vs. high density lipoprotein cholesterol ratio in two Taiwanese family samples

    Directory of Open Access Journals (Sweden)

    Yang Chi-Yu

    2003-04-01

    Full Text Available Abstract Background Triglyceride/HDL cholesterol ratio (TG/HDL-C is considered as a risk factor for cardiovascular events. Genetic components were important in controlling the variation in western countries. But the mode of inheritance and family aggregation patterns were still unknown among Asian-Pacific countries. This study, based on families recruited from community and hospital, is aimed to investigate the mode of inheritance, heritability and shared environmental factors in controlling TG/HDL-C. Results Two populations, one from community-based families (n = 988, 894 parent-offspring and 453 sibling pairs and the other from hospital-based families (n = 1313, 76 parent-offspring and 52 sibling pairs were sampled. The population in hospital-based families had higher mean age values than community-based families (54.7 vs. 34.0. Logarithmic transformed TG/ HDL-C values, after adjusted by age, gender and body mass index, were for genetic analyses. Significant parent-offspring and sibling correlations were also found in both samples. The parent-offspring correlation coefficient was higher in the hospital-based families than in the community-based families. Genetic heritability was higher in community-based families (0.338 ± 0.114, p = 0.002, but the common shared environmental factor was higher in hospital-based families (0.203 ± 0.042, p Conclusion Variations of TG/HDL-C in the normal ranges were likely to be influenced by multiple factors, including environmental and genetic components. Higher genetic factors were proved in younger community-based families than in older hospital-based families.

  11. Investigation of chemical modifiers for the determination of lead in fertilizers and limestone using graphite furnace atomic absorption spectrometry with Zeeman-effect background correction and slurry sampling

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; Dessuy, Morgana B. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil)

    2014-02-01

    In this work, chemical modifiers in solution (Pd/Mg, NH{sub 4}H{sub 2}PO{sub 4} and NH{sub 4}NO{sub 3}/Pd) were compared with permanent modifiers (Ir and Ru) for the determination of lead in fertilizer and limestone samples using slurry sampling and graphite furnace atomic absorption spectrometry with Zeeman-effect background correction. The analytical line at 283.3 nm was used due to some spectral interference observed at 217.0 nm. The NH{sub 4}H{sub 2}PO{sub 4} was abandoned due to severe spectral interference even at the 283.3-nm line. For Pd/Mg and NH{sub 4}NO{sub 3}/Pd the optimum pyrolysis and atomization temperatures were 900 °C and 1900 °C, respectively. For Ru and Ir, the integrated absorbance signal was stable up to pyrolysis temperatures of 700 °C and 900 °C, respectively, and up to atomization temperature of 1700 °C. The limit of detection (LOD) was 17 ng g{sup −1} using Pd/Mg and 29 ng g{sup −1} using NH{sub 4}NO{sub 3}/Pd. Among the permanent modifiers investigated, the LOD was 22 ng g{sup −1} Pb for Ir and 10 ng g{sup −1} Pb for Ru. The accuracy of the method was evaluated using the certified reference material NIST SRM 695. Although Ru provided lower LOD, which can be attributed to a lower blank signal, only the modifiers in solution showed concordant values of Pb concentration for the NIST SRM 695 and the most of analyzed samples. Moreover, the Pd/Mg modifier provided the highest sensitivity and for this reason it is more suitable for the determination of Pb in fertilizers samples in slurry; besides this it presented a better signal-to-noise ratio than NH{sub 4}NO{sub 3}/Pd. - Highlights: • Lead has been determined in fertilizers using slurry sampling GF AAS. • The mixture of palladium and magnesium nitrates was found to be the ideal chemical modifier. • Calibration could be carried out against aqueous standard solutions. • The proposed method is much faster than the EPA method, which includes sample digestion.

  12. Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

    Science.gov (United States)

    Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

    2013-11-15

    A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Visualization and quantification of heterogeneous diffusion rates in granodiorite samples by X-ray absorption imaging. Diffusion within gouge materials, altered rim and intact rock matrix

    International Nuclear Information System (INIS)

    Altman, S.J.; Tidwell, V.C.; Uchida, M.

    2001-01-01

    Matrix diffusion is one of the most important contaminant migration retardation processes in crystalline rocks. Performance assessment calculations in various countries assume that only the area of the fracture surface where advection is active provides access to the rock matrix. However, accessibility to the matrix could be significantly enhanced with diffusion into stagnant zones, fracture fillings, and through an alteration rim in the matrix. Laboratory visualization experiments were conducted on granodiorite samples to investigate and quantify diffusion rates within different zones of a Cretaceous granodiorite. Samples were collected from the Kamaishi experimental site in the northern part of the main island of Japan. Diffusion of iodine out of the sample is visualized and rates are measured using x-ray absorption imaging. X-ray images allow for measurements of relative iodine concentration and relative iodine mass as a function of time and two-dimensional space at a sub-millimeter spatial resolution. In addition, two-dimensional heterogeneous porosity fields (at the same resolution as the relative concentration fields) are measured. This imaging technique allows for a greater understanding of the spatial variability of diffusion rates than can be accomplished with standard bulk measurements. It was found that diffusion rates were fastest in partially gouge-filled fractures. Diffusion rates in the recrystallized calcite-based fracture-filling material were up to an order of magnitude lower than in gouge-filled fractures. Diffusion in altered matrix around the fractures was over an order of magnitude lower than that in the gouge-filled fractures. Healed fractures did not appear to have different diffusion rates than the unaltered matrix

  14. Visualization and quantification of heterogeneous diffusion rates in granodiorite samples by X-ray absorption imaging. Diffusion within gouge materials, altered rim and intact rock matrix

    Energy Technology Data Exchange (ETDEWEB)

    Altman, S.J.; Tidwell, V.C. [Sandia National Laboratories, Albuquerque, NM (United States); Uchida, M. [Japan Nuclear Cycle Development Inst., Ibaraki (Japan)

    2001-08-01

    Matrix diffusion is one of the most important contaminant migration retardation processes in crystalline rocks. Performance assessment calculations in various countries assume that only the area of the fracture surface where advection is active provides access to the rock matrix. However, accessibility to the matrix could be significantly enhanced with diffusion into stagnant zones, fracture fillings, and through an alteration rim in the matrix. Laboratory visualization experiments were conducted on granodiorite samples to investigate and quantify diffusion rates within different zones of a Cretaceous granodiorite. Samples were collected from the Kamaishi experimental site in the northern part of the main island of Japan. Diffusion of iodine out of the sample is visualized and rates are measured using x-ray absorption imaging. X-ray images allow for measurements of relative iodine concentration and relative iodine mass as a function of time and two-dimensional space at a sub-millimeter spatial resolution. In addition, two-dimensional heterogeneous porosity fields (at the same resolution as the relative concentration fields) are measured. This imaging technique allows for a greater understanding of the spatial variability of diffusion rates than can be accomplished with standard bulk measurements. It was found that diffusion rates were fastest in partially gouge-filled fractures. Diffusion rates in the recrystallized calcite-based fracture-filling material were up to an order of magnitude lower than in gouge-filled fractures. Diffusion in altered matrix around the fractures was over an order of magnitude lower than that in the gouge-filled fractures. Healed fractures did not appear to have different diffusion rates than the unaltered matrix.

  15. Preconcentration and determination of boron in milk, infant formula, and honey samples by solid phase extraction-electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, I.; Vinas, P.; Romero-Romero, R. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, M. [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain)], E-mail: hcordoba@um.es

    2009-02-15

    This work presents alternative procedures for the electrothermal atomic absorption spectrometric determination of boron in milk, infant formulas, and honey samples. Honey samples (10% m/v) were diluted in a medium containing 1% v/v HNO{sub 3} and 50% v/v H{sub 2}O{sub 2} and introduced in the atomizer. A mixture of 20 {mu}g Pd and 0.5 {mu}g Mg was used for chemical modification. Calibration was carried out using aqueous solutions prepared in the same medium, in the presence of 10% m/v sucrose. The detection limit was 2 {mu}g g{sup -1}, equivalent to three times the standard error of the estimate (s{sub y/x}) of the regression line. For both infant formulas and milk samples, due to their very low boron content, we used a procedure based on preconcentration by solid phase extraction (Amberlite IRA 743), followed by elution with 2 mol L{sup -1} hydrochloric acid. Detection limits were 0.03 {mu}g g{sup -1} for 4% m/v honey, 0.04 {mu}g g{sup -1} for 5% m/v infant formula and 0.08 {mu}g mL{sup -1} for 15% v/v cow milk. We confirmed the accuracy of the procedure by comparing the obtained results with those found via a comparable independent procedure, as well by the analysis of four certified reference materials.

  16. Novel analytical reagent for the application of cloud-point preconcentration and flame atomic absorption spectrometric determination of nickel in natural water samples

    International Nuclear Information System (INIS)

    Suvardhan, K.; Rekha, D.; Kumar, K. Suresh; Prasad, P. Reddy; Kumar, J. Dilip; Jayaraj, B.; Chiranjeevi, P.

    2007-01-01

    Cloud-point extraction was applied as a preconcentration of nickel after formation of complex with newly synthesized N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13] pentaoxacyclopentadecin-15-yl-methanimine, and later determined by flame atomic absorption spectrometry (FAAS) using octyl phenoxy polyethoxy ethanol (Triton X-114) as surfactant. Nickel was complexed with N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12 octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine in an aqueous phase and was kept for 15 min in a thermo-stated bath at 40 deg. C. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. The chemical variables affecting the cloud-point extraction were evaluated, optimized and successfully applied to the nickel determination in various water samples. Under the optimized conditions, the preconcentration system of 100 ml sample permitted an enhancement factor of 50-fold. The detailed study of various interferences made the method more selective. The detection limits obtained under optimal condition was 0.042 ng ml -1 . The extraction efficiency was investigated at different nickel concentrations (20-80 ng ml -1 ) and good recoveries (99.05-99.93%) were obtained using present method. The proposed method has been applied successfully for the determination of nickel in various water samples and compared with reported method in terms of Student's t-test and variance ratio f-test which indicate the significance of present method over reported and spectrophotometric methods at 95% confidence level

  17. Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

    Science.gov (United States)

    Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

    2017-12-01

    In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO 3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 2 7-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg -1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size < 54µm and adding 25mL of 20% w/w glycerol. The use of 1μg Rh and 50μg citric acid was found satisfactory for the analyte stabilization. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was confirmed by analysis of two certified reference materials (NIST SRM 2702 Inorganics in Marine Sediment and IGI BIL-1 Baikal Bottom Silt) and by comparison of the results obtained for ten real samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Orani, Anna Maria; Han, Eunmi; Mandjukov, Petko; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

  19. Solid sampling graphite furnace atomic absorption spectrometry for the direct analysis of microextraction solvent bars used for metal ultra-trace pre-concentration

    Science.gov (United States)

    González-Álvarez, Rafael Jesús; Pinto, Juan J.; Bellido-Milla, Dolores; Moreno, Carlos

    2017-09-01

    The potential applicability of the continuum source solid sampling graphite furnace atomic absorption spectroscopy (CS SS-GF AAS) technique has been studied to carry out the direct analysis of microextraction solvent bars used for metal ultra-trace pre-concentration in natural waters. An optimisation of the temperature program was developed for this purpose. Preliminary chamber furnace studies were performed in order to understand the behaviour of the bars with the increasing temperature. Solvent bars were filled with an acceptor solution, impregnated with an organic extractant and placed into the chamber furnace to carry out several temperature programs. Results led to perform a correct optimisation of the drying and pyrolysis steps of the furnace temperature program, which was tested with silver once completed. Blank solvent bars as well as standards containing silver were measured, obtaining a calibration curve with a correlation coefficient of 0.991. The results exhibited good repeatability and reproducibility, with relative standard deviations below 10% in both cases, indicating a promising applicability of the CS SS-GF AAS technique to directly determine metallic species in microextraction solvent bars.

  20. Preconcentration and determination of iron and copper in spice samples by cloud point extraction and flow injection flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sahin, Cigdem Arpa, E-mail: carpa@hacettepe.edu.tr [Hacettepe University, Chemistry Department, 06800 Beytepe, Ankara (Turkey); Tokgoez, Ilknur; Bektas, Sema [Hacettepe University, Chemistry Department, 06800 Beytepe, Ankara (Turkey)

    2010-09-15

    A flow injection (FI) cloud point extraction (CPE) method for the determination of iron and copper by flame atomic absorption spectrometer (FAAS) has been improved. The analytes were complexed with 3-amino-7-dimethylamino-2-methylphenazine (Neutral Red, NR) and octylphenoxypolyethoxyethanol (Triton X-114) was added as a surfactant. The micellar solution was heated above 50 {sup o}C and loaded through a column packed with cotton for phase separation. Then the surfactant-rich phase was eluted using 0.05 mol L{sup -1} H{sub 2}SO{sub 4} and the analytes were determined by FAAS. Chemical and flow variables influencing the instrumental and extraction conditions were optimized. Under optimized conditions for 25 mL of preconcentrated solution, the enrichment factors were 98 and 69, the limits of detection (3s) were 0.7 and 0.3 ng mL{sup -1}, the limits of quantification (10s) were 2.2 and 1.0 ng mL{sup -1} for iron and copper, respectively. The relative standard deviation (RSD) for ten replicate measurements of 10 ng mL{sup -1} iron and copper were 2.1% and 1.8%, respectively. The proposed method was successfully applied to determination of iron and copper in spice samples.

  1. Separation and determination of copper in bottled water samples by combination of dispersive liquid--liquid microextraction and microsample introduction flame atomic absorption spectrometry.

    Science.gov (United States)

    Citak, Demirhan; Tuzen, Mustafa

    2013-01-01

    A new and simple method for the determination of trace amounts of Cu(II) was developed by combination of dispersive liquid-liquid microextraction (DLLME) preconcentration and microsample introduction flame atomic absorption spectrometry. In this method, ethanol and chloroform were chosen as disperser and extraction solvents, respectively, and 1-nitroso-2-naphthol was used as the complexing agent. The factors affecting the extraction efficiency and determination of Cu(II), including extraction and disperser solvent nature and volume, concentration of the complexing agent, pH of the solution, extraction time, and matrix ions, were investigated. Under optimal conditions, the LOD for Cu(II) was 0.95 microg/L with a preconcentration factor of 70. The RSD was 1.9%. The accuracy of the developed DLLME method was verified by determination of Cu(II) in a certified reference material (NRCC-SLRS-4 river water). The relative error was -3.31%. The developed preconcentration procedure was successfully applied to the analysis of bottled drinking water samples.

  2. Applicability of cloud point extraction for the separation trace amount of lead ion in environmental and biological samples prior to determination by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Sayed Zia Mohammadi

    2016-09-01

    Full Text Available A sensitive cloud point extraction procedure(CPE for the preconcentration of trace lead prior to its determination by flame atomic absorption spectrometry (FAAS has been developed. The CPE method is based on the complex of Pb(II ion with 1-(2-pyridylazo-2-naphthol (PAN, and then entrapped in the non-ionic surfactant Triton X-114. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PAN and Triton X-114, equilibration temperature and time, were investigated in detail. A preconcentration factor of 30 was obtained for the preconcentration of Pb(II ion with 15.0 mL solution. Under the optimal conditions, the calibration curve was linear in the range of 7.5 ng mL−1–3.5 μg mL−1 of lead with R2 = 0.9998 (n = 10. Detection limit based on three times the standard deviation of the blank (3Sb was 5.27 ng mL−1. Eight replicate determinations of 1.0 μg mL−1 lead gave a mean absorbance of 0.275 with a relative standard deviation of 1.6%. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in biological and water samples with satisfactory results.

  3. Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mirabi, Ali; Dalirandeh, Zeinab [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Rad, Ali Shokuhi, E-mail: a.shokuhi@qaemshahriau.ac.ir [Department of Chemical Engineering, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of)

    2015-05-01

    A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe{sub 3}O{sub 4} as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L{sup −1} HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml{sup −1} and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results. - Highlights: • MNPs method is economical, simple, rapid and sensitive for trace analysis of Cd. • High preconcentration factor was obtained easily through this method. • A detection limit at ng mL{sup −1} level was achieved with 100.0 mL of sample. • This method provides good repeatability and extraction efficiency in a short time.

  4. Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Mirabi, Ali; Dalirandeh, Zeinab; Rad, Ali Shokuhi

    2015-01-01

    A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe 3 O 4 as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L −1 HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml −1 and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results. - Highlights: • MNPs method is economical, simple, rapid and sensitive for trace analysis of Cd. • High preconcentration factor was obtained easily through this method. • A detection limit at ng mL −1 level was achieved with 100.0 mL of sample. • This method provides good repeatability and extraction efficiency in a short time

  5. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS)

    International Nuclear Information System (INIS)

    Guilhen, Sabine Neusatz

    2009-01-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method's performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 +- 11,70)mug.L -1 with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10μg.L -1 . The obtained results fall into a

  6. A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Kahe, Hadi; Chamsaz, Mahmoud

    2016-11-01

    A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L -1 Bi (III) with a limit of detection (LOD) of 0.16 μg L -1 (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L -1 of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

  7. Hollow fiber liquid phase microextraction combined with graphite furnace atomic absorption spectrometry for the determination of methylmercury in human hair and sludge samples

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Hongmei [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn; Chen Beibei; Zu Wanqing [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2008-07-15

    Two methods, based on hollow fiber liquid-liquid-liquid (three phase) microextraction (HF-LLLME) and hollow fiber liquid phase (two phase) microextraction (HF-LPME), have been developed and critically compared for the determination of methylmercury content in human hair and sludge by graphite furnace atomic absorption spectrometry (GFAAS). In HF-LPME, methylmercury was extracted into the organic phase (toluene) prior to its determination by GFAAS, while inorganic mercury remained as a free species in the sample solution. In HF-LLLME, methylmercury was first extracted into the organic phase (toluene) and then into the acceptor phase (4% thiourea in 1 mol L{sup -1} HCl) prior to its determination by GFAAS, while inorganic mercury remained in the sample solution. The total mercury was determined by inductively coupled plasma-mass spectrometry (ICP-MS), and the levels of inorganic mercury in both HF-LLLME and HF-LPME were obtained by subtracting methylmercury from total mercury. The factors affecting the microextraction of methylmercury, including organic solvent, extraction time, stirring rate and ionic strength, were investigated and the optimal extraction conditions were established for both HF-LLLPME and HF-LPME. With a consumption of 3.0 mL of the sample solution, the enrichment factors were 204 and 55 for HF-LLLPME and HF-LPME, respectively. The limits of detection (LODs) for methylmercury were 0.1 {mu}g L{sup -1} and 0.4 {mu}g L{sup -1} (as Hg) with precisions (RSDs (%), c = 5 {mu}g L{sup -1} (as Hg), n = 5) of 13% and 11% for HF-LLLPME-GFAAS and HF-LPME-GFAAS, respectively. For ICP-MS determination of total mercury, a limit of detection of 39 ng L{sup -} {sup 1} was obtained. Finally, HF-LLLME-GFAAS was applied to the determination of methylmercury content in human hair and sludge, and the recoveries for the spiked samples were in the range of 99-113%. In order to validate the method, HF-LLLME-GFAAS was also applied to the analysis of a certified reference

  8. Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples.

    Science.gov (United States)

    Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

    2008-03-03

    The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 microL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 microgL(-1) with a detection limit of 0.5 microgL(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 microgL(-1) of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 microgL(-1) ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method.

  9. A solid phase extraction procedure for the determination of Cd(II) and Pb(II) ions in food and water samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Daşbaşı, Teslima; Saçmacı, Şerife; Ülgen, Ahmet; Kartal, Şenol

    2015-05-01

    A relatively rapid, accurate and precise solid phase extraction method is presented for the determination of cadmium(II) and lead(II) in various food and water samples. Quantitation is carried out by flame atomic absorption spectrometry (FAAS). The method is based on the retention of the trace metal ions on Dowex Marathon C, a strong acid cation exchange resin. Some important parameters affecting the analytical performance of the method such as pH, flow rate and volume of the sample solution; type, concentration, volume, flow rate of the eluent; and matrix effects on the retention of the metal ions were investigated. Common coexisting ions did not interfere on the separation and determination of the analytes. The detection limits (3 σb) for Cd(II) and Pb(II) were found as 0.13 and 0.18 μg L(-1), respectively, while the limit of quantification values (10 σb) were computed as 0.43 and 0.60 μg L(-1) for the same sequence of the analytes. The precision (as relative standard deviation was lower than 4% at 5 μg L(-1) Cd(II) and 10 μg L(-1) Pb(II) levels, and the preconcentration factor was found to be 250. The accuracy of the proposed procedure was verified by analysing the certified reference materials, SPS-WW2 Batch 108 wastewater level 2 and INCT-TL-1 tea leaves, with the satisfactory results. In addition, for the accuracy of the method the recovery studies (⩾ 95%) were carried out. The method was applied to the determination of the analytes in the various natural waters (lake water, tap water, waste water with boric acid, waste water with H2SO4) and food samples (pomegranate flower, organic pear, radish leaf, lamb meat, etc.), and good results were obtained. While the food samples almost do not contain cadmium, they have included lead at low levels of 0.13-1.12 μg g(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples

    International Nuclear Information System (INIS)

    Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

    2008-01-01

    The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 μL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 μg L -1 with a detection limit of 0.5 μg L -1 . The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 μg L -1 of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 μg L -1 ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method

  11. Graphene oxide-TiO2 composite solid phase extraction combined with graphite furnace atomic absorption spectrometry for the speciation of inorganic selenium in water samples.

    Science.gov (United States)

    Zhang, Yanan; Chen, Beibei; Wu, Shaowei; He, Man; Hu, Bin

    2016-07-01

    In this paper, a method of graphene oxide (GO)-TiO2 composite solid phase extraction followed by graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the speciation of inorganic selenium in environmental waters. The adsorption behavior of inorganic Se(IV) and Se(VI) on the GO-TiO2(1:1) composite was investigated. It was found that Se(IV) was quantitatively retained on the GO-TiO2 composites within a wide pH range of 0.5-10, while Se(VI) was quantitatively adsorbed on GO-TiO2(1:1) composite at pH 0.5-2, and no obvious adsorption of Se(VI) within the pH range of 4-10 was found. By selecting pH 6.0, Se(IV) could be easily determined. After reduction of Se(VI), total Se was determined by the proposed method, and Se(VI) was calculated as the difference between the total Se and Se(IV). The factors affecting the separation/preconcentration of Se(IV) and Se(VI) were studied. Under the optimum conditions, the isothermal adsorption of Se(IV) on the GO-TiO2(1:1) composite fitted Langmuir model; a linear range over 0.1-12ngmL(-1) was obtained. The limit of detection (LOD) and precision of the method for Se(IV) was 0.04ngmL(-1) and 9.4% (cSe(IV)=0.5ngmL(-1), n=7), respectively. In order to verify the accuracy of the method, a standard water sample (GSBZ50031-94) was analyzed, and the determined value was in a good agreement to the certified value. The established method was applied to inorganic Se speciation in environmental water samples and the recovery of 87.4-102% was obtained for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples

    Directory of Open Access Journals (Sweden)

    Xiupei Yang

    2017-03-01

    Full Text Available A cloud point extraction (CPE method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I/diethyldithiocarbamate (DDTC complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL−1 Ag+ in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL−1 for both Zn2+ and Cu2+, 80 μg·mL−1 for Pb2+, 1000 μg·mL−1 for Mn2+, and 100 μg·mL−1 for both Cd2+ and Ni2+. The calibration curve was linear in the range of 1–500 ng·mL−1 with a limit of detection (LOD at 0.3 ng·mL−1. The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

  13. Development of an analytical model for the determination of 60Co in aqueous samples by atomic absorption and gamma spectrometry techniques

    International Nuclear Information System (INIS)

    Solis A, N. A.

    2015-01-01

    The applications of the nuclear energy in industry and medicine generate radioactive wastes that must be isolated and confined in order to limit its spread in the biosphere. These types of wastes are generated in hospitals, industry, research centers and nuclear power plants (during de fuel cycle). The radioactive elements (radionuclides) cannot be destroyed by any known method, either chemical or mechanical. Its final destruction is produced by radioactive decay, which makes them stable isotopes, or nuclear transmutation being bombarded with atomic particles. Consequently, the radioactive waste management is to control the radioactive discharges and reduce to tolerable limits, eliminating of effluents and wastes the radionuclides of interest, concentrating them so they can be stored or evacuated so that later not appear in dangerous concentration in the biosphere. In Mexico, the main generators of radioactive wastes are the nuclear power plant of Laguna Verde in Veracruz, Hospitals of the public and private sector, in addition Instituto Nacional de Investigaciones Nucleares (ININ) some institutes and facilities of the UNAM and Instituto Politecnico Nacional (IPN) and industries among others. The aqueous radioactive wastes, particularly those from the nuclear power plants contain traces of cobalt-60. Currently there is no model or analytical technique for the separation of this radionuclide, so it became necessary to develop an analytical model for separation and facilitate their disposal. In this paper was shown that atomic absorption and gamma spectrometry techniques can separate the active concentration of the inactive, which is important because the total concentration can be associated through direct relationships with the wear of metal parts of the nuclear reactor, since the metal alloys of the same reactor containing a fraction of cobalt. Also this analytical and mathematical model that can be reproducible and applicable to full sets of samples and that this

  14. Hollow fiber based liquid-phase microextraction for the determination of mercury traces in water samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, Ignacio; Rivas, Ricardo E. [Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence ' Campus Mare Nostrum' , University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, Manuel, E-mail: hcordoba@um.es [Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence ' Campus Mare Nostrum' , University of Murcia, E-30071 Murcia (Spain)

    2012-09-19

    Highlight: Black-Right-Pointing-Pointer Hg (II) traces are preconcentrated by means of a three-phase liquid microextraction system. Black-Right-Pointing-Pointer PAN and ammonium iodide are used in the donor and acceptor phase, respectively. Black-Right-Pointing-Pointer Hollow-fiber pores are continuously fed with toluene placed in the lumen. Black-Right-Pointing-Pointer Mercuric ions can be measured in waters below the {mu}g L{sup -1} level. - Abstract: A three-phase liquid microextraction procedure for the determination of mercury at low concentrations is discussed. To the aqueous sample placed at pH 7 by means of a phosphate buffer, 0.002% (m/v) 1-(2-pyridylazo)-2-naphthol (PAN) is incorporated, and the mixture submitted to microextraction with a hollow-fiber impregnated with toluene and whose lumen contains a 0.05 mol L{sup -1} ammonium iodide solution. The final measurement of the extract is carried out by electrothermal atomic absorption spectrometry (300 Degree-Sign C and 1100 Degree-Sign C for the calcination and atomization temperatures, respectively). The pyrolytic graphite atomizer is coated electrolytically with palladium. An enrichment factor of 270, which results in a 0.06 {mu}g L{sup -1} mercury for the detection limit is obtained. The relative standard deviation at the 1 {mu}g L{sup -1} mercury level is 3.2% (n = 5). The reliability of the procedure is verified by analyzing waters as well as six certified reference materials.

  15. Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples.

    Science.gov (United States)

    Yang, Xiupei; Jia, Zhihui; Yang, Xiaocui; Li, Gu; Liao, Xiangjun

    2017-03-01

    A cloud point extraction (CPE) method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS) The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I)/diethyldithiocarbamate (DDTC) complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I)/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL -1 Ag + in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL -1 for both Zn 2+ and Cu 2+ , 80 μg·mL -1 for Pb 2+ , 1000 μg·mL -1 for Mn 2+ , and 100 μg·mL -1 for both Cd 2+ and Ni 2+ . The calibration curve was linear in the range of 1-500 ng·mL -1 with a limit of detection (LOD) at 0.3 ng·mL -1 . The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

  16. Bovine serum albumin-Cu(II) hybrid nanoflowers: An effective adsorbent for solid phase extraction and slurry sampling flame atomic absorption spectrometric analysis of cadmium and lead in water, hair, food and cigarette samples

    Energy Technology Data Exchange (ETDEWEB)

    Yilmaz, Erkan [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey); Ocsoy, Ismail [Department of Analytical Chemistry, Faculty of Pharmacy, Erciyes University, Kayseri 38039 (Turkey); Nanotechnology Research Center (ERNAM), Erciyes University, Kayseri 38039 (Turkey); Ozdemir, Nalan [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey); Soylak, Mustafa, E-mail: soylak@erciyes.edu.tr [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey)

    2016-02-04

    Herein, the synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers (BSA-NFs) through the building blocks of bovine serum albumin (BSA) and copper(II) ions in phosphate buffered saline (PBS) and their use as adsorbent for cadmium and lead ions are reported. The BSA-NFs, for the first time, were efficiently utilized as novel adsorbent for solid phase extraction (SPE) of cadmium and lead ions in water, food, cigarette and hair samples. The method is based on the separation and pre-concentration of Cd(II) and Pb(II) by BSA-NFs prior to determination by slurry analysis via flame atomic absorption spectrometry (FAAS). The analytes were adsorbed on BSA-NFs under the vortex mixing and then the ion-loaded slurry was separated and directly introduced into the flame AAS nebulizer by using a hand-made micro sample introduction system to eliminate a number of drawbacks. The effects of analytical key parameters, such as pH, amount of BSA-NFs, vortexing time, sample volume, and matrix effect of foreign ions on adsorbing of Cd(II) and Pb(II) were systematically investigated and optimized. The limits of detection (LODs) for Cd(II) and Pb(II) were calculated as 0.37 μg L{sup −1} and 8.8 μg L{sup −1}, respectively. The relative standard deviation percentages (RSDs) (N = 5) for Cd(II) and Pb(II) were 7.2%, and 5.0%, respectively. The accuracy of the developed procedure was validated by the analysis of certified reference materials (TMDA-53.3 Fortified Water, TMDA-70 Fortified Water, SPS-WW2 Waste Water, NCSDC-73349 Bush Branches and Leaves) and by addition/recovery analysis. The quantitative recoveries were obtained for the analysis of certified reference materials and addition/recovery tests. The method was successfully applied to the analysis of cadmium and lead in water, food, cigarette and hair samples. - Highlights: • The synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers is reported. • The nanoflowers were utilized for solid phase microextraction of

  17. Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

    Science.gov (United States)

    dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

    2009-11-11

    A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

  18. Calcium absorption

    International Nuclear Information System (INIS)

    Carlmark, B.; Reizenstein, P.; Dudley, R.A.

    1976-01-01

    The methods most commonly used to measure the absorption and retention of orally administered calcium are reviewed. Nearly all make use of calcium radioisotopes. The magnitude of calcium absorption and retention depends upon the chemical form and amount of calcium administered, and the clinical and nutritional status of the subject; these influences are briefly surveyed. (author)

  19. Absorption studies

    International Nuclear Information System (INIS)

    Ganatra, R.D.

    1992-01-01

    Absorption studies were once quite popular but hardly anyone does them these days. It is easier to estimate the blood level of the nutrient directly by radioimmunoassay (RIA). However, the information obtained by estimating the blood levels of the nutrients is not the same that can be obtained from the absorption studies. Absorption studies are primarily done to find out whether some of the essential nutrients are absorbed from the gut or not and if they are absorbed, to determine how much is being absorbed. In the advanced countries, these tests were mostly done to detect pernicious anaemia where vitamin B 12 is not absorbed because of the lack of the intrinsic factor in the stomach. In the tropical countries, ''malabsorption syndrome'' is quire common. In this condition, several nutrients like fat, folic acid and vitamin B 12 are not absorbed. It is possible to study absorption of these nutrients by radioisotopic absorption studies

  20. Analysis Of Non-Volatile Toxic Heavy Metals (Cd, Pb, Cu,Cr And Zn) In ALLIUM SATIVUM (Garlic) And Soil Samples ,Collected From Different Locations Of Punjab, Pakistan By Atomic Absorption Spectroscopy

    OpenAIRE

    Ata S.; Tayyab S.; Rasool A.

    2013-01-01

    Garlic is one of the most widely used medicinal plants. The monitoring of toxic metals such as lead, Cadmium, Chromium, Copper and Zinc in garlic and the soil of garlic fields collected from ten different cities of Punjab is critical for preventing public health against the hazards of metal toxicity. The levels of toxic heavy metals in garlic and soil samples were investigated using Atomic absorption spectrometer. The metal content in garlic samples was found to be in increasing order as Cr> ...

  1. Self-consistent approach to the solution of the light transfer problem for irradiances in marine waters with arbitrary turbidity, depth, and surface illumination. I. Case of absorption and elastic scattering.

    Science.gov (United States)

    Haltrin, V I

    1998-06-20

    A self-consistent variant of the two-flow approximation that takes into account strong anisotropy of light scattering in seawater of finite depth and arbitrary turbidity is presented. To achieve an appropriate accuracy, this approach uses experimental dependencies between downward and total mean cosines. It calculates irradiances, diffuse attenuation coefficients, and diffuse reflectances in waters with arbitrary values of scattering, backscattering, and attenuation coefficients. It also takes into account arbitrary conditions of illumination and reflection from the bottom with the Lambertian albedo. This theory can be used for the calculation of apparent optical properties in both open and coastal oceanic waters, lakes, and rivers. It can also be applied to other types of absorbing and scattering medium such as paints, photographic emulsions, and biological tissues.

  2. Bovine serum albumin-Cu(II) hybrid nanoflowers: An effective adsorbent for solid phase extraction and slurry sampling flame atomic absorption spectrometric analysis of cadmium and lead in water, hair, food and cigarette samples.

    Science.gov (United States)

    Yilmaz, Erkan; Ocsoy, Ismail; Ozdemir, Nalan; Soylak, Mustafa

    2016-02-04

    Herein, the synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers (BSA-NFs) through the building blocks of bovine serum albumin (BSA) and copper(II) ions in phosphate buffered saline (PBS) and their use as adsorbent for cadmium and lead ions are reported. The BSA-NFs, for the first time, were efficiently utilized as novel adsorbent for solid phase extraction (SPE) of cadmium and lead ions in water, food, cigarette and hair samples. The method is based on the separation and pre-concentration of Cd(II) and Pb(II) by BSA-NFs prior to determination by slurry analysis via flame atomic absorption spectrometry (FAAS). The analytes were adsorbed on BSA-NFs under the vortex mixing and then the ion-loaded slurry was separated and directly introduced into the flame AAS nebulizer by using a hand-made micro sample introduction system to eliminate a number of drawbacks. The effects of analytical key parameters, such as pH, amount of BSA-NFs, vortexing time, sample volume, and matrix effect of foreign ions on adsorbing of Cd(II) and Pb(II) were systematically investigated and optimized. The limits of detection (LODs) for Cd(II) and Pb(II) were calculated as 0.37 μg L(-)(1) and 8.8 μg L(-)(1), respectively. The relative standard deviation percentages (RSDs) (N = 5) for Cd(II) and Pb(II) were 7.2%, and 5.0%, respectively. The accuracy of the developed procedure was validated by the analysis of certified reference materials (TMDA-53.3 Fortified Water, TMDA-70 Fortified Water, SPS-WW2 Waste Water, NCSDC-73349 Bush Branches and Leaves) and by addition/recovery analysis. The quantitative recoveries were obtained for the analysis of certified reference materials and addition/recovery tests. The method was successfully applied to the analysis of cadmium and lead in water, food, cigarette and hair samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Folate absorption

    International Nuclear Information System (INIS)

    Baker, S.J.

    1976-01-01

    Folate is the generic term given to numerous compounds of pteroic acid with glutamic acid. Knowledge of absorption is limited because of the complexities introduced by the variety of compounds and because of the inadequacy of investigational methods. Two assay methods are in use, namely microbiological and radioactive. Techniques used to study absorption include measurement of urinary excretion, serum concentration, faecal excretion, intestinal perfusion, and haematological response. It is probably necessary to test absorption of both pteroylmonoglutamic acid and one or more polyglutamates, and such tests would be facilitated by availability of synthesized compounds labelled with radioactive tracers at specifically selected sites. (author)

  4. Structural Consistency, Consistency, and Sequential Rationality.

    OpenAIRE

    Kreps, David M; Ramey, Garey

    1987-01-01

    Sequential equilibria comprise consistent beliefs and a sequentially ra tional strategy profile. Consistent beliefs are limits of Bayes ratio nal beliefs for sequences of strategies that approach the equilibrium strategy. Beliefs are structurally consistent if they are rationaliz ed by some single conjecture concerning opponents' strategies. Consis tent beliefs are not necessarily structurally consistent, notwithstan ding a claim by Kreps and Robert Wilson (1982). Moreover, the spirit of stru...

  5. Transient-Absorption Spectroscopy of Cis-Trans Isomerization of N,N-dimethyl-4,4'-Azodianiline with 3D-Printed Temperature-Controlled Sample Holder

    Science.gov (United States)

    Kosenkov, Dmytro; Shaw, James; Zuczek, Jennifer; Kholod, Yana

    2016-01-01

    The laboratory unit demonstrates a project based approach to teaching physical chemistry laboratory where upper-division undergraduates carry out a transient-absorption experiment investigating the kinetics of cis-trans isomerization of N,N-dimethyl-4,4'-azodianiline. Students participate in modification of a standard flash-photolysis spectrometer…

  6. Single and Double Infrared Transitions in Rapid Vapor Deposited Parahydrogen Solids: Application to Sample Thickness Determination and Quantitative Infrared Absorption Spectroscopy

    National Research Council Canada - National Science Library

    Tam, Simon

    2001-01-01

    ...) solid from its infrared (IR) absorption spectrum. Millimeters-thick pH2 solids of exceptional optical clarity can be produced by the rapid vapor deposition method M.E. Fajardo and S. Tam, J. Chem. Phys. 108, 4237 (1998...

  7. Quasar Absorption Studies

    Science.gov (United States)

    Mushotzky, Richard (Technical Monitor); Elvis, Martin

    2004-01-01

    The aim of the proposal is to investigate the absorption properties of a sample of inter-mediate redshift quasars. The main goals of the project are: Measure the redshift and the column density of the X-ray absorbers; test the correlation between absorption and redshift suggested by ROSAT and ASCA data; constrain the absorber ionization status and metallicity; constrain the absorber dust content and composition through the comparison between the amount of X-ray absorption and optical dust extinction. Unanticipated low energy cut-offs where discovered in ROSAT spectra of quasars and confirmed by ASCA, BeppoSAX and Chandra. In most cases it was not possible to constrain adequately the redshift of the absorber from the X-ray data alone. Two possibilities remain open: a) absorption at the quasar redshift; and b) intervening absorption. The evidences in favour of intrinsic absorption are all indirect. Sensitive XMM observations can discriminate between these different scenarios. If the absorption is at the quasar redshift we can study whether the quasar environment evolves with the Cosmic time.

  8. Water absorption in brick masonry

    NARCIS (Netherlands)

    Brocken, H.J.P.; Smolders, H.R.

    1996-01-01

    The water absorption in brick, mortar that was cured separately, and masonry samples was studied using NMR. Models of the moisture transport are usually formulated on the basis of a diffusion equation. In the case of water absorption in separate brick and mortar samples, the moisture diffusivity in

  9. Determinação de As em amostras orgânicas de interesse ambiental por espectrometria de absorção atômica com atomização eletrotérmica após combustão em bomba de O2 Determination of As in environmental organic samples by atomic absorption spectrometry with electrothermal atomization after O2 bomb combustion

    Directory of Open Access Journals (Sweden)

    Vera Maria da Costa Dias

    2003-10-01

    Full Text Available The toxicity of the major As species present in the environment justifies the effort for quantifying the element in environmental organic samples, which can vary from animal and vegetal tissues to coal and industrial residues. This paper comments about the applicability of the O2 bomb digestion, as a general procedure for all environmental organic materials. A rapid and straightforward method is suggested, which consists in burning the sample in the bomb at high O2 pressure, dissolving the vapours in diluted HNO3 and determining As in the resulting solution by atomic absorption spectrometry with electrothermal atomization. The method was applied to certified materials and plant samples.

  10. Nonlinear effects in collective absorption

    International Nuclear Information System (INIS)

    Uenoyama, Takeshi; Mima, Kunioki; Watanabe, Tsuguhiro.

    1981-01-01

    The collective absorption of high intensity laser radiation is analyzed numerically. Density profile modification due to the ponderomotive force associating laser radiation and the excited electron plasma waves is self-consistently taken into account, and the intensity dependences of the absorption efficiency are obtained. In the high intensity regime, the absorption efficiency is found to be strongly enhanced in the plasma without flow, but reduced with supersonic flow. (author)

  11. Luminescence and optical absorption determination in porous silicon

    International Nuclear Information System (INIS)

    Nogal, U.; Calderon, A.; Marin, E.; Rojas T, J. B.; Juarez, A. G.

    2012-10-01

    We applied the photoacoustic spectroscopy technique in order to obtain the optical absorption spectrum in porous silicon samples prepared by electrochemical anodic etching on n-type, phosphorous doped, (100)-oriented crystal-line silicon wafer with thickness of 300 μm and 1-5 ωcm resistivity. The porous layers were prepared with etching times of 13, 20, 30, 40 and 60 minutes. Also, we realized a comparison among the optical absorption spectrum with the photoluminescence and photo reflectance ones, both obtained at room temperature. Our results show that the absorption spectrum of the samples of porous silicon depends notably of the etching time an it consist of two distinguishable absorption bands, one in the Vis region and the other one in the UV region. (Author)

  12. A practical method for determining γ-ray full-energy peak efficiency considering coincidence-summing and self-absorption corrections for the measurement of environmental samples after the Fukushima reactor accident

    Energy Technology Data Exchange (ETDEWEB)

    Shizuma, Kiyoshi, E-mail: shizuma@hiroshima-u.ac.jp [Graduate School of Engineering, Hiroshima University, Higashi-Hiroshima 739-8527 (Japan); Oba, Yurika; Takada, Momo [Graduate School of Integrated Arts and Sciences, Hiroshima University, Higashi-Hiroshima 739-8521 (Japan)

    2016-09-15

    A method for determining the γ-ray full-energy peak efficiency at positions close to three Ge detectors and at the well port of a well-type detector was developed for measuring environmental volume samples containing {sup 137}Cs, {sup 134}Cs and {sup 40}K. The efficiency was estimated by considering two correction factors: coincidence-summing and self-absorption corrections. The coincidence-summing correction for a cascade transition nuclide was estimated by an experimental method involving measuring a sample at the far and close positions of a detector. The derived coincidence-summing correction factors were compared with those of analytical and Monte Carlo simulation methods and good agreements were obtained. Differences in the matrix of the calibration source and the environmental sample resulted in an increase or decrease of the full-energy peak counts due to the self-absorption of γ-rays in the sample. The correction factor was derived as a function of the densities of several matrix materials. The present method was applied to the measurement of environmental samples and also low-level radioactivity measurements of water samples using the well-type detector.

  13. Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

    Science.gov (United States)

    Ciftci, Harun; Er, Cigdem

    2013-03-01

    In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

  14. Narrative absorption

    DEFF Research Database (Denmark)

    Narrative Absorption brings together research from the social sciences and Humanities to solve a number of mysteries: Most of us will have had those moments, of being totally absorbed in a book, a movie, or computer game. Typically we do not have any idea about how we ended up in such a state. No...

  15. Absorptive products

    International Nuclear Information System (INIS)

    Assarsson, P.G.; King, P.A.

    1976-01-01

    Applications for hydrophile gels produced by the radiation induced cross-linking in aqueous solution of polyethylene oxide and starch, as described in Norwegian patent 133501 (INIS RN 281494), such as sanitary napkins (diapers) and sanitary towels, are discussed. The process itself is also discussed and results, expressed as the percentage of insoluble gel and its absorptive capacity for saline solution as functions of the ratio of polyethylene oxide to starch and the radiation dose, are presented. (JIW)

  16. Solid phase extraction method for the determination of lead, nickel, copper and manganese by flame atomic absorption spectrometry using sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) in water samples

    International Nuclear Information System (INIS)

    Rekha, D.; Suvardhan, K.; Kumar, J. Dilip; Subramanyam, P.; Prasad, P. Reddy; Lingappa, Y.; Chiranjeevi, P.

    2007-01-01

    A novel column solid phase extraction procedure was developed for the determination of lead, nickel, copper and manganese in various water samples by flame atomic absorption spectrometry (FAAS) after preconcentration on sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) supported by Amberlite XAD-7. The sorbed element was subsequently eluted with 1 M nitric acid and the acid eluates are analysed by Flame atomic absorption spectrometry (FAAS). Various parameters such as pH, amount of adsorbent, eluent type and volume, flow-rate of the sample solution, volume of the sample solution and matrix interference effect on the retention of the metal ions have been studied. The optimum pH for the sorption of above mentioned metal ions was about 6.0 ± 0.2. The loading capacity of adsorbent for Pb, Cu, Ni and Mn were found to 28, 26, 22 and 20 x 10 -6 g/mL, respectively. The recoveries of lead, copper, nickel and manganese under optimum conditions were found to be 96.7-99.2 at the 95% confident level. The limit of detection was 3.0, 3.2, 2.8 and 3.6 x 10 -6 g/mL for lead, copper, nickel and manganese, respectively by applying a preconcentration factor 50. The proposed enrichment method was applied for metal ions in various water samples. The results were obtained are good agreement with reported method

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  18. Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS for determination of trace Cu and Zn in water Samples

    Directory of Open Access Journals (Sweden)

    Ghorbani A.

    2014-07-01

    Full Text Available Dispersive liquid-liquid microextraction (DLLME combined with graphite furnace atomic absorption spectrometry (GFAAS was proposed for the determination of trace amounts of Copper and Zinc ions using 8-hydroxyquinoline (8-HQ as chelating agent. Several factors influencing the microextraction efficiency of Cu and Zn and their subsequent determinations, such as pH, extraction and disperser solvent type and their volume, concentration of the chelating agent and extraction time were studied, and the optimized experimental conditions were established. After extraction, the enrichment factors were 25 and 26 for Cu and Zn, respectively. The detection limits of the method were 0.025 and 0.0033 μg/L for Cu and Zn, and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Cu and Zn were 8.51% and 7.41%, respectively.

  19. Vitamin A absorption

    International Nuclear Information System (INIS)

    Baker, S.J.

    1976-01-01

    Investigation of the absorption of vitamin A and related substances is complicated by the multiplicity of forms in which they occur in the diet and by the possibility that they may be subject to different mechanisms of absorption. Present knowledge of these mechanisms is inadequate, especially in the case of carotenoids. Numerous tests of absorption have been developed. The most common has been the biochemical measurement of the rise in plasma vitamin A after an oral dose of retinol or retinyl ester, but standardization is inadequate. Radioisotope tests based upon assay of serum or faecal activity following oral administration of tritiated vitamin A derivaties hold considerable promise, but again standardization is inadequate. From investigations hitherto performed it is known that absorption of vitamin A is influenced by several diseases, although as yet the consistency of results and the correlation with other tests of intestinal function have often been poor. However, the test of vitamin A absorption is nevertheless of clinical importance as a specialized measure of intestinal function. (author)

  20. Direct and quantitative photothermal absorption spectroscopy of individual particulates

    International Nuclear Information System (INIS)

    Tong, Jonathan K.; Hsu, Wei-Chun; Eon Han, Sang; Burg, Brian R.; Chen, Gang; Zheng, Ruiting; Shen, Sheng

    2013-01-01

    Photonic structures can exhibit significant absorption enhancement when an object's length scale is comparable to or smaller than the wavelength of light. This property has enabled photonic structures to be an integral component in many applications such as solar cells, light emitting diodes, and photothermal therapy. To characterize this enhancement at the single particulate level, conventional methods have consisted of indirect or qualitative approaches which are often limited to certain sample types. To overcome these limitations, we used a bilayer cantilever to directly and quantitatively measure the spectral absorption efficiency of a single silicon microwire in the visible wavelength range. We demonstrate an absorption enhancement on a per unit volume basis compared to a thin film, which shows good agreement with Mie theory calculations. This approach offers a quantitative approach for broadband absorption measurements on a wide range of photonic structures of different geometric and material compositions

  1. UV Absorption Measurements of Nitric Oxide Compared to Probe Sampling Data for Measurements in a Turbine Engine Exhaust at Simulated Altitude Conditions

    National Research Council Canada - National Science Library

    Howard, R

    1997-01-01

    Nitric oxide measurements were conducted in the exhaust of a turbofan engine at simulated altitude conditions in a ground-level test cell using both optical nonintrusive and conventional gas sampling techniques...

  2. Determination of molybdenum, ruthenium, rhodium, and palladium in radioinactive simulated waste of the nuclear fuel cycle by solid sampling graphite furnace atomic absorption spectrometry (GFAAS)

    International Nuclear Information System (INIS)

    Schmiedel, G.; Mainka, E.; Ache, H.J.

    1989-01-01

    In relation with insoluble particles in the nuclear fuel cycle waste, the solid sampling GFAAS was used to determine molybdenum, ruthenium, rhodium, and palladium in such waste. Two methods for the direct determination of these elements are described. The samples must be handled in glove boxes or moreover in hot cells with a robot. The determination of the elements by the cup-in-tube technique needs a very sensitive balance (microbalance) for weighing in μg-range and the handling of this method is not practical in glove boxes and hot cells. An alternative technique of solid sampling GFAAS, which can be used without great problems in glove boxes and hot cells is the slurry technique. In this case two methods have been used. One method uses graphite powder as a diluter, the other is the direct suspension of the sample in a matrix modifier solution. In the case of slurry technique with predilution of the sample with graphite powder, recoveries between 91 and 102% and RSD between 4 and 8% were obtained, whereas in the case of slurry technique with direct suspension of the waste sample recoveries between 91 and 103% and RSD between 14 and 20% for the above mentioned elements were obtained. (orig.)

  3. The development and evaluation of airborne in situ N2O and CH4 sampling using a Quantum Cascade Laser Absorption Spectrometer (QCLAS)

    Science.gov (United States)

    Pitt, Joseph; Le Breton, Michael; Allen, Grant; Percival, Carl; Gallagher, Martin; Bauguitte, Stephane; O'Shea, Sebastian; Muller, Jennifer; Zahniser, Mark; Pyle, John; Palmer, Paul

    2016-04-01

    Spectroscopic measurements of atmospheric N2O and CH4 mole fractions were made on board the FAAM (Facility for Airborne Atmospheric Measurements) large Atmospheric Research Aircraft. We evaluate the performance of the mid-IR continuous wave Aerodyne Research Inc. Quantum Cascade Laser Absorption Spectrometer (QCLAS) employed over 17 flights conducted during summer 2014. Two different methods of correcting for the influence of water vapour on the spectroscopic retrievals are compared and evaluated. Test flight data demonstrating the sensitivity of the instrument to changes in cabin pressure is presented, and a new in-flight calibration procedure to account for this issue is described and assessed. Total 1σ uncertainties of 1.81 ppb for CH4 and 0.35 ppb for N2O are derived. We report a mean difference in 1 Hz CH4 mole fraction of 2.05 ppb (1σ = 5.85 ppb) between in-flight measurements made using the QCLAS and simultaneous measurements using a previously characterised Los Gatos Research Fast Greenhouse Gas Analyser (FGGA).

  4. Gamma absorption meter

    International Nuclear Information System (INIS)

    Dincklage, R.D. von.

    1984-01-01

    The absorption meter consists of a radiation source, a trough for the absorbing liquid and a detector. It is characterized by the fact that there is a foil between the detector and the trough, made of a material whose binding energy of the K electrons is a little greater than the energy of the photons emitted by the radiation source. The source of radiation and foil are replaceable. (orig./HP) [de

  5. Consistency argued students of fluid

    Science.gov (United States)

    Viyanti; Cari; Suparmi; Winarti; Slamet Budiarti, Indah; Handika, Jeffry; Widyastuti, Fatma

    2017-01-01

    Problem solving for physics concepts through consistency arguments can improve thinking skills of students and it is an important thing in science. The study aims to assess the consistency of the material Fluid student argmentation. The population of this study are College students PGRI Madiun, UIN Sunan Kalijaga Yogyakarta and Lampung University. Samples using cluster random sampling, 145 samples obtained by the number of students. The study used a descriptive survey method. Data obtained through multiple-choice test and interview reasoned. Problem fluid modified from [9] and [1]. The results of the study gained an average consistency argmentation for the right consistency, consistency is wrong, and inconsistent respectively 4.85%; 29.93%; and 65.23%. Data from the study have an impact on the lack of understanding of the fluid material which is ideally in full consistency argued affect the expansion of understanding of the concept. The results of the study as a reference in making improvements in future studies is to obtain a positive change in the consistency of argumentations.

  6. Determination of fluorine in herbs and water samples by molecular absorption spectrometry after preconcentration on nano-TiO2 using ultrasound-assisted dispersive micro solid phase extraction.

    Science.gov (United States)

    Krawczyk-Coda, Magdalena; Stanisz, Ewa

    2017-11-01

    This work presents ultrasound-assisted dispersive micro solid phase extraction (USA DMSPE) for preconcentration of fluorine (F) in water and herb samples. TiO 2 nanoparticles (NPs) were used as an adsorbent. The determination with slurry sampling was performed via molecular absorption of calcium monofluoride (CaF) at 606.440 nm using a high-resolution continuum source electrothermal absorption spectrometry (HR-CS ET MAS). Several factors influencing the efficiency of the preconcentration technique, such as the amount of TiO 2 , pH of sample solution, ultrasonication and centrifugation time and TiO 2 slurry solution preparation before injection to HR-CS ET MAS, were investigated in detail. The conditions of detection step (wavelength, calcium amount, pyrolysis and molecule-forming temperatures) were also studied. After extraction, adsorbent with the analyte was mixed with 200 μL of H 2 O to prepare a slurry solution. The concentration limit of detection was 0.13 ng mL -1 . The achieved preconcentration factor was 7. The relative standard deviations (RSDs, %) for F in real samples were 3-15%. The accuracy of this method was evaluated by analyses of certified reference materials after spiking: INCT-MPH-2 (Mixed Polish Herbs), INCT-SBF-4 (Soya Bean Flour), ERM-CAO11b (Hard Drinking Water) and TMDA-54.5 (Lake Ontario Water). The measured F contents in reference materials were in satisfactory agreement with the added amounts, and the recoveries were found to be 97-109%. Under the developed extraction conditions, the proposed method has been successfully applied for the determination of F in real water samples (lake, sea, tap water) and herbs.

  7. Internal consistency, concurrent validity, and discriminant validity of a measure of public support for policies for active living in transportation (PAL-T) in a population-based sample of adults.

    Science.gov (United States)

    Fuller, Daniel; Gauvin, Lise; Fournier, Michel; Kestens, Yan; Daniel, Mark; Morency, Patrick; Drouin, Louis

    2012-04-01

    Active living is a broad conceptualization of physical activity that incorporates domains of exercise; recreational, household, and occupational activities; and active transportation. Policy makers develop and implement a variety of transportation policies that can influence choices about how to travel from one location to another. In making such decisions, policy makers act in part in response to public opinion or support for proposed policies. Measures of the public's support for policies aimed at promoting active transportation can inform researchers and policy makers. This study examined the internal consistency, and concurrent and discriminant validity of a newly developed measure of the public's support for policies for active living in transportation (PAL-T). A series of 17 items representing potential policies for promoting active transportation was generated. Two samples of participants (n = 2,001 and n = 2,502) from Montreal, Canada, were recruited via random digit dialling. Analyses were conducted on the combined data set (n = 4,503). Participants were aged 18 through 94 years (58% female). The concurrent and discriminant validity of the PAL-T was assessed by examining relationships with physical activity and smoking. To explore the usability of the PAL-T, predicted scale scores were compared to the summed values of responses. Results showed that the internal consistency of the PAL-T was 0.70. Multilevel regression demonstrated no relationship between the PAL-T and smoking status (p > 0.05) but significant relationships with utilitarian walking (p public opinion can inform policy makers and support advocacy efforts aimed at making built environments more suitable for active transportation while allowing researchers to examine the antecedents and consequences of public support for policies.

  8. Feasibility, internal consistency and covariates of TICS-m (telephone interview for cognitive status-modified) in a population-based sample: findings from the KORA-Age study.

    Science.gov (United States)

    Lacruz, Me; Emeny, Rt; Bickel, H; Linkohr, B; Ladwig, Kh

    2013-09-01

    Test the feasibility of the modified telephone interview for cognitive status (TICS-m) as a screening tool to detect cognitive impairment in a population-based sample of older subjects. Data were collected from 3,578 participants, age 65-94 years, of the KORA-Age study. We used analysis of covariance to test for significant sex, age and educational differences in raw TICS-m scores. Internal consistency was analysed by assessing Cronbach's alpha. Correction for education years was undertaken, and participants were divided in three subgroups following validated cut-offs. Finally, a logistic regression was performed to determine the impact of sex on cognition subgroups. Internal consistency of the TICS-m was 0.78. Study participants needed approximately 5.4 min to complete the interview. Lower raw TICS-m scores were associated with male sex, older age and lower education (all p education years, 2,851 (79%) had a non-impaired cognitive status (score >31). Male sex was independently associated with having a score equal to or below 27 and 31 (OR = 1.9, 95% CI 1.4-2.5 and OR = 1.5, 95% CI 1.2-1.7, respectively). The TICS-m is a feasible questionnaire for community-dwelling older adults with normal cognitive function or moderate cognitive impairment. Lower cognitive performance was associated with being a man, being older, and having fewer years of formal education. Copyright © 2012 John Wiley & Sons, Ltd.

  9. Extraction method based on emulsion breaking for the determination of Cu, Fe and Pb in Brazilian automotive gasoline samples by high-resolution continuum source flame atomic absorption spectrometry

    Science.gov (United States)

    Leite, Clarice C.; de Jesus, Alexandre; Kolling, Leandro; Ferrão, Marco F.; Samios, Dimitrios; Silva, Márcia M.

    2018-04-01

    This work reports a new method for extraction of Cu, Fe and Pb from Brazilian automotive gasoline and their determination by high-resolution continuous source flame atomic absorption spectrometry (HR-CS FAAS). The method was based on the formation of water-in-oil emulsion by mixing 2.0 mL of extraction solution constituted by 12% (w/v) Triton X-100 and 5% (v/v) HNO3 with 10 mL of sample. After heating at 90 °C for 10 min, two well-defined phases were formed. The bottom phase (approximately 3.5 mL), composed of acidified water and part of the ethanol originally present in the gasoline sample, containing the extracted analytes was analyzed. The surfactant and HNO3 concentrations and the heating temperature employed in the process were optimized by Doehlert design, using a Brazilian gasoline sample spiked with Cu, Fe and Pb (organometallic compounds). The efficiency of extraction was investigated and it ranged from 80 to 89%. The calibration was accomplished by using matrix matching method. For this, the standards were obtained performing the same extraction procedure used for the sample, using emulsions obtained with a gasoline sample free of analytes and the addition of inorganic standards. Limits of detection obtained were 3.0, 5.0 and 14.0 μg L-1 for Cu, Fe and Pb, respectively. These limits were estimated for the original sample taking into account the preconcentration factor obtained. The accuracy of the proposed method was assured by recovery tests spiking the samples with organometallic standards and the obtained values ranged from 98 to 105%. Ten gasoline samples were analyzed and Fe was found in four samples (0.04-0.35 mg L-1) while Cu (0.28 mg L-1) and Pb (0.60 mg L-1) was found in just one sample.

  10. Diurnal Variation and Spatial Distribution Effects on Sulfur Speciation in Aerosol Samples as Assessed by X-Ray Absorption Near-Edge Structure (XANES

    Directory of Open Access Journals (Sweden)

    Siwatt Pongpiachan

    2012-01-01

    Full Text Available This paper focuses on providing new results relating to the impacts of Diurnal variation, Vertical distribution, and Emission source on sulfur K-edge XANES spectrum of aerosol samples. All aerosol samples used in the diurnal variation experiment were preserved using anoxic preservation stainless cylinders (APSCs and pressure-controlled glove boxes (PCGBs, which were specially designed to prevent oxidation of the sulfur states in PM10. Further investigation of sulfur K-edge XANES spectra revealed that PM10 samples were dominated by S(VI, even when preserved in anoxic conditions. The “Emission source effect” on the sulfur oxidation state of PM10 was examined by comparing sulfur K-edge XANES spectra collected from various emission sources in southern Thailand, while “Vertical distribution effects” on the sulfur oxidation state of PM10 were made with samples collected from three different altitudes from rooftops of the highest buildings in three major cities in Thailand. The analytical results have demonstrated that neither “Emission source” nor “Vertical distribution” appreciably contribute to the characteristic fingerprint of sulfur K-edge XANES spectrum in PM10.

  11. Solid Phase Extraction of Trace Copper in Aqueous Samples Using C18 Membrane Disks Modified by Benzildithiosemicarbazone Prior to Flame Atomic Absorption Spectrometric (FAAS Determination

    Directory of Open Access Journals (Sweden)

    M. Mohammadhosseini

    2013-08-01

    Full Text Available A highly convenient, selective and sensitive procedure for pre-concentration, separation and determination of sub-ppm levels of Cu2+ in aqueous samples based on modification of octadecyl silica bonded phase membrane (OSBPM disks is described using benzildithiosemicarbazone  (BDSC as a powerful modifier. It was revealed that each loaded OSBPM disk with 6.0 mg of BDSC serves as excellent bead for trapping, enrichment and isolation of trace copper. The analyte was trapped during introduction the aqueous solutions through the surface of each modified membrane, quantitatively, while other interfering ions passed through the disk to drain. The adsorbed Cu2+ ions were then stripped by appropriate eluting agents followed by monitoring of the eluates by FAAS. The effects of sample pH, amount of the modifier, stripping agent types and sample flow-rates were also investigated. The described method permitted a pre-concentration factor of about 200. The detection limit of the procedure was predicted to be about 0.013 ng L-1. The method was successfully employed for recovery and quantification of trace copper in different water samples

  12. Speciation of arsenic in water samples by high-performance liquid chromatography-hydride generation-atomic absorption spectrometry at trace levels using a post-column reaction system

    Energy Technology Data Exchange (ETDEWEB)

    Stummeyer, J. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany); Harazim, B. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany); Wippermann, T. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany)

    1996-02-01

    Anion-exchange HPLC has been combined with hydride generation - atomic absorption spectrometry (HG-AAS) for the routine speciation of arsenite, arsenate, monomethylarsenic acid and dimethylarsinic acid. The sensitivity of the AAS-detection was increased by a post-column reaction system to achieve complete formation of volatile arsines from the methylated species and arsenate. The system allows the quantitative determination of 0.5 {mu}g/l of each arsenic compound in water samples. The stability of synthetical and natural water containing arsenic at trace levels was investigated. To preserve stored water samples, a method for quantitative separation of arsenate at high pH-values with the basic anion-exchange resin Dowex 1 x 8 was developed. (orig.)

  13. Consistent model driven architecture

    Science.gov (United States)

    Niepostyn, Stanisław J.

    2015-09-01

    The goal of the MDA is to produce software systems from abstract models in a way where human interaction is restricted to a minimum. These abstract models are based on the UML language. However, the semantics of UML models is defined in a natural language. Subsequently the verification of consistency of these diagrams is needed in order to identify errors in requirements at the early stage of the development process. The verification of consistency is difficult due to a semi-formal nature of UML diagrams. We propose automatic verification of consistency of the series of UML diagrams originating from abstract models implemented with our consistency rules. This Consistent Model Driven Architecture approach enables us to generate automatically complete workflow applications from consistent and complete models developed from abstract models (e.g. Business Context Diagram). Therefore, our method can be used to check practicability (feasibility) of software architecture models.

  14. Bitcoin Meets Strong Consistency

    OpenAIRE

    Decker, Christian; Seidel, Jochen; Wattenhofer, Roger

    2014-01-01

    The Bitcoin system only provides eventual consistency. For everyday life, the time to confirm a Bitcoin transaction is prohibitively slow. In this paper we propose a new system, built on the Bitcoin blockchain, which enables strong consistency. Our system, PeerCensus, acts as a certification authority, manages peer identities in a peer-to-peer network, and ultimately enhances Bitcoin and similar systems with strong consistency. Our extensive analysis shows that PeerCensus is in a secure state...

  15. Lead ultra-trace on-line preconcentration and determination using selective solid phase extraction and electrothermal atomic absorption spectrometry: applications in seawaters and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Vereda Alonso, E.; Siles Cordero, M.T.; Garcia de Torres, A.; Cano Pavon, J.M. [University of Malaga, Department of Analytical Chemistry Faculty of Sciences, Malaga (Spain)

    2006-08-15

    In this work, a new chelating resin [1,5-bis (2-pyridyl)-3-sulphophenyl methylene] thiocarbonohydrazide immobilised on aminopropyl-controlled pore glass (550 Aa; PSTH-cpg) was synthesised and packed in a microcolumn which replaced the sample tip of the autosampler arm. The system was applied to the preconcentration of lead. When microliters of 10% HNO{sub 3}, which acts as elution agent, pass through the microcolumn, the preconcentrated Pb(II) is eluted and directly deposited in a tungsten-rhodium coated graphite tube. With the use of the separation and preconcentration step and the permanent modifiers, the analytical characteristics of the technique were improved. The proposed method has a linear calibration range from 0.012 to 10 ng ml{sup -1} of lead. At a sample frequency of 36 h{sup -1} with a 90 s preconcentration time, the enrichment factor was 20.5, the detection and determination limits were 0.012 and 0.14 ng ml{sup -1}, respectively and the precision, expressed as relative standard deviation, was 3.2% (at 1 ng ml{sup -1}). Results from the determination of Pb in biological certified reference materials were in agreement with the certified values. Seawaters and other biological samples were analysed too. (orig.)

  16. Consistent classical supergravity theories

    International Nuclear Information System (INIS)

    Muller, M.

    1989-01-01

    This book offers a presentation of both conformal and Poincare supergravity. The consistent four-dimensional supergravity theories are classified. The formulae needed for further modelling are included

  17. Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

    Science.gov (United States)

    Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

    2018-05-01

    In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

  18. Development of Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop for the Sensitive Determination of Trace Copper in Water and Beverage Samples by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Wu, Chunxia; Zhao, Bin; Li, Yingli; Wu, Qiuhua; Wang, Chun; Wang, Zhi

    2011-01-01

    A dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) has been developed as a new approach for the extraction of trace copper in water and beverage samples followed by the determination with flame atomic absorption spectrometry. In the DLLME-SFO, 8-hydroxy quinoline, 1-dodecanol, and methanol were used as chelating agent, extraction solvent and dispersive solvent, respectively. The experimental parameters related to the DLLME-SFO such as the type and volume of the extraction and dispersive solvent, extraction time, sample volume, the concentration of chelating agent and salt addition were investigated and optimized. Under the optimum conditions, the enrichment factor for copper was 122. The method was linear in the range from 0.5 to 300 ng mL -1 of copper in the samples with a correlation coefficient (r) of 0.9996 and a limit of detection of 0.1 ng mL -1 . The method was applied to the determination of copper in water and beverage samples. The recoveries for the spiked water and beverage samples at the copper concentration levels of 5.0 and 10.0 ng mL -1 were in the range between 92.0% and 108.0%. The relative standard deviations (RSD) varied from 3.0% to 5.6%

  19. Consistency of orthodox gravity

    Energy Technology Data Exchange (ETDEWEB)

    Bellucci, S. [INFN, Frascati (Italy). Laboratori Nazionali di Frascati; Shiekh, A. [International Centre for Theoretical Physics, Trieste (Italy)

    1997-01-01

    A recent proposal for quantizing gravity is investigated for self consistency. The existence of a fixed-point all-order solution is found, corresponding to a consistent quantum gravity. A criterion to unify couplings is suggested, by invoking an application of their argument to more complex systems.

  20. Quasiparticles and thermodynamical consistency

    International Nuclear Information System (INIS)

    Shanenko, A.A.; Biro, T.S.; Toneev, V.D.

    2003-01-01

    A brief and simple introduction into the problem of the thermodynamical consistency is given. The thermodynamical consistency relations, which should be taken into account under constructing a quasiparticle model, are found in a general manner from the finite-temperature extension of the Hellmann-Feynman theorem. Restrictions following from these relations are illustrated by simple physical examples. (author)

  1. Análise direta de sólidos por espectrometria de absorção atômica com atomização em forno de grafite: uma revisão Solid sampling graphite furnace atomic absorption spectrometry: a review

    Directory of Open Access Journals (Sweden)

    Cassiana Seimi Nomura

    2008-01-01

    Full Text Available This is a review of direct analysis using solid sampling graphite furnace atomic absorption spectrometry. Greater emphasis is dedicated to sample preparation, sample homogeneity, calibration and its application to microanalysis and micro-homogeneity studies. The main advantages and some difficulties related to the applicability of this technique are discussed. A literature search on the application of solid sampling graphite furnace atomic absorption spectrometry in trace element determination in many kinds of samples, including biological, clinical, technological and environmental ones, is also presented.

  2. Monitoring of trace amounts of heavy metals in different food and water samples by flame atomic absorption spectrophotometer after preconcentration by amine-functionalized graphene nanosheet.

    Science.gov (United States)

    Behbahani, Mohammad; Tapeh, Nasim Akbari Ghareh; Mahyari, Mojtaba; Pourali, Ali Reza; Amin, Bahareh Golrokh; Shaabani, Ahmad

    2014-11-01

    We are introducing graphene oxide modified with amine groups as a new solid phase for extraction of heavy metal ions including cadmium(II), copper(II), nickel(II), zinc(II), and lead(II). Effects of pH value, flow rates, type, concentration, and volume of the eluent, breakthrough volume, and the effect of potentially interfering ions were studied. Under optimized conditions, the extraction efficiency is >97 %, the limit of detections are 0.03, 0.05, 0.2, 0.1, and 1 μg L(-1) for the ions of cadmium, copper, nickel, zinc, and lead, respectively, and the adsorption capacities for these ions are 178, 142, 110, 125, and 210 mg g(-1). The amino-functionalized graphene oxide was characterized by thermogravimetric analysis, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared spectrometry. The proposed method was successfully applied in the analysis of environmental water and food samples. Good spiked recoveries over the range of 95.8-100.0 % were obtained. This work not only proposes a useful method for sample preconcentration but also reveals the great potential of modified graphene as an excellent sorbent material in analytical processes.

  3. Ion imprinted activated carbon solid-phase extraction coupled to flame atomic absorption spectrometry for selective determination of lead ions in environmental samples

    International Nuclear Information System (INIS)

    Naraghi, Kiyana; Panahi, Homayon Ahmad; Hassani, Amir Hesam; Moniri, Elham

    2014-01-01

    A simple lead ion imprinted sorbent was synthesized by coupling activated carbon with a known metal chelating compound, iminodiacetic acid. The ion imprinted sorbent has been characterized using Fourier transform infrared spectroscopy, elemental analysis and thermogravimetric analysis and subjected for the extraction and determination of trace Pb(II) in environmental water samples. The optimum pH value for sorption of the lead ion was 6.5. The sorption capacity of lead imprinted sorbent was 42.2 mg g"−"1. The chelating imprinted sorbent can be reused for five cycles of sorption-desorption without any significant change in sorption capacity. Compared with non-imprinted polymer particles, the lead ion imprinted sorbent showed high adsorption capacity, significant selectivity, good site accessibility for Pb(II). The equilibrium adsorption data of Pb(II) by modified resin were analyzed by Langmuir, Freundlich, Temkin and Redlich-Peterson models

  4. Dispersive liquid-liquid microextraction for the simultaneous separation of trace amounts of zinc and cadmium ions in water samples prior to flame atomic absorption spectrometry determination

    Directory of Open Access Journals (Sweden)

    Sayed Zia Mohammadi

    2012-01-01

    Full Text Available In the proposed method, carbon tetrachloride and ethanol were used as extraction and dispersive solvents. Several factors that may be affected on the extraction process, such as extraction solvent, disperser solvent, the volume of extraction and disperser solvent, pH of the aqueous solution and extraction time were optimized. Under the optimal conditions, linearity was maintained between 1.0 ng mL-1 to 1.5 mg mL-1 for zinc and 1.0 ng mL-1 to 0.4 mg mL-1 for cadmium. The proposed method has been applied for determination of trace amount of zinc and cadmium in standard and water samples with satisfactory results.

  5. Ion imprinted activated carbon solid-phase extraction coupled to flame atomic absorption spectrometry for selective determination of lead ions in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Naraghi, Kiyana; Panahi, Homayon Ahmad; Hassani, Amir Hesam [Islamic Azad University, Tehran (Korea, Republic of); Moniri, Elham [Islamic Azad University, Varamin (Iran, Islamic Republic of)

    2014-10-15

    A simple lead ion imprinted sorbent was synthesized by coupling activated carbon with a known metal chelating compound, iminodiacetic acid. The ion imprinted sorbent has been characterized using Fourier transform infrared spectroscopy, elemental analysis and thermogravimetric analysis and subjected for the extraction and determination of trace Pb(II) in environmental water samples. The optimum pH value for sorption of the lead ion was 6.5. The sorption capacity of lead imprinted sorbent was 42.2 mg g{sup −1}. The chelating imprinted sorbent can be reused for five cycles of sorption-desorption without any significant change in sorption capacity. Compared with non-imprinted polymer particles, the lead ion imprinted sorbent showed high adsorption capacity, significant selectivity, good site accessibility for Pb(II). The equilibrium adsorption data of Pb(II) by modified resin were analyzed by Langmuir, Freundlich, Temkin and Redlich-Peterson models.

  6. Analysis Of Non-Volatile Toxic Heavy Metals (Cd, Pb, Cu,Cr And Zn In ALLIUM SATIVUM (Garlic And Soil Samples ,Collected From Different Locations Of Punjab, Pakistan By Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    Ata S.

    2013-04-01

    Full Text Available Garlic is one of the most widely used medicinal plants. The monitoring of toxic metals such as lead, Cadmium, Chromium, Copper and Zinc in garlic and the soil of garlic fields collected from ten different cities of Punjab is critical for preventing public health against the hazards of metal toxicity. The levels of toxic heavy metals in garlic and soil samples were investigated using Atomic absorption spectrometer. The metal content in garlic samples was found to be in increasing order as Cr> Pb> Cd> Cu> Zn. Infield metal content in the soil also followed the same trend. In garlic samples, Pb, Cd, Cr, Zn and Cu ranged from 0.039mg/L to 0.757mg/L, N.D to 1.211mg/L, 0.03mg/L to 0.451mg/L, 0.02mg/Lto0.42mg/L and 0.451mg/L to 0.893mg/L respectively. In soil samples, Pb, Cd, Cr, Zn and Cu were ranged from 0.459mg/L to 0.797mg/L, 0.205mg/L to1.062mg/L, 0.074mg/L to 2.598mg/L, 0.124mg/L to 0.276mg/L and 0.494mg/L to 0.921mg/L respectively. In our study, the Pb and Cd was found more in garlic from Gujranwala and Jaranwala, Cu and Zn were more in samples from Kasur while Cr was predominant in sample from Sheikhupura. Heavy metal content in soil and garlic samples was within the permissible limits proposed by World Health Organization (WHO.

  7. Flame atomic absorption spectrometric determination of trace amounts of Pb(II) and Cr(III) in biological, food and environmental samples after preconcentration by modified nano-alumina

    International Nuclear Information System (INIS)

    Afkhami, A.; Madrakian, T.; Saber-Tehrani, M.; Bagheri, H.

    2011-01-01

    A new solid-phase extraction sorbent was used for the preconcentration of Pb(II) and Cr(III) ions prior to their determination by flame atomic absorption spectrometry. It was prepared by immobilization of 2,4-dinitrophenylhydrazine on nano-alumina coated with sodium dodecyl sulfate. The sorbent was characterized by scanning electron microscopy, N 2 adsorption and Fourier transform infrared spectrometry, and used for preconcentration and separation of Pb(II) and Cr(III) from aqueous solutions. The ions on the sorbent were eluted with a mixture of nitric acid and methanol. The effects of sample pH, flow rates of samples and eluent, type of eluent, breakthrough volume and potentially interfering ions were studied. Linearity is maintained between 1.2 and 350 μg L -1 of Pb(II), and between 2.4 and 520 μg L -1 of Cr(III) for an 800-mL sample. The detection limit (3 s, N=10) for Pb(II) and Cr(III) ions is 0.43 and 0.55 μg L -1 , respectively, and the maximum preconcentration factor is 267. The method was successfully applied to the evaluation of these trace and toxic metals in various water, food, industrial effluent and urine samples. (author)

  8. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Science.gov (United States)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  9. Subgap absorption in conjugated polymers

    Energy Technology Data Exchange (ETDEWEB)

    Sinclair, M.; Seager, C.H. (Sandia National Labs., Albuquerque, NM (USA)); McBranch, D.; Heeger, A.J. (California Univ., Santa Barbara, CA (USA)); Baker, G.L. (Bell Communications Research, Inc., Red Bank, NJ (USA))

    1991-01-01

    Along with X{sup (3)}, the magnitude of the optical absorption in the transparent window below the principal absorption edge is an important parameter which will ultimately determine the utility of conjugated polymers in active integrated optical devices. With an absorptance sensitivity of < 10{sup {minus}5}, Photothermal Deflection Spectroscopy (PDS) is ideal for determining the absorption coefficients of thin films of transparent'' materials. We have used PDS to measure the optical absorption spectra of the conjugated polymers poly(1,4-phenylene-vinylene) (and derivitives) and polydiacetylene-4BCMU in the spectral region from 0.55 eV to 3 eV. Our spectra show that the shape of the absorption edge varies considerably from polymer to polymer, with polydiacetylene-4BCMU having the steepest absorption edge. The minimum absorption coefficients measured varied somewhat with sample age and quality, but were typically in the range 1 cm{sup {minus}1} to 10 cm{sup {minus}1}. In the region below 1 eV, overtones of C-H stretching modes were observed, indicating that further improvements in transparency in this spectral region might be achieved via deuteration of fluorination. 11 refs., 4 figs.

  10. Emulsification based dispersive liquid microextraction prior to flame atomic absorption spectrometry for the sensitive determination of Cd(II) in water samples

    International Nuclear Information System (INIS)

    Rahimi-Nasrabadi, Mehdi; Banan, Alireza; Zahedi, Mir Mahdi; Pourmortazavi, Seied Mahdi; Nazari, Zakieh; Asghari, Alireza

    2013-01-01

    We report on the application of emulsification-based dispersive liquid micro extraction (EB-DLME) to the preconcentration of Cd(II). This procedure not only possesses all the advantages of routine DLLME, but also results in a more stable cloudy state which is particularly useful when coupling it to FAAS. In EB-DLME, appropriate amounts of the extraction solvent (a solution of dithizone in chloroform) and an aqueous solution of sodium dodecyl sulfate (SDS; acting as a disperser) are injected into the samples. A stable cloudy microemulsion is formed and Cd(II) ion is extracted by chelation. After phase separation, the sedimented phase is subjected to FAAS. Under optimized conditions, the calibration curve for Cd(II) is linear in the range from 0.1 to 25 μg L −1 , the limit of detection (at S/N = 3) is 30 pg L −1 , the relative standard deviations for seven replicate analyses (at 0.56 μg L −1 of Cd(II)) is 4.6 %, and the enrichment factor is 151. EB-DLME in our opinion is a simple, efficient and rapid method for the preconcentration of Cd(II) (and most likely of many other ions) prior to FAAS determination. (author)

  11. Atomic absorption spectrophotometer

    International Nuclear Information System (INIS)

    Stockdale, T. J.

    1985-01-01

    In atomic absorption spectrophotometer, a reference path may be provided for radiation which excludes the flame. This radiation provides a signal from a detector which varies only with the instrumental drift produced by variations in the radiation source brightness and by variations in detector gain. The signal can be used to compensate for drift in other signals received through a sample path including the flame. In the present invention, radiation passes through the sample path continuously during measurement, and only through the reference path between sample measurements. Movable mirrors shift the radiation between the paths upon externally applied commands. Conveniently, the reference path measurement is made while the flame is stabilized during the change between samples. The reference path measurements are stored and used to correct for drift

  12. On-line preconcentration using a resin functionalized with 3,4-dihydroxybenzoic acid for the determination of trace elements in biological samples by thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Lemos, Valfredo A.; Bezerra, Marcos A.; Amorim, Fabio A.C.

    2008-01-01

    In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with 3,4-dihydroxybenzoic acid (XAD4-DHB) packed in a minicolumn was used as sorbent material. The metals were retained on the XAD-DHB resin, from which it could be eluted directly to the thermospray flame furnace system. The detection limits were 28 (Cd), 100 (Cu) and 77 ng L -1 (Zn) for 60 s preconcentration time, at a sample flow rate of 7.0 mL min -1 . Enrichment factors were 102, 91 and 62, for cadmium, copper and zinc, respectively. The procedure has been applied successfully to metal determination in biological standard reference materials

  13. Consistency between GRUAN sondes, LBLRTM and IASI

    Directory of Open Access Journals (Sweden)

    X. Calbet

    2017-06-01

    Full Text Available Radiosonde soundings from the GCOS Reference Upper-Air Network (GRUAN data record are shown to be consistent with Infrared Atmospheric Sounding Instrument (IASI-measured radiances via LBLRTM (Line-By-Line Radiative Transfer Model in the part of the spectrum that is mostly affected by water vapour absorption in the upper troposphere (from 700 hPa up. This result is key for climate data records, since GRUAN, IASI and LBLRTM constitute reference measurements or a reference radiative transfer model in each of their fields. This is specially the case for night-time radiosonde measurements. Although the sample size is small (16 cases, daytime GRUAN radiosonde measurements seem to have a small dry bias of 2.5 % in absolute terms of relative humidity, located mainly in the upper troposphere, with respect to LBLRTM and IASI. Full metrological closure is not yet possible and will not be until collocation uncertainties are better characterized and a full uncertainty covariance matrix is clarified for GRUAN.

  14. Near-infrared free carrier absorption in heavily doped silicon

    International Nuclear Information System (INIS)

    Baker-Finch, Simeon C.; McIntosh, Keith R.; Yan, Di; Fong, Kean Chern; Kho, Teng C.

    2014-01-01

    Free carrier absorption in heavily doped silicon can have a significant impact on devices operating in the infrared. In the near infrared, the free carrier absorption process can compete with band to band absorption processes, thereby reducing the number of available photons to optoelectronic devices such as solar cells. In this work, we fabricate 18 heavily doped regions by phosphorus and boron diffusion into planar polished silicon wafers; the simple sample structure facilitates accurate and precise measurement of the free carrier absorptance. We measure and model reflectance and transmittance dispersion to arrive at a parameterisation for the free carrier absorption coefficient that applies in the wavelength range between 1000 and 1500 nm, and the range of dopant densities between ∼10 18 and 3 × 10 20  cm −3 . Our measurements indicate that previously published parameterisations underestimate the free carrier absorptance in phosphorus diffusions. On the other hand, published parameterisations are generally consistent with our measurements and model for boron diffusions. Our new model is the first to be assigned uncertainty and is well-suited to routine device analysis

  15. Cloud point extraction of copper, lead, cadmium, and iron using 2,6-diamino-4-phenyl-1,3,5-triazine and nonionic surfactant, and their flame atomic absorption spectrometric determination in water and canned food samples.

    Science.gov (United States)

    Citak, Demirhan; Tuzen, Mustafa

    2012-01-01

    A cloud point extraction procedure was optimized for the separation and preconcentration of lead(II), cadmium(II), copper(II), and iron(III) ions in various water and canned food samples. The metal ions formed complexes with 2,6-diamino-4-phenyl-1,3,5-triazine that were extracted by surfactant-rich phases in the nonionic surfactant Triton X-114. The surfactant-rich phase was diluted with 1 M HNO3 in methanol prior to its analysis by flame atomic absorption spectrometry. The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, surfactant concentration, temperature, and incubation time, were optimized. LOD values based on three times the SD of the blank (3Sb) were 0.38, 0.48, 1.33, and 1.85 microg/L for cadmium(II), copper(II), lead(II), and iron(III) ions, respectively. The precision (RSD) of the method was in the 1.86-3.06% range (n=7). Validation of the procedure was carried out by analysis of National Institute of Standards and Technology Standard Reference Material (NIST-SRM) 1568a Rice Flour and GBW 07605 Tea. The method was applied to water and canned food samples for determination of metal ions.

  16. Solid-phase extraction of copper(II) in water and food samples using silica gel modified with bis(3-aminopropyl)amine and determination by flame atomic absorption spectrometry.

    Science.gov (United States)

    Cagirdi, Duygu; Altundag, Hüseyin; Imamoglu, Mustafa; Tuzen, Mustafa

    2014-01-01

    A simple and selective separation and preconcentration method was developed for the determination of Cu(ll) ions. This method is based on adsorption of Cu(ll) ions from aqueous solution on a bis(3-aminopropyl)amine modified silica gel column and flame atomic absorption spectrometric determination after desorption. Various analytical parameters such as pH, type of eluent solution and its volume, flow rate of sample and eluent, and sample volume were optimized. Effects of some cation, anion, and transition metal ions on the recoveries of Cu(ll) ions were also investigated. Cu(ll) ions were quantitatively recovered at pH 6; 5.0 mL of 2 M HCI was used as the eluent. The preconcentration factor was found to be 150. The LOD was 0.12 microg/L for Cu(ll). The accuracy of the method was confirmed by analysis of Tea Leaves (INCT-TL-1) and Fish Protein (DORM-3) certified reference materials. The optimized method was applied to various water and food samples for the determination of Cu(ll).

  17. Modified Activated Carbon Prepared from Acorn Shells as a New Solid-Phase Extraction Sorbent for the Preconcentration and Determination of Trace Amounts of Nickel in Food Samples Prior to Flame Atomic Absorption Spectrometry.

    Science.gov (United States)

    Ebrahimi, Bahram

    2017-03-01

    A new solid-phase extraction (SPE) sorbent was introduced based on acidic-modified (AM) activated carbon (AC) prepared from acorn shells of native oak trees in Kurdistan. Hydrochloric acid (15%, w/w) and nitric acid (32.5%, w/w) were used to condition and modify AC. The IR spectra of AC and AM-AC showed that AM lead to the formation of increasing numbers of acidic functional groups on AM-AC. AM-AC was used in the SPE method for the extraction and preconcentration of Ni+2 prior to flame atomic absorption spectrometric determination at ng/mL levels in model and real food samples. Effective parameters of the SPE procedure, such as the pH of the solutions, sorbent dosage, extraction time, sample volume, type of eluent, and matrix ions, were considered and optimized. An enrichment factor of 140 was obtained. The calibration curve was linear with an R2 of 0.997 in the concentration range of 1-220 ng/mL. The RSD was 5.67% (for n = 7), the LOD was 0.352 ng/mL, and relative recoveries in vegetable samples ranged from 96.7 to 103.7%.

  18. Speciation of Tl(III and Tl(I in hair samples by dispersive liquid–liquid microextraction based on solidification of floating organic droplet prior to flame atomic absorption spectrometry determination

    Directory of Open Access Journals (Sweden)

    S.Z. Mohammadi

    2016-11-01

    Full Text Available Dispersive liquid–liquid microextraction based on solidification of floating organic droplet was successfully used as a sample preparation method prior to flame atomic absorption determination of trace amounts of Tl(III and Tl(I in hair samples. In the proposed method, 1-(2-pyridylazo-2-naphthol, 1-dodecanol and ethanol were used as chelating agent, extraction and dispersive solvent, respectively. Several factors that may be affected in the extraction process, such as type and volume of extraction and disperser solvents, pH, salting out effect, ionic strength and extraction time were studied. Under the optimal conditions, linearity was maintained between 6.0 and 900.0 ng mL−1 for Tl(III. The relative standard deviation for seven replicate determinations of 0.2 μg mL−1 Tl(III was 2.5%. The detection limit based on 3Sb for Tl(III in the original solution was 2.1 ng mL−1. The proposed method has been applied for the determination of trace amounts of thallium in hair samples and satisfactory results were obtained.

  19. Air-assisted Liquid Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry for Preconcentration and Determination of Trace Amount of Co(II and Ni(II Ions in Water Samples

    Directory of Open Access Journals (Sweden)

    Saeed Mohammad Sorouraddin

    2017-12-01

    Full Text Available A simple, rapid and efficient method has been developed for the extraction, preconcentration and determination of cobalt (II and nickel (II ions in water samples by air-assisted liquid-liquid microextraction (AALLME coupled with graphite furnace atomic absorption spectrometry (GFAAS. In the proposed method, much less volume of an organic solvent was used as the extraction solvent in the absence of disperser solvent. Fine organic droplets were formed by sucking and injecting of the mixture of aqueous sample solution and extraction solvent with a syringe for several times in a conical test tube. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by GFAAS. Several variables that could affect the extraction efficiency were investigated and optimized. Calibration graphs were linear in the range of 6.5-100 ng L-1. Detection limits for Co and Ni were 2.3 ng L-1 and 3 ng L-1, respectively. The accuracy of the developed procedure was checked by analyzing NRCC-SLRS4 Riverine water as a certified reference material. Finally, the proposed method has been successfully applied for the determination of cobalt (II and nickel (II ions in tap, surface and river water samples.

  20. Consistency in PERT problems

    OpenAIRE

    Bergantiños, Gustavo; Valencia-Toledo, Alfredo; Vidal-Puga, Juan

    2016-01-01

    The program evaluation review technique (PERT) is a tool used to schedule and coordinate activities in a complex project. In assigning the cost of a potential delay, we characterize the Shapley rule as the only rule that satisfies consistency and other desirable properties.

  1. Two-dimensional thermometry by using neutron resonance absorption spectrometer DOG

    International Nuclear Information System (INIS)

    Kamiyama, T.; Noda, H.; Kiyanagi, Y.; Ikeda, S.

    2001-01-01

    We applied the neutron resonance absorption spectroscopy to thermometry of a bulk object. The measurement was done by using the neutron resonance absorption spectrometer, DOG, installed at KENS, High Energy Accelerator Research Organization Neutron Source, which enables us to investigate effective temperature of a particular element by analyzing line width of resonance absorption spectrum. The effective temperature becomes consistence with the sample temperature above room temperature. For the analysis we applied the computed tomography method to reconstruct the temperature distribution on the object cross section. The results and the calculated distribution by the heat conducting equation are well agreed on the temperature difference inside the object. (author)

  2. Reporting consistently on CSR

    DEFF Research Database (Denmark)

    Thomsen, Christa; Nielsen, Anne Ellerup

    2006-01-01

    This chapter first outlines theory and literature on CSR and Stakeholder Relations focusing on the different perspectives and the contextual and dynamic character of the CSR concept. CSR reporting challenges are discussed and a model of analysis is proposed. Next, our paper presents the results...... of a case study showing that companies use different and not necessarily consistent strategies for reporting on CSR. Finally, the implications for managerial practice are discussed. The chapter concludes by highlighting the value and awareness of the discourse and the discourse types adopted...... in the reporting material. By implementing consistent discourse strategies that interact according to a well-defined pattern or order, it is possible to communicate a strong social commitment on the one hand, and to take into consideration the expectations of the shareholders and the other stakeholders...

  3. Geometrically Consistent Mesh Modification

    KAUST Repository

    Bonito, A.

    2010-01-01

    A new paradigm of adaptivity is to execute refinement, coarsening, and smoothing of meshes on manifolds with incomplete information about their geometry and yet preserve position and curvature accuracy. We refer to this collectively as geometrically consistent (GC) mesh modification. We discuss the concept of discrete GC, show the failure of naive approaches, and propose and analyze a simple algorithm that is GC and accuracy preserving. © 2010 Society for Industrial and Applied Mathematics.

  4. Subgap Absorption in Conjugated Polymers

    Science.gov (United States)

    Sinclair, M.; Seager, C. H.; McBranch, D.; Heeger, A. J; Baker, G. L.

    1991-01-01

    Along with X{sup (3)}, the magnitude of the optical absorption in the transparent window below the principal absorption edge is an important parameter which will ultimately determine the utility of conjugated polymers in active integrated optical devices. With an absorptance sensitivity of materials. We have used PDS to measure the optical absorption spectra of the conjugated polymers poly(1,4-phenylene-vinylene) (and derivitives) and polydiacetylene-4BCMU in the spectral region from 0.55 eV to 3 eV. Our spectra show that the shape of the absorption edge varies considerably from polymer to polymer, with polydiacetylene-4BCMU having the steepest absorption edge. The minimum absorption coefficients measured varied somewhat with sample age and quality, but were typically in the range 1 cm{sup {minus}1} to 10 cm{sup {minus}1}. In the region below 1 eV, overtones of C-H stretching modes were observed, indicating that further improvements in transparency in this spectral region might be achieved via deuteration of fluorination.

  5. Anomalous infrared absorption in granular superconductors

    International Nuclear Information System (INIS)

    Carr, G.L.; Garland, J.C.; Tanner, D.B.

    1983-01-01

    Granular superconductors are shown to have a far-infrared absorption that is larger when the samples are superconducting than when they are normal. By constrast, theoretical models for these materials predict that when the samples become superconducting, the absorption should decrease

  6. A photo-oxidation procedure using UV radiation/H{sub 2}O{sub 2} for decomposition of wine samples - Determination of iron and manganese content by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Walter N.L. dos [Departamento de Ciencias Exatas e da Terra, Universidade do Estado da Bahia, Salvador, Bahia (Brazil); Universidade Federal da Bahia, Instituto de Quimica, Campus Ondina, Salvador, Bahia, 40170-290 Brazil (Brazil)], E-mail: wlopes@uneb.br; Brandao, Geovani C.; Portugal, Lindomar A.; David, Jorge M.; Ferreira, Sergio L.C. [Universidade Federal da Bahia, Instituto de Quimica, Campus Ondina, Salvador, Bahia, 40170-290 Brazil (Brazil)

    2009-06-15

    This paper proposes the use of photo-oxidation with UV radiation/H{sub 2}O{sub 2} as sample pretreatment for the determination of iron and manganese in wines by flame atomic absorption spectrometry (FAAS). The optimization involved the study of the following variables: pH and concentration of buffer solution, concentrated hydrogen peroxide volume and irradiation time. The evaluation of sample degradation was monitored by measuring the absorbance at the maximum wavelength of red wine (530 nm). Using the experimental conditions established during the optimization (irradiation time of 30 min, oxidant volume of 2.5 mL, pH 10, and a buffer concentration of 0.15 mol L{sup - 1}), this procedure allows the determination of iron and manganese with limits of detection of 30 and 22 {mu}g L{sup - 1}, respectively, for a 5 mL volume of digested sample. The precision levels, expressed as relative standard deviation (RSD), were 2.8% and 0.65% for iron and 2.7% and 0.54% for manganese for concentrations of 0.5 and 2.0 mg L{sup - 1}, respectively. Addition/recovery tests for evaluation of the accuracy were in the ranges of 90%-111% and 95%-107% for iron and manganese, respectively. This digestion procedure has been applied for the determination of iron and manganese in six wine samples. The concentrations varied from 1.58 to 2.77 mg L{sup - 1} for iron and from 1.30 to 1.91 mg L{sup - 1} for manganese. The results were compared with those obtained by an acid digestion procedure and determination of the elements by FAAS. There was no significant difference between the results obtained by the two methods based on a paired t-test (at 95% confidence level)

  7. The Rucio Consistency Service

    CERN Document Server

    Serfon, Cedric; The ATLAS collaboration

    2016-01-01

    One of the biggest challenge with Large scale data management system is to ensure the consistency between the global file catalog and what is physically on all storage elements. To tackle this issue, the Rucio software which is used by the ATLAS Distributed Data Management system has been extended to automatically handle lost or unregistered files (aka Dark Data). This system automatically detects these inconsistencies and take actions like recovery or deletion of unneeded files in a central manner. In this talk, we will present this system, explain the internals and give some results.

  8. Use of Doehlert and constrained mixture designs in the development of a photo-oxidation procedure using UV radiation/H2O2 for decomposition of landfill leachate samples and determination of metals by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Marcos A. Bezerra

    2015-03-01

    Full Text Available This work proposes the use of photo-oxidation degradation with UV radiation/H2O2 as sample treatment for the determination of Fe, Zn, Mn, Ni and Co in municipal solid waste landfill leachate by flame atomic absorption spectrometry (FAAS. Three variables (pH, irradiation time and buffer concentration were optimized using Doehlert design and the proportions of mixture components submitted to UV radiation (leachate sample, buffer solution and H2O2 30%, v/v were optimized using a constrained mixture design. Using the experimental conditions established, this procedure allows limits of detection of 0.075, 0.025, 0.010, 0.075 and 0.041 µg mL-1, and the precision levels expressed as relative standard (%RSD, 0.5 µg mL-1 were 3.6, 1.8, 1.3, 3.3 and 1.7%, for Fe, Mn, Zn, Ni and Co respectively. Recovery tests were carried out for evaluation of the procedure accuracy and recoveries were between 92 and 106% for the studied metals. This procedure has been applied for the analysis of the landfill leachate collected in Jequié, a city of the southwestern region of the State of Bahia, Brazil. The results were compared with those obtained by acid digestion. There was no significant difference between the results obtained by the two methods based on paired t-test at 95% confidence level.

  9. Ligandless surfactant mediated solid phase extraction combined with Fe₃O₄ nano-particle for the preconcentration and determination of cadmium and lead in water and soil samples followed by flame atomic absorption spectrometry: multivariate strategy.

    Science.gov (United States)

    Jalbani, N; Soylak, M

    2014-04-01

    In the present study, a microextraction technique combining Fe3O4 nano-particle with surfactant mediated solid phase extraction ((SM-SPE)) was successfully developed for the preconcentration/separation of Cd(II) and Pb(II) in water and soil samples. The analytes were determined by flame atomic absorption spectrometry (FAAS). The effective variables such as the amount of adsorbent (NPs), the pH, concentration of non-ionic (TX-114) and centrifugation time (min) were investigated by Plackett-Burman (PBD) design. The important variables were further optimized by central composite design (CCD). Under the optimized conditions, the detection limits (LODs) of Cd(II) and Pb(II) were 0.15 and 0.74 µg/L, respectively. The validation of the proposed procedure was checked by the analysis of certified reference materials of TMDA 53.3 fortified water and GBW07425 soil. The method was successfully applied for the determination of Cd(II) and Pb(II) in water and soil samples. Copyright © 2014 Elsevier Inc. All rights reserved.

  10. Synthesis and application of a nanoporous ion-imprinted polymer for the separation and preconcentration of trace amounts of vanadium from food samples before determination by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Dehghanpoor Frashah, Shahab

    2016-04-01

    A vanadium ion-imprinted polymer was synthesized in the presence of V(V) and N-benzoyl-N-phenyl hydroxyl amine using 4-vinyl pyridine as the monomer, ethylene glycol dimethacrylate as the cross linker and 2,2'-azobis(isobutyronitrile) as the initiator. The imprinted V(V) ions were completely removed by leaching the polymer with 5 mol/L nitric acid, and the polymer structure was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The ion-imprinted polymer was used as the sorbent in the development of the solid-phase extraction method for V(V) prior to its determination by electrothermal atomic absorption spectrometry. The maximum sorption capacity for V(V) ions was 26.7 mg/g at pH 4.0. Under the optimum conditions, for a sample volume of 150.0 mL, an enrichment factor of 289.0 and a detection limit of 6.4 ng/L were obtained. The developed method was successfully applied to the determination of vanadium in parsley, zucchini, black tea, rice, and water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. A highly selective and sensitive ultrasonic assisted dispersive liquid phase microextraction based on deep eutectic solvent for determination of cadmium in food and water samples prior to electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Zounr, Rizwan Ali; Tuzen, Mustafa; Deligonul, Nihal; Khuhawar, Muhammad Yar

    2018-07-01

    A simple, fast, green, sensitive and selective ultrasonic assisted deep eutectic solvent liquid-phase microextraction technique was used for preconcentration and extraction of cadmium (Cd) in water and food samples by electrothermal atomic absorption spectrometry (ETAAS). In this technique, a synthesized reagent (Z)-N-(3,5-diphenyl-1H-pyrrol-2-yl)-3,5-diphenyl-2H-pyrrol-2-imine (Azo) was used as a complexing agent for Cd. The main factors effecting the pre-concentration and extraction of Cd such as effect of pH, type and composition of deep eutectic solvent (DES), volume of DES, volume of complexing agent, volume of tetrahydrofuran (THF) and ultrasonication time have been examined in detail. At optimum conditions the value of pH and molar ratio of DES were found to be 6.0 and 1:4 (ChCl:Ph), respectively. The detection limit (LOD), limit of quantification (LOQ), relative standard deviation (RSD) and preconcentration factor (PF) were observed as 0.023 ng L -1 , 0.161 ng L -1 , 3.1% and 100, correspondingly. Validation of the developed technique was observed by extraction of Cd in certified reference materials (CRMs) and observed results were successfully compared with certified values. The developed procedure was practiced to various food, beverage and water samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  12. Determination of Ultra-trace Rhodium in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction Using 2-(5-Iodo-2-Pyridylazo)-5-Dimethylaminoaniline as a Chelating Agent.

    Science.gov (United States)

    Han, Quan; Huo, Yanyan; Wu, Jiangyan; He, Yaping; Yang, Xiaohui; Yang, Longhu

    2017-03-24

    A highly sensitive method based on cloud point extraction (CPE) separation/preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection has been developed for the determination of ultra-trace amounts of rhodium in water samples. A new reagent, 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA), was used as the chelating agent and the nonionic surfactant TritonX-114 was chosen as extractant. In a HAc-NaAc buffer solution at pH 5.5, Rh(III) reacts with 5-I-PADMA to form a stable chelate by heating in a boiling water bath for 10 min. Subsequently, the chelate is extracted into the surfactant phase and separated from bulk water. The factors affecting CPE were investigated. Under the optimized conditions, the calibration graph was linear in the range of 0.1-6.0 ng/mL, the detection limit was 0.023 ng/mL for rhodium and relative standard deviation was 3.67% ( c = 1.0 ng/mL, n = 11).The method has been applied to the determination of trace rhodium in water samples with satisfactory results.

  13. Solid-phase extraction of Mn(II), Co(II), Ni(II), Cu(II), Cd(II) and Pb(II) ions from environmental samples by flame atomic absorption spectrometry (FAAS)

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-07-19

    A new method using a column packed with Amberlite XAD-2010 resin as a solid-phase extractant has been developed for the multi-element preconcentration of Mn(II), Co(II), Ni(II), Cu(II), Cd(II), and Pb(II) ions based on their complex formation with the sodium diethyldithiocarbamate (Na-DDTC) prior to flame atomic absorption spectrometric (FAAS) determinations. Metal complexes sorbed on the resin were eluted by 1 mol L{sup -1} HNO{sub 3} in acetone. Effects of the analytical conditions over the preconcentration yields of the metal ions, such as pH, quantity of Na-DDTC, eluent type, sample volume and flow rate, foreign ions etc. have been investigated. The limits of detection (LOD) of the analytes were found in the range 0.08-0.26 {mu}g L{sup -1}. The method was validated by analyzing three certified reference materials. The method has been applied for the determination of trace elements in some environmental samples.

  14. Is cosmology consistent?

    International Nuclear Information System (INIS)

    Wang Xiaomin; Tegmark, Max; Zaldarriaga, Matias

    2002-01-01

    We perform a detailed analysis of the latest cosmic microwave background (CMB) measurements (including BOOMERaNG, DASI, Maxima and CBI), both alone and jointly with other cosmological data sets involving, e.g., galaxy clustering and the Lyman Alpha Forest. We first address the question of whether the CMB data are internally consistent once calibration and beam uncertainties are taken into account, performing a series of statistical tests. With a few minor caveats, our answer is yes, and we compress all data into a single set of 24 bandpowers with associated covariance matrix and window functions. We then compute joint constraints on the 11 parameters of the 'standard' adiabatic inflationary cosmological model. Our best fit model passes a series of physical consistency checks and agrees with essentially all currently available cosmological data. In addition to sharp constraints on the cosmic matter budget in good agreement with those of the BOOMERaNG, DASI and Maxima teams, we obtain a heaviest neutrino mass range 0.04-4.2 eV and the sharpest constraints to date on gravity waves which (together with preference for a slight red-tilt) favor 'small-field' inflation models

  15. Consistent Quantum Theory

    Science.gov (United States)

    Griffiths, Robert B.

    2001-11-01

    Quantum mechanics is one of the most fundamental yet difficult subjects in physics. Nonrelativistic quantum theory is presented here in a clear and systematic fashion, integrating Born's probabilistic interpretation with Schrödinger dynamics. Basic quantum principles are illustrated with simple examples requiring no mathematics beyond linear algebra and elementary probability theory. The quantum measurement process is consistently analyzed using fundamental quantum principles without referring to measurement. These same principles are used to resolve several of the paradoxes that have long perplexed physicists, including the double slit and Schrödinger's cat. The consistent histories formalism used here was first introduced by the author, and extended by M. Gell-Mann, J. Hartle and R. Omnès. Essential for researchers yet accessible to advanced undergraduate students in physics, chemistry, mathematics, and computer science, this book is supplementary to standard textbooks. It will also be of interest to physicists and philosophers working on the foundations of quantum mechanics. Comprehensive account Written by one of the main figures in the field Paperback edition of successful work on philosophy of quantum mechanics

  16. Determination of palladium, platinum and rhodium in used automobile catalysts and active pharmaceutical ingredients using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Resano, Martín, E-mail: mresano@unizar.es [Department of Analytical Chemistry, Aragón Institute of Engineering Research (I3A), University of Zaragoza, Pedro Cerbuna 12, 50009 Zaragoza (Spain); Flórez, María del Rosario [Department of Analytical Chemistry, Aragón Institute of Engineering Research (I3A), University of Zaragoza, Pedro Cerbuna 12, 50009 Zaragoza (Spain); Queralt, Ignasi [Institute of Earth Sciences Jaume Almera ICTJA-CSIC, Sole Sabarís s/n, 08028 Barcelona (Spain); Marguí, Eva [Department of Chemistry, Faculty of Sciences, Universitat de Girona, Campus Montilivi s/n, 17071 Girona (Spain)

    2015-03-01

    This work investigates the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for the direct determination of Pd, Pt and Rh in two samples of very different nature. While analysis of active pharmaceutical ingredients is straightforward and it is feasible to minimize matrix effects, to the point that calibration can be carried out against aqueous standard solutions, the analysis of used automobile catalysts is more challenging requiring the addition of a chemical modifier (NH{sub 4}F·HF) to help in releasing the analytes, a more vigorous temperature program and the use of a solid standard (CRM ERM®-EB504) for calibration. However, in both cases it was possible to obtain accurate results and precision values typically better than 10% RSD in a fast and simple way, while only two determinations are needed for the three analytes, since Pt and Rh can be simultaneously monitored in both types of samples. Overall, the methods proposed seem suited for the determination of these analytes in such types of samples, offering a greener and faster alternative that circumvents the traditional problems associated with sample digestion, requiring a small amount of sample only (0.05 mg per replicate for catalysts, and a few milligrams for the pharmaceuticals) and providing sufficient sensitivity to easily comply with regulations. The LODs achieved were 6.5 μg g{sup −1} (Pd), 8.3 μg g{sup −1} (Pt) and 9.3 μg g{sup −1} (Rh) for catalysts, which decreased to 0.08 μg g{sup −1} (Pd), 0.15 μg g{sup −1} (Pt) and 0.10 μg g{sup −1} (Rh) for pharmaceuticals. - Highlights: • Solid sampling HR CS GFAAS permits the fast and direct determination of Pd, Pt and Rh. • 2 determinations suffice for the 3 elements (2 of them can be measured simultaneously). • Samples as different as car catalysts and pharmaceuticals can be accurately analyzed. • Aqueous standards (pharmaceuticals) or a solid CRM (catalysts) is used for calibration.

  17. Selective and sensitive speciation analysis of Cr(VI) and Cr(III), at sub-μgL-1 levels in water samples by electrothermal atomic absorption spectrometry after electromembrane extraction.

    Science.gov (United States)

    Tahmasebi, Zeinab; Davarani, Saied Saeed Hosseiny

    2016-12-01

    In this work, electromembrane extraction in combination with electrothermal atomic absorption spectrometry (ET-AAS) was investigated for speciation, preconcentration and quantification of Cr(VI) and Cr(III) in water samples through the selective complexation of Cr(VI) with 1,5-diphenylcarbazide (DPC) as a complexing agent. DPC reduces Cr(VI) to Cr(III) ions and then Cr(III) species are extracted based on electrokinetic migration of their cationic complex (Cr(III)-DPC) toward the negative electrode placed in the hollow fiber. Also, once oxidized to Cr(VI), Cr(III) ions in initial sample were determined by this procedure. The influence of extraction parameters such as pH, type of organic solvent, chelating agent concentration, stirring rate, extraction time and applied voltage were evaluated following a one-at-a-time optimization approach. Under optimized conditions, the extracted analyte was quantified by ETAAS, with an acceptable linearity in the range of 0.05-5ngmL -1 (R 2 value=0.996), and a repeatability (%RSD) between 3.7% and 12.2% (n=4) for 5.0 and 1.0ngmL -1 of Cr(VI), respectively. Also, we obtained an enrichment factor of 110 that corresponded to the recovery of 66%. The detection limit (S/N ratio of 3:1) was 0.02ngmL -1 . Finally, this new method was successfully employed to determine Cr(III) and Cr(VI) species in real water samples. Copyright © 2016. Published by Elsevier B.V.

  18. Atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Haswell, S.J.

    1991-01-01

    Atomic absorption spectroscopy is now well established and widely used technique for the determination of trace and major elements in a wide range analyte types. There have been many advances in the atomic spectroscopy over the last decade and for this reason and to meet the demand, it was felt that there was a need for an updated book. Whilst interest in instrumental design has tended to dominate the minds of the spectrocopist, the analyst concerned with obtaining reliable and representative data, in diverse areas of application, has been diligently modifying and developing sample treatment and instrumental introduction techniques. Such methodology is de fundamental part of analysis and form the basis of the fourteen application chapters of this book. The text focuses in the main on AAS; however, the sample handling techniques described are in many cases equally applicable to ICP-OES and ICP-MS analysis. (author). refs.; figs.; tabs

  19. Factors Contributing to Cognitive Absorption and Grounded Learning Effectiveness in a Competitive Business Marketing Simulation

    Science.gov (United States)

    Baker, David Scott; Underwood, James, III; Thakur, Ramendra

    2017-01-01

    This study aimed to establish a pedagogical positioning of a business marketing simulation as a grounded learning teaching tool and empirically assess the dimensions of cognitive absorption related to grounded learning effectiveness in an iterative business simulation environment. The method/design and sample consisted of a field study survey…

  20. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

  1. Determination of lead at trace levels in mussel and sea water samples using vortex assisted dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry.

    Science.gov (United States)

    Erarpat, Sezin; Özzeybek, Gözde; Chormey, Dotse Selali; Bakırdere, Sezgin

    2017-12-01

    In this study, dispersive liquid-liquid microextraction (DLLME) and slotted quartz tube (SQT) were coupled to flame atomic absorption spectrometry (FAAS) to increase the sensitivity of lead. Conditions such as the formation of the lead-dithizone complex, efficiency of the DLLME method and the output of the SQT were systematically optimized to improve the detection limit for the analyte. The conventional FAAS system was improved upon by about 3.0 times with SQT-FAAS, 32 times with DLLME-FAAS and 142 times with DLLME-SQT-FAAS. The method was applicable over a wide linear range (10-500 μg L -1 ). The limit of detection (LOD) determined by DLLME-SQT-FAAS for seawater and mussel were 2.7 μg L -1 and 270 μg kg -1 , respectively. The percent recoveries obtained for mussel and seawater samples (spiked at 20 and 50 μg L -1 ) were 95-96% and 98-110%, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

    Science.gov (United States)

    de Babos, Diego Victor; Bechlin, Marcos André; Barros, Ariane Isis; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta; de Oliveira, Silvana Ruella

    2016-05-15

    A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Persistent sample circulation microextraction combined with graphite furnace atomic absorption spectroscopy for trace determination of heavy metals in fish species marketed in Kermanshah, Iran, and human health risk assessment.

    Science.gov (United States)

    Safari, Yahya; Karimaei, Mostafa; Sharafi, Kiomars; Arfaeinia, Hossein; Moradi, Masoud; Fattahi, Nazir

    2018-06-01

    Persistent sample circulation microextraction (PSCME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed as a high pre-concentration technique for the determination of heavy metals in fish species. In this method, a few microliters of organic solvent (40.0 µL carbon tetrachloride) was transferred to the bottom of a conical sample cup. Then 10.0 mL of aqueous solution was transformed to fine droplets while passing through the organic solvent. At this stage, metal-ligand hydrophobic complex was extracted into the organic solvent. After extraction, 20 µL of extraction solvent was injected into the graphite tube using an auto-sampler. Under optimal conditions, enrichment factors and enhancement factor were in the range of 180-240 and 155-214, respectively. The calibration curves were linear in the range of 0.03-200 µg kg -1 and the limits of detection (LODs) were in the range of 0.01-0.05 µg kg -1 . Repeatability (intra-day) and reproducibility (inter-day) for 0.50 µg L -1 Hg and 0.10 µg L -1 Cd and Pb were in the range of 3.1-4.2% (n = 7) and 4.3-6.1% (n = 7), respectively. Potential human health risk assessment was conducted by calculating estimated weekly intake (EWI) of the metals from eating fish and comparison of these values with provisional tolerable weekly intake (PTWI) values. EWI data for the studied metals through fish consumption were lower than the PTWI values. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  4. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    Science.gov (United States)

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  5. The Role of Trait and State Absorption in the Enjoyment of Music

    Science.gov (United States)

    2016-01-01

    Little is known about the role of state versus trait characteristics on our enjoyment of music. The aim of this study was to investigate the influence of state and trait absorption upon preference for music, particularly preference for music that evokes negative emotions. The sample consisted of 128 participants who were asked to listen to two pieces of self-selected music and rate the music on variables including preference and felt and expressed emotions. Participants completed a brief measure of state absorption after listening to each piece, and a trait absorption inventory. State absorption was strongly positively correlated with music preference, whereas trait absorption was not. Trait absorption was related to preference for negative emotions in music, with chi-square analyses demonstrating greater enjoyment of negative emotions in music among individuals with high trait absorption. This is the first study to show that state and trait absorption have separable and distinct effects on a listener’s music experience, with state characteristics impacting music enjoyment in the moment, and trait characteristics influencing music preference based on its emotional content. PMID:27828970

  6. The Role of Trait and State Absorption in the Enjoyment of Music.

    Science.gov (United States)

    Hall, Sarah E; Schubert, Emery; Wilson, Sarah J

    2016-01-01

    Little is known about the role of state versus trait characteristics on our enjoyment of music. The aim of this study was to investigate the influence of state and trait absorption upon preference for music, particularly preference for music that evokes negative emotions. The sample consisted of 128 participants who were asked to listen to two pieces of self-selected music and rate the music on variables including preference and felt and expressed emotions. Participants completed a brief measure of state absorption after listening to each piece, and a trait absorption inventory. State absorption was strongly positively correlated with music preference, whereas trait absorption was not. Trait absorption was related to preference for negative emotions in music, with chi-square analyses demonstrating greater enjoyment of negative emotions in music among individuals with high trait absorption. This is the first study to show that state and trait absorption have separable and distinct effects on a listener's music experience, with state characteristics impacting music enjoyment in the moment, and trait characteristics influencing music preference based on its emotional content.

  7. Ultrafast THz Saturable Absorption in Semiconductors

    DEFF Research Database (Denmark)

    Turchinovich, Dmitry; Hoffmann, Matthias C.

    2011-01-01

    We demonstrate THz saturable absorption in n-doped semiconductors GaAs, GaP, and Ge in a nonlinear THz time-domain spectroscopy experiment. Saturable absorption is caused by sample conductivity modulation due to electron heating and satellite valley scattering in the field of a strong THz pulse....

  8. D-xylose absorption

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003606.htm D-xylose absorption To use the sharing features on this page, please enable JavaScript. D-xylose absorption is a laboratory test to determine ...

  9. Analyzing Water's Optical Absorption

    Science.gov (United States)

    2002-01-01

    A cooperative agreement between World Precision Instruments (WPI), Inc., and Stennis Space Center has led the UltraPath(TM) device, which provides a more efficient method for analyzing the optical absorption of water samples at sea. UltraPath is a unique, high-performance absorbance spectrophotometer with user-selectable light path lengths. It is an ideal tool for any study requiring precise and highly sensitive spectroscopic determination of analytes, either in the laboratory or the field. As a low-cost, rugged, and portable system capable of high- sensitivity measurements in widely divergent waters, UltraPath will help scientists examine the role that coastal ocean environments play in the global carbon cycle. UltraPath(TM) is a trademark of World Precision Instruments, Inc. LWCC(TM) is a trademark of World Precision Instruments, Inc.

  10. Implementation of suitable flow injection/sequential-sample separation/preconcentration schemes for determination of trace metal concentrations using detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2002-01-01

    Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS...

  11. Correlation between Wavelength Dispersive X-ray Fluorescence (WDXRF) analysis of hardened concrete for chlorides vs. Atomic Absorption (AA) analysis in accordance with AASHTO T- 260; sampling and testing for chloride ion in concrete and concrete raw mater

    Science.gov (United States)

    2014-04-01

    A correlation between Wavelength Dispersive X-ray Fluorescence(WDXRF) analysis of Hardened : Concrete for Chlorides and Atomic Absorption (AA) analysis (current method AASHTO T-260, procedure B) has been : found and a new method of analysis has been ...

  12. Minority carrier diffusion lengths and absorption coefficients in silicon sheet material

    Science.gov (United States)

    Dumas, K. A.; Swimm, R. T.

    1980-01-01

    Most of the methods which have been developed for the measurement of the minority carrier diffusion length of silicon wafers require that the material have either a Schottky or an ohmic contact. The surface photovoltage (SPV) technique is an exception. The SPV technique could, therefore, become a valuable diagnostic tool in connection with current efforts to develop low-cost processes for the production of solar cells. The technique depends on a knowledge of the optical absorption coefficient. The considered investigation is concerned with a reevaluation of the absorption coefficient as a function of silicon processing. A comparison of absorption coefficient values showed these values to be relatively consistent from sample to sample, and independent of the sample growth method.

  13. Absorption and excretion tests

    International Nuclear Information System (INIS)

    Berberich, R.

    1988-01-01

    The absorption and excretion of radiopharmaceuticals is still of interest in diagnostic investigations of nuclear medicine. In this paper the most common methods of measuring absorption and excretion are described. The performance of the different tests and their standard values are discussed. More over the basic possibilities of measuring absorption and excretion including the needed measurement equipments are presented. (orig.) [de

  14. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-01-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L −1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L −1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic

  15. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L{sup −1} and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L{sup −1} of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic.

  16. Direct microcomputer controlled determination of zinc in human serum by flow injection atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Nielsen, Bent; Jensen, Arne

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve......, programmable from the microcomputer, to control the sample volume. No pre-treatment of the samples is necessary. The limit of detection is 0.14 mg l–1, and only small amounts of serum (

  17. Modernization of Atomic Absorption Spectrophotometer

    International Nuclear Information System (INIS)

    Tasic, Visa; Milivojevic, Dragan; Karabasevic, Dejan

    2003-01-01

    In Copper Institute in Bor, connection has been made between absorption spectrophotometer and standard PC with the aim to make its operation more reliable and comfortable. Applied solution includes both software and hardware components. An I/O interface module has been installed in PC [1]. Software component consists of programs for measuring and interpretation of results. Paper presents details of this job realization.(Author)

  18. Calcium absorption and achlorhydria

    International Nuclear Information System (INIS)

    Recker, R.R.

    1985-01-01

    Defective absorption of calcium has been thought to exist in patients with achlorhydria. The author compared absorption of calcium in its carbonate form with that in a pH-adjusted citrate form in a group of 11 fasting patients with achlorhydria and in 9 fasting normal subjects. Fractional calcium absorption was measured by a modified double-isotope procedure with 0.25 g of calcium used as the carrier. Mean calcium absorption (+/- S.D.) in the patients with achlorhydria was 0.452 +/- 0.125 for citrate and 0.042 +/- 0.021 for carbonate (P less than 0.0001). Fractional calcium absorption in the normal subjects was 0.243 +/- 0.049 for citrate and 0.225 +/- 0.108 for carbonate (not significant). Absorption of calcium from carbonate in patients with achlorhydria was significantly lower than in the normal subjects and was lower than absorption from citrate in either group; absorption from citrate in those with achlorhydria was significantly higher than in the normal subjects, as well as higher than absorption from carbonate in either group. Administration of calcium carbonate as part of a normal breakfast resulted in completely normal absorption in the achlorhydric subjects. These results indicate that calcium absorption from carbonate is impaired in achlorhydria under fasting conditions. Since achlorhydria is common in older persons, calcium carbonate may not be the ideal dietary supplement

  19. Studies of mercury, arsenic and selenium levels in human hair, nail and blood samples from the Wassa West District of Ghana, using neutron activation analysis and atomic absorption spectrophotometric technique

    International Nuclear Information System (INIS)

    Samlafu, V.B.

    2011-06-01

    This study examines Arsenic, mercury and selenium levels in human hair, nail and blood samples collected from Wassa West District, a mining impacted site in contrast with Akatsi and its environs, a non-mining impacted site using INAA facility at Ghana Research Reactor-1 (GHARR-1), Kwabenya, Accra. Other elements determined alongside the elements of interest were Na, K, Ca, Al, Mg, Mn, V, Cl, I, Br, Au, La, Cu, Zn, Sr, Ni and Ag. An alternative method was developed for the Preconcentration Neutron Activation Analysis using dithizone/CHCl 3 mixture as the chelating agent for very low levels of mercury and arsenic in human blood. Factors that affect dithizone complexation such as PH, and concentration were investigated. Selenium levels in all the matrices were determined by Hydride Generation Atomic Absorption Spectrophotometric (HGAAS) technique. Speciation of Se(IV) and Se(VI) was carried out on selected blood samples using HNO 3 /H 2 O 2 as digestion reagent. The precision of the analytical methods used were evaluated by Schewart control chart for internal quality assessment purposes. The results were within the acceptable limits of Xσ. Four certified reference materials namely GBW 09101, DOME-2, Lichen IAEA-336 and Peach leave SRM 1547 were also used to validate the analytical methods for external quality assessment. The results obtained in this work were in good agreement with the certified values. The levels of total mercury in hair ranged from 1.65 μg/g to 20.46 μg/g. Mercury in nail samples ranged from 0.97μg/g to 31.94 μg/g and blood samples ranged from 0.01μg/mL to 0.70 μg/mL in experimental subjects. Mercury levels in control subjects ranged from 0.24 μg/g to 7.15 μg/g in hair, 0.2 μg/g to 1.83 μg/g of mercury in nail and 0.01 μg/mL to 2.38 μg/mL of mercury in blood. Generally the decreasing order of accumulation of mercury in the three matrices in the experimental subjects were as follows nail > hair > blood, while the control subjects had the

  20. [Study on lead absorption in pumpkin by atomic absorption spectrophotometry].

    Science.gov (United States)

    Li, Zhen-Xia; Sun, Yong-Dong; Chen, Bi-Hua; Li, Xin-Zheng

    2008-07-01

    A study was carried out on the characteristic of lead absorption in pumpkin via atomic absorption spectrophotometer. The results showed that lead absorption amount in pumpkin increased with time, but the absorption rate decreased with time; And the lead absorption amount reached the peak in pH 7. Lead and cadmium have similar characteristic of absorption in pumpkin.

  1. H I absorption in nearby compact radio galaxies

    Science.gov (United States)

    Glowacki, M.; Allison, J. R.; Sadler, E. M.; Moss, V. A.; Curran, S. J.; Musaeva, A.; Deng, C.; Parry, R.; Sligo, M. C.

    2017-05-01

    H I absorption studies yield information on both active galactic nucleus (AGN) feeding and feedback processes. This AGN activity interacts with the neutral gas in compact radio sources, which are believed to represent the young or recently re-triggered AGN population. We present the results of a survey for H I absorption in a sample of 66 compact radio sources at 0.040 100 km s-1) features, indicative of disturbed gas kinematics. Such broad, shallow and offset features are also found within low-excitation radio galaxies which is attributed to disturbed circumnuclear gas, consistent with early-type galaxies typically devoid of a gas-rich disc. Comparing mid-infrared colours of our galaxies with H I detections indicates that narrow and deep absorption features are preferentially found in late-type and high-excitation radio galaxies in our sample. These features are attributed to gas in galactic discs. By combining XMM-Newton archival data with 21-cm data, we find support that absorbed X-ray sources may be good tracers of H I content within the host galaxy. This sample extends previous H I surveys in compact radio galaxies to lower radio luminosities and provides a basis for future work exploring the higher redshift universe.

  2. Absorption heat pumps

    International Nuclear Information System (INIS)

    Formigoni, C.

    1998-01-01

    A brief description of the difference between a compression and an absorption heat pump is made, and the reasons why absorption systems have spread lately are given. Studies and projects recently started in the field of absorption heat pumps, as well as criteria usually followed in project development are described. An outline (performance targets, basic components) of a project on a water/air absorption heat pump, running on natural gas or LPG, is given. The project was developed by the Robur Group as an evolution of a water absorption refrigerator operating with a water/ammonia solution, which has been on the market for a long time and recently innovated. Finally, a list of the main energy and cost advantages deriving from the use of absorption heat pumps is made [it

  3. The Portuguese language version of social phobia and Anxiety Inventory: analysis of items and internal consistency in a Brazilian sample of 1,014 undergraduate students Versão para o português do Inventário de Fobia Social e Ansiedade: análise de itens e consistência interna numa amostra de 1.014 estudantes universitários brasileiros

    Directory of Open Access Journals (Sweden)

    Patrícia Picon

    2006-01-01

    Full Text Available OBJECTIVE: Theoretical and empirical analysis of items and internal consistency of the Portuguese-language version of Social Phobia and Anxiety Inventory (SPAI-Portuguese. METHODS: Social phobia experts conducted a 45-item content analysis of the SPAI-Portuguese administered to a sample of 1,014 university students. Item discrimination was evaluated by Student's t test; interitem, mean and item-to-total correlations, by Pearson coefficient; reliability was estimated by Cronbach's alpha. RESULTS: There was 100% agreement among experts concerning the 45 items. On the SPAI-Portuguese 43 items were discriminative (p OBJETIVO: Análise teórica e empírica dos itens e da consistência interna da versão em português do Social Phobia and Anxiety Inventory (SPAI-Português e subescalas. MÉTODOS: Peritos em fobia social conduziram análise de conteúdo dos 45 itens do SPAI-Português, administrado a 1.014 estudantes universitários. A discriminação dos itens foi avaliada por teste t de Student; correlações interitens, médias e item/total por coeficientes de Pearson; fidedignidade pelo alfa de Cronbach. RESULTADOS: Concordância plena entre os peritos para os 45 itens. SPAI-Português com 43 itens discriminativos (p < 0,05. Alguns itens, entre as subescalas, apresentaram coeficientes abaixo de 0,2. As médias das correlações interitens foram: 0,41 na subescala fobia social; 0,32 na subescala agorafobia; e 0,32 no SPAI-Português. As correlações item/total foram maiores do que 0,3 (p < 0,001. Alfas de Cronbach foram: 0,95 no SPAI-Português; 0,96 na subescala de fobia social; 0,85 na subescala de agorafobia. CONCLUSÃO: O conteúdo dos itens foi relacionado aos constructos subjacentes (agorafobia e fobia social, com discriminabilidade de 43 itens do SPAI-Português. As correlações médias interitens e alfas revelaram consistência interna de SPAI-Português e subescalas, além de multidimensionalidade das mesmas. Nenhum item foi suprimido

  4. Absorption lines, Faraday rotation, and magnetic field estimates for QSO absorption-line clouds

    International Nuclear Information System (INIS)

    Kronberg, P.P.; Perry, J.J.

    1982-01-01

    We have estimated the extragalactic component of Faraday rotation for a sample of 37 QSOs for which there is good absorption line data, which we have also analyzed. Statistical evidence is presented which suggests that we have isolated a component of Faraday rotation which is occurring in the absorption clouds of some QSOs

  5. Solar absorption surface panel

    Science.gov (United States)

    Santala, Teuvo J.

    1978-01-01

    A composite metal of aluminum and nickel is used to form an economical solar absorption surface for a collector plate wherein an intermetallic compound of the aluminum and nickel provides a surface morphology with high absorptance and relatively low infrared emittance along with good durability.

  6. Nutrition and magnesium absorption

    NARCIS (Netherlands)

    Brink, E.J.

    1992-01-01

    The influence of various nutrients present in dairy products and soybean-based products on absorption of magnesium has been investigated. The studies demonstrate that soybean protein versus casein lowers apparent magnesium absorption in rats through its phytate component. However, true

  7. Zeeman atomic absorption spectroscopy

    International Nuclear Information System (INIS)

    Loos-Vollebregt, M.T.C. de.

    1980-01-01

    A new method of background correction in atomic absorption spectroscopy has recently been introduced, based on the Zeeman splitting of spectral lines in a magnetic field. A theoretical analysis of the background correction capability observed in such instruments is presented. A Zeeman atomic absorption spectrometer utilizing a 50 Hz sine wave modulated magnetic field is described. (Auth.)

  8. Control of water absorption by purification of graphite

    International Nuclear Information System (INIS)

    Simpkins, J.E.; Strehlow, R.A.; Mioduszewski, P.K.; Uckan, T.

    1988-01-01

    It is well known that graphite can absorb large quantities of water, which can represent an abundant source of oxygen impurities in fusion plasmas if the corresponding components are not properly outgassed. We have outgassed various fusion-relevant graphites (e.g., POCO AXF-5Q) for 1.5 h at 1500/degree/C to release absorbed water and have subsequently exposed the samples to air for various periods of time. Re-absorption of water during the air exposure was estimated by measuring the amount of water produced in subsequent outgassing runs. The results show that the amount of water re-absorbed increases by a factor of approximately 10 within 8 h compared to the sample in the outgassed state but with no air exposure. The water content of the 'as received' material is reached after approximately 30 days. Re-absorption of water was significantly reduced by purification of the investigated graphite samples. This purification process, which consists of heating the sample at 2800/degree/C for 30 min in an argon atmosphere, reduces the levels of trace impurities which can be responsible for catalytic surface reactions on the internal surfaces of the graphite. After exposing an outgassed sample to an electron cyclotron heated plasma followed by 1 h air exposure, the amount of water desorbed was observed to increase by a factor of 6. Data will be presented to correlate this effect with trace impurities. 9 refs., 2 figs., 5 tabs

  9. The comparison of benzene and CO2 absorption methods for radioisotope 14C dating

    International Nuclear Information System (INIS)

    Satrio and Zainal Abidin

    2007-01-01

    It had been conducted to research of age determination of carbon samples using CO 2 absorption method. This method as alternative to benzene synthesis method for radioisotope 14 C dating.The aim of the method is to support some hydrology research's especially groundwater dating using environmental radioisotope 14 C.The results which obtain by CO 2 absorption method then compared with the results of benzene synthesis method consists of background counter, standard counter, activity and age limit, age, and material cost or component. The research show that compared with benzene synthesis method, sample preparation using CO 2 absorption method is more simple and relatively low cost. The use of CO 2 absorption method can save the cost about 75 %. The different of both methods is age limit detection. The results of age limit detection when using CO 2 absorption and synthesis benzene methods are 33,310 years and 47,533 years respectively. Whereas, based on t test, the age results of both methods for the same sample are obtained relatively equal. (author)

  10. Aerosol Absorption Measurements in MILAGRO.

    Science.gov (United States)

    Gaffney, J. S.; Marley, N. A.; Arnott, W. P.; Paredes-Miranda, L.; Barnard, J. C.

    2007-12-01

    to carbonyl- and nitro- functional groups on conjugated and aromatic organic structures (e.g. PAH, and terpene derived products). Using 12-hour fine (0.1-1.0 micron) aerosol samples collected in the field on quartz filters, uv/vis and infrared spectra were obtained in the laboratory using integrating spheres and diffuse reflectance spectroscopy, respectively. An inter-comparison of the "real-time" measurements made by the photo-acoustic, aethalometer and MAAP techniques have been described. In addition, the in situ aethalometer (seven-channel) results are compared with continuous integrating sphere uv-visible spectra to examine the angstrom absorption coefficient variance. These results will be briefly overviewed and the specific posters detailing these results will be highlighted highlighted. This work was performed as part of the Department of Energy's Megacity Aerosol Experiment - Mexico City under the support of the Atmospheric Science Program. "This researchwas supported by the Office of Science (BER), U. S. Department of Energy, Grant No. DE-FG02-07ER64329.

  11. Measuring process and knowledge consistency

    DEFF Research Database (Denmark)

    Edwards, Kasper; Jensen, Klaes Ladeby; Haug, Anders

    2007-01-01

    When implementing configuration systems, knowledge about products and processes are documented and replicated in the configuration system. This practice assumes that products are specified consistently i.e. on the same rule base and likewise for processes. However, consistency cannot be taken...... for granted; rather the contrary, and attempting to implement a configuration system may easily ignite a political battle. This is because stakes are high in the sense that the rules and processes chosen may only reflect one part of the practice, ignoring a majority of the employees. To avoid this situation......, this paper presents a methodology for measuring product and process consistency prior to implementing a configuration system. The methodology consists of two parts: 1) measuring knowledge consistency and 2) measuring process consistency. Knowledge consistency is measured by developing a questionnaire...

  12. Effect of granulation of geological samples in neutron transport measurements

    International Nuclear Information System (INIS)

    Woznicka, Urszula; Drozdowicz, Krzysztof; Gabanska, Barbara; Krynicka, Ewa; Igielski, Andrzej

    2001-01-01

    The thermal neutron absorption cross section is one of the parameters describing the transport of thermal neutrons in a medium. Theoretical descriptions and experiments which determine the absorption cross section have a wide literature for homogeneous media. The situation comes true e.g. for fluids or amorphous solids. There are many other media which should be treated as heterogeneous. Among others - geological materials. The material heterogeneity for the thermal neutron transport in a considered volume is understood here as an existence of many small regions which differ significantly in their macroscopic neutron diffusion parameters (defined by the absorption and transport cross sections). The final difference, which influences the neutron transport, comes from a combination of the absolute differences between the parameters and of sizes of regions (related to the neutron mean free paths). A rock can be naturally heterogeneous in the above meaning. Besides, it can happen that a preparation of the rock sample for a neutron measurement can increase its natural heterogeneity. (For example, when the rock material is crushed and the measured sample consists of the obtained grains). The question is which granulation is allowed to treat the sample material as still homogeneous, and from which size of the rock grains we have to consider a two-component medium. It has been experimentally proved that the effective absorption of thermal neutrons in a heterogeneous two-component material can significantly differ from the absorption in a homogeneous one which consists of the same elements. The final effect is dependent on a few factors: the macroscopic absorption cross sections of the components, their total mass contributions, and the size of the grains. The ratio of the effective absorption cross section of the heterogeneous material to the cross section of the equivalent homogeneous, is a measure of the heterogeneity effect on the thermal neutron absorption

  13. Consistency of the MLE under mixture models

    OpenAIRE

    Chen, Jiahua

    2016-01-01

    The large-sample properties of likelihood-based statistical inference under mixture models have received much attention from statisticians. Although the consistency of the nonparametric MLE is regarded as a standard conclusion, many researchers ignore the precise conditions required on the mixture model. An incorrect claim of consistency can lead to false conclusions even if the mixture model under investigation seems well behaved. Under a finite normal mixture model, for instance, the consis...

  14. Uranium absorption study pile

    International Nuclear Information System (INIS)

    Raievski, V.; Sautiez, B.

    1959-01-01

    The report describes a pile designed to measure the absorption of fuel slugs. The pile is of graphite and comprises a central section composed of uranium rods in a regular lattice. RaBe sources and BF 3 counters are situated on either side of the center. A given uranium charge is compared with a specimen charge of about 560 kg, and the difference in absorption between the two noted. The sensitivity of the equipment will detect absorption variations of about a few ppm boron (10 -6 boron per gr. of uranium) or better. (author) [fr

  15. Total photon absorption

    International Nuclear Information System (INIS)

    Carlos, P.

    1985-06-01

    The present discussion is limited to a presentation of the most recent total photonuclear absorption experiments performed with real photons at intermediate energy, and more precisely in the region of nucleon resonances. The main sources of real photons are briefly reviewed and the experimental procedures used for total photonuclear absorption cross section measurements. The main results obtained below 140 MeV photon energy as well as above 2 GeV are recalled. The experimental study of total photonuclear absorption in the nuclear resonance region (140 MeV< E<2 GeV) is still at its beginning and some results are presented

  16. Intrinsic defect oriented visible region absorption in zinc oxide films

    Science.gov (United States)

    Rakhesh, V.; Shankar, Balakrishnan

    2018-05-01

    Zinc Oxide films were deposited on the glass substrate using vacuum arc sputtering technology. Films were prepared in oxygen ambience for 10mA and 15 mA deposition current separately. The UV-Visible spectroscopy of the samples showed that both samples possess sharp absorption near 3.5eV which is the characteristic band gap absorption energy of ZnO films. The absorption coefficient were calculated for the samples and the (αℎϑ)2 vs energy plot is drawn. The plot suggested that in addition to the sharp band edge absorption, the sample prepared at 10mA deposition current showed sharp absorption edge near 1.51eV and that at 15 mA showed absorption edge near 1.47eV. This refers to the presence of an intrinsic defect level which is likely to be deep in the band gap.

  17. Absorption heat pump system

    Science.gov (United States)

    Grossman, G.

    1982-06-16

    The efficiency of an absorption heat pump system is improved by conducting liquid from a second stage evaporator thereof to an auxiliary heat exchanger positioned downstream of a primary heat exchanger in the desorber of the system.

  18. Zeeman atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Hadeishi, T.; McLaughlin, R.

    1978-08-01

    The design and development of a Zeeman atomic absorption spectrometer for trace element analysis are described. An instruction manual is included which details the operation, adjustment, and maintenance. Specifications and circuit diagrams are given

  19. Revisiting Absorptive Capacity

    DEFF Research Database (Denmark)

    de Araújo, Ana Luiza Lara; Ulhøi, John Parm; Lettl, Christopher

    Absorptive capacity has mostly been perceived as a 'passive' outcome of R&D investments. Recently, however, a growing interest into its 'proactive' potentials has emerged. This paper taps into this development and proposes a dynamic model for conceptualizing the determinants of the complementary...... learning processes of absorptive capacity, which comprise combinative and adaptive capabilities. Drawing on survey data (n=169), the study concludes that combinative capabilities primarily enhance transformative and exploratory learning processes, while adaptive capabilities strengthen all three learning...

  20. Comment on resonant absorption

    International Nuclear Information System (INIS)

    Hammerling, P.

    1977-01-01

    An average over angles of incidence of the usual resonant absorption function is presented. This form is appropriate under experimental conditions where the angles of incidence vary greatly and in an unknown manner. For comparison a lens-ellipsoidal mirror illumination system with a known longitudinal aberration is considered. In the latter example the angles of incidence are readily obtained and the resulting resonance absorption function evaluated. The associated fields are calculated in a similar fashion. (author)

  1. Optical absorption measurement system

    International Nuclear Information System (INIS)

    Draggoo, V.G.; Morton, R.G.; Sawicki, R.H.; Bissinger, H.D.

    1989-01-01

    This patent describes a non-intrusive method for measuring the temperature rise of optical elements under high laser power optical loading to determine the absorption coefficient. The method comprises irradiating the optical element with a high average power laser beam, viewing the optical element with an infrared camera to determine the temperature across the optical element and calculating the absorption of the optical element from the temperature

  2. Coordinating user interfaces for consistency

    CERN Document Server

    Nielsen, Jakob

    2001-01-01

    In the years since Jakob Nielsen's classic collection on interface consistency first appeared, much has changed, and much has stayed the same. On the one hand, there's been exponential growth in the opportunities for following or disregarding the principles of interface consistency-more computers, more applications, more users, and of course the vast expanse of the Web. On the other, there are the principles themselves, as persistent and as valuable as ever. In these contributed chapters, you'll find details on many methods for seeking and enforcing consistency, along with bottom-line analys

  3. Sampling and sample preparation methods for the analysis of trace elements in biological material

    International Nuclear Information System (INIS)

    Sansoni, B.; Iyengar, V.

    1978-05-01

    The authors attempt to give a most systamtic possible treatment of the sample taking and sample preparation of biological material (particularly in human medicine) for trace analysis (e.g. neutron activation analysis, atomic absorption spectrometry). Contamination and loss problems are discussed as well as the manifold problems of the different consistency of solid and liquid biological materials, as well as the stabilization of the sample material. The process of dry and wet ashing is particularly dealt with, where new methods are also described. (RB) [de

  4. Aerosol Angstrom Absorption Coefficient Comparisons during MILAGRO.

    Science.gov (United States)

    Marley, N. A.; Marchany-Rivera, A.; Kelley, K. L.; Mangu, A.; Gaffney, J. S.

    2007-12-01

    Measurements of aerosol absorption were obtained as part of the MAX-Mex component of the MILAGRO field campaign at site T0 (Instituto Mexicano de Petroleo in Mexico City) by using a 7-channel aethalometer (Thermo- Anderson) during the month of March, 2006. The absorption measurements obtained in the field at 370, 470, 520, 590, 660, 880, and 950 nm were used to determine the aerosol Angstrom absorption exponents by linear regression. Since, unlike other absorbing aerosol species (e.g. humic like substances, nitrated PAHs), black carbon absorption is relatively constant from the ultraviolet to the infrared with an Angstrom absorption exponent of -1 (1), a comparison of the Angstrom exponents can indicate the presence of aerosol components with an enhanced UV absorption over that expected from BC content alone. The Angstrom exponents determined from the aerosol absorption measurements obtained in the field varied from - 0.7 to - 1.3 during the study and was generally lower in the afternoon than the morning hours, indicating an increase in secondary aerosol formation and photochemically generated UV absorbing species in the afternoon. Twelve-hour integrated samples of fine atmospheric aerosols (Petroleo (IMP) and CENICA.

  5. Choice, internal consistency, and rationality

    OpenAIRE

    Aditi Bhattacharyya; Prasanta K. Pattanaik; Yongsheng Xu

    2010-01-01

    The classical theory of rational choice is built on several important internal consistency conditions. In recent years, the reasonableness of those internal consistency conditions has been questioned and criticized, and several responses to accommodate such criticisms have been proposed in the literature. This paper develops a general framework to accommodate the issues raised by the criticisms of classical rational choice theory, and examines the broad impact of these criticisms from both no...

  6. Self-consistent quark bags

    International Nuclear Information System (INIS)

    Rafelski, J.

    1979-01-01

    After an introductory overview of the bag model the author uses the self-consistent solution of the coupled Dirac-meson fields to represent a bound state of strongly ineteracting fermions. In this framework he discusses the vivial approach to classical field equations. After a short description of the used numerical methods the properties of bound states of scalar self-consistent Fields and the solutions of a self-coupled Dirac field are considered. (HSI) [de

  7. Time-consistent and market-consistent evaluations

    NARCIS (Netherlands)

    Pelsser, A.; Stadje, M.A.

    2014-01-01

    We consider evaluation methods for payoffs with an inherent financial risk as encountered for instance for portfolios held by pension funds and insurance companies. Pricing such payoffs in a way consistent to market prices typically involves combining actuarial techniques with methods from

  8. Development of an in situ solvent formation microextraction and preconcentration method based on ionic liquids for the determination of trace cobalt (II in water samples by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Jamali

    2017-02-01

    Full Text Available A simple in situ solvent formation microextraction (ISFME methodology based on the application of ionic liquid (IL as an extractant solvent and sodium hexafluorophosphate (NaPF6 as an ion-pairing agent was proposed for the preconcentration of the trace levels of cobalt ions. In this method cobalt was complexed with 2-(5-bromo-2-pyridylazo-5-diethylaminophenol (5-Br-PADAP and extracted into an ionic liquid phase. After phase separation, the enriched analyte in the final solution is determined by flame atomic absorption spectrometry (FAAS. Some effective factors that influence the microextraction efficiency were investigated and optimized. Under the optimum experimental conditions, the limit of detection and the enrichment factor were 0.97 μg L−1 and 50, respectively. The relative standard deviation (R.S.D. was obtained as 2.4%. The proposed method was assessed through the analysis of certified reference water and recovery experiments.

  9. Determination of hafnium by atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yoshida, Isao; Kobayashi, Hiroshi; Ueno, Keihei.

    1977-01-01

    Optimum conditions for atomic absorption spectrophotometric determination of hafnium were investigated by use of a Jarrel-Ash AA-1 instrument which was equipped with a premixed gas burner slotted 50 mm in length and 0.4 mm in width. Absorption of hafnium, which was atomized in an nitrous oxide-acetylene flame, was measured on a resonance line at 307.29 nm. The absorption due to hafnium was enhanced in the presence of ammonium fluoride and iron(III) ion, as shown in Figs. 2 and 3, depending on their concentration. The highest absorption was attained by the addition of (0.15 -- 0.3)M ammonium fluoride, 0.07 M of iron(III) ion and 0.05 M of hydrochloric acid. An excess of the additives decreased the absorption. The presence of zirconium, which caused a significant interference in the ordinary analytical methods, did not affect the absorption due to hafnium, if the zirconium concentration is less than 0.2 M. A standard procedure was proposed; A sample containing a few mg of hafnium was dissolved in a 25-ml volumetric flask, and ammonium fluoride, ferric nitrate and hydrochloric acid were added so that the final concentrations were 0.3, 0.07 and 0.05 M, respectively. Atomic absorption was measured on the aqueous solution in a nitrous oxide-acetylene flame and the hafnium content was calculated from the absorbance. Sensitivity was as high as 12.5 μg of Hf/ml/l% absorption. The present method is especially recommendable to the direct determination of hafnium in samples containing zirconium. (auth.)

  10. Quasar outflow energetics from broad absorption line variability

    Science.gov (United States)

    McGraw, S. M.; Shields, J. C.; Hamann, F. W.; Capellupo, D. M.; Herbst, H.

    2018-03-01

    Quasar outflows have long been recognized as potential contributors to the co-evolution between supermassive black holes (SMBHs) and their host galaxies. The role of outflows in active galactic nucleus (AGN) feedback processes can be better understood by placing observational constraints on wind locations and kinetic energies. We utilize broad absorption line (BAL) variability to investigate the properties of a sample of 71 BAL quasars with P V broad absorption. The presence of P V BALs indicates that other BALs like C IV are saturated, such that variability in those lines favours clouds crossing the line of sight. We use these constraints with measurements of BAL variability to estimate outflow locations and energetics. Our data set consists of multiple-epoch spectra from the Sloan Digital Sky Survey and MDM Observatory. We detect significant (4σ) BAL variations from 10 quasars in our sample over rest-frame time-scales between ≤0.2-3.8 yr. Our derived distances for the 10 variable outflows are nominally ≲ 1-10 pc from the SMBH using the transverse-motion scenario, and ≲ 100-1000 pc from the central source using ionization-change considerations. These distances, in combination with the estimated high outflow column densities (i.e. NH ≳ 1022 cm-2), yield outflow kinetic luminosities between ˜ 0.001 and 1 times the bolometric luminosity of the quasar, indicating that many absorber energies within our sample are viable for AGN feedback.

  11. Mechanism of pion absorption in complex nuclei

    International Nuclear Information System (INIS)

    Doss, K.G.N.; Wharton, W.R.

    Basic geometrical arguments are used to analyze the A dependence of the total pion absorption cross section, the effective number of nucleons sharing the pion momentum and energy, and the proton yields from π + - and π - -induced reactions. The results are consistent with the pions penetrating some distance through the nuclear volume and annihilating on a pair of nucleons. 3 figures

  12. Market-consistent actuarial valuation

    CERN Document Server

    Wüthrich, Mario V

    2016-01-01

    This is the third edition of this well-received textbook, presenting powerful methods for measuring insurance liabilities and assets in a consistent way, with detailed mathematical frameworks that lead to market-consistent values for liabilities. Topics covered are stochastic discounting with deflators, valuation portfolio in life and non-life insurance, probability distortions, asset and liability management, financial risks, insurance technical risks, and solvency. Including updates on recent developments and regulatory changes under Solvency II, this new edition of Market-Consistent Actuarial Valuation also elaborates on different risk measures, providing a revised definition of solvency based on industry practice, and presents an adapted valuation framework which takes a dynamic view of non-life insurance reserving risk.

  13. The Principle of Energetic Consistency

    Science.gov (United States)

    Cohn, Stephen E.

    2009-01-01

    A basic result in estimation theory is that the minimum variance estimate of the dynamical state, given the observations, is the conditional mean estimate. This result holds independently of the specifics of any dynamical or observation nonlinearity or stochasticity, requiring only that the probability density function of the state, conditioned on the observations, has two moments. For nonlinear dynamics that conserve a total energy, this general result implies the principle of energetic consistency: if the dynamical variables are taken to be the natural energy variables, then the sum of the total energy of the conditional mean and the trace of the conditional covariance matrix (the total variance) is constant between observations. Ensemble Kalman filtering methods are designed to approximate the evolution of the conditional mean and covariance matrix. For them the principle of energetic consistency holds independently of ensemble size, even with covariance localization. However, full Kalman filter experiments with advection dynamics have shown that a small amount of numerical dissipation can cause a large, state-dependent loss of total variance, to the detriment of filter performance. The principle of energetic consistency offers a simple way to test whether this spurious loss of variance limits ensemble filter performance in full-blown applications. The classical second-moment closure (third-moment discard) equations also satisfy the principle of energetic consistency, independently of the rank of the conditional covariance matrix. Low-rank approximation of these equations offers an energetically consistent, computationally viable alternative to ensemble filtering. Current formulations of long-window, weak-constraint, four-dimensional variational methods are designed to approximate the conditional mode rather than the conditional mean. Thus they neglect the nonlinear bias term in the second-moment closure equation for the conditional mean. The principle of

  14. Consistent guiding center drift theories

    International Nuclear Information System (INIS)

    Wimmel, H.K.

    1982-04-01

    Various guiding-center drift theories are presented that are optimized in respect of consistency. They satisfy exact energy conservation theorems (in time-independent fields), Liouville's theorems, and appropriate power balance equations. A theoretical framework is given that allows direct and exact derivation of associated drift-kinetic equations from the respective guiding-center drift-orbit theories. These drift-kinetic equations are listed. Northrop's non-optimized theory is discussed for reference, and internal consistency relations of G.C. drift theories are presented. (orig.)

  15. Weak consistency and strong paraconsistency

    Directory of Open Access Journals (Sweden)

    Gemma Robles

    2009-11-01

    Full Text Available In a standard sense, consistency and paraconsistency are understood as, respectively, the absence of any contradiction and as the absence of the ECQ (“E contradictione quodlibet” rule that allows us to conclude any well formed formula from any contradiction. The aim of this paper is to explain the concepts of weak consistency alternative to the standard one, the concepts of paraconsistency related to them and the concept of strong paraconsistency, all of which have been defined by the author together with José M. Méndez.

  16. Consistent force fields for saccharides

    DEFF Research Database (Denmark)

    Rasmussen, Kjeld

    1999-01-01

    Consistent force fields for carbohydrates were hitherto developed by extensive optimization ofpotential energy function parameters on experimental data and on ab initio results. A wide range of experimental data is used: internal structures obtained from gas phase electron diffraction and from x......-anomeric effects are accounted for without addition of specific terms. The work is done in the framework of the Consistent Force Field which originatedin Israel and was further developed in Denmark. The actual methods and strategies employed havebeen described previously. Extensive testing of the force field...

  17. Glass consistency and glass performance

    International Nuclear Information System (INIS)

    Plodinec, M.J.; Ramsey, W.G.

    1994-01-01

    Glass produced by the Defense Waste Processing Facility (DWPF) will have to consistently be more durable than a benchmark glass (evaluated using a short-term leach test), with high confidence. The DWPF has developed a Glass Product Control Program to comply with this specification. However, it is not clear what relevance product consistency has on long-term glass performance. In this report, the authors show that DWPF glass, produced in compliance with this specification, can be expected to effectively limit the release of soluble radionuclides to natural environments. However, the release of insoluble radionuclides to the environment will be limited by their solubility, and not glass durability

  18. High temperature measurement of water vapor absorption

    Science.gov (United States)

    Keefer, Dennis; Lewis, J. W. L.; Eskridge, Richard

    1985-01-01

    An investigation was undertaken to measure the absorption coefficient, at a wavelength of 10.6 microns, for mixtures of water vapor and a diluent gas at high temperature and pressure. The experimental concept was to create the desired conditions of temperature and pressure in a laser absorption wave, similar to that which would be created in a laser propulsion system. A simplified numerical model was developed to predict the characteristics of the absorption wave and to estimate the laser intensity threshold for initiation. A non-intrusive method for temperature measurement utilizing optical laser-beam deflection (OLD) and optical spark breakdown produced by an excimer laser, was thoroughly investigated and found suitable for the non-equilibrium conditions expected in the wave. Experiments were performed to verify the temperature measurement technique, to screen possible materials for surface initiation of the laser absorption wave and to attempt to initiate an absorption wave using the 1.5 kW carbon dioxide laser. The OLD technique was proven for air and for argon, but spark breakdown could not be produced in helium. It was not possible to initiate a laser absorption wave in mixtures of water and helium or water and argon using the 1.5 kW laser, a result which was consistent with the model prediction.

  19. Time-consistent actuarial valuations

    NARCIS (Netherlands)

    Pelsser, A.A.J.; Salahnejhad Ghalehjooghi, A.

    2016-01-01

    Time-consistent valuations (i.e. pricing operators) can be created by backward iteration of one-period valuations. In this paper we investigate the continuous-time limits of well-known actuarial premium principles when such backward iteration procedures are applied. This method is applied to an

  20. Dynamically consistent oil import tariffs

    International Nuclear Information System (INIS)

    Karp, L.; Newbery, D.M.

    1992-01-01

    The standard theory of optimal tariffs considers tariffs on perishable goods produced abroad under static conditions, in which tariffs affect prices only in that period. Oil and other exhaustable resources do not fit this model, for current tariffs affect the amount of oil imported, which will affect the remaining stock and hence its future price. The problem of choosing a dynamically consistent oil import tariff when suppliers are competitive but importers have market power is considered. The open-loop Nash tariff is solved for the standard competitive case in which the oil price is arbitraged, and it was found that the resulting tariff rises at the rate of interest. This tariff was found to have an equilibrium that in general is dynamically inconsistent. Nevertheless, it is shown that necessary and sufficient conditions exist under which the tariff satisfies the weaker condition of time consistency. A dynamically consistent tariff is obtained by assuming that all agents condition their current decisions on the remaining stock of the resource, in contrast to open-loop strategies. For the natural case in which all agents choose their actions simultaneously in each period, the dynamically consistent tariff was characterized, and found to differ markedly from the time-inconsistent open-loop tariff. It was shown that if importers do not have overwhelming market power, then the time path of the world price is insensitive to the ability to commit, as is the level of wealth achieved by the importer. 26 refs., 4 figs

  1. HI Absorption in Merger Remnants

    Science.gov (United States)

    Teng, Stacy H.; Veileux, Sylvain; Baker, Andrew J.

    2012-01-01

    It has been proposed that ultraluminous infrared galaxies (ULIRGs) pass through a luminous starburst phase, followed by a dust-enshrouded AGN phase, and finally evolve into optically bright "naked" quasars once they shed their gas/dust reservoirs through powerful wind events. We present the results of our recent 21- cm HI survey of 21 merger remnants with the Green Bank Telescope. These remnants were selected from the QUEST (Quasar/ULIRG Evolution Study) sample of ULIRGs and PG quasars; our targets are all bolometrically dominated by AGN and sample all phases of the proposed ULIRG -> IR-excess quasar -> optical quasar sequence. We explore whether there is an evolutionary connection between ULIRGs and quasars by looking for the occurrence of HI absorption tracing neutral gas outflows; our results will allow us to identify where along the sequence the majority of a merger's gas reservoir is expelled.

  2. Consistently violating the non-Gaussian consistency relation

    International Nuclear Information System (INIS)

    Mooij, Sander; Palma, Gonzalo A.

    2015-01-01

    Non-attractor models of inflation are characterized by the super-horizon evolution of curvature perturbations, introducing a violation of the non-Gaussian consistency relation between the bispectrum's squeezed limit and the power spectrum's spectral index. In this work we show that the bispectrum's squeezed limit of non-attractor models continues to respect a relation dictated by the evolution of the background. We show how to derive this relation using only symmetry arguments, without ever needing to solve the equations of motion for the perturbations

  3. Separation and preconcentration of lead(II), cobalt(II), and nickel(II) on EDTA immobilized activated carbon cloth prior to flame atomic absorption spectrometric determination in environmental samples

    OpenAIRE

    ALOTHMAN, ZEID ABDULLAH; YILMAZ, ERKAN; HABİLA, MOHAMED; SOYLAK, MUSTAFA

    2015-01-01

    The synthesis and characterization of ethylenediaminetetraacetic acid immobilized activated carbon cloth was performed in the present work. It was used for preconcentration-separation of lead(II), cobalt(II), and nickel(II) at trace levels as an adsorbent. Factors including pH, concentration and volume of eluent, sample and eluent flow rates, sample volume, and effect of coexisting ions on the solid phase extraction of analytes were examined. The preconcentration factor was 50. The detection ...

  4. A new type of artificial structure to achieve broadband omnidirectional acoustic absorption

    KAUST Repository

    Zheng, L.-Y.; Wu, Y.; Zhang, X.-L.; Ni, X.; Chen, Z.-G.; Lu, M.-H.; Chen, Y.-F.

    2013-01-01

    We present a design for a two-dimensional omnidirectional acoustic absorber that can achieve 98.6% absorption of acoustic waves in water, forming an effective acoustic black hole. This artificial black hole consists of an absorptive core coated

  5. Neutron resonance absorption theory

    International Nuclear Information System (INIS)

    Reuss, P.

    1991-11-01

    After some recalls on the physics of neutron resonance absorption during their slowing down, this paper presents the main features of the theoretical developments performed by the french school of reactor physics: the effective reaction rate method so called Livolant-Jeanpierre theory, the generalizations carried out by the author, and the probability table method [fr

  6. Noble gas absorption process

    International Nuclear Information System (INIS)

    Thomas, J.W.

    1975-01-01

    A method of removing a noble gas from air comprising the use of activated carbon filters in stages in which absorption and desorption steps in succession are conducted in order to increase the capacity of the filters is described. (U.S.)

  7. Total photon absorption

    International Nuclear Information System (INIS)

    Carlos, P.

    1985-01-01

    Experimental methods using real photon beams for measurements of total photonuclear absorption cross section σ(Tot : E/sub γ/) are recalled. Most recent σ(Tot : E/sub γ/)results for complex nuclei and in the nucleon resonance region are presented

  8. Chemical Absorption Materials

    DEFF Research Database (Denmark)

    Thomsen, Kaj

    2011-01-01

    Chemical absorption materials that potentially can be used for post combustion carbon dioxide capture are discussed. They fall into five groups, alkanolamines, alkali carbonates, ammonia, amino acid salts, and ionic liquids. The chemistry of the materials is discussed and advantages and drawbacks...

  9. Particulate absorption properties in the Red Sea from hyperspectral particulate absorption spectra

    KAUST Repository

    Tiwari, Surya Prakash

    2018-03-16

    This paper aims to describe the variability of particulate absorption properties using a unique hyperspectral dataset collected in the Red Sea as part of the TARA Oceans expedition. The absorption contributions by phytoplankton (aph) and non-algal particles (aNAP) to the total particulate absorption coefficients are determined using a numerical decomposition method (NDM). The NDM is validated by comparing the NDM derived values of aph and aNAP with simulated values of aph and aNAP are found to be in excellent agreement for the selected wavelengths (i.e., 443, 490, 555, and 676nm) with high correlation coefficient (R2), low root mean square error (RMSE), mean relative error (MRE), and with a slope close to unity. Further analyses showed that the total particulate absorption coefficients (i.e., ap(443)average = 0.01995m−1) were dominated by phytoplankton absorption (i.e., aph(443)average = 0.01743m−1) with a smaller contribution by non-algal particles absorption (i.e., aNAP(443)average = 0.002524m−1). The chlorophyll a is computed using the absorption based Line Height Method (LHM). The derived chlorophyll-specific absorption ((a⁎ph = aph(λ)/ChlLH)) showed more variability in the blue part of spectrum as compared to the red part of spectrum representative of the package effect and changes in pigment composition. A new parametrization proposed also enabled the reconstruction of a⁎ph(λ) for the Red Sea. Comparison of derived spectral constants with the spectral constants of existing models showed that our study A(λ) values are consistent with the existing values, despite there is a divergence with the B(λ) values. This study provides valuable information derived from the particulate absorption properties and its spectral variability and this would help us to determine the relationship between the phytoplankton absorption coefficients and chlorophyll a and its host of variables for the Red Sea.

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

    Science.gov (United States)

    Altunay, Nail; Yıldırım, Emre; Gürkan, Ramazan

    2018-04-15

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

  11. Consistence of Network Filtering Rules

    Institute of Scientific and Technical Information of China (English)

    SHE Kun; WU Yuancheng; HUANG Juncai; ZHOU Mingtian

    2004-01-01

    The inconsistence of firewall/VPN(Virtual Private Network) rule makes a huge maintainable cost.With development of Multinational Company,SOHO office,E-government the number of firewalls/VPN will increase rapidly.Rule table in stand-alone or network will be increased in geometric series accordingly.Checking the consistence of rule table manually is inadequate.A formal approach can define semantic consistence,make a theoretic foundation of intelligent management about rule tables.In this paper,a kind of formalization of host rules and network ones for auto rule-validation based on SET theory were proporsed and a rule validation scheme was defined.The analysis results show the superior performance of the methods and demonstrate its potential for the intelligent management based on rule tables.

  12. Self-consistent radial sheath

    International Nuclear Information System (INIS)

    Hazeltine, R.D.

    1988-12-01

    The boundary layer arising in the radial vicinity of a tokamak limiter is examined, with special reference to the TEXT tokamak. It is shown that sheath structure depends upon the self-consistent effects of ion guiding-center orbit modification, as well as the radial variation of E /times/ B-induced toroidal rotation. Reasonable agreement with experiment is obtained from an idealized model which, however simplified, preserves such self-consistent effects. It is argued that the radial sheath, which occurs whenever confining magnetic field-lines lie in the plasma boundary surface, is an object of some intrinsic interest. It differs from the more familiar axial sheath because magnetized charges respond very differently to parallel and perpendicular electric fields. 11 refs., 1 fig

  13. Lagrangian multiforms and multidimensional consistency

    Energy Technology Data Exchange (ETDEWEB)

    Lobb, Sarah; Nijhoff, Frank [Department of Applied Mathematics, University of Leeds, Leeds LS2 9JT (United Kingdom)

    2009-10-30

    We show that well-chosen Lagrangians for a class of two-dimensional integrable lattice equations obey a closure relation when embedded in a higher dimensional lattice. On the basis of this property we formulate a Lagrangian description for such systems in terms of Lagrangian multiforms. We discuss the connection of this formalism with the notion of multidimensional consistency, and the role of the lattice from the point of view of the relevant variational principle.

  14. Consistency and Communication in Committees

    OpenAIRE

    Inga Deimen; Felix Ketelaar; Mark T. Le Quement

    2013-01-01

    This paper analyzes truthtelling incentives in pre-vote communication in heterogeneous committees. We generalize the classical Condorcet jury model by introducing a new informational structure that captures consistency of information. In contrast to the impossibility result shown by Coughlan (2000) for the classical model, full pooling of information followed by sincere voting is an equilibrium outcome of our model for a large set of parameter values implying the possibility of ex post confli...

  15. Deep Feature Consistent Variational Autoencoder

    OpenAIRE

    Hou, Xianxu; Shen, Linlin; Sun, Ke; Qiu, Guoping

    2016-01-01

    We present a novel method for constructing Variational Autoencoder (VAE). Instead of using pixel-by-pixel loss, we enforce deep feature consistency between the input and the output of a VAE, which ensures the VAE's output to preserve the spatial correlation characteristics of the input, thus leading the output to have a more natural visual appearance and better perceptual quality. Based on recent deep learning works such as style transfer, we employ a pre-trained deep convolutional neural net...

  16. Attenuation studies near K-absorption edges using Compton ...

    Indian Academy of Sciences (India)

    The results are consistent with theoretical values derived from the XCOM package. Keywords. Photon interaction; 241Am; gamma ray attenuation; Compton scattering; absorption edge; rare earth elements. PACS Nos 32.80.-t; 32.90.+a. 1. Introduction. Photon interaction studies at energies around the absorption edge have ...

  17. Consistency Analysis of Nearest Subspace Classifier

    OpenAIRE

    Wang, Yi

    2015-01-01

    The Nearest subspace classifier (NSS) finds an estimation of the underlying subspace within each class and assigns data points to the class that corresponds to its nearest subspace. This paper mainly studies how well NSS can be generalized to new samples. It is proved that NSS is strongly consistent under certain assumptions. For completeness, NSS is evaluated through experiments on various simulated and real data sets, in comparison with some other linear model based classifiers. It is also ...

  18. Optimization of Flame Atomic Absorption Spectrometry for ...

    African Journals Online (AJOL)

    Optimization of Flame Atomic Absorption Spectrometry for Measurement of High Concentrations of Arsenic and Selenium. ... This procedure allowed a rapid determination of As from minimum 4.462 mg/L to higher concentrations without sample pretreatment. Besides As, this method successfully measured Se concentrations ...

  19. A method optimization study for atomic absorption ...

    African Journals Online (AJOL)

    A sensitive, reliable and relative fast method has been developed for the determination of total zinc in insulin by atomic absorption spectrophotometer. This designed study was used to optimize the procedures for the existing methods. Spectrograms of both standard and sample solutions of zinc were recorded by measuring ...

  20. Evaluation of atomic absorption Spectrophotometry (ashing, non ...

    African Journals Online (AJOL)

    Three commonly used techniques, namely atomic absorption spectrophotometry (AAS-Ashing and AAS-Non Ashing) and titrimetry (potassium permanganate titration) have been evaluated in this study to determine the calcium content in six food samples whose calcium levels ranged from 0 to more than 250mg/100g ...

  1. Absorption-Edge-Modulated Transmission Spectra for Water Contaminant Monitoring

    Science.gov (United States)

    2016-03-31

    Naval Research Laboratory Washington, DC 20375-5320 NRL/MR/6390--16-9675 Absorption- Edge -Modulated Transmission Spectra for Water Contaminant...ABSTRACT c. THIS PAGE 18. NUMBER OF PAGES 17. LIMITATION OF ABSTRACT Absorption- Edge -Modulated Transmission Spectra for Water Contaminant Monitoring...contaminants, within a volume of sampled solution, requires sufficient sensitivity. The present study examines the sensitivity of absorption- edge

  2. The determination of some heavy metals in food samples by flame atomic absorption spectrometry after their separation-preconcentration on bis salicyl aldehyde, 1,3 propan diimine (BSPDI) loaded on activated carbon

    International Nuclear Information System (INIS)

    Ghaedi, M.; Shokrollahi, A.; Kianfar, A.H.; Mirsadeghi, A.S.; Pourfarokhi, A.; Soylak, M.

    2008-01-01

    A sensitive and simple method for the simultaneous preconcentration of Cr 3+ , Fe 3+ , Cu 2+ , Ni 2+ , Co 2+ and Zn 2+ in real samples has been reported. The method is based on the adsorption of analytes on bis salicyl aldehyde, 1,3 propan diimine (BSPDI) loaded on activated carbon. The adsorbed metals on modified activated carbon were eluted using 8 mL of 2 mol L -1 nitric acid in acetone or 10 mL of 4 mol L -1 HNO 3 . The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally quantitative. The method has been successfully applied for these metals content evaluation in some food samples

  3. Sustainable Absorption Panels from Agricultural Wastes

    Directory of Open Access Journals (Sweden)

    Ismail F.Z.

    2014-01-01

    Full Text Available Noise has become a serious environmental problem and there are demands for alternative sustainable materials which capable to reduce the noise level at various frequency ranges. Therefore, the aim of this research is to study the potential of turning the agricultural waste and waste paper into a sound absorption panel. For the purpose of this study, combination of two materials was under studied; coconut coir fibre from agriculture waste and shredded waste paper from the office. There were two main objective of the research; first is to develop absorption panels from coconut coir powder that available locally with a combination of shredded paper at different percentage of mixture. Second objective is to identify the absorption rate of the panels. The study encompasses the fabrication of the particle board using the coconut husk powder mix with shredded waste paper and using the gypsum powder as the binder for the two materials. Four acoustic panels of size 0.5m x 0.5m and 0.012 m thick were fabricated with different mix ratio; 25% of coconut coir powder mixed with 75% of shredded waste papers for sample 1, 50% both of the material for sample 2, 75% of coconut coir powder mixed with 25% of shredded waste paper for sample 3, and lastly 100% of coconut coir powder for sample 4. The absorption coefficient of the panels was tested in a reverberation chamber and in accordance with ISO 354:1985 standards. Based on the results, sample 1 gave the highest absorption coefficient compared to sample 2, 3 and 4. It can be concluded that the acoustic panel made from a mixture of 25% coconut coir powder with 75% shredded waste paper provided higher absorption coefficient compared to the performance of the other samples. This might be caused by the size of the coir powder which is very small, creating less void space in between the panel and thus causing it to absorb less sound. Since sound absorption is very much affected by the availability of void space of

  4. Gamma ray auto absorption correction evaluation methodology

    International Nuclear Information System (INIS)

    Gugiu, Daniela; Roth, Csaba; Ghinescu, Alecse

    2010-01-01

    Neutron activation analysis (NAA) is a well established nuclear technique, suited to investigate the microstructural or elemental composition and can be applied to studies of a large variety of samples. The work with large samples involves, beside the development of large irradiation devices with well know neutron field characteristics, the knowledge of perturbing phenomena and adequate evaluation of correction factors like: neutron self shielding, extended source correction, gamma ray auto absorption. The objective of the works presented in this paper is to validate an appropriate methodology for gamma ray auto absorption correction evaluation for large inhomogeneous samples. For this purpose a benchmark experiment has been defined - a simple gamma ray transmission experiment, easy to be reproduced. The gamma ray attenuation in pottery samples has been measured and computed using MCNP5 code. The results show a good agreement between the computed and measured values, proving that the proposed methodology is able to evaluate the correction factors. (authors)

  5. Spherical sampling

    CERN Document Server

    Freeden, Willi; Schreiner, Michael

    2018-01-01

    This book presents, in a consistent and unified overview, results and developments in the field of today´s spherical sampling, particularly arising in mathematical geosciences. Although the book often refers to original contributions, the authors made them accessible to (graduate) students and scientists not only from mathematics but also from geosciences and geoengineering. Building a library of topics in spherical sampling theory it shows how advances in this theory lead to new discoveries in mathematical, geodetic, geophysical as well as other scientific branches like neuro-medicine. A must-to-read for everybody working in the area of spherical sampling.

  6. Automated sequential injection-microcolumn approach with on-line flame atomic absorption spectrometric detection for implementing metal fractionation schemes of homogeneous and non-homogeneous solid samples of environmental interest

    DEFF Research Database (Denmark)

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    spectrometric detection and used for the determination of Cu as a model analyte, the potentials of this novel hyphenated approach are demonstrated by the ability of handling up to 300 mg sample of a nonhomogeneous sewage amended soil (viz., CRM 483). The three steps of the endorsed Standards, Measurements...

  7. Surfactant-assisted emulsification dispersive liquid-liquid microextraction using 2-thenoyltrifluoroacetone as a chelating agent coupled with electrothermal atomic absorption spectrometry for the speciation of chromium in water and rice samples.

    Science.gov (United States)

    Dokpikul, Nattawut; Chaiyasith, Wipharat Chuachuad; Sananmuang, Ratana; Ampiah-Bonney, Richmond J

    2018-04-25

    A novel method was developed by SAE-DLLME for chromium speciation in water and rice samples using 2-thenoyltrifluoroacetone (TTA) as a chelating reagent by ETAAS. The speciation of Cr(III) and Cr(VI) was achieved by complexation of Cr(III)-TTA and the total Cr was measured after reduction of Cr(VI) to Cr. The calibration graph was linear in the range of 0.02-2.50 µg L -1 , with a detection limit of 0.0052 µg L -1 . The %RSD was in range of 2.90-3.30% at 0.5, 1.5 and 2.5 µg L -1 of Cr(III), n = 5 and the EF was 54.47. The method was applied to chromium speciation and total chromium determination in real samples and gave recoveries in the range of 96.2-103.5% and 97.1-102.7% for Cr(III) and Cr(VI) in water samples and 93.7-103.5% of total Cr in rice samples. The accuracy of the method was evaluated by analysis of SRM 1573a with good agreement compared to the certified value. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Determination of inorganic mercury and total mercury in biological and environmental samples by flow injection-cold vapor-atomic absorption spectrometry using sodium borohydride as the sole reducing agent

    International Nuclear Information System (INIS)

    Rio Segade, Susana; Tyson, Julian F.

    2003-01-01

    A simple, fast, precise and accurate method to determine inorganic mercury and total mercury in biological and environmental samples was developed. The optimized flow-injection mercury system permitted the separate determination of inorganic mercury and total mercury using sodium borohydride as reducing agent. Inorganic mercury was selectively determined after reduction with 10 -4 % w/v sodium borohydride, while total mercury was determined after reduction with 0.75% w/v sodium borohydride. The calibration graphs were linear up to 30 ng ml -1 . The detection limits of the method based on three times the standard deviation of the blank were 24 and 3.9 ng l -1 for total mercury and inorganic mercury determination, respectively. The relative standard deviation was less than 1.5% for a 10 ng ml -1 mercury standard. As a means of checking method performance, deionized water and pond water samples were spiked with methylmercury and inorganic mercury; quantitative recovery for total mercury and inorganic mercury was obtained. The accuracy of the method was verified by analyzing alkaline and acid extracts of five biological and sediment reference materials. Microwave-assisted extraction procedures resulted in higher concentrations of recovered mercury species, lower matrix interference with mercury determination and less time involved in sample treatment than conventional extraction procedures. The standard addition method was only needed for calibration when biological samples were analyzed. The detection limits were in the range of 1.2-19 and 6.6-18 ng g -1 in biological and sediment samples for inorganic mercury and total mercury determination, respectively

  9. Time-resolved absorption measurements on OMEGA

    International Nuclear Information System (INIS)

    Jaanimagi, P.A.; DaSilva, L.; Delettrez, J.; Gregory, G.G.; Richardson, M.C.

    1986-01-01

    Time-resolved measurements of the incident laser light that is scattered and/or refracted from targets irradiated by the 24 uv-beam OMEGA laser at LLE, have provided some interesting features related to time-resolved absorption. The decrease in laser absorption characteristic of irradiating a target that implodes during the laser pulse has been observed. The increase in absorption expected as the critical density surface moves from a low to a high Z material in the target has also been noted. The detailed interpretation of these results is made through comparisons with simulation using the code LILAC, as well as with streak data from time-resolved x-ray imaging and spectroscopy. In addition, time and space-resolved imaging of the scattered light yields information on laser irradiation uniformity conditions on the target. The report consists of viewgraphs

  10. Linear absorptive dielectrics

    Science.gov (United States)

    Tip, A.

    1998-06-01

    Starting from Maxwell's equations for a linear, nonconducting, absorptive, and dispersive medium, characterized by the constitutive equations D(x,t)=ɛ1(x)E(x,t)+∫t-∞dsχ(x,t-s)E(x,s) and H(x,t)=B(x,t), a unitary time evolution and canonical formalism is obtained. Given the complex, coordinate, and frequency-dependent, electric permeability ɛ(x,ω), no further assumptions are made. The procedure leads to a proper definition of band gaps in the periodic case and a new continuity equation for energy flow. An S-matrix formalism for scattering from lossy objects is presented in full detail. A quantized version of the formalism is derived and applied to the generation of Čerenkov and transition radiation as well as atomic decay. The last case suggests a useful generalization of the density of states to the absorptive situation.

  11. Consistent ranking of volatility models

    DEFF Research Database (Denmark)

    Hansen, Peter Reinhard; Lunde, Asger

    2006-01-01

    We show that the empirical ranking of volatility models can be inconsistent for the true ranking if the evaluation is based on a proxy for the population measure of volatility. For example, the substitution of a squared return for the conditional variance in the evaluation of ARCH-type models can...... variance in out-of-sample evaluations rather than the squared return. We derive the theoretical results in a general framework that is not specific to the comparison of volatility models. Similar problems can arise in comparisons of forecasting models whenever the predicted variable is a latent variable....

  12. Iron absorption studies

    International Nuclear Information System (INIS)

    Ekenved, G.

    1976-01-01

    The main objective of the present work was to study iron absorption from different iron preparations in different types of subjects and under varying therapeutic conditions. The studies were performed with different radioiron isotope techniques and with a serum iron technique. The preparations used were solutions of ferrous sulphate and rapidly-disintegrating tablets containing ferrous sulphate, ferrous fumarate and ferrous carbonate and a slow-release ferrous sulphate tablet of an insoluble matrix type (Duroferon Durules). The serum iron method was evaluated and good correlation was found between the serum iron response and the total amount of iron absorbed after an oral dose of iron given in solution or in tablet form. New technique for studying the in-vivo release properties of tablets was presented. Iron tablets labelled with a radio-isotope were given to healthy subjects. The decline of the radioactivity in the tablets was followed by a profile scanning technique applied to different types of iron tablets. The release of iron from the two types of tablets was shown to be slower in vivo than in vitro. It was found that co-administration of antacids and iron tablets led to a marked reduction in the iron absorption and that these drugs should not be administered sumultaneously. A standardized meal markedly decreased the absorbability of iron from iron tablets. The influence of the meal was more marked with rapidly-disintegrating than with slow-release ferrous sulphate tablets. The absorption from rapidly-disintegrating and slow-release ferrous sulphate tablets was compared under practical clinical conditions during an extended treatment period. The studies were performed in healthy subjects, blood donors and patients with iron deficiency anaemia and it was found that the absorption of iron from the slow-release tablets was significantly better than from the rapidly-disintegrating tablets in all three groups of subjects. (author)

  13. Total Absorption Spectroscopy

    International Nuclear Information System (INIS)

    Rubio, B.; Gelletly, W.

    2007-01-01

    The problem of determining the distribution of beta decay strength (B(GT)) as a function of excitation energy in the daughter nucleus is discussed. Total Absorption Spectroscopy is shown to provide a way of determining the B(GT) precisely. A brief history of such measurements and a discussion of the advantages and disadvantages of this technique, is followed by examples of two recent studies using the technique. (authors)

  14. Maintaining consistency in distributed systems

    Science.gov (United States)

    Birman, Kenneth P.

    1991-01-01

    In systems designed as assemblies of independently developed components, concurrent access to data or data structures normally arises within individual programs, and is controlled using mutual exclusion constructs, such as semaphores and monitors. Where data is persistent and/or sets of operation are related to one another, transactions or linearizability may be more appropriate. Systems that incorporate cooperative styles of distributed execution often replicate or distribute data within groups of components. In these cases, group oriented consistency properties must be maintained, and tools based on the virtual synchrony execution model greatly simplify the task confronting an application developer. All three styles of distributed computing are likely to be seen in future systems - often, within the same application. This leads us to propose an integrated approach that permits applications that use virtual synchrony with concurrent objects that respect a linearizability constraint, and vice versa. Transactional subsystems are treated as a special case of linearizability.

  15. Self-consistent asset pricing models

    Science.gov (United States)

    Malevergne, Y.; Sornette, D.

    2007-08-01

    self-consistency condition derives a risk-factor decomposition in the multi-factor case which is identical to the principal component analysis (PCA), thus providing a direct link between model-driven and data-driven constructions of risk factors. This correspondence shows that PCA will therefore suffer from the same limitations as the CAPM and its multi-factor generalization, namely lack of out-of-sample explanatory power and predictability. In the multi-period context, the self-consistency conditions force the betas to be time-dependent with specific constraints.

  16. Identifying the perfect absorption of metamaterial absorbers

    Science.gov (United States)

    Duan, G.; Schalch, J.; Zhao, X.; Zhang, J.; Averitt, R. D.; Zhang, X.

    2018-01-01

    We present a detailed analysis of the conditions that result in unity absorption in metamaterial absorbers to guide the design and optimization of this important class of functional electromagnetic composites. Multilayer absorbers consisting of a metamaterial layer, dielectric spacer, and ground plane are specifically considered. Using interference theory, the dielectric spacer thickness and resonant frequency for unity absorption can be numerically determined from the functional dependence of the relative phase shift of the total reflection. Further, using transmission line theory in combination with interference theory we obtain analytical expressions for the unity absorption resonance frequency and corresponding spacer layer thickness in terms of the bare resonant frequency of the metamaterial layer and metallic and dielectric losses within the absorber structure. These simple expressions reveal a redshift of the unity absorption frequency with increasing loss that, in turn, necessitates an increase in the thickness of the dielectric spacer. The results of our analysis are experimentally confirmed by performing reflection-based terahertz time-domain spectroscopy on fabricated absorber structures covering a range of dielectric spacer thicknesses with careful control of the loss accomplished through water absorption in a semiporous polyimide dielectric spacer. Our findings can be widely applied to guide the design and optimization of the metamaterial absorbers and sensors.

  17. Dynamics of water absorption through superabsorbent polymer

    Science.gov (United States)

    Chang, Sooyoung; Kim, Wonjung

    2017-11-01

    Superabsorbent polymers (SAPs) consist of hydrophilic cross-linked polymer networks that can absorb and retain a great amount of water relative to their own mass, so that they are widely used for disposable diapers and holding soil moisture in agriculture. SAPs are typically available in the form of submillimeter-sized particles, and the water absorption is driven by capillary flows between particles as well as diffusion that entail swelling. Although the control of water absorption of SAPs is important in engineering applications, but the dynamics of water absorption in SAP particles has not been fully understood. We examine the dynamics of the water absorption of sodium polyacrylate, one of the most common SAP. We experimentally measured the water absorption of sodium polyacrylate particles in one-dimensional confined channel. The water flows through the particles were analyzed by capillarity dominant at the early stage and by diffusion involving volume expansion critical at a later stage. The results provide a quantitative basis of the hydrodynamic analysis of the water flow through SAP particles from a macroscopic point of view, facilitating the prediction of water uptake of SAPs in hygienic and agricultural applications. This work was supported by the National Research Foundation of Korea (NRF) Grant funded by the Korea government (MSIP) (No.2015R1A2A2A04006181).

  18. Microwave absorption studies of MgB 2 superconductor

    Indian Academy of Sciences (India)

    Microwave absorption studies have been carried out on MgB2 superconductor using a standard X-band EPR spectrometer. The modulated low-field microwave absorption signals recorded for polycrystalline (grain size ∼ 10m) samples suggested the absence of weak-link character. The field dependent direct microwave ...

  19. Possible stretched exponential parametrization for humidity absorption in polymers.

    Science.gov (United States)

    Hacinliyan, A; Skarlatos, Y; Sahin, G; Atak, K; Aybar, O O

    2009-04-01

    Polymer thin films have irregular transient current characteristics under constant voltage. In hydrophilic and hydrophobic polymers, the irregularity is also known to depend on the humidity absorbed by the polymer sample. Different stretched exponential models are studied and it is shown that the absorption of humidity as a function of time can be adequately modelled by a class of these stretched exponential absorption models.

  20. Errors in instumental neutron activation analysis caused by matrix absorption

    International Nuclear Information System (INIS)

    Croudace, I.W.

    1979-01-01

    Instrumental neutron activation analysis of the geochemically important rare earth elements, together with Ta, Hf and U involves energies below 150 keV where absorption of radiation by the sample becomes inceasingly important. Determinations of the total mass absorption coefficients have been made. (C.F.)

  1. Sound absorption with green materials

    Science.gov (United States)

    Trematerra, Amelia; Lombardi, Ilaria

    2017-07-01

    Green materials are a valid alternative to traditional materials that are by-products of processing oil. At the end of their useful life, green materials can be disposed of without polluting the environment. They are now being used in the construction and automotive industries. While, studies are currently being carried out in the aviation sector on the use of green materials for non-structural components of airplanes. Green materials can be used to improve the acoustic comfort inside buildings as well as mitigate reverberation, echoes effects and reduce the transmission of noise between rooms. In this paper, the acoustic measurements of the properties of green materials are reported. The absorption coefficient of samples of the materials were measured in the frequency range from 200 Hz to 2,000 Hz with an impedance tube, with the flow resistance being measured.

  2. Decentralized Consistent Updates in SDN

    KAUST Repository

    Nguyen, Thanh Dang

    2017-04-10

    We present ez-Segway, a decentralized mechanism to consistently and quickly update the network state while preventing forwarding anomalies (loops and blackholes) and avoiding link congestion. In our design, the centralized SDN controller only pre-computes information needed by the switches during the update execution. This information is distributed to the switches, which use partial knowledge and direct message passing to efficiently realize the update. This separation of concerns has the key benefit of improving update performance as the communication and computation bottlenecks at the controller are removed. Our evaluations via network emulations and large-scale simulations demonstrate the efficiency of ez-Segway, which compared to a centralized approach, improves network update times by up to 45% and 57% at the median and the 99th percentile, respectively. A deployment of a system prototype in a real OpenFlow switch and an implementation in P4 demonstrate the feasibility and low overhead of implementing simple network update functionality within switches.

  3. MNC Knowledge Transfer, Subsidiary Absorptive Capacity and HRM

    DEFF Research Database (Denmark)

    Minbaeva, Dana; Pedersen, Torben; Björkman, Ingmar

    2014-01-01

    Based on a sample of 169 subsidiaries of multinational corporations (MNCs) operating in the USA, Russia, and Finland, this paper investigates the relationship between MNC subsidiary HRM practices, absorptive capacity and knowledge transfer. First, we examine the relationship between the application...... of specific HRM practices and the level of the absorptive capacity. Second, we suggest that absorptive capacity should be conceptualized as being comprised of both employees’ ability and motivation. Further, results indicate that both ability and motivation (absorptive capacity) are needed to facilitate...

  4. Gold analysis by the gamma absorption technique

    International Nuclear Information System (INIS)

    Kurtoglu, Arzu; Tugrul, A.B.

    2003-01-01

    Gold (Au) analyses are generally performed using destructive techniques. In this study, the Gamma Absorption Technique has been employed for gold analysis. A series of different gold alloys of known gold content were analysed and a calibration curve was obtained. This curve was then used for the analysis of unknown samples. Gold analyses can be made non-destructively, easily and quickly by the gamma absorption technique. The mass attenuation coefficients of the alloys were measured around the K-shell absorption edge of Au. Theoretical mass attenuation coefficient values were obtained using the WinXCom program and comparison of the experimental results with the theoretical values showed generally good and acceptable agreement

  5. Absorption of carbon dioxide in waste tanks

    International Nuclear Information System (INIS)

    Hobbs, D.T.

    1987-01-01

    Air flow rates and carbon dioxide concentrations of air entering and exiting eight H-Area waste tanks were monitored for a period of one year. The average instanteous concentration of carbon dioxide in air is within the range reported offsite, and therefore is not affect by operation of the coal-fired power plant adjacent to the tank farm. Waste solutions in each of the tanks were observed to be continuously absorbing carbon dioxide. The rate of absorption of carbon dioxide decreased linearly with the pH of the solution. Personnel exposure associated with the routine sampling and analysis of radioactive wastes stored at SRP to determine the levels of corrosion inhibitors in solution could be reduced by monitoring the absorption of carbon dioxide and using the relationship between pH and carbon dioxide absorption to determine the free hydroxide concentration in solution

  6. Absorption of ultraviolet radiation by antarctic phytoplankton

    Energy Technology Data Exchange (ETDEWEB)

    Vernet, M.; Mitchell, B.G. (Univ. of California-San Diego, La Jolla (United States))

    1990-01-09

    Antarctic phytoplankton contain UV-absorbing compounds that may block damaging radiation. Compounds that absorb from 320-340 nm were observed in spectral absorption of both particulates and in methanol extracts of the particulates. The decrease in the total concentration of these UV compounds with respect to chlorophyll a, as measured by the ratio of in vitro absorption at 335 nm to absorption at 665 nm is variable and decreases with depth. We observed up to 5-fold decrease in this ratio for samples within the physically mixes surface layer. The absorption of UV radiation in methanol extracts, which peaks from 320 to 340 nm, may be composed of several compounds. Shifts in peak absorption with depth (for example, from 331 nm at surface to 321 nm at 75 m), may be interpreted as a change in composition. Ratios of protective yellow xanthophylls (diadinoxanthin + diatoxanthin) to photosynthetic fucoxanthin-like pigments have highest values in surface waters. As these pigments also absorb in the near UV, their function might extend to protection as well as utilization of UV radiation for photosynthesis. We document strong absorption in the UV from 320-330 nm for Antarctic marine particulates. Below this region of the solar energy spectrum, absolute energy levels of incident radiation drop off dramatically. Only wavelengths shorter than about 320 nm will be significantly enhanced due to ozone depletion. If the absorption we observed serves a protective role for phytoplankton photosynthesis, it appears the peak band is in the region where solar energy increases rapidly, and not in the region where depletion would cause significant variations in absolute flux.

  7. Comparative study of five varieties of spodumene through optical absorption

    International Nuclear Information System (INIS)

    Fujii, A.T.; Isotani, S.

    1983-11-01

    A comparative study of five varieties of spodumene crystals from Brazil through optical absorption spectroscopy, classified according to the colours lylac, colourless I, colourless II, yellow and green is reported. This series shows a consistent increase of the [Fe]/[Mn] ratio. The principal bands in the yellow sample are at 7,000 and 9,000 cm -1 , and in the green sample besides these bands a band at 16,000 cm -1 is observed. In lylac, colourless I and colourless II samples, the principal bands are at 18,000 cm -1 and when irradiated two new bands appears at 15,700 cm -1 (E perpendicular to c) and 11,000 cm -1 (K perpendicular to c). It is suggested that in green and yellow samples the bands are due to Fe 2+ (at 7,000 cm -1 and 9,000 cm -1 ) and due to Fe 2+ - Fe 3+ charge transfer (at 16,000 cm -1 ). In lylac and colourless I samples the model for Mn 3+ at two different sites is applied. The colourless II corresponds to the case in which Mn 3+ is at one site alone, being prohibited from occupying the second site due to higher Fe concentration. (Author) [pt

  8. Self-consistent electrodynamic scattering in the symmetric Bragg case

    International Nuclear Information System (INIS)

    Campos, H.S.

    1988-01-01

    We have analyzed the symmetric Bragg case, introducing a model of self consistent scattering for two elliptically polarized beams. The crystal is taken as a set of mathematical planes, each of them defined by a surface density of dipoles. We have considered the mesofield and the epifield differently from that of the Ewald's theory and, we assumed a plane of dipoles and the associated fields as a self consistent scattering unit. The exact analytical treatment when applied to any two neighbouring planes, results in a general and self consistent Bragg's equation, in terms of the amplitude and phase variations. The generalized solution for the set of N planes was obtained after introducing an absorption factor in the incident radiation, in two ways: (i) the analytical one, through a rule of field similarity, which says that the incidence occurs in both faces of the all crystal planes and also, through a matricial development with the Chebyshev polynomials; (ii) using the numerical solution we calculated, iteratively, the reflectivity, the reflection phase, the transmissivity, the transmission phase and the energy. The results are showed through reflection and transmission curves, which are characteristics as from kinematical as dynamical theories. The conservation of the energy results from the Ewald's self consistency principle is used. In the absorption case, the results show that it is not the only cause for the asymmetric form in the reflection curves. The model contains basic elements for a unified, microscope, self consistent, vectorial and exact formulation for interpretating the X ray diffraction in perfect crystals. (author)

  9. Optical absorption in dendrimers

    International Nuclear Information System (INIS)

    Supritz, C.; Engelmann, A.; Reineker, P.

    2004-01-01

    Dendrimers are highly branched molecules, which are expected to be useful, for example, as efficient artificial light harvesting systems in nano-technological applications. There are two different classes of dendrimers: compact dendrimers with constant distance between neighboring branching points throughout the macromolecule and extended dendrimers, where this distance increases from the system periphery to the center. We investigate the linear absorption spectra of these dendrimer types using the Frenkel exciton concept. The electron-phonon interaction is taken into account by introducing a heat bath that interacts with the exciton in a stochastic manner

  10. Rapidly variable relatvistic absorption

    Science.gov (United States)

    Parker, M.; Pinto, C.; Fabian, A.; Lohfink, A.; Buisson, D.; Alston, W.; Jiang, J.

    2017-10-01

    I will present results from the 1.5Ms XMM-Newton observing campaign on the most X-ray variable AGN, IRAS 13224-3809. We find a series of nine absorption lines with a velocity of 0.24c from an ultra-fast outflow. For the first time, we are able to see extremely rapid variability of the UFO features, and can link this to the X-ray variability from the inner accretion disk. We find a clear flux dependence of the outflow features, suggesting that the wind is ionized by increasing X-ray emission.

  11. Geospatial Absorption and Regional Effects

    Directory of Open Access Journals (Sweden)

    IOAN MAC

    2009-01-01

    Full Text Available The geospatial absorptions are characterized by a specific complexity both in content and in their phenomenological and spatial manifestation fields. Such processes are differentiated according to their specificity to pre-absorption, absorption or post-absorption. The mechanisms that contribute to absorption are extremely numerous: aggregation, extension, diffusion, substitution, resistivity (resilience, stratification, borrowings, etc. Between these mechanisms frequent relations are established determining an amplification of the process and of its regional effects. The installation of the geographic osmosis phenomenon in a given territory (a place for example leads to a homogenization of the geospatial state and to the installation of the regional homogeneity.

  12. H2, CO, and dust absorption through cold molecular clouds

    Science.gov (United States)

    Lacy, John H.; Sneden, Chris; Kim, Hwihyun; Jaffe, Daniel Thomas

    2017-06-01

    We have made observations with IGRINS on the Harlan J. Smith telescope at McDonald Observatory of near-infrared absorption by H2, CO, and dust toward stars behind molecular clouds, primarily the TMC. Prior to these observations, the abundance of H2 in molecular clouds, relative to the commonly used tracer CO, had only been measured toward a few embedded stars, which may be surrounded by atypical gas. The new observations provide a representative sample of these molecules in cold molecular gas. We find N(H2)/Av ~ 0.9e+21, N(CO)/Av ~ 1.6e+17, and H2/CO ~ 6000. The measured H2/CO ratio is consistent with that measured toward embedded stars in various molecular clouds, but half that derived from mm-wave observations of CO emission and star counts or other determinations of Av.

  13. Gastrointestinal absorption of plutonium by the Marshall Islanders

    International Nuclear Information System (INIS)

    Sun, L.C.; Meinhold, C.B.

    1997-01-01

    The gastrointestinal absorption constant (f 1 ) is a critical parameter in assessing systemic uptake following the ingestion of a radioactive material and in monitoring such intakes. This study addresses the latter, particularly, for plutonium. and from environmental measurements derives an f 1 value of 4 x 10 -4 for the Marshallese population. The uncertainty associated with the methodology and measurements used in this f 1 value assessment is evaluated. This evaluation takes into account the results from 24-h urine samples and the particular lifestyle of the Marshallese. Plutonium intake resulting from soil consumption is a primary parameter in this evaluation; for this study, it was assumed to be 500 mg d -1 . The f 1 , value determined here is consistent with the values in ICRP Publication 67 of 5 x 10 -4 for ages 1 to adult, and is the same as that suggested by the NRPB. 80 refs., 5 tabs

  14. Determinação de fósforo em aços por espectrometria de absorção atômica no forno de grafite Determination of phosphorus in steel samples by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Adilson José Curtius

    1998-06-01

    Full Text Available A method for the determination of phosphorus in steel samples by graphite furnace atomic absorption spectrometry, using the Zeeman effect background correction and the STPF conditions is proposed. The effect of iron (III on the phosphorus signal was studied. It was verified, through the pyrolysis temperature curves, that iron (III is an efficient chemical modifier, thermically stabilizing phosphorus up to 1400ºC. The phosphorus signal increases with the iron (III concentration, but in the range, which corresponds to the usual concentrations of iron in the sample solutions, the increase is small. Phosphorus was determined in three standard reference materials, after its dissolution in a mixture of hydrochloric and perchloric acids in a PTFE bomb. The agreement with the certified concentration values was excellent. Iron (III was added to the reference analytical solutions prepared in the blank of the dissolution, while the sample solutions were measured directly, since they already contained the modifier. The detection limit (k = 2 was 0.0042% of phosphorus in the steel sample.

  15. Absorption spectra of trapped holes in anatase TiO2

    DEFF Research Database (Denmark)

    Zawadzki, Pawel

    2013-01-01

    absorption spectroscopy (TAS), but the understanding of the optical absorption due to trapped carriers in TiO2 is incomplete. On the basis of the generalized Δ self-consistent field density functional theory (Δ-SCF DFT) calculations, we attribute the experimentally observed absorption band at 430-550 nm...

  16. Consistency of color representation in smart phones.

    Science.gov (United States)

    Dain, Stephen J; Kwan, Benjamin; Wong, Leslie

    2016-03-01

    One of the barriers to the construction of consistent computer-based color vision tests has been the variety of monitors and computers. Consistency of color on a variety of screens has necessitated calibration of each setup individually. Color vision examination with a carefully controlled display has, as a consequence, been a laboratory rather than a clinical activity. Inevitably, smart phones have become a vehicle for color vision tests. They have the advantage that the processor and screen are associated and there are fewer models of smart phones than permutations of computers and monitors. Colorimetric consistency of display within a model may be a given. It may extend across models from the same manufacturer but is unlikely to extend between manufacturers especially where technologies vary. In this study, we measured the same set of colors in a JPEG file displayed on 11 samples of each of four models of smart phone (iPhone 4s, iPhone5, Samsung Galaxy S3, and Samsung Galaxy S4) using a Photo Research PR-730. The iPhones are white LED backlit LCD and the Samsung are OLEDs. The color gamut varies between models and comparison with sRGB space shows 61%, 85%, 117%, and 110%, respectively. The iPhones differ markedly from the Samsungs and from one another. This indicates that model-specific color lookup tables will be needed. Within each model, the primaries were quite consistent (despite the age of phone varying within each sample). The worst case in each model was the blue primary; the 95th percentile limits in the v' coordinate were ±0.008 for the iPhone 4 and ±0.004 for the other three models. The u'v' variation in white points was ±0.004 for the iPhone4 and ±0.002 for the others, although the spread of white points between models was u'v'±0.007. The differences are essentially the same for primaries at low luminance. The variation of colors intermediate between the primaries (e.g., red-purple, orange) mirror the variation in the primaries. The variation in

  17. The redshift number density evolution of Mg II absorption systems

    International Nuclear Information System (INIS)

    Chen Zhi-Fu

    2013-01-01

    We make use of the recent large sample of 17 042 Mg II absorption systems from Quider et al. to analyze the evolution of the redshift number density. Regardless of the strength of the absorption line, we find that the evolution of the redshift number density can be clearly distinguished into three different phases. In the intermediate redshift epoch (0.6 ≲ z ≲ 1.6), the evolution of the redshift number density is consistent with the non-evolution curve, however, the non-evolution curve over-predicts the values of the redshift number density in the early (z ≲ 0.6) and late (z ≳ 1.6) epochs. Based on the invariant cross-section of the absorber, the lack of evolution in the redshift number density compared to the non-evolution curve implies the galaxy number density does not evolve during the middle epoch. The flat evolution of the redshift number density tends to correspond to a shallow evolution in the galaxy merger rate during the late epoch, and the steep decrease of the redshift number density might be ascribed to the small mass of halos during the early epoch.

  18. Determination of molybdenum in flotation concentrates by atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Ise, Kazuo

    1978-01-01

    Molybdenum was determined by atomic absorption spectrophotometry in 0.05 N ammoniacal solution after the decomposition of the concentrate with aqua regia. Negros ore from Philippines was used as a flotation feed, which contained chalcopyrites and calcium-magnesium minerals. Among the metals tested copper, iron and the alkaline earths interfered. Less than 50 ppm of copper yielded lower results for molybdenum. Higher results came out with more than 50 ppm of copper. In the presence of iron and citric acid (0.4 g/100 ml) which is a suppressor for hydroxide formation, a lower estimation resulted for molybdenum. Calcium interfered, lower results by 2 and >10% being obtained with respective 2.5 and 20 ppm of calcium. More than 20 ppm of magnesium behaved similarly. Sodium sulfate (0.5 g/100 ml) served as the suppressor for copper, iron and citric acid; 100 ppm each of copper and iron did not interfere in this way. Interferences due to calcium and magnesium (less than 60 ppm) was able to be masked by the addition of sodium silicate (200 ppm as silica). The analysis of flotation products and synthetic samples consisting of molybdenite, chalcopyrite, calcium chloride and magnesium sulfate revealed that the atomic absorption method can be applied to the analysis of the concentrates for molybdenum with an error of about 2%. (auth.)

  19. Self-consistency and sum-rule tests in the Kramers-Kronig analysis of optical data: Applications to aluminum

    International Nuclear Information System (INIS)

    Shiles, E.; Sasaki, T.; Inokuti, M.; Smith, D.Y.

    1980-01-01

    An iterative, self-consistent procedure for the Kramers-Kronig analysis of data from reflectance, ellipsometric, transmission, and electron-energy-loss measurements is presented. This procedure has been developed for practical dispersion analysis since experimentally no single optical function can be readily measured over the entire range of frequencies as required by the Kramers-Kronig relations. The present technique is applied to metallic aluminum as an example. The results are then examined for internal consistency and for systematic errors by various optical sum rules. The present procedure affords a systematic means of preparing a self-consistent set of optical functions provided some optical or energy-loss data are available in all important spectral regions. The analysis of aluminum discloses that currently available data exhibit an excess oscillator strength, apparently in the vicinity of the L edge. A possible explanation is a systematic experimental error in the absorption-coefficient measurements resulting from surface layers: possibly oxides: present in thin-film transmission samples. A revised set of optical functions has been prepared by an ad hoc reduction of the reported absorption coefficient above the L edge by 14%. These revised data lead to a total oscillator strength consistent with the known electron density and are in agreement with dc-conductivity and stopping-power measurements as well as with absorption coefficients inferred from the cross sections of neighboring elements in the periodic table. The optical functions resulting from this study show evidence for both the redistribution of oscillator strength between energy levels and the effects on real transitions of the shielding of conduction electrons by virtual processes in the core states

  20. Outflow and hot dust emission in broad absorption line quasars

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Shaohua; Zhou, Hongyan [Polar Research Institute of China, 451 Jinqiao Road, Shanghai 200136 (China); Wang, Huiyuan; Wang, Tinggui; Xing, Feijun; Jiang, Peng [Key Laboratory for Research in Galaxies and Cosmology, University of Science and Technology of China, Chinese Academy of Sciences, Hefei, Anhui 230026 (China); Zhang, Kai, E-mail: zhangshaohua@pric.gov.cn, E-mail: whywang@mail.ustc.edu.cn [Key Laboratory for Research in Galaxies and Cosmology, Shanghai Astronomical Observatory, Chinese Academy of Sciences, 80 Nandan Road, Shanghai 200030 (China)

    2014-05-01

    We have investigated a sample of 2099 broad absorption line (BAL) quasars with z = 1.7-2.2 built from the Sloan Digital Sky Survey Data Release Seven and the Wide-field Infrared Survey. This sample is collected from two BAL quasar samples in the literature and is refined by our new algorithm. Correlations of outflow velocity and strength with a hot dust indicator (β{sub NIR}) and other quasar physical parameters—such as an Eddington ratio, luminosity, and a UV continuum slope—are explored in order to figure out which parameters drive outflows. Here β{sub NIR} is the near-infrared continuum slope, which is a good indicator of the amount of hot dust emission relative to the accretion disk emission. We confirm previous findings that outflow properties moderately or weakly depend on the Eddington ratio, UV slope, and luminosity. For the first time, we report moderate and significant correlations of outflow strength and velocity with β{sub NIR} in BAL quasars. It is consistent with the behavior of blueshifted broad emission lines in non-BAL quasars. The statistical analysis and composite spectra study both reveal that outflow strength and velocity are more strongly correlated with β{sub NIR} than the Eddington ratio, luminosity, and UV slope. In particular, the composites show that the entire C IV absorption profile shifts blueward and broadens as β{sub NIR} increases, while the Eddington ratio and UV slope only affect the high and low velocity part of outflows, respectively. We discuss several potential processes and suggest that the dusty outflow scenario, i.e., that dust is intrinsic to outflows and may contribute to the outflow acceleration, is most likely.