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  • 11
    Electronic Resource
    Electronic Resource
    Springer
    Journal of radioanalytical and nuclear chemistry 180 (1994), S. 187-196 
    ISSN: 1588-2780
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering
    Notes: Abstract The extraction behavior of Sm(III), Eu(III) and Dy(III) with 1-nitroso-2-naphthol (HA) and trioctylphosphine oxide (TOPO) in methyl isobutyl ketone (MIBK) from aqueous NaClO4 solutions in the pH range 4–9 at 0.1M ionic strength has been studied. The equilibrium concentrations of Sm and Dy were measured using their short-lived neutron activation products,155Sm and165mDy, respectively. In the case of Eu, the concentrations were assayed through the152,154Eu radiotracer. The distribution ratios of these elements were determined as a function of pH, 1-nitroso-2-naphthol and TOPO concentrations. The extractions of Sm, Eu and Dy were found to be quantitative with MIBK solutions in the pH range 5.9–7.5, 5.6–7.5 and 5.8–7.5, respectively. Quantitative extraction of Eu was also obtained between pH 5.8 and 8.8 with chloroform solutions. The results show that these lanthanides (Ln) are extracted as LnA3 chelates with 1-nitroso-2-naphthol alone, and in the presence of TOPO as LnA3(TOPO) and LnA3(TOPO)2 adducts. The extraction constants and the adduct formation constants of these complexes have been calculated.
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  • 12
    Electronic Resource
    Electronic Resource
    Springer
    Journal of radioanalytical and nuclear chemistry 195 (1995), S. 343-354 
    ISSN: 1588-2780
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering
    Notes: Abstract The equilibrium extraction behavior of Sm(III), Eu(III) and Dy(III) from aqueous NaClO4 solutions in the pH range of 4–9 at 0.1 M ionic strength into organic solutions of 1-nitroso-2-naphthol (HA) and 1,10-phenanthroline (Phen) has been studied. The equilibrium concentrations of Eu were assayed through the 344 keV photopeak of the152Eu radiotracer used. The concentrations of Sm and Dy were measured by irradiating one mL portions of the organic extract and analyzing the 104 and 108 keV photopeaks of the short-lived neutron activation products,155Sm and165mDy, respectively. Quantitative extraction of Eu with 5×10−2 M HA alone was obtained in the pH range of 6.7–7.8 with n-butanol, 7.4–8.5 with chloroform, 8.0–8.7 with ethyl acetate, 7.7–8.5 with isoamyl alcohol and 6.1–8.0 with methyl isobutyl ketone (MIBK). But, Eu was extracted only to a maximum of 78% and 83% in the pH range of 8.3–8.9 and 7.4–8.1 with carbon tetrachloride and xylene, respectively. The extraction of Sm and Dy were found quantitative in the pH range of 6.3–7.0 and 6.6–7.1, respectively, with 5×10−2 M HA alone in MIBK solutions. The synergistic extraction of Eu was quantitative in the pH range of 6.6–9.8 with chloroform, 7.8–8.9 with ethyl acetate, 7.7–8.5 with isoamyl alcohol and 6.0–9.6 with MIBK when 1×10−2 M each of HA and Phen were employed. Sm and Dy were quantitatively extracted into MIBK solutions containing 5×10−2 M each of HA and Phen in the pH range 6.0–7.5 and 6.1–7.5, respectively. The distribution ratios of these lanthanides (Ln) were determined as a function of pH, and HA and Phen concentrations. The analysis of the data suggests that these Ln are extracted as LnA3 chelates when HA alone is used. In the presence of HA and Phen, both LnA3(Phen) and LnA3(Phen)2 adducts are formed only in the MIBK system while LnA3(Phen) complexes are the predominant ones in all other solvent systems studied. The extraction constants and the adduct formation constants of these complexes have been calculated.
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  • 13
    ISSN: 1588-2780
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering
    Notes: Abstract A simple preconcentration method is described for the simultaneous coprecipitation of Cd(II), Co(II), Cu(II), Mo(VI), U(VI), V(V) and Zn(II) from surface water samples followed by quantitation using neutron activation analysis. Ammonium pyrrolidinedithiocarbanate (APDC), anthranilic acid and 8-hydroxyquinoline have been investigated as possible coprecipitating agents. The suitability of Bi3+, Fe3+, Ni2+ and Pb2+ ions as metal carriers has also been studied. It has been found that the above elements can be quantitatively coprecipitated with APDC in the presence of Bi3+ carrier at pH 4. The precision and accuracy of the method for all elements are found to be between ±2 and 10%. The enrichment factors are of the order of 103. The detection limits are in the ppb range varying between 0.04 ng · ml−1 for Co and V and 5 ng · ml−1 for Zn. The method has been applied to tap and well waters, and river and lake water samples collected from Halifax County, Nova Scotia.
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  • 14
    ISSN: 1588-2780
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering
    Notes: Abstract A method has been developed for the simultaneous preconcentration of Cd(II), Co(II), Cu(II), Hg(II), Mn(II), Th(IV), U(VI), V(IV) and Zn(II) from 500–1000 ml of water samples by coprecipitation using a combination of 1-(2-thiazolylazo)-2-naphthol, ammonium pyrrolidinedithiocarbamate and ammonium salt of N-nitroso-phenylhydroxylamine. The elemental contents have been measured by neutron activation analysis using different schemes of irradiation, decay and counting periods. Quantitative recoveries of all the above elements have been achieved between pH 6.0 and 7.2. For most of the elements, the enrichment factors are of the order of 104. The precision, expressed in terms of relative standard deviation, and accuracy of measurements are within ±5–10%. The detection limits are in the ppb range. The method has been applied to sea and drinking water samples and biological materials.
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  • 15
    Electronic Resource
    Electronic Resource
    Springer
    Journal of radioanalytical and nuclear chemistry 197 (1995), S. 133-148 
    ISSN: 1588-2780
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering
    Notes: Abstract A systematic study of separating the actinides from each other in 1 M hydrochloric acid media has been carried out using selective oxidation/reduction processes followed by coprecipitation with neodymium fluoride. We have optimized two such procedures, one with bromate and another with permanganate, for the sequential separation of Am, Pu, Np, and U isotopes. The first procedure involves oxidation of Pu, Np, and U to +6 state in 1 M HCl media at 85° C with 30% NaBrO3 and separation from trivalent Am by collecting the latter on the first NdF3 coprecipitated source. Plutonium is then reduced and converted to +4 oxidation state with 40% NaNO2 at 85°C, while Np and U are kept oxidized with additional bromate in 50–70°C hot solution, thus separating Pu by collection on a second NdF3 source. At this stage, Np present in the filtrate is reduced with hydroxylamine hydrochloride and separated from U by collecting on a third source. Subsequently, U is reduced with 30% TiCl3 and co-precipitated on a final source. The second procedure, which employs KMnO4 in 1 M HCl media at 60–85°C for oxidizing Pu, Np, and U, and separating from Am, produced MnO2 which is collected along with Am on the coprecipitated NdF3. This MnO2 is dissolved on the filter itself with 1 mL of acidified 1.5% H2O2 without any degradation of the α-spectra. After evaporating the filtrate to destroy H2O2, Pu, Np, and U are separated by following steps similar to those in the bromate procedure. The recoveries of the actinides with both procedurés are 〉99%. The decontamination factors are between 103 and 104. The precision and accuracy of measurements, as expressed by the relative standard deviation of replicate analyses, are within 5%. Absolute detection limits for a one-day count on a 600 mm2 detector at 32% counting efficiency and 450 mm2 detector at 27% counting efficiency are about 2.7×10−4 and 3.2×10−4 Bq, respectively. These procedures have been applied to the analysis of actinides in environmental samples.
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  • 16
    Electronic Resource
    Electronic Resource
    Springer
    Journal of radioanalytical and nuclear chemistry 151 (1991), S. 167-175 
    ISSN: 1588-2780
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering
    Notes: Abstract The homogeneity of four reference materials was evaluated for Se by cyclic instrumental neutron activation analysis (CINAA). The relative standard deviation for Se measurements at ppb levels by CINAA was 〈12% for NIST Wheat Flour (SRM 1567) in 5–10 mg samples, while it was 〈11% for Chinese Hair (HH−CH-1), 〈13% for IAEA Animal Muscle (H-4) and 25% for IAEA Animal Blood (A-13) in 50 mg samples. The highest relative subsampling uncertainties were observed in the mass range of samples ≤50 mg for Chinese Hair, ≤100 mg for Wheat Flour and Animal Muscle and ≤300 mg for Animal Blood. The results of a one-way analysis of variance indicate that all reference materials above these mass ranges are adequately homogeneous with respect to Se distribution. Our data suggest that these materials, except Animal Blood, can be used as reference standards for Se in Quality assurance programs well below the sample masses re commended by the issuing agencies.
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  • 17
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 352 (1995), S. 136-142 
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A pilot project was initiated to study the feasibility of preparing milk as a candidate reference material for 14C near environmental levels. Two materials, MK-B at natural level of 14C and MK-C4 at an elevated level, have been prepared from pasteurized 2% dairy milk. MK-C4 was spiked with an appropriate amount of 14C-methylated casein tracer to achieve the elevated level. Several samples from MK-B and MK-C4 have been analyzed to test the homogeneity of these materials for the distribution of 14C. The samples were combusted in oxygen under 20 atmospheres pressure using a Parr bomb. The 14C concentrations were determined by liquid scintillation counting using Carbo-Sorb/Permafluor E+ cocktail. The results indicate that these materials are homogeneous with respect to 14C concentration even in sub-sample sizes of 0.25 g of the freeze-dried material. The precision of our 14C measurements, as expressed by the % relative standard deviation, is within 5%. The accuracy has been tested by analyzing replicate samples of the IAEA 14C quality assurance materials, C-3 (cellulose) and C-6 (ANU sucrose) and found to be within 3%. The lower limits of detection are 0.08, 0.05 and 0.02 Bq.g−1 of carbon for 20 ml of liquid scintillation mixture (Carbo-Sorb/Permafluor E+ = ∼0.67) loaded with up to 0.4 g of carbon from the sample and counted for 3 cycles of 60, 180 and 1000 min each, respectively. Our measurements of 14C specific activities of MK-B and MK-C4 are 0.26±0.01 and 15.3±0.4 Bq.g−1 of carbon, respectively.
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  • 18
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 352 (1995), S. 53-57 
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Epithermal instrumental neutron activation analysis (EINAA) methods have been optimized and applied to several biological reference materials and selected food items for the determination of iodine. The method involves irradiation of the samples for different periods in epi-cadmium and/or epi-boron flux of the Dalhousie University SLOWPOKE-2 reactor and direct counting without any pre-treatment on a 25-cm3 hyperpure Ge detector. The 443 keV photopeak of 128I is used for assaying the iodine content. Precision of measurements, expressed as the relative standard deviation, is 10–15% at 200–500 ppb and 3–12% at 500–6000 ppb levels of iodine. Accuracy of iodine measurements is within 5%. The detection limits for iodine in several biological materials with cadmium and boron, either alone or a combination of the two, as thermal neutron shields have been found to vary between 0.1 and 0.4 mg · kg−1 for different periods of irradiation, decay and counting. The results suggest that the EINAA methods can be successfully applied to biological materials for routine analysis of iodine at levels higher than 200 ppb.
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  • 19
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 338 (1990), S. 399-407 
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A cyclic instrumental neutron activation analysis method has been used to calculate sampling constants and to evaluate homogeneity for Se in five biological reference and certified reference materials, namely NRC lobster hepatopancreas (RM TORT-1), IAEA horse kidney (RM-H8), and NIST bovine liver (SRM-1577a), oyster tissue (SRM-1566) and mixed diet (RM-8431). The between-weight-range heterogeneity has been observed to be no greater than the within-weight-range heterogeneity. The subsampling standard deviation (S s) has been found to be less than the measurement standard deviation (S m) for H-8 (〉5 mg sample) and TORT-1 (〉50 mg). For 1577a, S s is almost equal to S m; while S s is 2–3 times higher than S m for the other two materials. The sampling constants varied between 0.04 and 3.0 g for four materials while the mixed diet had a value of 31 g.
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  • 20
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    International Journal for Numerical Methods in Fluids 18 (1994), S. 821-842 
    ISSN: 0271-2091
    Keywords: Free-surface ; Interphase mass transfer ; Finite element two-phase flow ; Coating ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: The application of the finite element method to multiphase flow problems with interphase mass and heat transfer is described. A general forinulation is used that determines the position of the interfacial boundary and allows for multiple solvents, differential volatilities and concentration- and temperature-dependent thermophysical properties. Species phase change and the dramatic volume change that acompanies interphase mass transfer make implementation of the theory challening, since these events lead to discontinuous velocities and concentrations at phase boundaries. These discontinuities are especially large in processes involving rapid evaporation or condensation. As examples we examine the effects of rapid drying on film and fibre formation of sol--gel materials, which are often laden with volatile species.
    Additional Material: 10 Ill.
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