Photoemission from tin and lead cluster anions

Photoelectrons from mass-identified jet-cooled tin and lead cluster anions (Sn _n ^? , Pb _n ^? ) are detached by ultraviolet laser light (hν=3.68 eV). The photoelectron energy spectra give the detachment energies of ground state cluster anions (electron affinities) as well as excitation energies of neutral clusters in the geometry of the anions. The energy spectra for Sn _n ^? are dominated by flat thresholds with ann-dependence similar to that of other group IV clusters. In contrast, for Pb _n ^? we find pronounced narrow lines close to threshold, generally followed by a 0.3–1.4 eV gap which indicates closed-shell behaviour of Pb _n ^? for nearly alln.     

Cadmium and lead recovery from yeast biomass

Properties of metal solution, environmental conditions and the type of biomaterials (microorganism genus, species or even strain) influence the mechanism of metal biosorption and consequently metal adsorption capacity, affinity and specificity. Cell surface properties determine the metal-microorganism interactions to a large extent. In this work the relationship between yeast surface properties and yeast’s ability to bind cadmium, lead and copper was studied. Surface charge and hydrophobicity before and after biosorption were determined using dye retention and solvent partition assays, respectively. There were differences in the surface charge and relative hydrophobicity among different yeast strains. A higher metal adsorption capacity for more negatively charged yeast cells was observed. Biosorption of heavy metals resulted in modifications to the surface charge and hydrophobicity of yeast cells. However, there were not statistically significant changes in the yeast surface charge and hydrophobicity after binding of heavy metals depending on the nature of the metal, initial metal concentration and solution pH.     

INAA,AAS, and lead isotope analysis of ancient lead anchors from the Black Sea

Lead stocks of wooden-lead anchors found along the Bulgarian Black Sea coast and typologically dated VI c. B.C.-III c. A. D. have been analyzed for chemical composition and lead isotope ratios by INAA, AAS and mass spectrometry. Using multivariate methods for analysis as well as simple bivariate plots the lead for production of the stocks was localized as originating from Laurion, Thassos, Troas, Chalkidike and the Rhodopes. In general, the chemical composition is not recommended to be used for provenance study of lead artefacts. Combining the results from this study with the existing typological classification certain conclusions about the production and distribution of lead anchors in the Aegean region are made.     

Antifilarial lead molecules isolated from Trachyspermum ammi

Lymphatic filariasis is caused by infection with the parasitic filarial nematodes Wuchereria bancrofti, Brugia malayi and B. timori, transmitted by mosquitoes. The lack of an adulticidal drug poses a challenge to filariasis elimination, hence it is essential to develop an effective antifilarial drug which could either kill or permanently sterilize the adult worms. In the reported work the in vitro activity of a methanolic extract of fruits of Trachyspermum ammi (Apiaceae) against adult bovine filarial Setaria digitata worms has been investigated. A bioassay-guided fractionation was carried out by subjecting the crude extract to flash chromatography. HPLC analysis was done for the crude extract and active fraction. The crude extract and the active fraction showed significant activity against the adult S. digitata by both a worm motility and MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] reduction assays. The isolated active principle was chemically characterized by IR, (1)H-NMR and MS analysis and identified as a phenolic monoterpene. It was screened for in vivo antifilarial activity against the human filarial worm B. malayi in Mastomys coucha, showing macrofilaricidal activity and female worm sterility in vivo against B. malayi. The findings thus provide a new lead for development of a macrofilaricidal drug from natural products.     

Nucleation of lead chromate from homogeneous solution

On the basis of the Christiansen-Nielsen model for nucleation, the nucleus of lead chromate precipitated from homogeneous solution has been found to consist of about five ions. The critical supersaturation values of solutions of lead chromate are dependent upon the method of filtration; however, a change in supersaturation of about 25 % is without effect on the size of the critical nucleus.     

Oscillatory diffuse X-ray scattering from lead chalcogenides

New inorganic compounds having the general formula (Bi₂O₃)_1−x (Lu₂O₃) _x (x ranges from 0.1 to 0.5) displaying orange colours have been synthesized by traditional solid-state route, as viable alternatives to lead, cadmium and chromium based yellow toxic inorganic pigments. The host lattice of these pigments is Bi₂O₃ that is doped by Lu³⁺ ions. The goal was to develop conditions for the synthesis of these compounds and to determine the influence of calcination temperature and lutetium content on their colouring effects. The simultaneous TG-DTA measurements were used for determination of the temperature region of the pigment formation and thermal stability of pigments. The pigments were also evaluated from the standpoint of their structure and particle sizes.     

Radiochemical separation of radiothallium from proton-irradiated lead

Absorption of carrier-free T1 from nitric acid solutions of lead by ammonium 12-molybdophosphate fixed in the matrix of porous Teflon (AMP-sorbent) has been investigated. Effective separation of T1 and Pb is shown to take place. Elution processes of T1 from AMP-sorbent have been investigated. It is found that complete extraction of T1 is achieved upon dissolving AMP in concentrated ammonia. Further purification and concentration of T1 are performed by means of cation exchange chromatography on Dowex-50 or KU-2 resins. Investigation of high temperature behaviour of T1 ultramicroamounts in Pb melt showed that T1 is quantitatively separated out into the gas phase when fluorinating additions of PbF₂ or NaF solid salts covering the melt surface are used. The volatile compounds of radiothallium formed were transported by a stream of inert gas (He or N₂) from the evaporation zone to the thermochromatographic column, where they were sorbed on the surface in a limited zone with the maximum at 240 °C. Liquid and gas thermochromatographic methods for separation of carrier free radiothallium from protonirradiated lead material have been developed. The radiochemical, chemical and radionuclidic purity of T1 samples complies with requirements of nuclear medicine for²⁰¹T1 product. Both methods ensure 95% chemical yield of T1 and take about two hours each.     

Isolation of lead from water samples and determination of Pb

This paper describes the procedures of isolating lead and strontium from the larger volume of seawater and drinking water samples that enable the determination of ²¹⁰Pb on gamma spectrometer and ^89,90Sr on liquid scintillation counter. In one procedure, lead is directly isolated from water sample on the column filled with Sr resin by binding of lead on the Sr resin column from 0.2 M HCl in water sample, and successive elution with 0.2 and 8 M HCl. In others, lead and strontium are precipitated from sample with (NH₄)₂CO₃, followed by isolation on an anion exchange column. Lead, strontium and yttrium are bound onto anion exchange column (filled with Amberlite CG-400 in nitrate form) from alcoholic solutions of nitric acid. Lead, Sr and Y are separated from Mg, Ca, K, and other elements by elution with 0.25 M HNO₃ in the mixture of ethanol and methanol. After that, strontium and yttrium are separated from lead by elution with 0.25 M HNO₃ in the mixture of ethanol and water.

The procedure with the Sr resin (direct isolation) is simpler and faster in the phase of isolation on the column in comparison with the procedure with the anion exchanger. The procedure with the anion exchanger, however, makes possible the simultaneous isolation of lead, yttrium and strontium and rapid determination of ^89,90Sr. These procedures were tested by determination of ²¹⁰Pb and ^89,90Sr in real sample. Obtained results showed that Pb can be efficiently isolated (with high recovery) from sample and activity of 6 mBq l⁻¹ of ²¹⁰Pb and higher can be determined.     

Cation-exchange separation of copper from zinc, nickel and lead

Summary Copper is separated from zinc, nickel and lead on the cation-exchange resin Dowex 50 W X-16 by selective elution. 0.5 M ammonium acetate solution is used for the elution of copper, 1.0 M ammonium chloride solution for zinc, 1.2 M hydrochloric acid for nickel and 0.25 M ammonium acetate solution for lead. The method is applied to the separation of copper from brass and gun metal. The errors are about ± 2.5%.

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Zusammenfassung Ein Verfahren zur Trennung des Kupfers von Zink, Nickel und Blei durch selektive Elution am Kationenaustauscher Dowex 50 W X-16 wird beschrieben. Zur Elution von Kupfer dient 0,5 M Ammoniumacetatlösung, für Zink wird 1,0 M Ammoniumchloridlösung benutzt, für Nickel 1,2 M Salzsäure und für Blei 0,25 M Ammoniumacetatlösung. Die Fehler liegen bei ± 2,5%. Die Methode wird zur Abtrennung von Kupfer aus Messing und Bronze benutzt.

     

Formation of PbS materials from lead xanthate precursors

Six lead xanthate adducts Pb(S(2)COR)(2).L [R = Et, (n)Bu, L = bipy, TMEDA (tetramethylethylenediamine), PMDETA (pentamethyldiethylenetriamine)] have been synthesised and the structures of all, save Pb(S(2)COBu(n))(2).TMEDA (4) which is an oil, determined. Pb(S(2)COEt)(2).TMEDA (3) is seven-coordinate at lead through three chelating ligands and one weak intermolecular Pb‥S interaction. Both Pb(S(2)COR)(2).bipy [R = Et (1), (n)Bu (2)] are dimers in which one xanthate is terminal and the other μ(2) bridging at each sulphur, generating an eight-coordinate lead when the bipy donor is included. Both Pb(S(2)COR)(2).PMDETA [R = Et (5), (n)Bu (6)] are seven-coordinate at lead by virtue of two bidentate chelating xanthate ligands and a tridentate PMDETA; there are no intermolecular interactions. Trends in the (207)Pb NMR chemical shifts mirror the changes in the intramolecular coordination number across the series. Pb(S(2)COEt)(2).TMEDA (3) has been used to deposit PbS films on glass, Mo-coated glass and Si by AACVD. Pb(S(2)COEt)(2) also generated PbS nanocubes when decomposed under an autogenerated pressure.     

A novel route to perovskite lead titanate from lead and titanium glycolates via the sol–gel process

Pure perovskite lead titanate powder (PbTiO₃) is successfully produced via the sol–gel process using lead and titanium glycolates as starting precursors and has been synthesized by the oxide one spot synthesis process. The obtained lead titanate is of the tetragonal form of the perovskite phase, with high purity and nearly zero moisture content. From high‐resolution mass spectra, the XRD technique, Raman‐FTIR and TGA‐DTA analysis, the lead–titanium glycolates undergo sol–gel transition through the formation of Pb? O? Ti bonds. From the SEM micrographs, the PbTiO₃ particle shape transforms from an agglomerate sphere to a needle and fiber‐like shapes as the calcination temperature is varied above T_c. The corresponding molecular structural transformation, from the tetragonal form to the cubic form, occurs at 430 °C. The lead titanate powder calcined at 300 °C for 3 h has the highest dielectric constant and electrical conductivity values, namely 17470 and 1.83 × 10^?3, respectively. Copyright © 2006 John Wiley & Sons, Ltd.     

Lead-tin mirror formation from mixtures of red lead and tin sulphide

Mosaic gold, tin (IV) sulphide, is a yellow pigment which was known in antiquity but whose use was superseded by other more easily obtainable yellow pigments by the Renaissance. The identification of mosaic gold residues in a burnished golden mirror decoration on a XIIIth Century Spanish polychrome statue is important in that the first reference to the use of mosaic gold in the European literature dates from the XIVth Century, although the use of this material in China had been recorded some time before. In this paper, Raman spectroscopy, XRD and SEM are used in the analysis of the conditions required for the formation of golden mirrors using tin (IV) sulphide in admixture with dilead (II) lead (IV) tetroxide and mercury (II) sulphide. From these results, it is proposed that the major reactions are the reduction of Sn(IV) to Sn(0) with the accompanying oxidation of lead (II) oxide to lead (IV) oxide and the formation of lead (0) and lead (II) sulphide. From these results it was possible to explain the process of creation of the golden mirror from mosaic gold in the XIIIth Century.     

Bremsstrahlung spectra from lead and tantalum at 6 MeV electron energy

Bremsstrahlung spectral distributions have been experimentally measured for thick targets of lead and tantalum at 6 MeV electron energy, using Compton scattering technique. The experimental results are in agreement with the theoretical results.     

Electrodeposition of micro- and nanocrystalline lead selenide from alkaline selenosulfate solutions

Cathodic electrodeposition of PbSe is carried out in aqueous alkaline selenosulfate (SeSO ₃ ^2? ) bath of lead complex ions at various conditions of electrolysis. Micro- and nanocrystalline PbSe thin films were grown onto glassy carbon (GC) substrates by potentiostatic and cyclic voltammetric (CV) methods respectively. Structure and surface morphology of thin films were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). X-ray diffraction indicates that the PbSe films have cubic structure without any impurities. The SEM micrograph showed the films cover GC substrate completely and consisted of irregular shaped grains.     

Generalized STU-parameters for elastic electron scattering from thallium and lead atoms

Numerical results for the complete set of generalized STU-parameters are presented for elastic scattering of polarized electrons from unpolarized thallium and lead atoms. Some of these parameters can only be measured in “triple scattering experiments”, since the change of the initial polarization vector has to be determined. The agreement between the predictions of semirelativistic Breit-PauliR-matrix calculations and recent experimental data of the Münster group for the Sherman functionS is excellent in the case of thallium while further improvements of the theoretical model are necessary for the lead target.     

Oxidation of perfluoronaphthols by lead tetraacetate and lead dioxide

Depending on the reaction conditions, oxidation of perfluoronaphthols by Pb(OAc)₄ proceeds by two routes. Under mild conditions (20°C) oxidation leads to the products of dimerisation of perfluoronaphthoxy radicals. At a higher temperature (80°C) the reaction leads to acetoxydienones. The mechanistic aspects of oxidation of perfluoronaphthols by Pb(OAc)₄ are discussed.     

Extraction chromatography preconcentration of impurities from high purity lead

Summary The method of multielement preconcentration of impurities from high-purity lead utilizing an extraction Chromatographie separation in tri-n-octylamine-HCl system is developed. Unlike a well-known procedure based on precipitation of lead nitrate this method is applicable to very small samples. Being used in combination with the precipitation procedure mentioned, this method provides a considerable increase in the effectiveness of the latter.     

Adsorption of radiocobalt on lead dioxide from aqueous solution

Adsorption of cobalt on lead dioxide from aqueous solutions has been studied in relation to shaking time, amount of adsorbent, pH, and concentration of the adsorbate. The data fitted very well Langmuir, Freundlich, and Dubinin-Radushkevich isotherms and their corresponding constants were calculated. In another set of experiments the influence of different anions and cations on the adsorption of cobalt under the optimum experimental conditions have been determined. EDTA, tartrate, citrate, thiocyanate, oxalate, U(VI), Al(III), Fe(III), Cr(III), and Th(IV), drastically reduced adsorption of cobalt. Therefore these anions and cations should be removed before adsorption of cobalt on lead dioxide. Adsorption of other metal ions on the oxide were measured under identical conditions. TheK _D values indicate that cobalt can be separated successfully from Hg(II), Ag(I), Ta(V), In(III) and Tc(VII).     

Characterisation of lead rhodizonate as barium and radium adsorber from fresh water

A series of metal -diketonates were irradiated with bremsstrahlung of maximum energy of 50 MeV and the recoil behavior of⁷Be, formed from¹²C of ligands through¹²C(, n)⁷Be reaction, was investigated.⁷Be nuclides thus formed were detected partially as central metal atoms of the complexes. Complex yields of⁷Be were compared and an anomalously high yield was observed in tris-acetylacetonatocobalt(III) [Co(acac)₃].     

The lead amalgam/lead sulfate electrode redesigned and reassessed

To make the (Pb)Hg‖PbSO₄‖SO ₄ ²⁻ electrode really usable and attractive for extensive application to thermodynamic studies, a new, simplified design and a convenient preparative procedure have been introduced, ensuring stable amalgams and reproducible electrode potentials. The electrode so prepared has been exhaustively characterized both thermodynamically and as a SO ₄ ²⁻ -sensing electrode, in different sulfate solutions, including H₂SO₄. The past discrepancies of standard potentials-mainly due to preparation and/or handling problems-are discussed and, for a final resolution of the question, a practical standardization procedure is proposed.