Dünnschichtchromatographie als Hilfsmittel in der Radiochemie. 4. Mitteilung Trennung von 113Sn und 113mIn

Thin-layer chromatography is applied to the separation of ^113mIn from ¹¹³Sn. Different factors influencing migration and separation of the ions are investigated. The method can be used for the examination of the purity of isolated ^113mIn solutions.     

Separation of trace elements,In(III), Sn(IV), Sb(V) and Te(IV) by adsorption on activated carbon and graphite

Adsorption behaviour of trace elements, In(III), Sn(IV), Sb(V) and Te(IV) on activated carbon and graphite powder was studied. Adsorption characteristics of the ions enabled the separation of In(III)–Sn(IV), Sn(IV)–Sb(V) and Sb(V)–Te(IV) pairs. Applications to practical separation, milking of^113mIn from¹¹³Sn, removal of tin impurity from¹¹⁹Sb, and milking of¹¹⁹Sb from^119mTe, are presented.     

Neutron activation analysis of tin in biological materials and their ash using123Sn and125Sn

Tin has been determined in biological materials by NAA of the γ-emitting 40-min¹²³Sn and 9,7-min¹²⁵Sn isotopes at the sub-ppm level. For¹²³Sn, samples are wet-ashed after irradiation, whereas to allow fast radiochemistry for¹²⁵Sn, the samples are dry-ashed prior to the irradiation. Both separation techniques rely on selective solvent extraction of tin(IV) iodide, and NaI(TI) counting. Comparative analyses of several materials by both methods gave good agreement, indicating that tin is not lost on dry-ashing and that simple dissolution of the ash in an HCl?HI mixture is complete. Results by both techniques are presented for the standard materials Bowen's Kale and NBS Orchard Leaves, and for some other materials.     

Colloidal behavior of carrier-free125mTe in aqueous solutions

NaCl solutions containing carrier-free^125mTe(IV) and^125mTe(VI) have been prepared. The effect of the presence of various substances on the colloidal behavior of^125mTe in solution has been studied by ultracentrifugation. It has been found that phosphate, sulfide and oxalate ions which complex with various elements decrease the colloidal formation of^125mTe. In order to estimate the size of colloidal particles, the NaCl solutions containing carrier-free^125mTe have been microfiltered through membrane filters with various pore size.     

Kathodenstrahlpolarographische Bestimmung von Spurenelementen in Tetrachlorogolds?ure nach ionenaustausch-chromatographischer Trennung

Zusammenfassung Die kathodenstrahlpolarographische Bestimmung von Ni, Pb, Cu, Co, Fe, Mo, Te, Sn, Zn, Bi, Cd, Tl in Tetrachlorogoldsäure wird beschrieben. Die Nachweisgrenzen liegen im 10^–4%- bzw. 10^–5%-Bereich (Ni, Co, Mo). Die Spuren werden über einen Ionenaustauscher AG 1X8 untereinander und von der Matrix getrennt.

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Cathode-ray polarographic determination of trace elements in tetrachloroauric acid after separation by ion exchange

A method is described for the cathode-ray polarographic determination of traces of Ni, Pb, Cu, Co, Fe, Mo, Te, Sn, Zn, Bi, Cd, Tl in H(AuCl₄). Gold is separated from the trace metals by absorption on the strongly basic anion-exchange resin AG 1X8. The detection limits are within the ranges of 10^–4% and 10^–5% ((Ni, Co, Mo).

     

Adsorption and colloidal behavior of traces of hexavalent tellurium in aqueous solutions

The solutions of carrier-free^125mTe(VI) have been prepared by oxidizing^125mTe(IV) with bromine. Using carrier-free^125mTe(VI) as a tracer, the effects of pH, NaCl concentration, and tellurium(VI) concentration on the adsorption and colloidal properties of tellurium(VI) in NaCl solution have been studied. It has been found that traces of tellurium(VI) are adsorbed on filter paper and show colloidal behavior in the basic region. A method has been devised for the separation of carrier-free^125mTe from its parent nuclide¹²⁵Sb, based on the adsorption properties of^125mTe(VI) in basic solutions.     

Etude des generateurs d'indium-113m

Methods are proposed for the determination of¹¹³Sn in the eluate of an^113mIn generator as well as for the analysis of its chemical and radionuclidic purity. Two generators of different origin have been studied. The presence of the radioisotopes¹¹³Sn,¹²⁵Sb,^125mTe and the elements Zr, Si and Fe have been found in the eluate. Recommendations are given for the use of such generators.     

Preparation of a118Te/118Sb radionuclide generator

The development of a new radionuclide generator, based on¹¹⁸Te/¹¹⁸Sb, has been studied. The 3.5 minute¹¹⁸Sb daughter activity decays principally by positron emission and has potential use as a flow tracer. The¹¹⁸Te parent is conveniently produced by proton bombardment of antimony targets. A simple and efficient scheme for the separation of radiotellurium from proton-irradiated antimony targets has been developed, and thin-target cross sections for¹²¹Sb(p, 4n)¹¹⁸Te and competing reactions have been determined. For antimony targets irradiated with 46 MeV protons, the yields (mCi/g Ah) of¹¹⁸Te,^119mTe and¹¹⁹Te were measured to be 0.71, 0.33 and 1.9, respectively. The adsorption and elution characteristics of activated carbon for tellurium have been evaluated for use as a column chromatography adsorbent in a¹¹⁸Te/¹¹⁸Sb generator. The conditions for optimal¹¹⁸Sb elution and minimal¹¹⁸Te breakthrough for promising systems are presented.     

Mössbauer study of defect119Sn atoms with ligands from silver to iodine

Mössbauer emission spectra of defect¹¹⁹Sn atoms arising from¹¹⁹Sb were measured in InSb, GaSb, CdSb, ZnSb, In₂Te₃, CdTe, and Ag₂Te labeled with¹¹⁹Sb or its parent^119mTe. Together with the results of our previous studies, the isomer shifts of defect and normal¹¹⁹Sn were shown to correlate with the electronegativity of ligands from silver to iodine.     

Darstellung und Kristallstruktur von ANi10P3 (A: Zn,Ga, Sn,Sb)

Preparation and Crystal Structure of A Ni₁₀P₃ ( A : Zn, Ga, Sn, Sb) Four compounds ANi₁₀P₃ (A: Zn, Ga, Sn, Sb) were prepared by heating mixtures of the elements and investigated by means of X‐ray methods. Single crystal structure determinations of ZnNi₁₀P₃ (a = 7.665(1), c = 9.360(1) Å) and SnNi₁₀P₃ (a = 7.674(1), c = 9.621(1) Å) respectively showed, that they are isotypic and crystallize in a new structure (P3m1; Z = 3). This type is characterized by 3²⁰ and 3²⁴ cages of Ni atoms (Frank Kasper polyhedra), which are connected with each other. A atoms are located in the centres of these polyhedra and have no direct bonds to the P atoms.     

Eigenschaften von Tellur-Tellur-Bindungen. IV. Dismutationsreaktionen von Di-p-tolylditellurid mit Tetra-tert-butyldiphosphan und Tetra-isopropyldiphosphan

Properties of Te? Te Bonds. IV. Dismutation Reactions of Di-p-tolylditelluride with Tetra-tert-butyldiphosphane and Tetra-isopropyldiphosphane Di-p-tolylditelluride reacts with tetra-tert-butyldiphosphane and tetra-isopropyldiphosphane (prepared from the corresponding chlorophosphanes with potassium in toluene) with formation of new tellurophosphinous acid esters p-CH₃C₆H₄TePR₂ (R = t-C₄H₉, i-C₃H₇). Distillation leads to pure yellow liquids that have been characterized by ¹H-, ¹³C-, ³¹P-, and ¹²⁵Te-NMR, by elemental analysis and by mass spectroscopy.     

125Te-NMR-spektren von organotellurhalogeniden

Tetraorganotin compounds react with tellurium tetrachloride or tellurium tetrabromide with formation of the corresponding organotellurium trihalides and diorganotellurium dihalides. ¹²⁵Te NMR spectra of the reaction mixtures are used to determine the reaction products.     

Kristallstruktur,Schwingungs- und NMR-Spektren von Dodecaphenylcyclohexastannan (Ph2Sn)6

Crystal Structure, Vibrational and N.M.R. Spectra of Dodecaphenylcyclohexastannane (Ph₂Sn)₆ The six-membered homocycle (Ph₂Sn)₆ was obtained under condition described for the preparation of the five-membered ring (Ph₂Sn)₅. The homocycles (Ph₂M)₆, M ? Si, Ge, Sn exist in three crystalline forms, without solvent, containing seven moles of crystal benzene, and with two moles alkylbenzene. The crystal structure of (Ph₂Sn)₆ · 2 Toluene was determined and refined until R = 0.041. The parameters of the Sn₆ ring are: Sn? Sn bond length 278.0 pm, bond angle 112.5°, and torsion angle 51.6°. The homorings (Ph₂M)₆ form a nearly identical series of rigid normal conformations and spherical space filling. IR and Raman spectra of (Ph₂Sn)₆ are given and discussed. There is a strong coupling between Sn₆ ring vibrations and mass sensitive vibrations of the phenyl groups. ¹¹⁹Sn und ¹³C N.M.R. spectra exhibit long range couplings with Sn nuclei. The values of the coupling constants indicate only a minor effective charge at the Sn atoms.     

Separation of radioindium (N.C.A.) from neutron irradiated tin and cadmium on hydrated antimony pentoxide

Hydrated antimony pentoxide (HAP) as an absorbent for column operation has been prepared by hydrolysis of SbCl₅ with deionized water. Sorption behavior of Sn, Cd, Sb and In was studied on HAP in HCl medium. Radiochemical separation of no-carrier added^113mIn from¹¹³Sn/¹²⁵Sb and^115mIn from¹¹⁵Cd wa achieved over a HAPO column. The separated products were of high radionuclidic purity.     

Zirconium silicotungstate matrix as a prospective sorbent material for the preparation of <Superscript>113</Superscript>Sn/<Superscript>113m</Superscript>In generator

The zirconium silicotungstate (ZrSiW) was studied as an effective sorbent material to be used in the ¹¹³Sn/^113mIn generator. The results elucidated that the distribution coefficient of ¹¹³Sn (3700 mL/g) is greater than ^113mIn (275 mL/g) from 0.1 M HCl acid solution to the ZrSiW material. The maximum sorption capacity of Sn (IV) was found to be 33 mg per gram ZrSiW (~?0.3 mmol/g). The elution yield of ^113mIn was found to be >?78?±?6.4% with an acceptable purity of radionuclidic and radiochemical (≥?99.99 and 96.8%, respectively). The rigorous separation of ^113mIn from the ¹²⁵Sb was carried out due to its long half-life (2.758 years) and beta emission that causes tissue damage. Zr, W and Si levels are below the permitted limit in the ^113mIn eluate.     

Trennung von spaltprodukten durch Extraktionschromatographie

The separation of fission products which form anionic species in mineral acids and of uranium and neptunium from samples of neutron-irradiated uranium is described. The method used is extraction chromatography with tri-n-butylphosphate (TBP) and di-(2-ethylhexyl)-orthophosphoric acid (HDEHP) as extractants and polytrifluoromonochloroethylene powder as the solid support. In the first column Zr, U and Np are extracted with TBP from 8N HNO₃/NaClO₃. In the second column, HDEHP is applied as extractant and 9N HCl/NaClO₃ as the mobile phase for the isolation of Nb, Sb, and I, and in the third column (HDEHP), the rare earths and Mo are extracted from 0.1N HCl. Finally with the fourth column (TBP), Te and Tc are isolated from 6N HCl. These four groups of elements are further separated by elution from the columns. From the final effluent containing Ru, Rh, Cs, Sr, and Ba, Ru is distilled from HClO₄, and Rh is precipitated with NH₄OH. The determination of chemical yields with X-ray fluorescence techniques is described for Zr, Mo, Te, Cs, Ce and U.

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Aus einer Dissertation, Mainz 1967.     

Dünnschichtchromatographie als Hilfsmittel in der Radiochemie. 3. Mitteilung [1]. Trennung von 99Mo und 99Tc

The separation of ⁹⁹Tc from neutron irradiated ammonium molybdate by thin-layer chromatography is described.     

Sequential segregation of Sn and Sb in a Cu(111) single crystal

The sequential segregation of Sn and Sb to the surface of a Cu(111) single crystal was measured in the temperature range 400–1100 K by Auger electron spectroscopy. It was found that Sn with the higher diffusion coefficient first segregates to the surface and then is replaced by the slower‐segregating Sb. The results were fitted by a ternary segregation model yielding segregation energies (ΔG_Sn = 76.3 kJ mol^?1, ΔG_Sb = 95.9 kJ mol^?1), interaction parameters (Ω_SnCu = 3.8 kJ mol^?1, Ω_SbCu = 16.2 kJ mol^?1, Ω_SnSb = ?5.3 kJ mol^?1) and diffusion coefficients (D_0(Sn) = 1.8 × 10^?5 m² s^?1, E_Sn = 173 kJ mol^?1, D_0(Sb) = 6.0 × 10^?5 m² s^?1, E_Sb = 205 kJ mol^?1) for both species. The validity of the interaction coefficients and segregation energies was verified using the Guttman equations for equilibrium segregation in ternary systems. Copyright © 2003 John Wiley & Sons, Ltd.     

Separation of113mIn from113Sn on an isotope generator with inorganic ionite

A method of preparation of hydrated zirconium oxide suitable for^113mIn generators was elaborated. A good separation of^113mIn from¹¹³Sn was obtained in the course of routine use of generator, with a very small admixture of zirconium in the eluate.     

Quasirelativistic study of 125Te nuclear magnetic shielding constants and chemical shifts

Calculations for ¹²⁵Te magnetic shielding constants and chemical shifts were carried out using a quasirelativistic Hamiltonian including the spin‐free relativistic, one‐ and two‐electron spin–orbit, and relativistic magnetic interaction terms. For the tellurium‐containing series Te(CH₃)₂, TeH₂, TeF₆, Te(CH₃)₄, and Te(CH₃)₂Cl₂, the relativistic effects amounted to as much as 1300 ppm and were very important for qualitatively reproducing the absolute value of the ¹²⁵Te shielding constants obtained experimentally. On the other hand, for the ¹²⁵Te chemical shifts the relativistic effects were less important, because they cancelled each other between the sample and reference compounds. © 2001 John Wiley & Sons, Inc. J Comput Chem 22: 1502–1508, 2001