Selective removal of radio-sodium from neutron-activated materials by retention on hydrated antimony pentoxide

A new method is presented to remove sodium interferences from neutron-activated materials. The method is based on passage of the samples, dissolved in a concentrated acid solution on a column of hydrated antimony pentoxide (HAP). The retention is quantitative with a maximum capacity of 31 mg Na/g HAP. Only tantalum, in addition to sodium, was retained by HAP out of the 60 elements tested. The method should find applications in neutron activation analysis, particularly of biological materials. Applications are also foreseen in other analytical techniques, such as emission spectroscopy and flame spectrophotometry, where high sodium concentrations in the sample can be a source of interference.     

Studies on the selectivity of Na+ separation on specially prepared hydrated antimony pentoxide

The selectivity of Na⁺ separation on especially prepared hydrated antimony pentoxide (HAP) was studied with respect to trace elements. For this purpose NaCl samples, doped with 0.5 μg each of altogether 21 selected elements in form of suitable neutron activated compounds, were in relation to practice subjected to column experiments. In some cases trace elements were used in different oxidation states. Considered were elements which are of particular interest for neutron activation analysis. With simultaneous retention of Na⁺ (DK≥10⁸) Cs, Ba, Sc, La, Ce, Eu, Cr, Mo, Mn, Co, Cu, Ag, Au, Zn, Cd, Hg, and Sb are completely eluted from the HAP column, using 7.5N HCl, whereby Cs and to some extent Ba and Sc in comparison to the elements mentioned above required a higher elution volume. Rb, Se and As on the contrary were almost quantitatively retained on HAP column, W partly as WO ₄ ^2? . The scope of validity of the results will be discussed.     

Structural conversions of hydrated antimony pentoxide during absorption of cations and polar adsorbates

X-ray diffraction analysis data has been used to calculate the electron-density distribution of a squared crystal of hydrated antimony pentoxide during sorption of water, nitric acid, and strontium cations. It has been shown that absorption of water and acid molecules causes reversible changes of the anionic framework of the ionite. Sorption of divalent cations is accompanied by irreversible phase transformations in the sorbent structure, which is also the cause of the particularly strong retention of particles of the material absorbed.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 22, No. 2, pp. 229–234, March–April, 1986.     

Separation of no-carrier-added radioactive scandium from neutron irradiated titanium

In this work, sorption of Ni(II) from aqueous solution to goethite as a function of various water quality parameters and temperature was investigated. The results indicated that the pseudo-second-order rate equation fitted the kinetic sorption well. The sorption of Ni(II) to goethite was strongly dependent on pH and ionic strength. A positive effect of HA/FA on Ni(II) sorption was found at pH < 8.0, whereas a negative effect was observed at pH > 8.0. The Langmuir, Freundlich, and D-R models were applied to simulate the sorption isotherms at three different temperatures of 293.15 K, 313.15 K and 333.15 K. The thermodynamic parameters (ΔH ⁰, ΔS ⁰ and ΔG ⁰) were calculated from the temperature dependent sorption, and the results indicated that the sorption was endothermic and spontaneous. At low pH, the sorption of Ni(II) was dominated by outer-sphere surface complexation or ion exchange with Na⁺/H⁺ on goethite surfaces, whereas inner-sphere surface complexation was the main sorption mechanism at high pH.     

Separation of heavier rare earths from neutron irradiated uranium targets

A radiochemical method is described for the separation of heavier rare earths from the fission of uranium. The method is particularly suitable for the separation of low yield (10⁻⁵%–10⁻⁷%), highly asymmetric rare earth fission products viz.^179,177Lu,¹⁷⁵Yb,¹⁷³Tm,^172,171Er,¹⁶⁷Ho and^161,160Tb in the neutron induced fission of natural and depleted uranium targets. Additional separation steps have been incorporated for decontamination from²³⁹Np (an activation product) and^93-90Y (a high fission-yield product) which show similar chemical behaviour to rare earths. Separation of individual rare earths is achieved by a cation exchange method performed at 80°C by elution with α-hydroxyisobutyric acid (α-HIBA).     

Studies on the preparation of hydrated antimony pentoxide (HAP) to separate Na+ in the field of radioanalytical investigations

Summary Hydrated antimony pentoxide with favourable chemical and mechanical properties could be produced from an aqueous suspension of antimonic acid by a two stage drying process.A decisive factor for the pre-drying is that the compound should be given the chance to form crystalline structure, the existence of which is the primary condition for the retentive effect of HAP on Na⁺-ions.The post-drying leads to a decrease of elutability of Na⁺-ions. This is accompanied by a reduction of the lattice constant and the water content of the products.

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Über die Herstellung von wasserhaltigem Antimonpentoxid zur Abtrennung von Na⁺ bei radioanalytischen Untersuchungen

Zusammenfassung Wasserhaltiges Antimonpentoxid mit ausgezeichneten chemischen und mechanischen Eigenschaften läßt sich durch einen zweistufigen Trocknungsprozeß aus einer wäßrigen Suspension von Antimon-V-säure herstellen. Entscheidend für die Vortrocknung ist, daß die Verbindung kristalline Struktur annimmt. Dies ist die erste Bedingung für den Retentionseffekt gegenüber Na-Ionen. Die Nachtrocknung führt zur Abnahme der Auswaschbarkeit dieser Ionen. Daneben erfolgt eine Herabsetzung der Gitterkonstante und des Wassergehaltes der Produkte.

     

Determination of selected trace metals in scallops by flame atomic absorption spectrometry after removal of sodium on hydrated antimony pentoxide

Hydrated antimony pentoxide is used to remove sodium ion for the determination of trace metals in scallop specimens of Plactopecten magellanicus. The concentrations of Cd, Cr, Co, Cu, Au, Fe, Pb, Mn, Hg, Ni, Ag and Zn were determined in the samples and in a standard reference material. This method yields improved detection limits with simple apparatus.     

Separation of antimony from synthetic cloth: Application in forensic science using neutron activation analysis

Summary A simple ion-exchange separation procedure was developed for selective removal of antimony from synthetic cloth to facilitate determination of several trace elements frequently used to identify gunshot residues by neutron activation analysis. Radiotracers of Sb, Ba, Cu, Co, As, Zn, Hg and Ag were employed to optimize the developed procedure. The method involves the quantitative retention of the above elements, except of Sb, from 0.2M ammonium carbonate solution using Chelex 100 resin and subsequent quantitative elution of the elements of interest with 2M nitric acid for gamma-ray spectrometry. The procedure was tested by simulated gunshot residues.     

The determination of traces of antimony,tin and arsenic in cadmium by pulse polarography

Traces of antimony, tin and arsenic in cadmium products were determined by pulse polarography. Arsenic was distilled, while antimony and tin were precipitated as hydroxides with manganese dioxide as carrier; some lead was coprecipitated with tin, hence these elements were further separated by distillation. In all cases quantitative recoveries were obtained. Antimony(III) was determined in a hydrochloric acid-sodium hypophosphite mixture, tin(IV) in a hydrochloric-hydrobromic acid mixture and arsenic(III) in sulphuric acid as supporting electrolytes; for arsenic(III), methylene blue had to be added. A sample weight of 10 g and an end volume of 10 ml allowed the determination down to about 0.004 p.p.m. antimony, 0.006 p.p.m. tin and 0.003 p.p.m. arsenic in cadmium. Several synthetic samples and commercially available cadmium products were analysed.     

Determination of indium in metallic tin and cadmium by substoichiometric neutron activation analysis

The paper deseribes the determination of indium in metallic tin and cadmium metals by the direct method, which is a variant of substoichiometric radioactivation analysis. It is based on substoichiometric extraction of indium diethyldithiocarbamate into carbon tetrachloride. Indium in tin metal was determined by^116mIn (T=54 min), while^115mIn (T=4.5 h), formed by the reaction¹¹⁴Cd(n, γ)¹¹⁵Cd was used for cadmium samples. The irradiated sample was dissolved and the radioactivity of^116mIn or^115mIn, A, was measured. After the separation of indium from the matrix, a known amount of indium, m, was separated substoichiometrically and the radioactivity, a, was measured. Indium was calculated as M_x=m A/a. If a known amount of the element, M, is added to the irradiated sample in advance, the equation for calculation is given as M_x-m A/a−M. By this method, indium can be determined without any consideration of self-shielding and secondary nuclear reaction of the matrix.     

Separation of antimony(V) from iron(III), copper(II), cobalt(II) and cadmium(II) by ion-exchange

With excess of tartaric acid, antimony(V) forms a stable anionic complex that completely escapes adsorption on a cation-exchange ream, Zeo-Carb-225, while Cu(II), Fe(IIl), Co(II) or Cd(II) is quantitatively retained. Antimony(V) can be separated from these ions in this way.     

C13 NMR investigation of solutions of organic bases in tin and antimony halides

Theoretical and Experimental Chemistry -     

Separation of no-carrier-added 113,117mSn and 113m,114mIn from alpha particle irradiated natural cadmium target

A natural cadmium foil was irradiated by 42 MeV α-particles to produce ^113,117mSn, ^{111,113m,114m}In simultaneously in the target matrix. After the complete decay of short lived radionuclides, long-lived NCA products were separated sequentially from the bulk cadmium by liquid–liquid extraction using di-(2-ethylhexyl)phosphoric acid (HDEHP) dissolved in cyclohexane as organic phase and HCl as aqueous phase. At the optimum condition, 10^?2 M HCl and 5 % HDEHP, NCA In along with NCA Sn radionuclides (75 %) were separated from the bulk Cd resulting to high separation factors of 2.7 × 10⁴ (D _In/D _Cd) and 500 (D _Sn/D _Cd), respectively. The NCA In was stripped back completely to the aqueous phase by 6 M HCl leaving NCA Sn in the HDEHP phase with a separation factor (D _Sn/D _In) of 3.94 × 10⁶.     

Separations involving sulphides : Separation of rhenium and antimony from mercury

It has been shown that it is possible to estimate rhenium or antimony in the presence of mercury by decomposing their thiosalts but not platinum, gold. selenium and tin.     

Thermal radiation from C(N)+ and La@C(N)+

The radiative cooling of positively charged fullerene and endohedral fullerene fragments of C60, C70, C84, and La@C82 has been measured in a time-of-flight mass spectrometer. The radiative cooling is measured via its influence on the metastable decay. The emissivity extracted from the data is between 4x10(-4) and 13x10(-4). These values agree fairly well with the emissivity calculated from considering the low-energy tail of the surface plasmon. No major difference is found in the emission behavior of empty and endohedral fullerenes.     

Separation of different valency states of iron,arsenic, antimony,mercury, tin and chromium by thin-layer chromatography

Summary Different valency states of iron, mercury, tin, arsenic, antimony and chromium were separated by the thin-layer chromatography on starch and cellulose, using nine different solvent systems.     

A procedure for simultaneous determination of arsenic,cadmium, copper,tin and zinc in beef extract by neutron activation analysis

A radiochemical procedure developed by the authors for neutron activation analysis of As, Cd, Cu, Sn, and Zn in beef extract samples is described, based on combined precipitation steps to isolate the elements to be determined. Nuclides are separated with high degree of purity and good chemical yields. Interferences from threshold reactions are discussed and calculated. Results are shown for analysis of six samples.     

A radiochemical neutron activation analysis method for the determination of tin,arsenic, copper and antimony for the forensic comparison of bullet lead specimens

Trace element characterization of bullet lead by instrumental neutron activation analysis (INAA) is hampered by the high spectral background due to antimony, normally present in high concentration in bullet lead. Tin is indicated to be a very useful element for characterization purposes. Beta-active¹²¹Sn is a suitable nuclide for quantitation of tin provided it is separated in high radiochemical purity. A radiochemical procedure capable of determining tin down to 10 ppm in bullet lead, a sequential procedure for its determination along with copper, arsenic and antimony and the application of this procedure for the determination of the contents of these elements in various bullet leads are described. This method has been applied to a “Rhinoceros shoot-out” case, referred to our laboratory.