The determination of tin in rocks by thermal neutron activation

A fast routine method for the determination of tin in rocks is discussed. The method is based on coprecipitation of tetravalent tin with ferric hydroxide, followed by a short irradiation in a high thermal neutron flux, extraction in toluene from 1∶1 sulphuric acid which is 5N in potassium iodide, and counting of^123mSn (T=40 m) or^125mSn (T=9.7 m) with a well-type NaI detector. In the present work^125mSn was used. The lower limit of determination is governed by the blank of the reagents. For a sample of at least one gram it is ≌ 0.2 μg Sn·g⁻¹.     

Subtoichiometric determination of indium and tin by radioactivation analysis

A method of radioactivation analysis has been developed for the determination of indium and tin. It is based on substoichiometric extraction of indium diethyldithiocarbamate into carbon tetrachloride from a slightly ammoniacal solution in the presence of potassium cyanide. With this method, indium can be determined via^116m In (T=54 min) and tin via^113m In (T=104 min) which is formed by the reaction¹¹²Sn(n, ψ)¹¹³Sn. The method has been applied to the determination of indium in metallic zinc and of tin in tin-doped gallium arsenide, and 0.4 ppb of indium was analyzed in a zinc sample.     

Interferences in the determination of trace elements in high-purity tin

Reactor neutron activation analysis of antimony, indium and cadmium in high-purity tin is interfered with by nuclear reactions on the tin matrix. For a number of interfering reactions the cross-sections were determined. The following results were obtained:¹²²Sn(n,γ)^123mSn:σ_th=0.145 barn, I=0.79 barn;¹²²Sn(n,γ)¹¹³Sn:σ_th=0.52, I=25.4 barn;¹¹²Sn(n, 2n)¹¹¹Sn: microbarn;¹¹⁸Sn(n, α)¹¹⁵Cd: microbarn; and¹¹⁴Sn(n, p)^114m1In: microbarn.     

The determination of tin in biological samples

A rapid method is described for the determination of tin in biological material, using¹²³Sn (T=40 m). The chemical procedure is based on the nearly quantitative extraction of tetravalent tin into toluene from an acid 1.3M iodide solution. The recovery is determined by spiking the solution with¹¹³Sn and measuring the activity of the^113mIn daughter in the counting sample. The lower limit of the determination is ?0.01μg. Results are given for standard kale powder and dried animal blood.     

Instrumental activation analysis for determining the composition of micro-ingots of multi-constituent alloys

A procedure for the instrumental neutron activation analysis of micro-ingots of alloys containing In, Sb, Au, Ga, Ni, Sn and Bi is proposed. The non-destructive analysis of the irradiated samples is performed by γ-spectrometry techniques including one-crystal scintillation detectors, dual-crystal sum-coincidence scintillation detectors and Ge(Li) semiconductor detectors. As a result, the cumbersome operations of radiochemical separation can be eliminated. The sensitivity of quantitative determinations using scintillation detectors in alloys of the above composition is 10⁻¹⁰ g for indium, gold, antimony and gallium and 10⁻⁶ g for nickel and tin. The use of semiconductor detectors yields sensitivities of 10⁻¹⁰ g for indium and gold and 10⁻⁹ g for gallium and antimony.     

Tin(II) Phthalocyaninate and Tin(IV) bis-Phthaloc Yaninate: A Quantum Chemical Study

The structural parameters of tin(II) phthalocyaninate PcSn and tin(IV) bis-phthalocyaninate Pc₂Sn as well as of their cations are determined by B3LYP/SDD and PBE0/SDD quantum chemical methods. The PcSn molecule is characterized by C_4v symmetry, and SnN bond lengths are 2.307/2.299 ? (B3LYP/PBE0). The Sn nucleus is by 1.11 ? (B3LYP, PBE0, single crystal X-ray diffraction analysis) higher than the plane of four neighboring nitrogen nuclei. The “hindered” configuration (D _4d symmetry) with a high (27–30 kcal/mole) internal rotation barrier corresponds to the Pc₂Sn energy minimum. The calculated equilibrium lengths of eight equivalent SnN bonds of 2.366/2.347 (B3LYP/PBE0) are similar to the average SnN bond length of 2.347 ? (single crystal X-ray diffraction). Vertical and adiabatic ionization potentials are calculated: I^v 6.40/6.48 eV, I^A 6.38/6.45 eV for PcSn and I^v 5.63/5.66 eV, I^A 5.60/5.63 eV for Pc₂Sn.     

Labeling bombesin-like peptide with <Superscript>99m</Superscript>Tc via hydrazinonicotinamide: description of optimized radiolabeling conditions

Bombesin (BNN)-like peptides have very high binding affinity for the gastrin-releasing peptide (GRP) receptor. The goal of the current study was to optimize the labeling conditions of a new ^99mTc-radiolabeled BNN-like peptide based on the bifunctional chelating ligand HYNIC using different co-ligands (EDDA and tricine). The radiolabeling conditions (pH, amount of co-ligand, amount of stannous chloride, temperature and reaction time) for newly-formed ^99mTc-tricine-HYNIC-Q-Litorin and ^99mTc-EDDA-HYNIC-Q-Litorin were optimized and evaluated by RHPLC and RTLC. Radiochemical yields for ^99mTc-tricine-HYNIC-Q-Litorin and ^99mTc-EDDA-HYNIC-Q-Litorin were 98.0 ± 1.7 and 97.5 ± 2.5%, respectively. When EDDA was used as co-ligand, the labeling of ^99mTc-EDDA-HYNIC-Q-Litorin was optimal in the following reaction mixture: HYNIC-peptide: EDDA: 10 μg/5 mg, pH 3, SnCl₂ concentration: 12 μg/0.1 mL, reaction temperature: 100 °C, reaction time: 15 min. Besides, the optimum conditions were HYNIC-peptide:tricine: 10 μg/50 mg, pH 5, SnCl₂ concentration: 12 μg/0.1 mL, reaction temperature: 100 °C, reaction time: 15 min for preparing ^99mTc-tricine-HYNIC-Q-Litorin. The manufactured ^99mTc-HYNIC-Q-Litorin conjugates may offer new possibilities for imaging cancer cells expressing bombesin receptors.     

Codeposition of copper and tin from acidic sulfate solutions containing polyethylene glycols. Effect of length of the hydrocarbon chain

Voltammetry and electrochemical impedance spectroscopy technique were applied to study the effect of polyethylene glycols (PEG) with different molecular mass on Cu(II) and Sn(II) reduction kinetics in acidic sulfate solutions. Tetraethylene glycol was found to be the surface-active oligomer on both Cu and Sn substrates that holds the shortest (–CH₂–CH₂–O–)_m chain. The exchange current density of the rate-limiting step Cu²⁺ + e → Cu⁺ falls drastically with an increase in the molecular mass of PEG. An addition of PEG into halide-free Sn(II) solutions results in the significant inhibition of Sn(II) reduction in the entire range of cathodic polarizations including the region of limiting current. Inhibition degree also increases with PEG molecular mass. In contrast with Cu|Cu(II) system, formation of adsorption layers on Sn electrodes proceeds significantly slower. Underpotential deposition of Sn(II) is observed in the region of Cu(II)-limiting current. The characteristic current minimum arises in the region where free Sn phase is thermodynamically stable. It deepens with the length of the hydrocarbon chain of PEG. The fall of current density seems to arise from the inhibitive PEG adsorption on tin atoms that are still not incorporated into general Cu–Sn lattice.     

Sorption kinetics of tributyltin on Elbe river biofilms

For the first time detailed sorption kinetics of tributyltin on native Elbe river biofilms are presented. For this purpose a modified annular rotating continuous flow reactor has been used to develop a reproducible biofilm. Important parameters, such as flow rates, sheer forces, and nutrient concentrations could be varied independently and adjusted to natural conditions. Time-resolved sorption kinetics have been carried out with tributyltin, the most toxic compound in many antifouling paints. The highest sorption rates of tributyltin were observed during the first 0–10 min (0.60±0.05 g Sn m^–2min^–1) than they decreased to a value of 0.10±0.10 g Sn m^–2min^–1 (10–90 min) and increased to a value of 0.20±0.05 g Sn m^–2min^–1 (90–120 min).     

Synthesis and Characterization of Tin Oxide Nanoparticles by Solid State Chemical Reaction Method

High purity tin oxide nanopowders have been synthesized by using a solid-state chemical reaction technique with annealing at elevated temperature. The effects of two parameters, specifically by controlling the annealing temperature and kind of alkaline chlorides as precursors, the effect on particle size, morphology and IR spectra of synthesized tin oxide nanopowder were investigated. From the X-ray pattern, the crystal structure of the synthesized powders was confirmed as a tetragonal structure. Based on the recorded FTIR spectrum of SnO₂, the IR bands due to SnO₂ vibrations and its lattice modes were observed at 625 and 690 cm⁻¹, respectively. In addition, an important characterization peak has been identified at 1,450 cm⁻¹ due to Sn–O–Sn bridges observed only when LiCl was used as precursor. The formation of Sn–O–Sn bridges was confirmed by TGA–DTA analysis. According to the SEM images, it is obvious to notice that the kind of alkaline chlorides as precursors play a dominant role in controlling the morphology of tin oxide nanopowders.     

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.     

The effect of tin precursors on the formation of Zr<Subscript>0.8</Subscript>Sn<Subscript>0.2</Subscript>TiO<Subscript>4</Subscript> nano-powder by sol gel process

Different precursors can have different effects upon the properties of materials. In this paper, two different tin precursors, i.e., tin (IV) chloride pentahydrate (SnCl₄·5H₂O) and tin (IV) t-butoxide (Sn(OC₄H₉)₄) have been used to prepare Zr_0.8Sn_0.2TiO₄ powders. The dry gel and powder were characterized by Simultaneous DTA/TGA analysis (SDT), X-ray diffraction (XRD), Scanning electron microscopy (SEM), and Accelerated surface area and porosimetry analyzer (ASAP). The results show less weight loss for dry gel from precursor SnCl₄·5H₂O than that of Sn(OC₄H₉)₄. The onset of polycrystalline ZST nano powders occurred at 450 °C from precursor SnCl₄·5H₂O which is 50 °C lower than that of Sn(OC₄H₉)₄. Even though the powders from SnCl₄·5H₂O had a specific surface area of 30.4 m²/g which is higher than that of 28.7 m²/g from Sn(OC₄H₉)₄. The crystallite size of ZST powders were about the same around 15 nm. This may be due to the powders are more aggregated in Sn(OC₄H₉)₄ system. Two major mechanisms are proposed for above differences in morphology and the formation of powders.     

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.     

Production of <Superscript>122</Superscript>Sb for the study of environmental pollution

This article presents, ¹²²Sb (T _1/2 = 2.723 days, I _β- = 97.59%) was produced via the ^natSn(p,xn) nuclear process at the AMIRS (Cyclone-30, IBA, Belgium). The electrodeposition experiments were carried out by potassium stannate trihydrate (K₂Sn(OH)₆) and potassium hydroxide. The optimum conditions of the electrodeposition of tin were as follows: 40 g/L ^natSn, 20 g/L KOH, 115 g/L K₂Sn(OH)₆, DC current density of 5 A/dm² with a bath temperature of 75 °C. The electroplated Tin-target was irradiated with 26.5 MeV protons at current of 180 μA for 20 min. Solvent extraction of no-carrier-added ¹²²Sb from irradiated Tin-natural target hydrochloric solution was investigated using di-n-butyl ether (C₈H₁₈O). Yields of about 3.61 MBq/μAh were experimentally obtained.     

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.     

Separation of <Superscript>113m</Superscript>In from <Superscript>113</Superscript>Sn based on activated carbon used as column matrix

The activated carbon was prepared by using corncobs and characterized by sorpatometer for using as an exchanger material to separate the generated ^113mIn from ¹¹³Sn and ^124,125Sb. To optimize the separation process, the different parameters like acetone percentage, HCl concentration were studied. The exchange capacity of Sn(IV) is 7.6 meq/g onto the activated carbon and the elution efficiency of ^113mIn > 80% by using 10 mL of 0.2 M HCl-80% acetone with flow rate 1 mL/min. The radionuclidic purity and radiochemical purity of the eluted ^113mIn were examined and clarified the presence of ^124,125Sb with relatively high level as radio impurities, so further separation was carried out by using Dowex 1×8 as an anion exchanger below the activated carbon matrix on the same separation column to adsorb the ¹¹³Sn and ^124,125Sb, which escape from the activated carbon matrix.     

Determination of lead in sediments and sewage sludge by on-line hydride-generation axial-view inductively-coupled plasma optical-emission spectrometry using slurry sampling

Among the “traditional” hydride-forming elements, lead is probably the most difficult, and its determination in this form has rarely been reported in the literature. In this paper a simple and rapid method, axial-view inductively-coupled plasma optical-emission spectrometry using on-line hydride generation (HG–ICP–OES) from samples prepared as slurry, is proposed for determination of lead in environmental samples. The samples (20–50 mg, particle size ≤120 μm) were treated with 1 mL aqua regia in a 40-kHz ultrasonic bath for 60 min. The slurry was diluted to a final volume of 50 mL with a 10% m/v solution of (NH₄)₂S₂O₈. The concentrations of NaBH₄, tartaric acid, and (NH₄)₂S₂O₈, used for on-line plumbane generation were optimized by means of a complete factorial analysis applied to an aqueous standard solution and to the slurry of a sediment certified reference material (CRM). External calibration against aqueous standards in the concentration range 10–100 μg L⁻¹ was used for analysis of six CRM—three marine sediments, one river sediment, and two sewage sludges. Analysis of the filtered slurry showed that Pb was only partially extracted into the liquid phase. Several major concomitants tested did not affect the Pb signal. The detection limit (3s, n = 10) for 20 mg sample in a final volume of 50 mL was 5.0 μg g⁻¹. Tin was the only other hydride-forming analyte that could be determined satisfactorily with Pb; for tin the detection limit was 1.0 μg g⁻¹. The values obtained for Pb and Sn were not significantly different from the certified concentrations, according to the t-test at the 95% confidence level. Nine river sediments collected locally were also analyzed and the concentrations were in agreement with results obtained after total digestion.     

Inhibition activity of ethyleneglycol and its oligomers on tin electrode

Voltammetry and electrochemical impedance spectroscopy were applied to investigate the inhibition activity of ethyleneglycol and its oligomers on tin electrode in strong acidic sulfate solutions. Tetraethyleneglycol was found to be the most active substance among compounds HO–(CH₂–CH₂–O) _m –H (m≤4) that retards diffusion-controlled Sn(II) reduction due to its inhibitive adsorption. This rather slow process is controlled both by diffusion and electrosorption steps. A comparison of exchange current densities obtained in the presence of different polyethers shows that the length of the hydrocarbon chain is the main factor responsible for inhibition activity of such substances on tin electrode.     

MOR/SBA-15复合分子筛的合成、表征及其催化性能评价

采用MOR纳米晶和正硅酸四乙酯为硅源,P123三嵌段共聚物为模板剂水热合成MOR/SBA-15复合分子筛催化剂。采用XRD、SEM、TEM和EDX等手段对催化剂进行了表征,在固定床反应器中评价二甲醚制乙醇催化性能。结果表明,通过控制合适的MOR纳米晶种及MOR纳米晶种在SBA-15水热合成体系中的添加量,可以成功地将MOR纳米晶作为SBA-15的结构单元嫁接到SBA-15的介孔骨架中,水热合成的MOR/SBA-15复合分子筛催化剂同时具有MOR和SBA-15的XRD特征衍射峰,相比于SBA-15,其比表面积和总孔体积由756 m2·g~(-1),1.07 cm3·g~(-1)降低至628 m2·g~(-1),0.85 cm3·g~(-1),平均孔径由8.1 nm提高到9.3nm,Cu修饰的MOR/SBA-15复合分子筛催化剂同时具有Cu MOR羰基化和Cu SBA-15加氢的双功能催化性能,其催化剂评价结果显示二甲醚转化率为43.6%左右,乙醇选择性为95.3%,Cu MOR/SBA-15复合分子筛催化剂实现了二甲醚到乙醇的一步转化。     

Hydrogen peroxide induced formation of peroxystannate nanoparticles

Stable, amorphous potassium peroxystannate nanoparticles of controlled average size—in the range 10–100 nm—and of controlled hydrogen peroxide content—in the range of 19–30 wt%—were synthesized by hydrogen peroxide induced polymerization in water–potassium hexahydroxostannate solutions. The sol phase and the precipitate were characterized by vibrational spectroscopies, ¹¹⁹Sn NMR, XPS and XRD using crystalline K₂Sn(OH)₆ and K₂Sn(OOH)₆ reference materials. This is the first study to show that peroxocoordination induces polymerization of a main group element. ¹¹⁹Sn NMR studies show that peroxotin coordination and polymerization took place already in the hydrogen peroxide–water phase. The high abundance of peroxotin bonds revealed by ¹¹⁹Sn MAS NMR, vibrational spectroscopy, and XPS suggests that the particles are predominantly made of peroxo bridged tin networks. Although the particles are highly stable in the dry phase as well as in alcohol solutions and do not lose hydrogen peroxide upon storage, they release their stored hydrogen peroxide content by exposure to water.