Average cross-sections for (n, α) and (n,p) reactions on titanium in a fission-type reactor spectrum

The average cross-section in a fission-type reactor spectrum was determined experimentally for the reactions:⁴⁶Ti(n,p)⁴⁶Sc,⁴⁷Ti(n,p)⁴⁷Sc,⁴⁸Ti(n,p)⁴⁸Ti(n,α)⁴⁵Ca and⁵⁰Ti(n,α)⁴⁷Ca. In order to obtain the (n,p) cross-sections, reactor irradiation of titanium was followed by measurement of the induced scandium activities with a Ge(Li) detector of calibrated detection efficiency. For this no chemical separations had to be carried out. For the (n,α) reactions, however, the induced calcium activities were separeted and purified by oxalate precipitation, after the bulk of the radioactivity had been removed by precipitation of titanium hydroxide. The⁴⁷Ca disintegration rate was determined in the same way as for the scandium isotopes, whereas for⁴⁵Ca liquid scintillation counting was carried out. The shape of the reactor spectrum was investigated by irradiating reference threshold detectors with different effective threshold energies. To correct for (n,γ) interferences, irradiations were carried out with and without cadmium shielding. On the basis of \(\bar \sigma _F = 0.64\) mb for the reaction²⁷Al(n,α)²⁴Na, the average cross-sections were as follows:⁴⁶Ti(n,p)⁴⁶Sc:10.5±0.4 mb;⁴⁷Ti(n,p)⁴⁷Sc: 16.3±0.6 mb;⁴⁸Ti(n,p)⁴⁸Sc:0.272±0.005 mb;⁴⁸Ti(n,α)⁴⁵Ca: 34μb;⁵⁰Ti(n,α)⁴⁷Ca: 8.1±0.3 μb.     

The single-comparator method in thermal neutron activation analysis extended for some (n,p) reactions

From experimental studies of the rate of the reactions⁴⁷Ti(n, p)⁴⁷Sc,⁴⁸Ti(n, p)⁴⁸Sc and⁵⁸Ni(n, p)⁵⁸Co in four nuclear reactors, it is concluded that for the irradiation positions of the light water moderated reactors BR2 (Mol, Belgium) and HFR (Petten, Netherlands) a simple empirical relation exists between the fast neutron flux on the one hand and the thermal and epithermal neutron flux on the other. The graphite moderated reactor BR1 (Mol, Belgium) and the heavy water reactor FRJ2 (Jülich, Federal Republic of Germany), however, have relatively much lower fast fluxes and their irradiation facilities do not obey the empirical relation determined.     

Production of low and high specific activity <Superscript>64</Superscript>Cu in a reactor

Production of radioactive scandium by irradiating natural titanium metal in Pakistan Research Reactor-1 was evaluated. The production rate of ⁴⁷Sc and other radioactive scandium was estimated. High specific activity ⁴⁷Sc can be produced by irradiating enriched ⁴⁷Ti in sufficient quantities needed for therapeutic applications. A new separation technique based on column chromatography was developed. Neutron irradiated titanium was dissolved in hydrofluoric acid, which was evaporated and taken in distilled water. The resulting solution was loaded on silica gel column. The radioactive scandium comes out first and the inactive titanium is removed with 2 M HCl. More than 95% radioactive scandium was recovered, while chemical impurity of titanium determined by optical emission spectroscopy was less than 0.01 μg/mL in final product.     

Some problems of parametric neutron activation analysis based on the use of radioactive daughters of longer-lived mothers with low mother/daughter half-life ratios

The theoretical and practical aspects of the use of radioactive daughters originated from the decay of longer-lived radioactive mothers in parametric activation analysis, when the ratio: mother half-life to daughter half-life is less than 10, are discussed. The mother-daughter relationships: ⁴⁷Ca/⁴⁷Sc; ⁹⁵Zr/⁹⁵Nb; ¹⁴⁰Ba/¹⁴⁰La; ⁹⁹Mo/^99mTc and ¹¹⁵Cd/^115mIn are selected as models for the study. The cases when the radionuclide of interest is formed through both direct and indirect routes are also analyzed. As illustrative example, the direct reaction and the reaction chain: ⁴⁷Ti(n,p)⁴⁷Sc/⁴⁶Ca(n,γ)⁴⁷Ca(β⁻)⁴⁷Sc are evaluated with respect to the determination of the elements involved and their reciprocal interferences.     

Separation of carrier-free47Sc from titanium targets

The radiochemical separation of no-carrier-added (NCA)⁴⁷Sc from^natTi targets has been studied. Scandium-47, a medium-energy -emitter, is intended for use with labelled tumor associated monoclonal antibodies for radiotherapy. Several radiochemical methods for the separation of NCA⁴⁷Sc from macroquantities of titanium and other impurities were tested. Four different procedures based on ion exchange, solvent extraction and extraction chromatography are reported. For each method, parameters such as the distribution coefficient, kinetics and recoveries are reported. The selective separation can be performed rapidly by all methods.     

Measurement of calcium and titanium from 47sc by instrumental neutron activation analysis

A procedure is outlined for measuring calcium and titanium from ⁴⁷Sc by instrumental neutron activation analysis. Precise calcium measurements obtained from ⁴⁷Sc are compared with measurements based on ⁴⁷Ca and ⁴⁹Ca. The method is particularly suitable for low levels (ca. 1%) of calcium.     

Measurement of the50Ti(n,α)47Ca reaction cross section averaged over a235U fission neutron spectrum

The²³⁵U fission neutron spectrum averaged cross section for the⁵⁰Ti(n,)⁴⁷Ca reaction was experimentally determined by irradiation of titanium with reactor neutrons. A value of (9.7±1.1) b was found for this cross section, using (307±11) b for the⁴⁸Ti(n,p)⁴⁸Sc spectrum-averaged cross section that was used as a standard. The⁵⁰Ti(n,)⁴⁷Ca spectrum-averaged cross section was also semiempirically evaluated by numerically integrating, through the ENDF/B-V representation of the²³⁵U fission neutron spectrum, the available experimental differential cross section data.     

<Superscript>47</Superscript>Sc production development by cyclotron irradiation of <Superscript>48</Superscript>Ca

The therapeutic radionuclide ⁴⁷Sc was produced through the ⁴⁸Ca(p,2n) channel on a proton beam accelerator. The obtained results show that the optimum proton energies are in the range of 24–17 MeV, giving the possibility to produce ⁴⁷Sc radionuclide containing 7.4% of ⁴⁸Sc. After activation, the powdery CaCO₃ target material was dissolved in HCl and scandium isotopes were isolated from the targets. The performed separation experiments indicate that, due to the simplicity of the operations and the chemical purity of the obtained ⁴⁷Sc the best separation process is when scandium radioisotopes are separated on the 0.2 µm filter.     

Die Bestimmung von53Mn,Welches in Meteoritischem Material Durch Kosmische Strahlung Erzeugt Wurde,mit Hilfe der Neutronenaktivierung

Among a number of stable and unstable nuclides formed in material exposed to cosmic radiation the spallation nuclide⁵³Mn (T=2·10⁶ a) is investigated in meteoritic manganese by combined techniques of neutron activation and advanced γ-spectrometry. The need for an economic use of precious meteorites is so ensured best. Intense neutron bombardment transforms the long-livedK-emitter⁵³Mn into⁵⁴Mn, which is detected by its 0.84 MeV γ-rays. Using the (n,γ) cross section—recently derived byMillard—⁵³Mn-values in the range of 60–600 dpm/kg (10⁻¹¹ g/g) are found in a larger number of iron meteorite samples, which are only 1–3 g in weight. The determination is very specific and under appropriate conditions unaffected by side reactions. The attempt to use the⁴⁴Ti (n,γ)⁴⁵Ti reactions for the analysis of spallogenic titanium failed, because the σ_therm of⁴⁴Ti was found to be unexpectedly low (10 barns). Additionally,⁴⁵Sc was determined after (n,γ) reaction by the⁴⁶Sc γ,γ-cascades.      

Measurement of isomeric yield ratios for the 44m,gSc isomeric pairs produced from 45Sc and natTi targets at 50-, 60-, and 70-MeV bremsstrahlung

We measured the isomeric yield ratios for the ^44m,gSc isomeric pairs produced from different reaction channels ⁴⁵Sc(??,n)^44m,gSc and ^natTi(??,xnp)^44m,gSc by using the activation method and ??-ray spectroscopic methods at 50-, 60-, and 70-MeV bremsstrahlung energies. The high-purity natural Sc and Ti foils in disc shape were irradiated with uncollimated bremsstrahlung beams generated from an electron linear accelerator at Pohang Accelerator Laboratory. The induced activities in the irradiated foils were measured by the high-resolution ??-ray spectrometric system which consists of a high-purity Germanium detector and a multichannel analyzer. In order to improve the accuracy of the experimental results the necessary corrections were made in the ??-ray activity measurements and data analysis. The measured isomeric yield ratios for the ⁴⁵Sc(??,n)^44m,gSc reaction are 0.20 ± 0.02, 0.21 ± 0.02, and 0.21 ± 0.02 and those for the ^natTi(??,xnp)^44m,gSc reaction are 0.063 ± 0.012, 0.079 ± 0.014, and 0.124 ± 0.022 at 50-, 60-, and 70-MeV bremsstrahlung energies, respectively. The obtained results are compared with the corresponding values found in the literature. We observed that the isomeric yield ratios for the ⁴⁵Sc(??,n)^44m,gSc reaction increase rapidly with the increasing bremsstrahlung energies from the reaction threshold up to giant resonance region, and then those are almost constant in the energy range from about 30 to 2.5 GeV. The isomeric yield ratios for the ^natTi(??,xnp)^44m,gSc reaction increase with increasing bremsstrahlung energies in a wide range of bremsstrahlung energies from 50 to 2.5 GeV.     

Non-destructive compositional analysis of sol–gel synthesized lithium titanate (Li2TiO3) by particle induced gamma-ray emission and instrumental neutron activation analysis

Lithium titanate, one of the important tritium breeding materials in D–T based fusion reactor under ITER programme, was synthesized through sol–gel route. For chemical quality control of finished product, it was necessary to quantify the lithium and titanium contents. As this ceramic sample is difficult to dissolve, non-destructive analytical methods are preferred for compositional analysis. In the present work, two non-destructive nuclear analytical methods namely particle induced gamma-ray emission (PIGE) using proton beam and instrumental neutron activation analysis (INAA) using reactor neutrons were standardized for the determination of lithium and titanium concentrations, respectively and applied to eleven samples of lithium titanate. To the best of our knowledge, Li quantification in lithium titanate sample is being reported for the first time using PIGE. For quantifications of Li and Ti, 478 keV prompt gamma-ray from ⁷Li (p, p′γ) ⁷Li and 320 keV gamma-ray from ⁵⁰Ti (n,γ) ⁵¹Ti were measured, respectively, by high resolution gamma-ray spectrometry. The PIGE and INAA methods were validated using several synthetic samples containing lithium and titanium, respectively. Concentrations of lithium and titanium and Li/Ti mole ratios were evaluated and compared with the stoichiometric concentration of Li₂TiO₃.     

Isotope shift and hyperfine structure measurements in titanium I

High accuracy measurements of hyperfine structure due to⁴⁷Ti and⁴⁹Ti in the 3d ² 4s ² a ³ F ₂?3d ² 4s4p z ⁵ D ₁ absorption line at σ=18482.772 cm^?1 have been performed by use of a Doppler-free experiment, where a beam of titanium atoms is crossed by a CW single mode tunable dye laser. They have allowed for the determination of isotope shifts between⁴⁶Ti,⁴⁷Ti,⁴⁸Ti,⁴⁹Ti and⁵⁰Ti. By use of accurate values of mean square nuclear charge radii for the even isotopes, it has been possible to separate mass shifts from field shifts and to determine accurate values for the mean square nuclear charge radii of⁴⁷Ti and⁴⁹Ti. The field shift presents a marked odd-even staggering.     

Multi-element characterization of high-purity titanium dioxide by neutron activation analysis

A radiochemical neutron activation analysis method for the determination of 34 elements in titanium dioxide has been developed. For the assay of indicator radionuclides with short and with long half-lives, the radiochemical separation was performed by anion exchange on a Dowex 1 × 8 column and by combination of cation and anion exchange on a Dowex 50W × 8 and a Dowex 1 × 8 column from HF- and HF/NH₄F-medium, respectively. With both separation modes, a selective removal of the matrix-produced radionuclides ⁴⁶Sc, ⁴⁷Sc and ⁴⁸Sc was achieved. A selective extraction of copper with dithizone from 15 mol/L HF enabled counting the intensive but unspecific 511-keV rays of ⁶⁴Cu for the determination of Cu. The limits of detection achieved were between 0.004 ng/g for Sm and 0.8 μg/g for Sn (via ¹²⁵Sb). The elements La, Mn and Th were determined by instrumental neutron activation analysis only. These techniques were applied to the analysis of two titanium dioxide samples of different purity grade. The results and limits of detection are compared with those of other methods.     

Formation of Binuclear Zigzag Hexapentaene Titanium Complexes via a Titanacumulene [Ti=C=C=CH2] Intermediate

The reaction of bis(η⁵:η¹‐pentafulvene)titanium complexes with an allylidenephosphorylide Ph₃P=C(H)‐ C(H)=CH₂ leads to binuclear zigzag hexapentaene titanium complexes ( Ti2a , Ti2b ). The formation of the central C₆H₄ unit can be described as a spontaneous double C−H bond activation process, leading to an R₃P=C=C=CH₂ intermediate, as a synthon for a titanabutatriene fragment [(Cp^R)₂Ti=C=C=CH₂] (R: 2‐adamantyl, CH(p‐tol)₂). In a subsequent dimerization Ti2a and Ti2b are formed, proofed by single‐crystal X‐ray diffraction and NMR measurements. The reaction sequence is confirmed by DFT calculations.     

Separation of carrier-free 48Sc tracer and its determination by isotopic dilution

An easy method for speedy and quantitative separation of carrier-free scandium tracer formed by the (48)Ti(22)(n,p)(48)Sc(21) nuclear reaction has been developed. Separation of (48)Sc (1.83 days) from the target titanium metal was carried out by co-precipitating the tracer with calcium fluoride precipitated at pH approximately 4 from the solution of irradiated titanium in hydrofluoric acid. The freshly formed fluoride precipitate was dissolved in conc. hydrochloric acid, and the tracer extracted with tributyl phosphate and then stripped into aqueous medium. The carrier-free tracer was estimated by isotopic dilution. with calcium fluoride as non-isotopic diluent.     

Separation of 44Sc from 44Ti in the Context of A Generator System for Radiopharmaceutical Purposes with the Example of [44Sc]Sc-PSMA-617 and [44Sc]Sc-PSMA-I&T Synthesis

Today, ⁴⁴Sc is an attractive radionuclide for molecular imaging with PET. In this work, we evaluated a ⁴⁴Ti/⁴⁴Sc radionuclide generator based on TEVA resin as a source of ⁴⁴Sc. The generator prototype (5 MBq) exhibits high ⁴⁴Ti retention and stable yield of ⁴⁴Sc (91 ± 6 %) in 1 mL of eluate (20 bed volumes, eluent—0.1 M oxalic acid/0.2 M HCl) during one year of monitoring (more than 120 elutions). The breakthrough of ⁴⁴Ti did not exceed 1.5 × 10⁻⁵% (average value was 6.5 × 10⁻⁶%). Post-processing of the eluate for further use in radiopharmaceutical synthesis was proposed. The post-processing procedure using a combination of Presep^® PolyChelate and TK221 resins made it possible to obtain ⁴⁴Sc-radioconjugates with high labeling yield (≥95%) while using small precursor amounts (5 nmol). The proposed method takes no more than 15 min and provides ≥90% yield relative to the ⁴⁴Sc activity eluted from the generator. The labeling efficiency was demonstrated on the example of [⁴⁴Sc]Sc-PSMA-617 and [⁴⁴Sc]Sc-PSMA-I&T synthesis. Some superiority of PSMA-I&T over PSMA-617 in terms of ⁴⁴Sc labeling efficiency was demonstrated (likely due to presence of DOTAGA chelator in the precursor structure). It was also shown that microwave heating of the reaction mixture considerably shortened the reaction time and improved radiolabeling yield and reproducibility of [⁴⁴Sc]Sc-PSMA-617 and [⁴⁴Sc]Sc-PSMA-I&T synthesis.     

Studies in heavy ion activation analysis

¹⁸O induced radioactivation may be used for the trace detection of¹H via¹H (¹⁸O, n)¹⁸F. Matrices in which this reaction is interference-free include: Al, Si, S, K, Ti, V, Ni, Cu and Zn. However, due to numerous radioisotopes created at the bombarding energies used (E≥51 MeV), a post-irradiation chemical separation of¹⁸F is required.¹⁸O activation also appears as a promising means for the trace determination of S[S(¹⁸O, x)⁴⁷V], Si[Si(¹⁸O, x)^43–44Sc] and B[B(¹⁸O, x)³⁷Mg]. Part I: in Journal of Radioanalytical Chemistry, 53 (1979) 181.     

Production and chemical separation of <Superscript>48</Superscript>V

Summary Vanadium-48 was produced with an activity of 222 MBq (6 mCi) by the ^natTi(d,xn)⁴⁸V nuclear reactions in the U-120 cyclotron. The energy of the irradiating beam was 13 MeV, its intensity 5 μA, and the metallic Ti target dimension 11’11 mm² (0.1 mm thickness). For target cooling, circulated water in target backside was used. After 3 cooling days, only ⁴⁸V and some ⁴⁶Sc (T_1/2 = 83.8 d), produced by the side nuclear reaction ⁴⁸Ti(d,α)⁴⁶Sc were found in the target. For production of the radiotracer of ⁴⁸V and for the preparation of source for standardization of ⁴⁸V by 4πβ-γ coincidence, the Ti target was dissolved either in HF or in H₂SO₄. For both dissolving methods an ion-exchange separation procedure was developed.     

Synthesis and some properties of furylacrylates of aluminium(III) and titanium(IV)

Summary Compounds of the type [M(OPrⁱ)_m–n(FA)_n] (where m = 3 and n = 1 to 3 when M = Al; and m = 4 and n = 1 to 4 when M = Ti) have been synthesised by the reactions of aluminium and titanium isopropoxides with furylacrylic acid (HFA) in benzene. The corresponding tertiary butoxide derivatives, [M(OBu^t)_m–n(FA)_n], were also obtained by the alcohol-interchange technique. These compounds have been characterised by elemental analysis, and i.r. and p.m.r. spectra.     

New developments in the production of theranostic pairs of radionuclides

A brief historical background of the development of the theranostic approach in nuclear medicine is given and seven theranostic pairs of radionuclides, namely ^44gSc/⁴⁷Sc, ⁶⁴Cu/⁶⁷Cu, ⁸³Sr/⁸⁹Sr, ⁸⁶Y/⁹⁰Y, ¹²⁴I/¹³¹I, ¹⁵²Tb/¹⁶¹Tb and ¹⁵²Tb/¹⁴⁹Tb, are considered. The first six pairs consist of a positron and a β^?-emitter whereas the seventh pair consists of a positron and an α-particle emitter. The decay properties of all those radionuclides are briefly mentioned and their production methodologies are discussed. The positron emitters ⁶⁴Cu, ⁸⁶Y and ¹²⁴I are commonly produced in sufficient quantities via the (p,n) reaction on the respective highly enriched target isotope. A clinical scale production of the positron emitter ^44gSc has been achieved via the generator route as well as via the (p,n) reaction, but further development work is necessary. The positron emitters ⁸³Sr and ¹⁵²Tb are under development. Among the therapeutic radionuclides, ⁸⁹Sr, ⁹⁰Y and ¹³¹I are commercially available and ¹⁶¹Tb can also be produced in sufficient quantity at a nuclear reactor. Great efforts are presently underway to produce ⁴⁷Sc and ⁶⁷Cu via neutron, photon and charged particle induced reactions. The radionuclide ¹⁴⁹Tb is unique because it is an α-particle emitter. The present method of production of ¹⁵²Tb and ¹⁴⁹Tb involves the use of the spallation process in combination with an on-line mass separator. The role of some emerging irradiation facilities in the production of special radionuclides is discussed.