•An extraction resin utilizing 2-thenolyltrifluoroacetone selectively isolates gold.•Efficient gold isolation in complex nuclear forensics-relevant samples.•Zirconium, iron, gallium, and thallium can ...be extracted from complex samples.
Post-detonation nuclear forensics capabilities depend on the ability to rapidly isolate radionuclides to improve measurement quality. In this work an extraction chromatography resin was developed utilizing thenoyltrifluoroacetone and 1-octanol supported on Eichrom prefilter resin. The resin was tested in nitric and hydrochloric acid matrices. In nitric acid the resin was able to extract zirconium, while in hydrochloric acid matrices it was possible to extract iron and gallium. In all acid conditions tested, gold was retained but can be eluted from the column with 10 % thiourea.
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•A novel extraction chromatography resin containing a calix4arene-mono-crown-6 has been prepared.•The resin was found to be far superior to the only similar resin reported before.•The extraction of ...radio-cesium could be done from 3 M HNO3 and the stripping of the loaded activity was done by water.•The resin has good radiation stability and recyclability for about 5 cycles of loading and stripping.•The resin hold great potential for application in actual acidic radioactive feeds.
An extraction chromatography resin, prepared by the impregnation of bis-octyloxy-calix4arene-mono-crown-6 (BOCMC)onto an acrylic ester based polymeric support material, gave excellent uptake data for the removal of radio-cesium (Cs-137) from nitric acid feed solutions. The weight distribution coefficient (Kd) value of >300 obtained during the present study at 3 M HNO3 was the highest reported so far while using a calix-crown-6 based extraction chromatographic resin material. Analogous resin reported previously has yielded a Kd value <100 at comparable feed conditions. The sorbed metal ions could be efficiently desorbed with de-ionized water. Kinetic modeling of the uptake data indicated that both the film and the intra-particle diffusion mechanism are simultaneously operating in the sorption of Cs+ion onto the BOCMC resin. The metal ion sorption data were fitted to the sorption isotherm models and did not conform to the chemisorptions of physisorption models and indicated a pi-pi interaction between the benzene rings of the calix-crown-6 ligand and the Cs+ ion. The reusability of the resins was quite satisfactory after 5 cycles and the radiation stability of the resin material was very good upto an absorbed dose of 500 kGy. The results of column studies were quite encouraging with 15 mL (9 bed volumes) as the breakthrough volume while the elution was complete in about 12 bed volumes of de-ionized water.
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The radiotherapeutic 195mPt is among the most effective Auger electron emitters of the currently studied radionuclides that have a potential theranostic application in nuclear medicine. Production of ...195mPt through double neuron capture of enriched 193Ir followed by β−-decay to the radioisotope of interest carried out at the research reactor IBR-2 is described. Because of the high radiation background, radiochemical purification procedure of 195mPt from bulk of iridium was needed to be developed and is detailed here as well. For the first time, cross section and resonance integral for the reaction 194Ir(n,γ)195mIr were determined. Resonance neutrons contribution was established to exceed that of thermal neutrons, and resonance integral for the reaction 194Ir(n,γ)195mIr is calculated to be 2900 b. Specific activity of 195mPt was estimated to reach a value of 38.7 GBq/(g Pt) at IBR-2 by the end of bombardment (EOB).
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Silver-111 (111Ag, t1/2 = 7.47 d) is a β− emitter suitable for targeted cancer therapy due to favourable decay properties. The production of no-carrier added 111Ag via Isotope Separation On-Line ...(ISOL) technique is being investigated at the Legnaro National Laboratories of the Italian Institute of Nuclear Physics (ISOLPHARM project). Stable Cadmium-111 (111Cd) is co-produced as isobaric contaminant, hence a chemical separation process must be developed to selectively harvest 111Ag. In this study, a chromatographic procedure employing the commercially available CL resin was investigated by using stable Ag+ and Cd2+. Results indicate that CL resin allows to efficiently separate Ag+ from Cd2+ and recover the former with high yields.
•Silver-111 (t1/2 = 7.47 days) is a β− emitting radionuclide suitable for cancer therapy.•During 111Ag production via ISOL method, 111Cd is co-produced.•Chromatographic method using commercially available CL resin was developed to separate silver from cadmium.
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Formation of Yb and Tm radioisotopes upon irradiation of ytterbium of natural isotopic composition by bremsstrahlung photons with energies up to 55 MeV was studied. The yield of the medical ...radionuclide 167Tm was (7.8 ± 1.1) × 103 Bq × μA-1 × h−1 × cm2 × g−1. Thulium radioisotopes were separated from irradiated ytterbium target by extraction chromatography on the LN Resin sorbent in nitric media. Efficient separation of tracer amounts of thulium from tens of milligrams of ytterbium could be achieved. The method can be of practical importance for the production of 167Tm when using a 168Yb enriched target.
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•Simple process for At-211 recovery and purification from α-particle bombarded Bi-209.•Elegant recovery of At-211 directly from nitric acid media, yield greater than 95%.•Rapid ...purification of At-211 in under 20 min, decontamination factor greater than 105.
The near quantitative separation, purification, and recovery of 211At has been demonstrated through an extraction chromatography process which utilizes porous beads impregnated with 3-octanone, resulting in an elution yield of 92–95%. Moreover, the rapid nature of this process, <20 min, was achieved after dissolution of a Bi metal target in HNO3 following retrieval from the beamline after α-particle bombardment. The solution was directly loaded onto the column with no volume or acidity adjustment. The column was washed with HNO3 and H2O, and 211At was eluted with ethanol, collecting roughly 87–93% in 1 mL. This process of recovering high purity 211At, in near quantitative yields, represents a significant advance in At separations.
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•Extraction chromatography has proven to be a promising green technology for separating individual REEs.•The best separation efficiency for the entire REE series was obtained with HDEHP, followed by ...TBP and Aliquat-336.•The method achieves the separation of the entire REE series in single or fewer steps.•Separation of REEs into several subgroups achieved by overloading the extraction column.•Common mineral acids can be used as eluent to eliminate the use of toxic and flammable organic solvents.
The effectiveness of commonly used extractants for chromatographic separation of rare earth elements (REEs) was compared. Columns loaded with similar molar concentrations of tributyl phosphate (TBP), di-(2-ethylhexyl) phosphoric acid (HDEHP), and N-Methyl-N, N, N-tri-octyl-ammonium chloride (Aliquat-336), with mineral acid as eluent were evaluated. Retention factors were determined, and separation efficiency was assessed based on the resolution data of the REEs acquired under the same elution conditions for each column. HDEHP demonstrated the best separation efficiency for the entire REE series (mean Rs = 2.76), followed by TBP (mean Rs = 1.52), while Aliquat-336 exhibited the lowest performance (mean Rs = 1.42). The HDEHP-coated column was then used to optimize the extraction chromatographic separation of the REEs. The primary challenge was to completely elute the heavy REEs (Tb – Lu) while maintaining adequate separation of the light REEs (La – Gd) within a reasonably short time. The stepwise gradient elution procedure improved the resolution between adjacent REEs, allowing the complete separation of the entire REE series within 25 minutes. Better separation efficiency for light REEs was achieved at higher column temperatures and a mobile phase flow rate of 1.5 mL/min in the tested domain of 20–60 °C, and 0.5–2.0 mL/min, respectively, resulting in plate heights (H) ranging from 0.011 to 0.027 mm.
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•A resin containing Chromosorb W and Aliquat 336 was prepared and characterized.•Batch uptake studies were carried out using Th-234 and U-233 radiotracers.•Column studies were done to obtain ...breakthrough profile of Th-234 while U was not retained.•Th-234 was separated from bulk U with a decontamination factor as high as 500.•Kinetic modeling and sorption isotherm studies were carried out.
The uptake of Th(IV) from acidic feed solutions was investigated by solid phase extraction using a Chromosorb W based extraction chromatography (XC) material containing Aliquat 336 in the resin pores. Increase in Th(IV) uptake was seen with increasing aqueous acid concentration conforming to an anion exchange mechanism. There was negligible Uranium uptake under identical conditions suggesting possible separation of the metal ions. The Th(IV) uptake data were subjected to kinetic modeling and the sorption isotherm models which clearly conformed to the pseudo-second order kinetics and Langmuir isotherm. Column studies were carried out to obtain breakthrough and elution profiles of Th4+ while UO22+ was not held onto the column. The separation of 234Th from 238U was studied with encouraging results and a separation scheme was proposed.
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Separation of Am from Sm is very important for gamma spectrometric analysis of 242gAm in some specific samples, and also represents a very difficult challenge due to their similar chemical ...properties. Here we report a novel automated separation procedure based on two-stage HDEHP extraction chromatography to achieve the fast and highly efficient separation of Am from Sm. The two-stage HDEHP extraction chromatography was established by using HDEHP resin as the stationary phase, and DTPA-lactic acid and HNO3 as the mobile phases respectively. The automated separation method can be realized through process automation design. As a result, the recovery of Am is above 90%, and the decontamination factor (DF) for Sm reaches 2 × 107. The separation speed is improved and the radiation damage of radionuclides to the analysts is greatly reduced. So, this automated separation procedure developed in this work is certified to be convenient and efficient for the analysis of low activity 242gAm in the complex samples.
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•A novel two-stage HDEHP extraction chromatography was developed to separation Am from Sm.•Automated separation technique was established to rapidly isolate short-lived nuclide in strong radiation sample.•It presents a good separation performance and repeatability with high recovery of Am (above 90%) and high DF for Sm (2 × 107).•This method is applicable for the gamma spectrometric analysis of 242gAm in some specific samples.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
Sound strategies for marine chemical monitoring call for measurement systems capable of producing comparable analytical results with demonstrated quality. This work presents the development and ...validation of a new analytical procedure for the determination of the 241Am mass fraction in marine sediment and seawater samples at low levels. The procedure includes a tandem-column extraction chromatography for separation of 241Am and sector field-inductively coupled plasma mass spectrometry (SF ICP-MS) for its determination. The separation is based on the application of two new extraction resins, TK200 and TK221. The acid leaching method was employed for the pre-treatment of marine sediments, while Fe(OH)3 co-precipitation was used for Am pre-concentration in seawater samples. The extraction behaviors of Am on TK221 resins in the different acidic mediums were investigated. The removal capabilities of the tandem TK200-TK221 columns for the 241Am in the presence of interfering elements including Pu, Pb, Hg, Bi, Tl, Pt, Hf, U, and Th were carefully investigated and the corresponding decontamination factors (DFs) estimated to be in the range from 104 to 106. The main interfering element Pu was efficiently removed with a DF of about 6 × 105. Matrix rare earth elements (REEs) in marine sediments were further removed by the application of TEVA resins. 241Am mass fraction was quantified by the application of external calibration and SF ICP-MS. Following the recommendations of the ISO/IEC 17025 guidelines, the validation of the analytical procedure was accomplished by executing it on the certified reference material (CRM) IAEA-385 (marine sediment) and the seawater IAEA-443 reference materials (RM). The obtained results showed that 241Am mass fractions were accurately determined in both reference samples, with excellent reproducibility (2.1 % and 7.6 %) and low LODs (0.4 fg g−1 and 0.2 fg g−1). The relative expanded uncertainties (k = 2) obtained were 17.1 % and 29.0 %, respectively. The overall analytical times for the application of the proposed procedure on the marine sediment and seawater samples were evaluated to be only about 9 h and 6.5 h, respectively. It shows great advantages for its potential applications for emergency monitoring of 241Am contamination in the marine environment.
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•Determination of 241Am by SF ICP-MS after tandem-column extraction separation.•Decontamination factor as high as ∼6 × 105 for Pu was obtained.•Total analytical times for marine sediment and seawater were shortened to 6–9 h.•Rapid and accurate method for 241Am monitoring for marine environmental studies.
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