TEVA Resin Research Articles

Determination of 93Zr, 237Np and Th radionuclides in radioactive waste and mineral samples: extension of the method for determination of actinides

A novel method has been developed for the simultaneous determination of difficult-to-measure (DTM) nuclides 93Zr, 237Np, 232Th, 230Th and 228Th using a DGA resin® (containing N,N,N′,N′-tetra-n-octyl-diglycolamide) column for simultaneous separation of Zr and actinides followed by purification of Zr, Np and Th on a TEVA resin® (containing Aliquat 336) column. Samples are destroyed by fusion with sodium hydroxide or by acid destruction using HNO3, HCl and HF. Pre-concentration procedure tailored to the extraction chromatography is based on co-precipitation of Zr and actinides and removal of alumina, silica, iron and calcium. The concentrations of 93Zr, 237Np and Th nuclides are determined by ICP-MS and α spectrometry, respectively. High chemical recoveries (≥ 73%) and separation factors were obtained for Zr, Np and Th both in evaporation concentrates of an NPP and various samples of mineral origin such as soil and concrete. The procedure can be easily combined with the simultaneous separation of other actinides (Pu, Am, U) using the same DGA column that has been described in our previous papers (Cassette et al. in Appl Radiat Isot 68:122–130, 2010 and Groska et al. in J Radioanal Nucl Chem 309(3):1145–1158, 2016).

Quantification of [99Tc]TcO4- in urine by means of anion-exchange chromatography–aerosol desolvation nebulization–inductively coupled plasma–mass spectrometry

To sensitively determine 99Tc, a new method for internal quantification of its most common and stable species, [99Tc]TcO4-\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${\ ext{O}}_{4}^{-}$$\\end{document}, was developed. Anion-exchange chromatography (IC) was coupled to inductively coupled plasma–mass spectrometry (ICP-MS) and equipped with an aerosol desolvation system to provide enhanced detection power. Due to a lack of commercial Tc standards, an isotope dilution-like approach using a Ru spike and called isobaric dilution analysis (IBDA) was used for internal quantification of 99Tc. This approach required knowledge of the sensitivities of 99Ru and 99Tc in ICP-MS. The latter was determined using an in-house prepared standard manufactured from decayed medical 99mTc-generator eluates. This standard was cleaned and preconcentrated using extraction chromatography with TEVA resin and quantified via total reflection X-ray fluorescence (TXRF) analysis. IC coupled to ICP-MS enabled to separate, detect and quantify [99Tc]TcO4-\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${\ ext{O}}_{4}^{-}$$\\end{document} as most stable Tc species in complex environments, which was demonstrated in a proof of concept. We quantified this species in untreated and undiluted raw urine collected from a patient, who previously underwent scintigraphy with a 99mTc-tracer, and determined a concentration of 19.6 ± 0.5 ng L−1. The developed method has a high utility to characterize a range of Tc-based radiopharmaceuticals, to determine concentrations, purity, and degradation products in complex samples without the need to assess activity parameters of 99(m)Tc.Graphical

Electrochemical Reduction of Ytterbium in Non-Aqueous Solvents - Towards Production of Pure Medical Lutetium-177

In recent years targeted radionuclide therapy has become a topic of great interest as a growing number of cancers can potentially be treated with radionuclides like lutetium-177 and samarium-153. To facilitate this growth and meet the demand, preparation and purification of lutetium-177 is increasing in importance. In the most common production route, enriched ytterbium-176 targets are irradiated and the produced lutetium-177 is separated from the ytterbium target material. This challenging separation is commonly performed using ion exchange resins, a method limited in scalability as the chemical similarity between ytterbium and lutetium results in poor separation at higher concentrations.An alternative method to aid the separation of lutetium from ytterbium is the electrochemical reduction of ytterbium as a change in oxidation states changes chemical properties significantly. Ytterbium has an accessible divalent state, whereas lutetium has not. However, the very negative value of the Yb(III)/Yb(II) standard reduction potential (E0= -1.04 V vs. SHE) does pose some challenges as it becomes a necessity to work in non-aqueous solvents with a very low water content. Similar research has already been performed in our group, looking into the separation of samarium-153 from europium-154, reducing europium in nitrate media, followed by a separation over TEVA resin. In this study, we investigated the reduction of ytterbium in ethylene glycol, dimethyl sulfoxide, tetrahydrofuran and N,N-dimethyl formamide by cyclic voltammetry, linear sweep voltammetry and electronic impedance spectroscopy. The influence of multiple variables such as moisture content on the reduction kinetics and stability of Yb(II) was determined and a Koutecky-Levich analysis was performed. Our results demonstrate that the reduction of ytterbium in non-aqueous solvents is feasible but attempts to perform bulk electrolysis were not successful yet. Ethylene glycol, dimethyl sulfoxide and N,N-dimethyl formamide demonstrate favorable conditions and in each solvents clear reduction and oxidation peaks were observed. It was found that the solvents do affect the peak separation, reduction potential and sensitivity to passivation. Figure 1

Comparison for the simultaneous determination of 237Np and Pu isotopes between TEVA and TK200 resin

A reliable and stable method was developed to accurately analyze neptunium (237Np) and plutonium isotopes in environmental samples using 242Pu or 236Pu as a tracer. Key parameters, including the valence adjustment conditions and the stabilities of Pu and Np in the different resins, were investigated using TK200 and TEVA resin. It was found that Pu and Np could be efficiently extracted simultaneously using TK200 resin under the optimal loading conditions (6–12 M HNO3) with the addition of 0.01–0.12 M NaNO2 for valence adjustment. These isotopes were subsequently stripped out using a solution containing 0.1 M HCl, 0.05 M HF, and 0.01 M NH2OH·HCl. The separation efficiencies of Pu and Np were >93%, and the chemical yield ratio between Np and Pu was maintained steady at an average of 1.00 ± 0.03 (n > 50) under the optimal conditions. The analytical method was validated by analyzing environmental soil samples spiked with known amounts of 239Pu and 237Np standard solutions or certified reference materials. The measured values of 237Np, 239Pu, and 240Pu obtained by inductively coupled plasma tandem mass spectrometry were consistent with their International Atomic Energy Agency literature values within a 95% confidence interval. These results confirm the reliability and high analytical precision (<6%) of this developed method using Pu as a non-isotopic tracer for monitoring the chemical yield of 237Np. The developed method can also be used for environmental pollutant monitoring and for tracer studies of the 237Np and Pu isotopes.

DTPA(DOTA)-Nimotuzumab Radiolabeling with Generator-produced Thorium for Radioimmunotherapy of EGFR-overexpressing Carcinomas.

The feasibility of preparing the "in-house" generators and the Th- DTPA(DOTA)-Nimotuzumab radioimmunoconjugate was evaluated. 226Th is perspective for TAT, however, due to short half-life it is preferable to apply this radionuclide for readily available epithelial malignancies. Nimotuzumab being specific for EGFR expressing cells as a targeting moiety is considered to be suitable for thorium delivery. TEVA extraction chromatographic resin and anion exchange resin AG 1x8 were used as sorbents for 226Th generator. In order to determine features of labeling by Th4+ we applied 234Th as a longer-lived analog of short-lived 226Th and the immunoconjugates DTPA(DOTA)-Nimotuzumab were used for radiolabeling. The generator on the base of TEVA resin has shown higher volume activity of the product compared to the AG 1x8. The 226Th volume concentration was up to 80%/mL. The radiolabeling of BFCA by thorium radioisotopes reached 95% at the MR(Th:p-SCN-Bn-DTPA) = 1:100 and 86% for MR(Th:p-SCN-Bn-DOTA) = 1:5000 at 90°C. The procedure of Nimotuzumab labeling with Th4+ for radiotherapy of EGFR-overexpressing carcinomas was established. The overall labeling yield in both radioimmunoconjugates - DTPA and DOTA functionalized - was in the range of 45-50%. The immunoconjugate Nimotuzumab-p-SCN-Bn-DTPA was obtained with a molar ratio 1:25 (Nimotuzumab: BFCA), within 1 hour of conjugation at 25°C and labelled via postconjugation approach. Whereas Nimotuzumab-p-SCN-Bn-DOTA was obtained at the same conditions, but radiolabeled by the method of pre-conjugation. Thorium-234 incorporation into both radioimmunoconjugates reached 45-50%. It has been shown that Th-DTPA-Nimotuzumab radioimmunoconjugate specifically bound with EGFR overexpressing epidermoid carcinoma A431 cells.

A Novel Alkali Precipitation Method for Tungsten Separation and High‐Precision Isotopic Measurement in Geological Samples

Tungsten (W) isotopes are useful tools in geological and cosmochemical research, but the chemical separation of W is cumbersome for high‐precision measurement. Here, a novel alkali (sodium hydroxide, NaOH) precipitation method for separation and purification of W in geological samples is described, which simplifies the chemical procedure. The amphoteric character of W is exploited to separate it from most matrix elements in alkaline conditions. Subsequently, TEVA resin was applied to further purify W for measurements using a multi‐collector inductively coupled plasma‐mass spectrometer. Importantly, the introduction of a certain amount of Na in the W analyte can increase the signal intensity by approximately 1.6 times, which may be caused by Coulomb fission. Such Na‐triggered signal enhancement reduces the test portion mass required for analysis. Our results show that the Alfa Aesar W standard solution and geological reference materials JB‐3, BCR‐2 and BHVO‐2 yield 182W/184W ratios consistent with previously reported values within uncertainty. Repeated measurement of the Alfa Aesar W standard solution shows that the intermediate precision of 182W/184W was better than 5 ppm (2s), which is sufficient to identify subtle 182W isotope variations in terrestrial and extra‐terrestrial samples. Above all, the alkali precipitation method in this study optimises the experimental process and mass spectrometric analysis.

Behavior of selenium and arsenic in HCl and HNO3 on TRU, TEVA, DGA, and Pb extraction chromatography resins

Behavior of selenium and arsenic in HCl and HNO3 on TRU, TEVA, DGA, and Pb extraction chromatography resins

Rapid Elution of 226Th from a Two-Column 230U/226Th Generator with Diluted and Buffer Solutions.

A radionuclide generator of the short-lived alpha emitter 226Th was proposed. An original scheme consisting of two in-series chromatographic columns was developed for rapidly producing a neutral citric-buffered eluate of high purity 226Th. The first column filled with TEVA resin retained the parent 230U, while 226Th was eluted with 7 M HCl solution to be immediately adsorbed on the second column containing DGA resin or UTEVA resin. Having substituted the strongly acidic medium of second column with neutral salt solution, 226Th was desorbed with diluted citric buffer solution. One cycle of generator milking took 5-7 min and produced >90% of 226Th in 1.5 mL of eluate (pH 4.5-5.0) appropriate for direct use in radiopharmaceutical synthesis. The 230U impurity in 226Th eluate was less than 0.01%. The proposed two-column 230U/226Th generator was tested over 2 months including a second loading of 230U additionally accumulated from 230Pa.

Status report on AMS measurements of plutonium isotopes using the 1MV Tandetron Accelerator at IFIN-HH

Accelerator Mass Spectrometry is the most sensitive measurement method that allows us to determine 239, 240, and 244Pu radioisotopes in environmental samples with extremely low isotopic concentrations. By measuring plutonium isotopes, we focus our research activity on two main directions, monitoring of environmental nuclear pollution and nuclear astrophysics.This report gives an overview of the progress that was made in the determination of plutonium isotopes at IFIN-HH, and it starts with the studies performed for the transport and measurement of actinides using the 1MV Tandetron Accelerator. The 238U and 232Th isotopes were used as pilot beams for the determination of ion transport parameters, after which the isotopic ratios 239Pu/242Pu, 240Pu/242Pu, and 244Pu/242Pu were measured using the new Plutonium Standard ColPuS. The results obtained for the isotopic ratios agree with the consensus values of the standard. In addition, we developed radiochemical procedures for thorium, plutonium, and uranium separation, the chemical recoveries of uranium and thorium using UTEVA and TEVA resins are presented, where we used an Agilent ICP-MS system (Inductively Coupled Plasma Mass Spectrometry). The radiochemical separation is important mainly for obtaining target materials that can provide microscopic pilot beams as U and/or Th. Finally, a short overview is provided of the molecular interference challenges that are encountered when measuring plutonium isotopes.

Extraction of gold, mercury, and lead with TEVA resin from HCl and HNO3

Extraction of gold, mercury, and lead with TEVA resin from HCl and HNO3

Rapid americium separations from complex matrices using commercially available extraction chromatography resins

A method for rapid separation of americium from complex matrices by use of two commercially available extraction chromatography resins is reported. TRU resin is capable of purifying americium/lanthanides together from Group 1, Group 2 and transition metals. TRU resin tolerated high loadings of iron, aluminium, calcium sodium and potassium. TEVA resin purified americium/lanthanides by elution with ammonium thiocyanate. Decontamination factors > 20,000 were achieved within one working day. The affinity of TEVA resin for americium, curium and lanthanides as a function of ammonium thiocyanate concentration is reported. The possibility of americium/lanthanide separations on LN resin has been explored.

Ultrasensitive detection of 244Pu in environmental samples by accelerator mass spectrometry

Plutonium radiochemical separation using TEVA resin and chemical recoveries determined by alpha spectrometry. Zero background measurement of 244Pu by AMS from environmental sediments from Bikini Atoll island and the Pacific Ocean.

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.

Determination of ultra-trace levels of uranium and thorium in electrolytic copper using radiochemical neutron activation analysis

Uranium and thorium as natural radioactive elements are present everywhere in the environment. Their trace levels are also present in various materials, such as copper, used as a shielding material in gamma-ray spectrometry, usually located very close to the detector. Ultra-low levels of uranium and thorium in electrolytic copper were determined in this study using radiochemical neutron activation analysis (RNAA) via their induced nuclides U-239/Np-239 and Pa-233, respectively. After irradiation of copper together with uranium and thorium standards, various techniques were used for their separation from the matrix. To isolate of short-lived U-239, solvent extraction in a combination of tributyl phosphate (TBP) in toluene was used. To separate Np-239 and Pa-233, extraction chromatography using TEVA and TK-400 resins was applied. Special attention was paid to the estimation of radiochemical recovery, which was determined in each sample aliquot using U-235, Np-238 and Pa-231 tracers. For quantification of induced nuclides and tracers used in the experiment, gamma-ray spectrometry was used. Obtained results showed that electrolytic copper samples contained impurities of uranium and thorium in ultra-trace levels: up to 45 pg/g (550 nBq/g) for uranium and up to 80 pg/g (330 nBq/g) for thorium. The electrolytic copper also contained impurities of Ag, As, Au, Sb, Se and Zn as observed using the k0-INAA technique.

Rapid method for sequential determination of Pu and Am in soil and sediment samples by sector-field inductively coupled plasma mass spectrometry

New method was developed to analyze Pu and Am sequentially for soil and sediment by inductively coupled plasma mass spectrometry (ICPMS). The developed method uses conc. HNO3 to leach Pu and Am, Fe(OH)3 coprecipitation to remove alkali and alkaline metals, extraction chromatographic separation using UTEVA, DGA and TEVA resins to remove interfering elements (IEs) and separate Pu and Am from each other, and sector field-ICPMS to measure Pu and Am. The analysis of four standard reference materials showed that both Pu isotopes and 241Am were accurately determined by this method, as a result of its excellent decontamination ability of IEs. Especially the high decontamination factor of Pu [DF(Pu), 4.2 × 102] in Am fraction and high DF(Am) (7.0 × 103) in Pu fraction sufficiently eliminated the cross interference between 241Pu and 241Am in ICPMS measurement. In addition, stable and high chemical recoveries were achieved for Pu (71–91%) and Am (70–88%). The low LODs of Pu isotopes, short analytical time (14 h) and high DFs of IEs allows this method to sequentially analyze Pu and Am, for both global fallout and nuclear accident sourced samples.

Construction of a thorium/actinium generator at the Canadian Nuclear Laboratories

Targeted Alpha Therapy (TAT) has demonstrated considerable promise in the treatment of a range of cancers in both preclinical and, more recently clinical research. In particular, work with the alpha-emitting radionuclide 225Ac has been effectively employed due to the relatively rapid decay cascade that leads to 4 alpha and 2 beta emissions. One limitation for TAT has been caused by access to the vital radionuclide. Traditionally, 225Ac has been sourced from thorium/actinium generators based on the alpha decay of stockpiles of 229Th. 229Th is itself the alpha-decay product from 233U. Due to proliferation issues associated with 233U, only three thorium/actinium generators have been reported in the literature, capable of supporting clinical research. This paper describes the construction and operation of a thorium/actinium radionuclide generator at the Canadian Nuclear Laboratories, capable of supporting preclinical and limited clinical research in the area of TAT. Thorium was recovered and purified by a combination of anion exchange and extraction chromatography from aged 233U stockpiles. A separation scheme for 225Ra and 225Ac has been developed, based upon the chemical composition of the thorium material to allow for regular, routine milkings capable of supplying up to 3.7 GBq (100 mCi) of radiochemically pure 225Ac annually. This routine separation is accomplished using a combination of anion exchange chromatography to separate Ac and Ra isotopes from Th and extraction chromatography employing TEVA and DGA-N resins to separate actinium from radium and breakthrough thorium.

Determination of Ultra-Low Level Plutonium Isotopes in Large Volume Environmental Water Samples

Plutonium is an important artificial element, 239 Pu and 240 Pu are two major radioisotopes of plutonium in the environment released by human nuclear activities. Due to their high radiotoxicity and bio-toxicity, the determination of these radionuclides is critical in view of radiation protection and environmental radioactivity. It is still a major challenge to accurately determine these radionuclides in environmental water samples due to their extremely low concentrations. In this work, a sensitive analytical method for determination of 239 Pu and 240 Pu in environmental water samples was reported. By co-precipitation of plutonium with Ti(OH) 3 followed by separation of plutonium using extraction chromatography with TEVA resin, a recovery of more than 80% for plutonium and decontamination factor of 1.3 × 10 5 for uranium were achieved. A triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS) with dynamic collision/reaction cell was used for measurement of plutonium isotopes. By using NH 3 -He double gasses as collision/reaction gas, 238 U 1 H + polyatomic ion interference to measurement of 239 Pu was significantly suppressed and the final abundance sensitivity of 238 U to m/z 239 was reduced to < 1 × 10 –11 , and sensitivity of 239 Pu was improved to 990 cps/(pg/g). For 20 L water sample, the detection limits of the method for 239 Pu and 240 Pu reached 1.28 × 10 –7 Bq/L and 1.38 × 10 –7 Bq/L, respectively, which enabled accurate determination of 239 Pu and 240 Pu in normal environmental water samples. The developed method was successfully applied to determine 239 Pu and 240 Pu in the spiked water and real environmental water samples, and the results indicated that this method was reliable and could be practically applied. A sensitive method for determination of ultra-low level 239 Pu and 240 Pu was established by pre-concentration of plutonium from large volume water using Ti(OH) 3 co-precipitation, purification for plutonium using extraction chromatography with TEVA resin and triple quadrupole ICP-MS measurement of plutonium isotope. NH 3 -He was used as reaction gas for elimination of uranium hydride interference and increasing the measurement sensitivity using collision focusing. The method was successfully applied for analysis of environmental water samples from China.

Fundamental distribution coefficient data and separations using eichrom extraction chromatographic resins

Distribution coefficient (Kd) data provides the analyst with a powerful set of tools for designing elemental chemical separations. While considerable Kd data exists in the literature for traditional anion and cation exchange resins, a comprehensive Kd study for the majority of the periodic table has not been published to date for several newer Eichrom extraction chromatographic resins. Kd values for the sorption of 41 different of elements on TEVA, TRU, UTEVA, and Diphonix resin were determined in this work. The power of Kd data in designing chemical separations is then demonstrated through development of separation methods for several challenging chemical separations including U/Mo/Te, Zr/Nb/Mo, and Cd isolation. Separation methodologies are finally applied to soil samples, where the ability for each separation to perform under complex matrix conditions is evaluated.

Production of 230Pa from Proton-irradiated Thorium and Developing 230Pa/230U/226Th Tandem Generator

Targeted alpha-therapy of various oncology diseases is based on the coupling of alpha-emitting radionuclides to tumour-selective carrier molecules. 230U (t1/2 = 20.8 d) is accumulated via decay of 230Pa and has strong potential for alpha-therapy due to 5 emitting alpha particles with total energy 33.5 MeV. It can be used directly or as a parent of 226Th in a generator system. A prospective way for production of 230Pa/ 230U is irradiation of natural thorium with medium-energy protons. Curie amounts of 230Pa can be generated in one irradiation run together with other useful alpha-emitters 225Ac and 223Ra. After dissolving Th-target in 6M nitric acid with the addition of catalytic amounts of hydrofluoric acid Pa was isolated by liquid extraction with octanol. The water phase may be further used for isolation of 225Ac and 223Ra according the method, proposed in [1, 2]. Namely, the most part of thorium was removed by liquid extraction with di(2-ethylhexyl)phosphoric acid in toluene. Organic phase was kept for accumulation 223Ra from parent 227Th. 225Ac and 223Ra were concentrated from aqueous phase and then separated and purified by extraction chromatography. After re-extraction 230Pa was purified on silica gel using different oxalic acid solutions. Up to 85% of 230Pa with radionuclidic purity >99% was recovered and stored for 230U accumulation. Basing on distribution coefficients 230U was separated from 230Pa in diluted nitric acid solution on DGA resin. Obtained 230U may be used for development of 230U/226Th – generator. Distribution coefficients for U and Th were obtained for a wide range of extraction chromatographic resins. TEVA (mixture of trioctyl and tridecyl methyl ammonium chloride as an extractant) and WBEC (based on a mixture of tertiary octyl and decylamines) resins are most suitable for this purpose. [1]R.A. Aliev, S.V. Ermolaev, A.N. Vasiliev, V.S. Ostapenko, E.V. Lapshina, B.L. Zhuikov, N.V. Zakharov, V.V. Pozdeev, V.M. Kokhanyuk, B.F. Myasoedov, S.N. Kalmykov. Isolation of medicine-applicable actinium-225 from thorium targets irradiated by medium-energy protons. Solvent Extraction and Ion Exchange, 2014, v. 32, p. 468-477.[2]A.N. Vasiliev, V.S. Ostapenko , E.V. Lapshina, S.V. Ermolaev, S.S. Danilov, B.L. Zhuikov and S. N. Kalmykov. Recovery of Ra-223 from natural thorium irradiated by protons. Radiochimica Acta, 2016, v. 104, N.8, p. 539-547.

Flow-through magnetic-stirring assisted system for uranium(VI) extraction: First 3D printed device application

A 3D printed solid-phase extraction (SPE) device for uranium(VI) extraction has been fabricated using stereolithographic 3D printing. The 3D printed device is shaped as a stirred reactor chamber containing a network of small cubes, which were impregnated with TEVA resin for the extraction of U(VI) from water matrices without doing any previous pretreatment. A flow-through system was combined with off-line ICP-MS detection for the accurate and rapid determination of U(VI) at trace levels. The automatic system was satisfactorily optimized using experimental design, obtaining 0.03 and 0.09 ng U(VI) of detection and quantification limits, respectively, and a durability of 11 consecutive extractions. The reliability of the proposed system was confirmed through the analysis of a reference water material (CSN/CIEMAT 2011), and to water samples (tap, mineral and groundwater) by addition/recovery assays obtaining recoveries between 95 and 106%. This study present for the first time the design of a 3D printing SPE device impregnated with TEVA resin for the on-line extraction of U(VI), showing that 3D printing is a powerful tool for simplifying the construction of complex experimental devices and its operation in analytical procedures for pretreatment applications in water matrices.