Liquid-liquid extraction methods for the production of carrier-free 115cd and 89,90sr from fission products

The extraction of fission product elements with 1-phenyl-3-methyl-4-caprylpyrazolone-5 at various pH values has been investigated. The quantitative extraction of cadmium at pH 5.4 and that of strontium at pH 9.0 is utilised in devising procedures for the recovery of ¹¹⁵Cd and ^89,90Sr from the fission products. Good decontamination factors and more than 90% ¹¹⁵Cd and 80% ^89,90Sr activities were recovered.     

Radiochemical determination of 90Sr and 86Sr in soil

Summary A modified HCl-leach method for the radiochemical ⁹⁰Sr and ⁸⁹Sr determination in soil has been developed. The sample is leached by HCl in the presence of the Sr-carrier. Then bi- and trivalent ions are separated by a combination of complexation and ion exchange. The separation of strontium and calcium is performed by fuming nitric acid. After further purification, strontium carbonate is precipitated and the activity of ⁹⁰Sr and ⁸⁹Sr is measured. ⁹⁰Sr determined by the isolation of ⁹⁰Y and by measuring its activity. The ⁹⁰Sr and ⁸⁹Sr content in soil is calculated from the measured activities of yttrium oxide and strontium carbonate by considering the counting efficiencies for ⁹⁰Y, ⁹⁰Sr and ⁸⁹Sr beta rays, the chemical yields of strontium and yttrium and the time of ⁹⁰Y growth from ⁹⁰Sr.

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Radiochemische Bestimmung von ⁹⁰Sr und ⁸⁹Sr in Boden

Zusammenfassung Eine modifizierte Auslaugungsmethode für die radiochemische Bestimmung von ⁹⁰Sr und ⁸⁹Sr im Boden wurde entwickelt. Die Probe wird in HCl in Gegenwart des Sr-Trägers ausgelaugt und die zwei- und dreiwertigen Ionen dann durch eine Kombination von Komplexierung und Ionenaustausch getrennt. Die Strontiumtrennung von Calcium erfolgt mit rauchender Salpetersäure. Nach weiterer Reinigung wird SrCO₃ gefällt und die Aktivität von ⁹⁰Sr und ⁸⁹Sr bestimmt. ⁹⁰Sr wird durch Isolierung und Zählung von ⁹⁰Y ermittelt. Der ⁹⁰Sr- und ⁸⁹-Sr-Gehalt im Boden wird aus der Aktivität von Y₂O₃ und SrCO₃ unter Berücksichtigung der Zählausbeute für ⁹⁰Y-, ⁹⁰Sr- und ⁸⁹-Sr-beta-Strahlen, aus der gravimetrischen Bestimmung von Strontium und Yttrium und aus der Zeit der ⁹⁰Y-Entstehung aus ⁹⁰Sr bestimmt.

     

Methodology for determination of 89Sr and 90Sr in radiological emergency: I. Scenario dependent evaluation of potentially interfering radionuclides

Early determination of ⁸⁹Sr and ⁹⁰Sr in radiological emergency is hampered by the presence of interfering short-lived fission products. In this study, three commonly used radioanalytical strategies for ⁸⁹Sr and ⁹⁰Sr were evaluated theoretically considering their suitability in a nuclear explosion scenario. The methods were evaluated with respect to the need for decay time of interfering short-lived strontium and yttrium isotopes, and reduction of other known interfering nuclides prior to measurement. The strategy shown to be most successful included initial separation of strontium and determination of ⁸⁹Sr, followed by an yttrium separation and counting of ⁹⁰Y. ⁸⁹Sr and ⁹⁰Sr could be determined about 5 and 9 days after a nuclear explosion, respectively.     

The solvent extraction of carrier-free90Y from90Sr with crown ethers

A simple solvent extraction method has been developed for the separation of⁹⁰Y from⁹⁰Sr. Crown ether dissolved in chloroform was used as a selective reagent and organic picrate anion was chosen as a counter ion. The effect of various factors on the extraction separation of strontium and yttrium in the system have been studied. The extraction equilibrium constant of strontium logK _ex=9.15 was obtained from the study of the distribution coefficient versus the crown ether concentration. The separation method was simple, resulted high purity (>99.9%) and quantitative yield, and took less than half an hour.     

The use of liquid scintillation spectrometry for the determination of radionuclidic purity of 90Y from a radiochemical 90Y/90Srgenerator

Summary An extraction technique for the separation of ⁹⁰Sr from a high excess of⁹⁰Y has been developed. This procedure can be used for the determination of trace amounts of⁹⁰Sr in⁹⁰Y prepared by a radiochemical⁹⁰Y/⁹⁰Sr generator by liquid scintillation.     

Preparation of 90Y by the 90Sr-90Y Generator for Medical Purpose

The production of ⁹⁰Y by ⁹⁰Sr-⁹⁰Y generator was studied. ⁹⁰Sr was adsorbed on a column with Aminex A-5 resin. The daughter radionuclide ⁹⁰Y was eluted with 0.7M -hydroxyisobutyrate (-HIB, pH 5.4). Radionuclidic, radiochemical and chemical purities were >98% and yield >85%. After converting into chloride form ⁹⁰YCl₃-solution (pH:1) was used for preparing injectable yttrium citrate and labeling some other radiopharmaceuticals. Furthermore, a fast ITLC-method for the determination of ⁹⁰Sr in ⁹⁰Y-eluate was developed.     

Separation of 90Y from 90Sr using sequential multiple column extraction chromatography

The distribution coefficient measurements on Y(III) and Sr(II) were performed using ditertiarybutyl dicyclohexano 18-crown-6 (Sr-selective resin) and N,N,N′,N′-tetraoctyldiglycolamide (Y-selective resin) in HNO₃, HCl and HClO₄ media. Separation factors (⁹⁰Y/⁹⁰Sr) based on distribution coefficient data suggested that perchloric acid is distinctly better medium as compared to nitric acid/hydrochloric acid. The mechanism of extraction changes with the nature and concentration of acid and is responsible for the high selectivity in perchloric acid medium. Sequential column studies were carried out on tracers (radioactive/stable) employing Sr-selective/Y-selective extraction chromatographic resins as stationary phases. The final elution of ⁹⁰Y was done in 0.01 M EDTA at pH 4.0 which can be used for clinical applications after radiochemical processing.     

Trennung des Strontiums von Yttrium (90Sr/90Y) mit Anionenaustauscher-Sulfaten

Zusammenfassung Die selektive Fällungssorption von Strontium an Dowex-I-Sulfat im Säulenverfahren als SrSO₄ aus 50%ig methanolischer Lösung erlaubt die rasche Gewinnung von fremdstrahlungsfreiem Yttrium-90 aus dem Zerfallsprozeß . Die Kontrolle des Trenneffektes erfolgt durch Bestimmung der Halbwertszeit des ⁹⁰Y. Je nach Länge der Austauscherschicht kann unter Beachtung der Bildungsschnelligkeit von ⁹⁰Y dieses mehrfach entnommen werden.

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Summary Selective precipitating Sorption of strontium as SrSO₄ on Dowex-I-sulphate in a column operation, using aqueous methanol solution (11), permits the isolation of pure ⁹⁰Y, produced by the decay process . The effect of separation may be controlled by determination of the half-life of ⁹⁰Y. Taking into account the velocity of formation ⁹⁰Y can be obtained several times according to the length of the ion-exchanger column.

     

The simple radiochemical determination of 90Sr in environmental solid samples by solvent extraction

Determination of ⁹⁰Sr in environmental solid samples is a challenging task because of the presence of so many other radionuclides in samples of interest. This problem was dealt with by radiochemical separation of strontium followed by yttrium separation and Cerenkov counting of the high-energy ??-particle emissions of ⁹⁰Y in order to quantitate ⁹⁰Sr. In this work, an improved method is described for the determination of ⁹⁰Sr in soil samples, through the separation of the daughter ⁹⁰Y at equilibrium. The procedure is based on the HDEHP solvent extraction in combination with liquid scintillation spectrometry (LSS). A low background Quantulus has been optimized for low level counting of Cerenkov radiation emitted by the hard ??-emitter ⁹⁰Y. The analytical quality of the method has been checked by analyzing IAEA Soil-375 reference materials. The analytical method has also been successfully applied to the determination of ⁹⁰Sr for moss-soil samples in inter-laboratory exercises through IAEA??s ALMERA network. The chemical recovery for ⁹⁰Y extraction ranged from 80 to 85% and the counting efficiency was 73% in the window 25?C400 keV.     

Validation of an extraction paper chromatography (EPC) technique for estimation of trace levels of 90Sr in 90Y solutions obtained from 90Sr/90Y generator systems

While the extraction paper chromatography (EPC) technique constitutes a novel paradigm for the determination of few Becquerels of ⁹⁰Sr in MBq quantities of ⁹⁰Y obtained from ⁹⁰Sr/⁹⁰Y generator, validation of the technique is essential to ensure its usefulness as a real time analytical tool. With a view to explore the relevance and applicability of EPC technique as a real time quality control (QC) technique for the routine estimation of ⁹⁰Sr content in generator produced ⁹⁰Y, a systematic validation study was carried out diligently not only to establish its worthiness but also to broaden its horizon. The ability of the EPC technique to separate trace amounts of Sr²⁺ in the presence of large amounts of Y³⁺ was verified. The specificity of the technique for Y³⁺ was demonstrated with ⁹⁰Y obtained by neutron irradiation. The method was validated under real experimental conditions and compared with a QC method described in US Pharmacopeia for detection of ⁹⁰Sr levels in ⁹⁰Y radiopharmaceuticals.     

Separation of microamounts of yttrium from strontium by using nitrobenzene solution of sodium dicarbollylcobaltate in the presence of 18-crown-6

A rapid extraction separation of trace amounts of yttrium from strontium with a nitrobenzene solution of sodium dicarbollylcobaltate (NaDCC) and 18-crown-6 in the presence of tetrasodium salt of ethylenediamine-N,N,N",N"- tetraacetic acid (Na₄L) in the aqueous phase was developed. The separation factor a(Sr/Y) was substantially higher than 10⁶. This water-nitrobenzene extraction system can be applied for efficient separation of carrier-free ⁹⁰Y from ⁹⁰Sr/⁹⁰Y generator.     

Studies on soil samples mineralization conditions preceding the determination of 90Sr

Some results of the extraction of strontium and yttrium from soil samples by concentrated nitric acid are described. The concentration of Sr and Y in the solid was determined by XRF method. The results obtained allowed to elaborate the conditions of acid leaching and to propose an analytical procedure for the determination of ⁹⁰Sr in samples without their total dissolution.     

Bestimmung des Gehaltes an90Sr und89Sr in Proben tierischer und pflanzlicher Herkunft

A method is described for the determination of⁸⁹Sr and⁹⁰Sr in samples of plant and animal origin. The Rehak-Feddersen method was modified to measure⁹⁰Sr. Modification was made in the sample preparation and in the toluene-HDEHP [di(2-ethylhexyl)phosphoric acid] extraction. After the extraction of yttrium, strontium is separated with nitric acid and—calculating with a correction factor—⁸⁹Sr can directly be determined. Namely,⁸⁹Sr can be measured in an aqueous solution by a liquid scintillation technique with an efficiency of 30% while⁹⁰Sr with 1.4% only. Quenching of the solution—depending on the composition—which may influence the measurement of⁹⁰Y and⁸⁹Sr was also examined. Detection limits and reproducibilities are given. Finally, evaluation of the experimental data is reported.      

Extraction chromatographic separation of carrier-free90Y from90Sr/90Y generator by crown ether coated silica gels

A remarkable extraction chromatographic method for the preparation of⁹⁰Y of high radiochemical purity has been developed. The generator consists of silica gel coated crown ether. It functions as a strong adsorber for⁹⁰Sr and in the meantime high purity of⁹⁰Y is eluted with a dilute solution of picric acid after a suitable period. The experiments indicated that DC18C6 coated silica gel is better than that of DB18C6 coated. The extraction capacity of strontium on 3.8% DC18C6 coated silica gel is 5.6 mg Sr/g silica gel. Yttrium is obtained with more than 95% milking yield with radionuclide purity greater than 99.9%. The extraction chromatographic generator does not change its characteristics even after 5 elutions.     

An electrochemical pathway to prepare circular planar 90Sr/90Y sources for the calibration of surface contamination monitors

In this communication, we describe a novel method to prepare circular planar ⁹⁰Sr/⁹⁰Y sources (? = 16 mm) exploiting the intrinsic properties of the anodized titanium to electro-deposit predicted quantity of ⁹⁰Sr activity from an aqueous solution. The influences of various experimental parameters such as pH of the electrolyte, applied current density, electrodeposition time and carrier strontium concentration were thoroughly investigated to arrive at a condition resulting optimal deposition of the ⁹⁰Sr/⁹⁰Y activity on the substrate. An optimized electrochemical procedure to prepare ~3.7 MBq (~0.1 mCi) of circular planar ⁹⁰Sr/⁹⁰Y sources commensurate with regulatory safety requirement has been the positive outcome.     

Separation of microamounts of yttrium from strontium by using sodium dicarbollylcobaltate, Slovafol 909 and ethylenediamine - N, N, N', N'-tetraacetic acid in the water - nitrobenzene extraction system

Summary A rapid extraction separation of trace amounts of yttrium from strontium by a nitrobenzene solution of sodium dicarbollylcobaltate (NaDCC) in the presence of p-nonylphenylnonaethylene glycol (Slovafol 909) and tetrasodium salt of ethylenediamine - N,N,N',N' - tetraacetic acid (Na₄L) in the aqueous phase was developed. The separation factor a(Sr/Y) was substantially higher than 10⁵. This water-nitrobenzene extraction system can be applied for the efficient separation of carrier-free ⁹⁰Y from ⁹⁰Y/⁹⁰Sr generator.     

Rapid determination of 90Sr/90Y in water samples by liquid scintillation and Cherenkov counting

Strontium-90 (⁹⁰Sr) is a ubiquitous contaminant at nuclear facilities, found at high concentrations in spent nuclear fuel and radioactive waste. Due to its long half-life and ability to be transported in groundwater, an accurate method for measuring ⁹⁰Sr in water samples is critical to the monitoring program of any nuclear facility. To address this need, a rapid procedure for sequential separation of Sr/Y was developed and tested in groundwater samples collected from an area of riverbed affected by a ⁹⁰Sr groundwater plume. Sixteen samples, plus spike and water blanks, were analyzed. Five different measurements were performed to determine the ⁹⁰Sr and yttrium-90 (⁹⁰Y) activities in the samples: direct triple-to-double-coincidence ratio (TDCR) Cherenkov counting of ⁹⁰Y, liquid scintillation (LS) counting for ⁹⁰Sr following radiochemical separation, LS counting for ⁹⁰Y following radiochemical separation, Cherenkov counting for ⁹⁰Y following radiochemical separation and LS counting of the Sr samples for ⁹⁰Y in-growth. The counting was done using a low-level Hidex 300SL TDCR counter. Each measurement method was compared for accuracy, sensitivity and efficiency. The results following Cherenkov counting and radiochemical separation were in very good agreement with one another.     

A rapid method for the determination of strontium-90 in powdered milk

A method in which⁹⁰Y the daughter product of⁹⁰Sr decay is extracted by tributyl phosphate (TBP) from ashed powdered milk is described. The⁹⁰Y which is in equilibrium with⁹⁰Sr is back-extracted into the aqueous phase and coprecipitated with milligram amounts of ferric hydroxide. The proposed procedure makes it possible to obtain thin planar sources convenient for low level gas counters. The overall detection efficiency of 45.5% for⁹⁰Y (including chemical recovery of yttrium) was achieved. The detection limit for 200 g powdered milk samples and 10 000 s counting time was 0.065 Bq·kg^–1. The concentration of⁹⁰Sr in three-year old samples (after Chernobyl accident) ranged from 0.81 to 1.31 Bq·kg^–1.     

Strontium-90 determination in biological and environmental samples by direct milking of its daughter product, yttrium-90

A method is presented for the determination of ⁹⁰Sr in environmental samples by direct milking of ⁹⁰Y. Pyridine-2,6-dicarboxylic acid forms an anionic complex with yttrium which is retained on an anionic resin. Most of the matrix elements are washed out of the column as neutral or uncomplexed species and yttrium is eluted by increasing the ionic force of the eluent solution. This method gives yttrium recoveries between 65% to 85% for soil, grass, milk and bone samples with very high radiochemical purity (⁹⁰Y average half-life of 66±4 hours) and a detection limit of 0.3 Bq/kg of soil. The method supports a calcium content up to 3 g per sample without any decrease in yttrium yield, allowing the measurement of milk, milk-teeth and bone samples with no concentration step in one day.     

Development of rapid solvent extraction based radioanalytical technique for estimation of 90Sr in the presence of natural and anthropogenic radionuclides

A radiochemical technique for estimation of ⁹⁰Sr concentration by direct extraction of ⁹⁰Y with bis (2-ethylhexyl) phosphate (HDEHP) in toluene was developed and standardized. About 90% ⁹⁰Sr retained in the aqueous phase at the optimized pH 4–4.5. Cerenkov counting with 0.04 g mL⁻¹ sodium salicylate as a wavelength shifter resulted in 7.5 fold increase its Cerenkov counting efficiency. The method was validated by estimating ⁹⁰Sr in certified reference materials like, IAEA TEL 2016-03 drinking water, Spruce needle and IAEA-156 Clover. The interference of naturally occurring Ra and its β progeny especially Pb was eliminated by means of Cerenkov counting. Conventional radiochemical separation was used to compare ⁹⁰Sr activity in effluent samples.