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1.
A radiochemical procedure is described for the sensitive determination of89Sr and90Sr activity concentrations in soil and sediment samples. After leaching the sample with hydrochloric acid, Sr is separated from most of the soluble matrix constituents and Ca by solvent extraction using dicylclohexano-18-crown-6 in trichloromethane. After backextraction with a EDTA-solution (ethylene diamine tetra acetate), Sr is purified by several precipitation steps from traces of matrix constituents and radionuclides which might interfere the beta measurements of89Sr,90Sr and90Y. The detection limits are about 0.2 Bq/kg and 0.4 Bq/kg for90Sr and89Sr respectively. The procedure can be applied to all kind of environmental samples with small modifications of the sample preparation steps prior to analysis.  相似文献   

2.
A method is described for the determination of 90Sr in environmental samples using combination of developed in-house method, Eichrom Sr resin and Beta Counter. Strontium was efficiently, rapidly and simply separated from Ca and other interfering matrix components by Eichrom Sr resin. All the results in general showed good accuracy, high precision, reliable and in good agreement between these two measured and certified value of SRM (i.e. IAEA-375, IAEA-326, IAEA-152 and IAEA-414). As a whole, the procedure described in this work notably improves conventional methods in particular concerning the time needed, sample volume, safer and others. Thus, the introduced method was successfully performed and will be applied to actual sample for the determination of 90Sr in different environmental materials such as soil, sediments, milk, biological sample, water etc.  相似文献   

3.
This paper describes the procedures of isolating strontium and yttrium from seawater that enable the determination of 89,90Sr. In one procedure, strontium is directly isolated from seawater on the column filled with Sr resin by binding of strontium to the resin from 3 M HNO3 in a seawater, and successive elution with HNO3. In others, strontium is precipitated from seawater with (NH4)2CO3, followed by isolation on a Sr column or an anion exchange column. It is shown that strontium precipitation is optimal with concentration of 0.3 M (NH4)2CO3 at pH = 11. In these conditions, 100% Y, 78% Sr, 80% Ca and 50% Mg are precipitated. Strontium is bound on to Sr column from 5 to 8 M HNO3, separated from other elements by elution with 3 M HNO3 and 0.05 M HNO3. Strontium and yttrium are bound on to anion exchange column from alcoholic solutions of nitric acid. The optimum mixture of alcohols for sample binding is a mixture of ethanol and methanol with the volume ratio 1:3. Strontium and yttrium are separated from Mg, Ca, K, and other elements by elution with 0.25 M HNO3 in the mixture of ethanol and methanol. After the separation, yttrium and strontium are eluted from the column with water or methanol.In the procedure of direct isolation from 1 l of the sample, the average recovery of 50% was obtained. In the remaining two procedures, the strontium recovery was about 60% for the Sr column and 65% for anion exchange column. Recovery of yttrium is about 70% for the anion exchange column. It turned out that the procedure with the Sr resin (direct isolation and isolation after precipitation) is simpler and faster in the phase of the isolation on the column in comparison with the procedure with the anion exchanger. The procedure with the anion exchanger, however, enables the simultaneous isolation of yttrium and strontium and rapid determination of 89,90Sr. These procedures were tested by determination of 89,90Sr on liquid scintillation counter and Cherenkov counting in 5 M HNO3. Obtained results showed that activity of 50 mBq l−1 of 89,90Sr and higher can be simultaneously determined.  相似文献   

4.
A radiochemical procedure to extract plutonium, americium and strontium from soils is presented. Strontium was separated from americium and plutonium fraction at the beginning of the method to increase the Sr recovery. The studied soils coming from an Alpine wetland site contain a big amount of iron which was eliminated by an oxalate precipitation before the column step. The hydroxide precipitation should be made by adding iron of known quantity to avoid interference. The procedure was validated by reference soils from IAEA. Plutonium-238, 239, 240, 241Am, 90Sr and 137Cs activities are given and some isotopic ratios are calculated in order to know the origin of the radionuclides.  相似文献   

5.
A rapid analytical method, applicable for the selective separation and determination of90Sr and89Sr in river water, is described. Strontium is extracted from the water sample at pH 10.5 by TTA/TOPO in cyclohexane in the presence of Tiron as masking agent for interfering ß-emitters. Radiostrontium is measured by liquid scintillation after back-extraction into 1N nitric acid. The distribution coefficient of strontium is over 400 and the separation factors from other radionuclides are higher than 5.0×103.  相似文献   

6.
A rapid determination method in which beta-ray spectrometry was combined with solid phase extraction using Sr Rad Disk was developed for the determination of 89Sr and 90Sr in low-level radioactive waste. Various amounts of 89Sr, 90Sr, and 90Y retained by the Sr Rad Disk was measured by a beta-ray spectrometer, and it was found that both 89Sr and 90Sr were simultaneously determined with <30% error (2σ) at 89Sr/90Sr radioactivity ratio of 0.3 to 45. The present method was successfully applied to actual radioactive liquid waste samples arising from nuclear facilities in Japan Atomic Energy Agency. Strontium was simply separated from interfering nuclides such as 137Cs and 154Eu, and matrix components by the Sr Rad Disk, and the results obtained by beta-ray spectrometry was in good agreement with that of the conventional analysis.  相似文献   

7.
Activity concentration of 90 Sr and stable strontium concentration was analysed in 42 samples of animal (deer, roe-deer, elk and boar) bones, which mostly originated from north-eastern Poland. Strontium separation was performed by extraction chromatography. Determination of chemical yield was controlled by means of stable Sr determination using atomic spectrometry at the beginning and at the end of the separation procedure. Equilibrated 90 Sr and 90 Y activity was measured using a liquid scintillator spectrometer. Stable strontium range was from 55.4±1.7 ppm to 91.8±4.5 ppm, the mean was 71.84 ppm with a standard deviation (SD) of 9.31 ppm. The mean recovery of strontium was 26.7% with SD = 16.1%. The maximum activity of 90 Sr, equal to 629±13 Bq/kg (ash) was found for a deer sample from Augustów Primeval Forest. In average, deer show the highest radiostrontium level, followed by roe-deer, elk and the lowest level were observed for boar. Differences between boar and deer or roe-deer are significant in terms of Kruskal-Wallis statistical test. Animal bones from north-eastern Poland showed about twice the mean concentration of 90 Sr, compared to those of south-central Poland, but the difference was found not significant. Activities observed in roe-deer bones suggest the deposition of a concentration of 1.9 to 3.5 kBq/m2 in the average of Chernobyl-origin 90 Sr in 1986 in north-eastern Poland.  相似文献   

8.
This study presents analytical methods for the determination of gross beta, 90Sr, 226Ra and Pu isotopes using samples in the IAEA-TEL-2015-04 ALMERA Proficiency Test exercise. Samples for gross beta were prepared by evaporation and then analyzed using a gas proportional counter. 90Sr in the liquid sample was concentrated as SrCO3 precipitates and purified by Sr resin. Pu isotopes and 90Sr in the soil sample were extracted from the sample by mineral acid leaching and separated using TEVA and Sr resin, respectively. Pu isotopes were determined by alpha spectrometry and 90Sr were determined with a liquid scintillation counter. Radium in the soil sample was extracted by LiBO2 fusion, and the radon-emanation method using LSC was applied for the determination of 226Ra.  相似文献   

9.
This study presents a rapid and quantitative sequential radiochemical separation method for Pu, U, Am and Sr isotopes in environmental samples with extraction chromatographic resins. After radionuclides were leached from the samples with 6 M HNO3, Pu and U isotopes were adsorbed onto the UTEVA column and Am isotopes were adsorbed onto the TRU column connected with the UTEVA column. Also, 90Sr was adsorbed onto the Sr column connected with the TRU column. Pu and U isotopes were purified from other nuclides through the UTEVA column. In addition, Am isotopes were separated from other nuclides with the TRU column. Finally, 90Sr was purified with the Sr resin. After α source preparation for the purified Pu, U and Am isotopes with micro-coprecipitation method, Pu, U and Am isotopes were measured using alpha spectrometry. On the other hand, 90Sr was measured using a low level liquid scintillation counter. The radiochemical procedure for Pu, U, Am and Sr nuclides investigated in this study has been applied to environmental samples after validating the simulated samples.  相似文献   

10.
We studied the use of an extraction chromatography for determination of 90Sr in contaminated water samples. The aim of our work was to compare selected products from the point of view of the strontium chemical yields and analysis time. Three commercial products, 3M Empore? Strontium Rad Disk, AnaLig® Sr-01 gel, Sr®Resin, and two classical methods, liquid?Cliquid extraction with tributhylphosphate and carbonate co-precipitation, were tested for the separation of 90Sr. The water sample from nuclear power plant A1 Jaslovske Bohunice was used for radiochemical analysis of 90Sr volume activity. Samples were traced with 85Sr to monitor strontium chemical recovery and counted either by Cerenkov counting on TRI CARB 2900 TR liquid scintillation counter or low level alpha?Cbeta proportional counter.  相似文献   

11.
The analysis of actinides and radiostrontium in animal tissue samples is very important for environmental monitoring. There is a need to measure actinide isotopes and strontium with very low detection limits in animal tissue samples, including fish, deer, hogs, beef and shellfish. A new, rapid separation method has been developed that allows the measurement of plutonium, neptunium, uranium, americium, curium and strontium isotopes in large animal tissue samples (100–200 g) with high chemical recoveries and effective removal of matrix interferences. This method uses stacked TEVA Resin®, TRU Resin® and DGA Resin® cartridges from Eichrom Technologies (Darien, IL, USA) that allows the rapid separation of plutonium (Pu), neptunium (Np), uranium (U), americium (Am), and curium (Cm) using a single multi-stage column combined with alphaspectrometry. Strontium is collected on Sr Resin® from Eichrom Technologies (Darien, IL, USA). After acid digestion and furnace heating of the animal tissue samples, the actinides and 89/90Sr are separated using column extraction chromatography. This method has been shown to be effective over a wide range of animal tissue matrices. Vacuum box cartridge technology with rapid flow rates is used to minimize sample preparation time.  相似文献   

12.
A simple and rapid separation procedure was systemized for the determination of 99Tc, 90Sr, 94Nb, 55Fe and 59,63Ni in low and intermediate level radioactive wastes. The integrated procedure involves precipitation, anion exchange and extraction chromatography for the separation and purification of individual radionuclide from sample matrix elements and from other radionuclides. After separating Re (as a surrogate of 99Tc) on an anion change resin column, Sr, Nb, Fe and Ni were sequentially separated as follows; Sr was separated as Sr (Ca-oxalate) co-precipitates from Nb, Fe and Ni followed by purification using Sr-Spec extraction chromatographic resin. Nb was separated from Fe and Ni by anion exchange chromatography. Fe was separated from Ni by anion exchange chromatography. Ni was separated as Ni-dimethylglyoxime precipitates after the removal of 134,137Cs and 110mAg by Cs-phosphotungstate and AgCl precipitation, respectively. Finally, the radionuclide sources were prepared by precipitation for their radioactivity measurements. The reliability of the procedure was evaluated by measuring the recovery of chemical carriers added to a synthetic radioactive waste solution.  相似文献   

13.
Summary A procedure for the sequential radiochemical determination of plutonium, strontium, uranium and iron nuclides is described. The separation is carried out on a single anion exchange column. Pu(IV), U(VI) and Fe(III) are fixed on Bio Rad AG 1-X4 from 9 mol/l HCl, while the sample effluent is used for the determination of radio-strontium. Fe and U are eluted separately with 7 mol/l HNO3, and Pu(III) is eluted with 1.2 mol/l HCl containing hydrogen peroxide. Subsequently, Pu and U are electrolysed and counted by alpha spectrometry. Radiostrontium is purified by the nitrate method and counted in a low level beta proportional counter. Fe is purified by extraction and cation exchange and 55Fe is counted by X-ray spectrometry with a Si(Li) detector. The sample preparation and the application of the procedure to large samples, namely aerosols from 105 m3 of air, and monthly deposition samples from 0.6 m2 sampling area (10–100 l) are described. Chemical yields are for Pu 70±20, for Sr 80±15, for U 80–90, and for Fe 75±10%. As an example, the maximum airborne radionuclide concentrations determined with that procedure in fortnightly collected samples at Neuherberg after the Chernobyl accident were: 239+240Pu, 2.58; 238Pu, 1.40; 238U, 0.65; 234U, 0.67; 90Sr, 7600; and 55Fe, 990 Bqm–3.With appropriate changes in sample preparation, the procedure is applicable to other kinds of samples.  相似文献   

14.
A new rapid method for the determination of actinides and radiostrontium in vegetation samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used in emergency response situations or for routine analysis. The actinides in vegetation method utilizes a rapid sodium hydroxide fusion method, a lanthanum fluoride matrix removal step, and a streamlined column separation process with stacked TEVA, TRU and DGA Resin cartridges. Lanthanum was separated rapidly and effectively from Am and Cm on DGA Resin. Alpha emitters are prepared using rare earth microprecipitation for counting by alpha spectrometry. The purified 90Sr fractions are mounted directly on planchets and counted by gas flow proportional counting. The method showed high chemical recoveries and effective removal of interferences. The actinide and 90Sr in vegetation sample analysis can be performed in less than 8 h with excellent quality for emergency samples. The rapid fusion technique is a rugged sample digestion method that ensures that any refractory actinide particles or vegetation residue after furnace heating is effectively digested.  相似文献   

15.
The methodology for the rapid determination of 89,90Sr in wide range of activity concentration is given. Methodology is based on simultaneous separation of strontium and yttrium from samples by mixed solvent anion exchange chromatography, mutual separation of 89,90Sr from 90Y by hydroxide precipitation and quantitative 89,90Sr determination by Cherenkov counting within 3 days. It is shown that Y and Sr can be efficiently separated from alkaline, alkaline earth and transition elements as well as from lanthanides and actinides on the column filed by strong base anion exchanger in nitrate form and 0.25 M HNO3 in mixture of ethanol and methanol as eluent. Decontamination factor for Ba, La and other examined elements except calcium is low and can not affect quantitative determination in predictable circumstances. Methodology for quantitative determination by Cherenkov counting based on following the changes of sample activity over time is described and discussed. It has been shown that 89,90Sr can be determined with acceptable accuracy when 89Sr/90Sr ratio is over 10:1 and that separation of Y enables reliable determination of 89Sr and 90Sr in wide range of 89Sr/90Sr ratios (60:1) and in some cases in presence of other yttrium and strontium isotopes. The methodology was tested by determination of 89,90Sr in Analytics crosscheck samples (nuclear waste sample) and ERA proficiency testing samples (low level activity samples). Obtained results shows that by using of low level liquid scintillation counter it can be possible to determine 89Sr and 90Sr in wide range of concentration activity (1–1,000 Bq/L/kg) with uncertainty below 10% within 2–3 days. Results also show that accuracy of determination of 89Sr (and 90Sr) strongly depends on the determination of difference between separation and counting time when activity ratio of 89Sr/90Sr is high. Examination the influence of media and vial type on background radiation and counting efficiency has shown that lowest limit of determination can be obtained by using of HNO3 in plastic vials as counting media, because in this combination figure of merit is maximized. For the recovery of 50% and 100 min of counting time estimated MDA is 55 Bq and 90 Bq for 90Sr and 89Sr, respectively. Analysis of combined uncertainty shows that it mainly depends on uncertainty of efficiency and recovery determination, uncertainty of activities determination for both isotopes and level of background radiation.  相似文献   

16.
This work describes a procedure for the isolation of 90Sr and 210Pb from deer bones by anion exchange methods and their sequential measurement by LSC. To prevent collection of Pb on the Sr·Spec® resin we first separated Pb on a Dowex anion exchange column. Sr, which is not held back on the Dowex column, was then purified using Sr·Spec® resin: first Ca and the Ra isotopes were eluted with 3 M HNO3 and then Sr was eluted with distilled water. With this 2-steps procedure pure 210Pb and 90Sr spectra can be achieved. The chemical yield of both steps was determined by ICP-MS. Our 90Sr results show satisfying agreement with data obtained by a shorter Sr·Spec® method and also by the “classical” 90Sr determination using fuming nitric acid. Also 210Pb results were checked by re-measuring bone samples with already known 210Pb activities. Further our method was verified on the reference sample IAEA-A-12.  相似文献   

17.
Strontium Hydroxide Chloride and Strontium Hydroxide Bromide – Preparation, Crystal Structure, and IR and Raman Spectra The partly hitherto unknown compounds Sr(OH)Cl, Sr(OH)Br mC16 and Sr(OH)Br cP16 have been established by both dehydration of the hydrates (Sr(OH)Cl, Sr(OH)Br mC16) and melting together stoichiometric mixtures of Sr(OH)2 and SrCl2 or SrBr2 (Sr(OH)Cl, Sr(OH)Br cP16). The monoclinic polymorph of the bromide is monotropically changed above 650 K (high-temperature X-ray and high-temperature Raman studies) into the cubic modification. Sr(OH)Cl crystallizes in the Cd(OH)Cl structure type (space group P63mc, Z = 2, a = 414.41(2), c = 995.16(10) pm), Sr(OH)Br mC16 and cP16 crystallizing in own structures (C2/m, Z = 4, a = 1100.66(7), b = 429.55(3), c = 726.25(5) pm, β = 106.285(4)°, P213, Z = 4, a = 675.79(2) pm). The structures were refined from X-ray powder diffractograms (Sr(OH)Cl: RI = 11.4%, 4668 observations, Sr(OH)Br mon.: RI = 13%, 1082 observations), neutron powder diffractograms (Sr(OD)Br cub.: RI = 3,8%, 793 observations), and X-ray single-crystal studies, respectively (Sr(OH)Br cub.: R1 = 5.02%, 585 independent reflections). The positions of the hydrogen atoms of Sr(OH)Cl and Sr(OH)Br mon. were determined by the method of minimum cohesive energy. Sr(OH)Cl and Sr(OH)Br mon. crystallize in layered structures with monocapped distorted octahedrally (3 OH and 4 X) coordinated strontium ions. Sr(OH)Br cub. crystallizes in a structure built up of three-dimensional nets, the coordination of Sr, however, corresponds to that of Sr(OH)Cl and Sr(OH)Br mon. IR and Raman spectra are presented and discussed together with the structure data with respect to the strength of the O–H…X hydrogen bonds (stretching modes of matrix isolated OD ions: 2641 cm–1 (Sr(OH)Cl), 2662 cm–1 (Sr(OH)Br mon.), and 2614 cm–1 and 2572 cm–1 (Sr(OH)Br cub.) (295 K)) and the dependence of the librations of the OH ions on the strength of the hydrogen bonds and the packing of the structure. The OH ions of Sr(OH)Br cub. display a temperature dependent disorder between a thermodynamically more stable position with trifurcated hydrogen bonds and one with stronger, almost linear bonds.  相似文献   

18.
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.
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.
  相似文献   

19.
The paper describes a new high-precision method for the simultaneous precise determination of 88Sr/86Sr and 87Sr/86Sr ratios in a single portion of a geological sample by multicollector inductively coupled mass spectrometry (MC-ICP-MS). The isotope analysis is carried out with mass bias effect correction by a combination of internal normalization to the standard Zr-isotope ratio and bracketing standard method (external normalization). Our results for geochemical IAPSO and BCR-1 standard samples are in a good agreement with the published data. The reproducibility of the 88Sr/86Sr ratio varies from ±0.015 to ±0.05?? (depending on the sample features) and, together with the analysis accuracy, is superior to the previously reported methods of MC-ICP-MS analysis. Still ahead is only double spike thermal ionization mass spectrometry with its ±0.02?? reproducibility. However, the new method allows the simultaneous determination of 88Sr/86Sr and 87Sr/86Sr ratios and its productivity is higher by 5 to 6 times. On the other hand, in sample preparation, it is necessary to strive for at least 95% Sr yield from the chromatographic column; otherwise the sorption-desorption process may lead to a 0.6?? 88Sr/86Sr ratio bias relative to the true value.  相似文献   

20.
A sensitive and reliable metbod for the sequential separation and determination of plutonium,241Am and90Sr in soil samples was developed. Plutonium was separated by a Microthene-TNOA column. Then90Y (for90Sr determination) was separated from americium by a HDEHP column after elimination of large amounts of interfering stable or radioactive nuclides (iron,210Bi and210Po etc.) by an oxalate precipitation and a Microthene-TNOA column. Finally americium was purified by another HDEHP column and a PMBP-TOPO extraction. A special attention was paid to the decontamination of Pu and Am from210Po and of90Y from210Bi; the relevant decontamination factors resulted greater than 105, 106 and 104 respectively. The detection limits were 1.2 mBq/kg for Pu and 1.7 mBq/kg for241Am and 0.32 Bq/kg for90Sr. The procedure was checked by analyzing three certified samples supplied by IAEA. Some Italian soil samples were also analyzed giving average yields of 84.9±7.2% for Pu, 57.8±3.2%for Am and 96.7±1.6% for Y; the239+240Pu,238Pu,241Am and90Sr contents (Bq/kg) ranged from 0.347 to 1.53, from 0.013 to 0.048, from 0.126 to 0.556 and from 2.89 to 11.6 respectively and the average ratios were 0.037±0.017 for238Pu/239+240Pu, 0.357±0.040 for241Am/239+240Pu and 7.0±1.2 for90Sr/239+240Pu.  相似文献   

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