Rapid method for the determination of radiostrontium in milk

A radiochemical procedure comprising ion chromatography for preconcentration, oxalate precipitation for alkali/alkaline earth separation, strontium specific extraction chromatography with a crown ether for calcium/strontium separation, carbonate precipitation for counting on a low background proportional counter, provides a simple, rapid (48 h) and effective method for radiostrontium determination in emergency situation in milk. The separation scheme gives a strontium recovery rate of 62% and an empiric relative standard deviation of 11%. The detection limit for 500 ml milk and 3600-second counting time is 0.090 Bq^.l^-1.     

Determination of strontium radioisotopes in soils

Summary A method is proposed for determination of radiostrontium in soils which is based on selective strontium separation by liquid-liquid extraction with dicyclohexano-18-crown-6 in chloroform, loading of the extract on a thin-layer plate and TLC separation of strontium and yttrium radioisotopes using a circular procedure. The method allows the separate determination of ⁸⁹Sr and ⁹⁰Sr. The strontium chemical yield is more than 90%, the detection limit is about 0.5 Bk/g, RSD is equal to 2–5%.     

Analysis of90Sr in environmental and biological samples by extraction chromatography using a crown ether

The use of crown ethers is a simple and rapid method for the separation and determination of strontium in various samples. After sample dissolution oxalate precipitation was carried out to remove K. Chromatographic separation of strontium from most inactive and radioactive interference was done with a crown ether. The chemical recovery was determined gravimetrically. Radiostrontium was then determined by liquid scintillation counting.     

Rapid determination of radiostrontium in large soil samples

A new method for the determination of radiostrontium in large soil samples has been developed at the Savannah River Environmental Laboratory (Aiken, SC, USA) that allows rapid preconcentration and separation of strontium in large soil samples for the measurement of strontium isotopes by gas flow proportional counting. The need for rapid analyses in the event of a radiological dispersive device or improvised nuclear device event is well-known. In addition, the recent accident at Fukushima Nuclear Power Plant in March, 2011 reinforces the need to have rapid analyses for radionuclides in environmental samples in the event of a nuclear accident. The method employs a novel pre-concentration step that utilizes an iron hydroxide precipitation (enhanced with calcium phosphate) followed by a final calcium fluoride precipitation to remove silicates and other matrix components. The pre-concentration steps, in combination with a rapid Sr Resin separation using vacuum box technology, allow very large soil samples to be analyzed for ^89,90Sr using gas flow proportional counting with a lower method detection limit. The calcium fluoride precipitation eliminates column flow problems typically associated with large amounts of silicates in large soil samples.     

Rapid method for determination of radiostrontium in emergency milk samples

A new rapid separation method for radiostrontium in emergency milk samples was developed at the Savannah River Site (SRS) Environmental Bioassay Laboratory (Aiken, SC, USA) that will allow rapid separation and measurement of radiostrontium within 8 hours. The new method uses calcium phosphate precipitation, nitric acid dissolution of the precipitate to coagulate residual fat/proteins and a rapid strontium separation using Sr Resin (Eichrom Technologies, Darien, IL, USA) with vacuum-assisted flow rates. The method is much faster than the previous method that use calcination or cation-exchange pretreatment, has excellent chemical recovery, and effectively removes beta-interferences. When a 100 mL sample aliquot is used with a 20 minute count time, the method has a detection limit of 0.5 Bq·L⁻¹, well below generic emergency action levels.     

Rapid trace determination of radiostrontium in milk and drinking water

A rapid method for determining traces of radiostrontium in milk and drinking water is described. The technique involves a batch treatment of the milk sample with a cation exchanger (DOWEX 50W X8) followed by a solvent extraction with a crown ether (DC18C6) and a precipitation of SrCO₃. In the case of water, the strontium is extracted directly with the crown ether. The average separation yield is 74% for milk and 91% for water. The overall separation procedure takes about 8 hours. Activities as low as 0.03 Bq/1 can be determined with a low background GM-counter.     

Separation of strontium from large amounts of calcium, with application to radiostrontium analysis

The elution first of calcium and then of strontium by complex formation with cyclohexanediaminetetra-acetic acid (CyDTA) after sorption on ion-exchange columns, is shown to require careful control of pH and the concentrations of CyDTA and NH(4)(+). A procedure is described for volumetric analysis of calcium and strontium, and for use of this separation procedure before determination of (90)Sr in sea-water. Careful choice of reagents and materials is shown to be necessary for use of such a method in determination of trace amounts of radiostrontium.     

A Magnetic Sorbent for Radiocesium and Radiostrontium Removal from Clay and Soil Suspensions

A magnetic sorbent based on a mixture of magnetic iron and nickel oxides, and specific surface activation by ferrocyanide solution for enhancement of cesium adsorption is described. After equilibration of clay or soil suspension with the magnetic sorbent, the latter can be removed with exchangeable radiocesium and radiostrontium by means of magnetic separation. The distribution coefficients of the order 2·10³ l/kg for cesium and 5·10³ l/kg for strontium were determined. The efficiency of the sorbent was investigated in a 1% montmorillonite or soil suspension. At a soil:sorbent ratio 1:1–1:6 in the suspension, the fraction of exchangeable radiocesium in soil at a 2 hours contact was diminished from 56–59% to 48–12%, the decontamination factor of both the mobile cesium and strontium is about 3. The multistage process and sorbent recycling need further investigation.     

A rapid and accurate method for the determination of strontium-90 in environmental soil

A rapid and accurate method for the determination of⁹⁰Sr in environmental soil has been developed; the procedure includes soil leaching by hydrochloric acid, oxalate precipitation, decontamination from²¹⁰Bi, separation by HDEHP extraction chromatography column, yttrium oxalate precipitation and -counting. The interference of²¹⁰Bi was found and studies have been made for the decontamination of⁹⁰Y from²¹⁰Bi by Bi₂S₃ precipitation giving a decontamination factor of 1.05·10³. The analytical results obtained by the improved rapid method for 12 soil samples were comparable to that obtained by a previous method within a relative error of 20%. Studies of vertical distribution of⁹⁰Sr in an environmental soil profile have shown that 90% of the⁹⁰Sr deposits in the 30 cm surface soil of the earth with a highest concentration of 3.40 Bq/kg. When 50 g soil was analyzed, the yield of yttrium was 73±17% with a detection limit of 0.26 Bq/kg.     

Sr and stable strontium in bones of wild, herbivorous animals from Poland

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.     

Determination of90Sr by thin layer radiochromatography

A simple method for the determination of⁹⁰Sr by using thin layer chromatography on silica gel or cellulose pretreated with calcium oxalate is proposed. In these conditions a complete separation between strontium and its daughter yttrium is obtained. Radioactivity of separated elements was measured by a linear multiscanner analyzer and the results were computer processed to obtain the activity of⁹⁰Sr. The method has been applied to samples of water and milk subjected to a very simple extraction procedure. Under the experimental conditions used, the detection limit is about 25 mBq of deposited radioactivity, which corresponds to about 6 Bq/l.     

Kinetic-enzymatic determination of oxalate in urine by flow-injection analysis with double stopped flow

An enzymatic stopped-flow injection method for the determination of oxalate is proposed. Two sequential haltings of the flow are made, the first while the sample plug is in a reactor packed with controlled-pore glass and immobilized oxalate decarboxylase, and the second on merging of the sample plug with a stream containing an auxiliary enzyme (formate dehydrogenase) as the plug reaches the flow cell, where absorbance-time data are collected. The linear range of the calibration graphs is between 0.1 and 3.0 mM oxalate and their sensitivity depends on the interval over which measurements are made. The proposed method was applied to the determination of oxalate in urine without separation of the analyte by precipitation, with excellent results.     

Rapid method for radiostrontium determination in milk in emergency situations using PS resin

This study describes a new and rapid procedure for radiostrontium determination in milk samples based on the use of plastic scintillation resins (PS resins). The proposed method reduces the time of analysis by at least 2 h by combining separation and measurement preparation into a single step and optimizing the pre-treatment steps. The method is robust and reproducible, with good total recoveries (65% on average) and a relative bias for total radiostrontium activity (⁸⁹Sr + ⁹⁰Sr) below 7%. The minimum detectable activity for 100 mL of milk sample measured for 60 min is about 0.34 Bq L^?1. The proposed method can quantify radiostrontium content in 5 h, which makes it suitable for use in emergency situations.     

Radiochemical separation of strontium by isotopic exchange

Isotopic exchange has been used for the rapid separation of minute quantities of radio-strontium. A number of variables such as agitation time, concentration of strontium in both phases, mode of preparation and aging of the precipitates, were studied and optimized. With an optimized procedure, exchange yields of 96% and 94% respectively were obtained when strontium sulphate and strontium oxalate precipitates were used for the exchange. Decontamination studies made with radioactive tracers of 15 elements showed that the sulphate precipitate is more selective than the oxalate, most of the elements showing <1 % contamination except (140)Ba-(140)La and (110)Ag which show high contamination. This simple procedure has also been applied for the determination of radioactive strontium in rain-water samples.     

Estimation of <Superscript>90</Superscript>Sr activity in reprocessed uranium from the PUREX process

⁹⁰Sr estimation in reprocessed uranium was carried out by a series of solvent extraction and carrier precipitation techniques using strontium and lanthanum carriers. Fuming with HClO₄ was used to remove ¹⁰⁶Ru as RuO₄. Three step solvent extraction with 50% tri-n-butyl phosphate in xylene in presence of small amounts of dibutyl phosphate and thenoyl trifluoro acetone was carried out to eliminate uranium, plutonium, thorium and protactinium impurities. Lanthanum oxalate precipitation in acid medium was employed to scavenge the remaining multivalent ions. Strontium was precipitated as strontium oxalate in alkaline pH and ¹³⁷ Cs was removed by washing the precipitate with water. A strontium recovery well above 70% was obtained. Final estimation was carried out by radiometry using end window GM counter after drying the precipitate under an infra red lamp. The same procedure was extended to the estimation of ⁹⁰Sr in a diluted sample of the actual spent fuel solution. An additional lanthanum oxalate precipitation step was required to remove the entire ¹⁴⁴Ce impurity from this sample. This modified procedure was employed in the determination of ⁹⁰Sr in a number of reprocessed uranium samples and the over all precision of the method was found to be well within ±10%. An additional barium chromate precipitation step was necessary for the analysis of reprocessed uranium samples from high bumup fuels to eliminate trace amounts of short lived ²²⁴Ra produced during the decay of ²³²U and its daughters as they interfere in the estimation of ⁹⁰Sr.     

The application of novel extraction chromatographic materials to the characterization of radioactive waste solutions

A simple method for the separation and preconcentration of radiostrontium from acidic nuclear waste solutions for subsequent determination is described. The method involves passage of the waste solution, acidified to at least 2M with nitric acid, through an extraction chromatographic column consisting of a 1M solution of bis-4,4(5)[(t-butyl)cyclohexano]-18-crown-6 in 1-octanol sorbed on an inert polymeric substrate, which preferentially retains strontium. The strontium may then be stripped from the column with a small volume of either dilute (0.05M) nitric acid or water. Actinides present are removed quantitatively prior to strontium separation by passage of the sample through an actinide-specific extraction chromatographic column.Work performed under the auspices of the Office of Basic Energy Sciences, Division of Chemical Sciences, U. S. Department of Energy, under contract number W-31-109-ENG-38.     

Flow-Injection Spectrophotometric Determination of Oxalate,Citrate and Tartrate Based on Photochemical Reactions

Abstract

A flow-injection configuration for the spectrophotometric determination of oxalate, citrate and tartrate is proposed. The procedure is based on the photochemical decomposition of the complexes formed between iron(III) and these anions. The iron(II) produced in the photochemical reactions was detected by measuring the absorbance after complexation with ferrozine (λ_max=562 nm). Linear calibration graphs were obtained over the concentration ranges 5.0 × 10^?6 - 1.0 × 10^?4 M, 8 × 10^?6 - 1.8 × 10^?4 M and 1.0 × 10^?6 - 2 × 10^?5 M for oxalate, citrate and tartrate, respectively. The relative standard deviations at the 1x10^?5 M concentration level were within the range 1.29 - 1.47 %. The sampling frequency was about 40 samples h^?1. The usefulness of the method was tested in the determination of oxalate in urine and spinach, of citrate in pharmaceuticals and soft drinks and of tartrate in pharmaceuticals. For the determination of oxalate in urine samples a prior separation of the analyte by precipitation with calcium chloride is recommended.     

Determination of 90Sr in soil, grass and cereals

⁹⁰Sr was measured in environmental samples in Upper Austria in the year 2005. After the nuclear weapon tests the average deposition of ⁹⁰Sr in Austria amounted to 3.3 kBq/m². In 1986 the average deposition was 0.9 kBq/m² [1]. To assess the actual condition in soil, grass and cereals ⁹⁰Sr was measured in these samples. For all samples oxalate precipitation was conducted and strontium specific columns (Eichrom Industries, Inc.) were used. The calcium concentration in these samples was determined to estimate the amount of resin needed for the preparation. For grass and cereal samples columns were packed with the 100–150 μm resin to gain a lower limit of detection LLD below 2 and below 0.1 Bq/kg_{dry matter} respectively. The prepacked 2 mL columns with particle size 100–150 μm were used for soil (LLD below 2 Bq/kg_{dry matter}). After digestion of soil samples, hydroxide precipitation was used as an additional separation step. The ⁹⁰Sr was measured by liquid scintillation counting. For quality control reasons, first the initial strontium concentration in the sample was determined then a strontium carrier solution was added and after the separation steps the chemical recovery was determined by ICP-MS. Thus, no radioactive tracer and just a small amount of the measuring solution were needed. The results are presented and discussed. These results will be used as reference for further ⁹⁰Sr analyses which will be conducted in a 5 year period to detect any radiological impact of the nuclear power plant Temelin on the environment of Austria.     

Rapid column extraction method for actinides and strontium in fish and other animal tissue samples

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.     

Radiochemical analysis of90Sr in milk,soil and plants by solvent extraction

A universal and fast method of⁹⁰Sr determination in environmental matrices (raw and dried milk, plants, soils) has been elaborated. Solvent extraction method of daughter⁹⁰Y by tributyl phosphate was used. The method of strontium determination is compatible with determination of other transuranic elements (americium, plutonium) and there is no need to check the chemical yield of strontium.