Determination of 90Sr in environmental samples using solid phase extraction chromatography

The p-tert-butyl calix[4]arene thiophenol derivative was successfully synthesized with reflux condition and was characterized by FT-IR and ¹H-NMR. This work mainly adopted the method of controlling variables. The results showed that the optimum pH value, temperature and extraction time were respectively 4.5, 25 °C and 90 min. By calculating the data of the enthalpy change and gibbs free energy, indicating that the process of reaction was an exothermic and spontaneous process, and it demonstrated a close agreement with pseudo-second-order kinetic model. It is also found that the coexisting cations on the extraction of uranium had greater influence.

     

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.     

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.     

Determination of radiostrontium in soil samples using a crown ether

A simple and rapid method has been developed for the separation and determination of total radiostrontium in soil. The method consists of three basic steps: oxalate precipitation to remove bulk potassium, chromatographic separation of strontium from most inactive and radioactive interferences utilizing a crown ether (Sr. Spec, EIChroM Industries, Il. USA) and oxalate precipitation of strontium to evaluate the chemical yield. Radiostrontium is then determined by liquid scintillation counting of the dissolved precipitate. When 10 g samples of soil are used, the sensitivity of the method is about 10 Bq/kg. The chemical yield is about 80%. The separation and determination of radiostrontium can be carried out in about 8 hours.     

The determination of uranium in environmental samples using extraction chromatography

Many traditional methods for the determination of actinides in environmental samples have involved several solvent extraction and/or ion exchange steps that separate the radionuclide of interest from the bulk sample matrix. These methods are generally labor-intensive employ hazardous substances and generate considerable volume of toxic wastes. Extraction chromatographic resins have been developed that combine the power and selectivity of solvent extraction with the ease of use of ion exchange chromatographic resin. Some of these extraction chromatographic resins have been developed that will selectively sorb a particular radionuclide or groups of radionuclides from solution. A considerable amount of interest has recently been shown in these resins as they are claimed to be cost-effective in terms of increasing sample throughput, eliminating the need for expensive solvent extractants and being generally safer to handle. One such commercially available resin, U/TEVA.Spec^® will selectively absorb uranium and tetravalent actinides such as thorium and plutonium from an acidic nitrate solution. This paper describes the application of U/TEVA.Spec^® to the determination of uranium in a range of environmental samples.     

Determination of chloroethenes in environmental biological samples using gas chromatography coupled with solid phase micro extraction

Summary An analytical method has been developed to determine the chloroethene series, tetrachloroethene (PCE), trichloroethene (TCE),cisdichloroethene (cis-DCE) andtransdichloroethene (trans-DCE) in environmental biotreatment studies using gas chromatography coupled with a solid phase micro extraction (SPME) technique. The volatile chlorinated compounds in aqueous solution can be analyzed directly without solvent extraction, purge and trap, or thermal heating. The calibration curves have demonstrated good linear relationships within 50.0 to 3000.0 g L^–1 concentration range. Detection limits are 18.0, 5.0, 25.0, and 42.0 g L^–1, for PCE, TCE,cis-DCE andtrans-DCE, respectively. Factors which affect the SPME process, such as sample adsorption time, thermal desorption time, and concentration of salt in the matrix, have also been evaluated.     

Determination of90Sr in soil and sediment using lithium-borate fusion and extraction chromatography

A rapid and reliable method for determination of⁹⁰Sr in soil and sediment has been developed. The method is based on lithium-borate fusion and extraction chromatography with a Sr-resin. The samples can be dissolved and separated for Sr in approximately 5 hours of which the fusion and dissolution requires 20 minutes. The method has been applied to four reference materials, two soils and two sediments, and the results agree well with the recommended values. The mean recovery of Sr was 71%.     

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.     

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.     

A simple radiochemical determination of90Sr in environmental samples

A simple procedure for the determination of⁹⁰Sr in environmental samples is described. The method uses the different solubilities of the oxalates of calcium and strontium in presence of a large excess of calcium. For this reason the method is especially suited for Ca-rich samples, as e.g., bones or soils. However, after addition of supplementary calcium it works equally well for other types of samples. The method was tested by analyzing the IAEA Certified Reference Materials soil, animal bone and algae.     

The application of extraction chromatography to the determination of radionuclides in biological and environmental samples

The paper describes the application of extraction chromatography to the determination of several alpha and beta emitters in biological and environmental samples. Both column extraction chromatography and batch extraction process have been used to isolate the radionuclides from the samples. The effect of several parameters (extractant concentration, support granulometry, stirring time, temperature, presence of a complexing agent) on the extraction and elution has been examined. The application of redox extraction chromatography is also described.     

Measurement of (90)Sr in environmental samples by cation-exchange and liquid scintillation counting

A new method for the measurement of (90)Sr in environmental samples by cation-exchange and liquid scintillation counting is described. Strontium carbonate is purified by precipitation and ion-exchange, weighed for the determination of chemical yield, dissolved in hydrochloric acid and mixed with the liquid scintillator, Aquasol-2. Two channels of a low-background liquid scintillation counter are used to determine (90)Sr, (90)Y and (89)Sr, free from the effects of environmental tritium. The values of (90)Sr obtained by this method are in good agreement with those from ordinary (90)Y milking and the gas proportional counting method. The concentration of (90)Sr in the air at Tokai-mura in Japan has been measured by the new method.     

Determination of atrazine in environmental and biological samples using solid phase extraction and spectrophotometry

An analytical method employing a combination of solid phase extraction and spectrophotometry is proposed for the determination of a widely used herbicide atrazine. This combination is very simple and cheaper than chromatography and mass spectrometry based methods. The proposed method also reduced the use of toxic solvents. The method is based on the reaction of atrazine with pyridine to form a quaternary halide, which forms a carbinol base in the presence of alkali. Carbinol undergoes cleavage of heterocyclic ring to form glutaconic aldehyde that is subsequently coupled with sulphanilic acid to give a yellow orange dye which is measured spectrophotometrically at 460 nm. Beer’s law is obeyed in the range 0.07–0.7 μg/mL of atrazine. Molar absorptivity and Sandell’s sensitivity were found to be 2.2 × 10⁵ L/mol cm and 0.0009 μg/cm², respectively. Breakthrough volume is found to be more than 100 mL. The use of solid phase extraction increases the sensitivity ten times. The proposed method is sensitive and found to be free from the interference of a large number of foreign species and other pesticides. The developed method was applied to spiked environmental and biological samples, the recovery was in the range from 95.2 to 99.2% with RSD of 0.36%. The article is published in the original.     

Selective solid-phase extraction of tebuconazole in biological and environmental samples using molecularly imprinted polymers

Molecularly imprinted polymers (MIPs) were prepared by precipitation polymerization using tebuconazole (TBZ) as a template. Frontal chromatography and selectivity experiments were used to determine the binding capabilities and binding specificities of different MIPs. The polymer that had the highest binding selectivity and capability was used as the solid-phase extraction (SPE) sorbent for the direct extraction of TBZ from different biological and environmental samples (cabbage, pannage, shrimp, orange juice and tap water). The extraction protocol was optimized and the optimum conditions were: conditioning with 5 mL methanol:acetic acid (9:1), 5 mL methanol and 5 mL water respectively, loading with 5 mL aqueous samples, washing with 1.2 mL acetonitrile (ACN):phosphate buffer (5:5, pH3), and eluting with 3 mL methanol. The MIPs were able to selectively recognize, effectively trap and preconcentrate TBZ over a concentration range of 0.5–15 μmol/L. The intraday and interday RSDs were less than 9.7% and 8.6%, respectively. The limit of quantification was 0.1 μmol/L. Under optimum conditions, the MISPE recoveries of spiked cabbage, pannage, shrimp, orange juice and tap water were 62.3%, 75.8%, 71.6%, 89% and 93.9%, respectively. MISPE gave better HPLC separation efficiencies and higher recoveries than C18 SPE and strong cation exchange (SCX) SPE. Figure HPLC analysis of spiked pannage after MISPE (A) and after C18 SPE (B). HQ (1), E3 (2), p-NP (3), FTF (4), TBZ (5), PNZ (6), HXZ (7) Electronic supplementary material Supplementary material is available in the online version of this article at and is accessible for authorized users.     

Determination of polychlorinated biphenyls by fast chromatography mass-spectrometry in environmental and biological samples

A method for the determination of polychlorinated biphenyls (PCB) by fast gas chromatography coupled with mass-spectrometric detection in selective ion monitoring mode has been developed. Chromatographic separation was carried out with HT-8 column (30 m × 0.25 mm) under sharp temperature increase from 80 to 320°C at a rate of 40°C/min. Duration of chromatography is 10 min. Fast chromatography conditions suggested by authors makes it possible to increase S/N ratios 10 times and so to reduce significantly the representative weight of the sample and develop an effective sample preparation technique. The method was used for PCB determination in Baikal area samples such as soil, snow, sediments from Lake Baikal and its tributaries, tissues of Baikal omul (Coregonus migratorius, Georgi, 1775) and blubber of Baikal seal (Phoca sibirica Gm.). The sample preparation stage includes PCB extraction from environmental samples and hydrolyzate of biological material with the following cleanup of the extract on the compact silica gel and florisil cartridges (0.5 g of the sorbent). The method enables the measurements of total PCBs and isomer groups of the same chlorination level with interlaboratory precision of no greater than 10% and the determination of indicator congeners (PCBs 28, 52, 101, 118, 138, 153, and 180) with a precision not exceeding 15%.     

Determination of 90Sr in urine samples and 89Sr/90Sr in water samples by chemical separation and Cherenkov counting with LSC system

Journal of Radioanalytical and Nuclear Chemistry - In order to determine radiostrontium with a satisfactory chemical yield, calculated by an external standard, and a low level of MDC a...     

Solvent extraction separation of rubidium with a crown ether for neutron activation analysis in rock samples

The extraction behavior of rubidium with a crown ether has been studied and methods for the separation and determination of rubidium have been developed. Rubidium was separated with tetraphenylborate from sample solution, and then quantitatively extracted into nitrobenzene by 18-crown-6 from 0.05 mol/l picric acid (pH 6) and back-extracted by 6 mol/l hydrochloric acid. Rubidium was determined by the neutron activation method in rock samples.     

Ion-imprinted resin for use in an automated solid phase extraction system for determining 90Sr in environmental and human samples

Journal of Radioanalytical and Nuclear Chemistry - In 90Sr analysis, determining its daughter 90Y improves the sensitivity of the radiometric methods. We found that to imprint a cavity made of...     

Determination of traces of 237Np in environmental samples by ICP-MS after separation using TOA extraction chromatography

A simple, rapid, cost-efficient, and robust method for separation of 237Np with an extraction chromatographic column (TOA: tri-n-octylamine on Teflon powder) is outlined in detail and further improved for direct ICP-MS analysis. The column efficiently retained 237Np in 2 mol L(-1) HNO3 medium and all of the 237Np was easily eluted with 0.02 mol L(-1) oxalic acid in 0.16 mol L(-1) HNO3 at 95 degrees C. The separated solutions were free from most matrix elements and were aspirated into the ICP-MS directly. The decontamination factor for 238U is more than 10(4). The instrumental detection limit for 237Np was 0.46 pg mL(-1), which corresponds to 1.2 x 10(-5) Bq mL(-1). The method is more rapid than traditional radiometric techniques. It is also considered to be more suitable for environmental monitoring than existing methods based on TOA.     

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.