The determination of uranium by a fluorimetric method using a conventional spectrophotometer has been elaborated. The quenching effect of the matrix was reduced by separation with liquid-liquid extraction and emulsion liquid membrane extraction methods using D2EHPA as a selective extraction reagent. The method was employed for uranium determination in radioactive waste solutions and proved to be very fast and easy to perform. It was found that it is possible to determinate as low as 0.2 ppm of uranium in a 10 ml sample.
The separation and quantification of nitrophenol isomers in aqueous solutions by capillary isotachophoresis has been studied. Several electrolyte systems with different leading and terminating ions were used. The separation was carried out in a PTFE column in a device for column-coupling system.
Composite sorbents based on potassium nickel ferrocyanide embedded in silica gel matrix were prepared and characterised by
powdered X-ray diffraction analysis, IR spectra, Mössbauer spectra and electron microscopy. The sorbent exhibits very good
efficiency for cesium uptake and radiation resistance. The sorption capacity for cesium ions is comparable with the capacity
for the pure ferrocyanides.
The preconcentration of strontium from aqueous colloid solution containing di(2-ethylhexyl)-phosphoric acid as a surfactant was performed using micellar ultrafiltration technique. Filters with different pore size and materials (nitrocellulose, polysulfonate, glass fibers) were used to achieve a separation from liquid solutions. The strontium recoveries depending on the different conditions (pH, concentration of surfactant, background electrolytes) were determined and the results are explained in the terms of colloidal parameters of the system, viz. surface tension and turbidity.
The influence of background electrolytes (KCl, NH4Cl, CTABr) in different concentrations on the sorption ability of radiocesium by measuring the distribution coefficient has been studied. Sorption isotherms of cesium for characterization of soil sorption ability were used. Sorption of cesium depends on its concentration and at least three different sorption sites are active in the sorption process. In the case of low cesium concentration, two very selective sites with high distribution coefficients are responsible for the sorption. With increasing cesium concentration in the aqueous phase, distribution coefficient is decreasing. Frayed edge sites of illite in soil and exchangeable potassium are probably responsible for nonlinear isotherms at low cesium concentrations. From sorption isotherms and determination of potassium by activation analysis, it was found that the capacity of very selective sites for different concentrations of background electrolyte was up to 7 mmol·kg–1.
An extraction chromatography method was developed for the separation of 239Np from 243Am in nitric acid solution. A sorbent based on aliphatic quaternary amine Aliquat-336 and hydrophobized silica gel was prepared. 239Np reduced to the oxidation state(IV) with ferrous sulfamate in 2M or 6M HNO3 sorbs on the prepared silica gel column. After washing with 0.1M ferrous sulfamate in 2.5M HNO3, 239Np is eluted with 0.1M HNO3 containing 0.02M HF. The separation of 243Am from 239Np is very effective. The purity of 239Np was found to be better than 99.5%. The proposed 239Np milking procedure is suitable for the preparation of 239Np tracer that can be used for the determination of 237Np radiochemical yield.
The preconcentration of strontium using a solid phase separation technique with selective micelle forming complexant has been studied. Di-2-ethylhexylphosphoric acid and its thio- and dithio derivatives were used as modifiers. The goal of this work was to study the influence of physico-chemical parameters on recovery of strontium after its preconcentration on reverse phase (Si–C-18) using micelle modifiers.
Various silica gel materials were chemically modified with imidazole, diaza-18-crown-6 (DA18C6) and dibenzod-18-crown-6 (DB18C6). The degree of functionalization of the covalently attached molecule was calculated from C, H, N analysis and ranged between 0.270 and 0.552 mmol/g (for sorbents with imidazole) and between 0.043 and 0.062 mmol/g (for sorbents with DA18C6 and DB18C6). The degree of functionalization depends on the reflux time and silica gel matrix used. Experimental sorption capacity ranged between 0.038 and 0.228 mmol/g (for sorbents with imidazole) and between 0.019 and 0.050 mmol/g (for sorbents with DA18C6 and DB18C6). Synthesized hexagonal mesoporous silica matrix MCM-41 with uniform pore diameter <40 Å was used too. Change of pore diameters of silica gel support to larger pores should have a positive influence on access of cobalt ion to sorption centers to increase of sorption capacity of sorbents. The sorption kinetics of cobalt and the influence of cobalt concentration, pH of various kinds of silica gel matrix with immobilized imidazole group in static conditions on sorption were measured. The sorption of cobalt in various conditions (pH, contact time of phases) with constant liquid-solid ratio (V/m = 50 ml/g) was studied. The distribution coefficients ranged between 200 and 50 000 ml/g (for imidazole), 85 and 120 ml/g (for DB18C6) and between 230 and 500 ml/g (for DA18C6) according to silica gel matrix used and according to the method of sorbent preparation. pH plays important role in the sorption of cobalt on prepared sorbents with immobilized crown ethers due to protonization of crown ethers. Protons significantly competes to sorption of cobalt in acidic solutions. The influence of presence of other heavy or toxic metals (Hg(II), Cd(II), Mn(II), Zn(II), Cu(II), Fe(III), Cr(III), Al(III) and the influence of sodium and potassium on sorption Co(II) from aqueous solutions was investigated. Sorption of cobalt decreases in order Hg > Cu > Cd > Zn, Fe > Mn > Al, Cr. The presence of sodium and potassium ions at concentration 0.05 mol/l significantly influences on the sorption of cobalt with sorbent with immobilized DB18C6 functional group.
Cesium cation exchange reaction with K, Na, Ca and Mg ions on natural and modified clinoptilolite has been studied. Batch
cation-exchange experiments were performed by placing 0.5 g of clinoptilolite into 10 ml or 20 ml of 1·10−3M CsCl solution for differing times. Two type deposits of clinoptilolite zeolites from, Nižný Hrabovec (NH), Slovakia and
Metaxades (MX), Greece were used for ion-exchange study. The distribution coefficient (Kd) and sorption capacity (Γ) were evaluated. For the determination of K, Na, Ca and Mg isotachophoresis method, the most common
cations in exchange reaction was used. Cesium sorption was studied using 137Cs tracer and measured by γ-spectrometry.