Influence of hydrofluoric acid on extraction of thorium using a commercially available extraction chromatographic resin

The dependence of Th recovery on hydrofluoric acid (HF) concentration in nitric acid (HNO₃) solutions (1–5 mol/dm³) containing 1 × 10⁻⁶ mol/dm³ of Th and various concentrations of HF and the elution behavior were studied using a commercially available UTEVA (for uranium and tetravalent actinide) resin column. Thorium recovery decreased with an increase in HF concentration in the sample solutions. The concentration of HF at which Th recovery started to decrease was ∼1 × 10⁻⁴ mol/dm³ in 1 mol/dm³ HNO₃ solution, ∼1 × 10⁻³ mol/dm³ in 3 mol/dm³ HNO₃ solution, and ∼1 × 10⁻² mol/dm³ in 5 mol/dm³ HNO₃ solution. When Al(NO₃)₃ (0.2 mol/dm³) or Fe(NO₃)₃ (0.6 mol/dm³) was added as a masking agent for F⁻ to the Th solution containing 1 × 10⁻¹ mol/dm³ HF and 1 mol/dm³ HNO₃, Th recovery improved from 1.4 ± 0.3% to 95 ± 5% or 93 ± 3%. Effective extraction of Th using UTEVA resin was achieved by selecting the concentration of HNO₃ and/or adding masking agents such as Al(NO₃)₃ according to the concentration of HF in the sample solution.     

Separation of technetium from rhenium by liquid-liquid extraction with potassium xanthate

A method is described for separating technetium from rhenium in hydrochloric acid medium by liquid-liquid extraction with potassium xanthate and carbon tetrachloride. The effects of the concentration of various acids, concentration of xanthate, different solvents and diverse ions have been investigated.     

Gross alpha determination in salt rich water samples using an extraction chromatographic resin and LSC

The application of an extraction chromatographic resin to the determination of the gross alpha activity of drinking water samples with volumes greater than 100 ml and of salt rich aqueous samples, like mineral, waste or sea waters was tested. Alpha-emitters are extracted from the water sample onto the resin, the gross alpha activity is then determined by direct measurement of the dried resin using α/β discrimination LSC. The resin shows strong affinity for actinides, as well as for radium, out of pH 2 solutions. The extraction is robust against Ca, sulphate and other potential interferents. The method was tested by analyzing reference materials, intercomparison samples and spiked real samples. Results of good precision and accuracy were obtained in counting times notably shorter than routinely used for gas proportional counting.     

Solvent extraction of heptavalent technetium

An extraction study was performed on technetium in its highest oxidation state as a function of nitric acid concentration at 25, 50 and 70 °C. A long chain amine (tri-n-octylamine TOA) and an organophosphorus solvent (TBP) have been investigated. Addition of NH₄NO₃ has a salting-out effect on the extraction of TBP in the aqueous phase and therefore decreases the distribution coefficient for heptavalent technetium. The mechanism of extraction is discussed in the light of the results obtained.     

亲水作用色谱柱与阳离子交换树脂柱结合分离无机离子（英文）

A combination of hydrophilic interaction chromatographic(HILIC) column and a weakly acidic cation-exchange resin(WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography(IC).Firstly,the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions.The columns used were SeQuant ZIC-HILIC(ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase(ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase(HILIC-10).When using tartaric acid as the eluent,the HILIC columns indicated strong retentions for anions,based on ion-pair interaction.Especially,HILIC-10 could strongly retain anions compared with ZIC-HILIC.The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I-> NO-3 > Br-> Cl-> H2PO-4.However,since HILIC-10 could not separate analyte cations,a WCX column(TSKgel Super IC-A/C) was connected after the HILIC column in series.The combination column system of HILIC and WCX columns could successfully separate ten ions(Na+,NH+4,K+,Mg2+,Ca2+,H2PO-4,Cl-,Br-,NO-3 and I-) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6.The relative standard deviations(RSDs) of analyte ions by the system were in the ranges of 0.02%-0.05% in retention times and 0.18%-5.3% in peak areas through three-time successive injections.The limits of detection at signal-to-noise ratio of 3 were 0.24-0.30 μmol/L for the cations and 0.31-1.2 μmol/L for the anions.This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.     

Comparison of the TEVA-Spec resin and liquid-liquid extraction methods for the separation of technetium in soil samples

When ICP-MS is used for⁹⁹Tc measurements, elements which interfere with⁹⁹Tc counting should be removed. In this study, a separation method using a novel chromatographic resin (TEVA·Spec^® resin) was compared with a liquid-liquid extraction (LLX) method for separation and concentration of⁹⁹Tc which was trapped in a solution after combustion of environmental soil samples. The results showed that Tc could be separated from Ru at high recoveries with both separation methods. Molybdenum, however, was not removed by LLX, while more than 99% of Mo in soil samples were removed by TEVA·Spec resin.     

Evaporation behavior of water and concentration of technetium and rhenium using thin film evaporator

The nuclear energy cycle requires the recycling of nuclear fuel, water, chemical reagents, and the volume reduction of radioactive liquid wastes. A fundamental technique for continuous recovery of water using a thin-film evaporator was examined. Appropriate recovery measurements were: an evaporator heat temperature of 323 K, a feed rate of 0.23 cm³s⁻¹, a vacuum pressure of 15 mmHg (2 kPa), and impeller rotational speeds of 500–600 rpm (min⁻¹). The concentration of trace technetium and rhenium in aqueous solutions was also studied. A decontamination factor of 10⁵ for rhenium was obtained.     

Separation of strontium from associated elements with selective specific resin and extraction chromatography

In this paper,separation of Sr from associated elements（Na,K,Ca,Mg,and Ba） was carried out using an extraction chromatographic column packed with Sr selective specific resin consisting of an octanol solution of 4,4’（5’）-bis（t-butylcyclohexo）-18-crown-6 sorbed on an inert polymeric support.Using 8.0 mol/L HNO₃ as the eluent,Ba and associated elements were eluted immediately from the column, whereas Sr was strongly retained.The adsorbed Sr could then be stripped from the column as the eluent was changed to 0.05 mol/L HNO₃.Complete Sr/Ba separation was demonstrated to be feasible in that Ba could be washed from the column leaving pure Sr by adequate rinsing with 8.0 mol/L HNO₃. Furthermore,matrix effect could be effectively eliminated and the selectivity of the method was improved.The method was applied for the determination of Sr in the high purity barium carbonate （BaCO₃） product and seawater.The recoveries of Sr in 2 samples were determined to be 93.2%and 109%, respectively.     

Development of a temperature-responsive agarose-based ion-exchange chromatographic resin

A temperature-responsive ion-exchange resin (ItBA) has been prepared by grafting poly(N-isopropylacrylamide-co-acrylic acid-co-tert-butylacrylamide; ItBA) onto cross-linked agarose. A carboxymethylated ion exchanger (CM) of similar charge density was also prepared. Maximum adsorption capacities (B_max) for lactoferrin at 20 °C and 50 °C were determined for both resins by batch adsorption procedures. Dynamic adsorption and desorption characteristics of the CM and ItBA with lactoferrin were established, as well as the ability of ItBA to selectively adsorb and desorb lactoferrin in the presence of other proteins. With the CM-agarose resin there was no significant difference between the B_max values obtained at 20 °C and 50 °C. However, for the agarose-based ItBA resin the B_max value at 50 °C was almost three times higher than the B_max value at 20 °C. Dynamically, lactoferrin adsorbed to the ItBA packed column at 50 °C with a significant proportion of the adsorbed lactoferrin desorbed by reducing the temperature to 20 °C. In addition, anionic proteins did not adsorb to the ItBA packed column, and did not interfere with the dynamic adsorption/desorption behaviour of lactoferrin. These results indicate that this new temperature-responsive agarose-based ItBA resin has potential for the fractionation of whey proteins, with good selectivity for cationic proteins.     

An improved extraction chromatographic resin for the separation of uranium from acidic nitrate media

The preparation and characterization of a new extraction chromatographic resin exhibiting extraordinarily strong retention of hexavalent uranyl ion over a wide range of nitric acid concentrations and very high selectivity for U(VI) over Fe(III) and numerous other cations is described. This new material (designated U/TEVA-2) comprises a novel liquid stationary phase consisting of an equimolar mixture of diamyl amylphosphonate (DA[AP]) and Cyanex 923^® (a commercially available trialkyl-phosphine oxide, TRPO) sorbed on silanized silica or Amberchrom CG-71. Cyanex 923 is shown to be preferable to a related TRPO, Cyanex 925^®, due to its lower viscosity and higher selectivity for U(VI) over Fe(III). The retention of uranyl nitrate by the U/TEVA-2 resin, as measured by the k′ values (number of free column values to peak maximum) is >5000 from approximately 0.1 to 8 M HNO₃. The ability of the new resin to strongly and selectively retain U(VI) from such a wide range of acid concentrations, along with its favorable physical properties, make it a good candidate for application in the separation and preconcentration of U(VI) from complex environmental, biological, and nuclear waste samples for subsequent determination.     

Separation preconcentration method for platinum and rhodium from environmental samples using a chelating resin

A method of determining trace levels of platinum and rhodium in different samples was investigated. The method involves separation and preconcentration of the platinum and rhodium from the matrix by flow injection (FI) on-line coupled with electrothermal atomic absorption spectrometry (ETAAS) with Zeeman effect background correction. Platinum and rhodium were adsorbed on a microcolumn packed with 1,5-bis(di-2-pyridyl)methylene thiocarbohydrazide immobilized on silica gel (DPTH-gel). The sorbed metals were directly eluted with nitric acid into the graphite furnace and determined by AAS.     

Separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt

Methods were developed for the separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt, Zephiramine. Tungsten was extracted into chloroform as an ion associate of tungsten(V)-thiocyanate complex and Zephiramine cation was retained on a column of Teflon powder coated with Zephiramine, but molybdenum(III) was neither extracted nor retained. The extraction chromatographic method was successfully applied to the determination of trace amounts of tungsten in molybdenum by neutron activation analysis.     

Separation and concentration of some platinum metal ions with a new chelating resin containing thiosemicarbazide as functional group

A new chelating ion-exchange resin containing thiosemicarbazide as functional group and based on macroreticular polystyrene-divinylbenzene (8%) has been prepared. Its sorption characteristics for palladium(II), platinum(IV), rhodium(III), ruthenium(III) and iridium(III) have been studied. These platinum metal ions can be quantitatively separated by sorption on this chelating resin and selective elution. The resin is highly stable in acid and alkaline solution.     

Characterization of an extraction chromatographic resin for the separation and determination of 36Cl and 129I

The monitoring of long-lived radionuclides is of great importance in the context of the surveillance of nuclear facilities, during their operation as well as during their decommissioning. This is especially true for radionuclides of rather volatile elements, such as chlorine and iodine, the main interest being in ³⁶Cl and ¹²⁹I. Liquid Scintillation Counting (LSC) is a widely used measurement technique especially for the determination of ³⁶Cl that requires a thorough and selective sample preparation in order to give accurate results. Sample preparation methods frequently employed such as volatilization and/or repeated precipitation steps can be rather elaborate and time consuming. Therefore, an attempt has been made to develop an ‘easy to use’ extraction chromatographic resin that allows extraction, and subsequent separation, of chloride and iodide from pretreated environmental and decommissioning samples for their determination via LSC. First results of the characterization of the resin including D _w values of Cl^?, I^? and potential interferents, and of the method development are presented as well as the result of the analysis of a simulated real sample.     

Rapid sequential separation of actinides using Eichrom's extraction chromatographic material

The presence of ²²⁶ Ra in an estuary formerly affected by direct discharges of waste from a phosphate fertilizer complex has been investigated. Specific activities ranging from 3.6 to 45.2 mBq/l have been detected. In general, activity levels are lower than those detected when direct discharges were carried out. However, there is still a clear contamination due to the disposal of phosphogypsum in open air piles by the river. Moreover, it seems that ²²⁶ Ra is being redissolved from the contaminated bed sediments, which also contributes to an enhancement in the activity levels of the estuary waters.     

Separation and determination of saturated very-long-chain free fatty acids in plasma of patients with adrenoleukodystrophy using solid-phase extraction and high-performance liquid chromatographic analysis

An improved method was developed for the isolation of very-long-chain free fatty acids (VLCFFAs) in plasma and their separation and determination by high-performance liquid chromatography (HPLC). The method includes sample clean-up using solid-phase extraction, fluorophoric labelling of the FFAs and reversed-phase HPLC separation. The solid-phase extraction was carried out with aminopropyl-bonded phase columns. The FFAs were then derivatized with 9-anthryldiazomethane (fluorescent) reagent and separated by HPLC on an RP-18 column with methanol as the mobile phase. Using this method, the concentrations of C20:0, C22:0, C24:0 and C26:0 were determined in the plasma of five adrenoleukodystrophy (ALD) patients, one obligatory heterozygote, four healthy male volunteers and one child with cerebral leukodystrophy but without any other ALD symptoms. Statistically significant differences were found in the levels of C24 and C26 and in the ratios C24/C22 and C26/C22 in ALD patients and in normal controls. The values were higher in patients with X-ALD. This method therefore provides a rapid and accurate procedure for the laboratory confirmation of X-ALD.     

Solvent extraction of technetium in urine with TBP

The solvent extraction of technetium from urine with TBP has been investigated. The distribution ratio of technetium was determined as a function of HCl concentration and reaction time. The distribution ratio in the HCl-TBP system containing urine is consistently lower than that without urine. The chemical forms of technetium in urine, analyzed by paper chromatography, indicated that pertechnetate was reduced in the presence of HCl and that the reduction of pertechnetate was enhanced by urine. The observed decrease in the distribution ratio was attributed to the enhanced reduction of pertechnetate by urine.     

Separation, recovery and recycling of a fluorous-tagged nickel catalyst using fluorous solid-phase extraction

Highly efficient separation, recovery and recycling of the fluorous-tagged catalyst, [Ni[F13C6C(O)CHC(O)C6F13]2], can be achieved with fluorous solid-phase extraction, after the Lewis acid catalysed synthesis of enaminodiones in conventional organic solvents.