Separation and quantification of 238U, 232Th and rare earths in monazite samples by ion chromatography coupled with on-line flow scintillation detector.
An alternative procedure has been described for efficient separation and quantitative determination of uranium (U), thorium (Th) and rare earth elements (REEs) in monazite mineral by high performance ion chromatographic system (IC). Different variables affecting the distribution coefficient, the retention and hence separation efficiency such as eluent flow rate and concentrations of HCI and ammonium sulfate (NH4)2SO4 containing the mobile phase were studied. The developed separation protocol of U, Th and REEs was optimized using an Ion Pac CS5 separation column followed by post-column derivatization reaction with Arsenaso III and UV-VIS spectrophotometric detection. Comparative evaluation of U, Th and REEs concentration in monazite mineral was demonstrated using two different on-line detection modes including flow through cell scintillation detector (FSD) and UV-VIS spectrophotometer. Response of the FSD was found to be linear over the full range of activities investigated (4-100 Bq). The lower limits of detection (LLD) for the investigated radionuclides were 3.0+0.1 Bq for 238U and 6.0 +/- 0.1 Bq for 232Th. The detection of 238U and 232Th by FSD shows good agreement with the corresponding determination by UV-VIS spectrophotometer. The content of ThO2 and U3O8 in monazite sample were found to be 4.7 +/- 0.1% and 0.42 +/- 0.04% using UV-VIS detector and 4.3 +/- 0.1% and 0.45 +/- 0.1% using FSD, respectively.
Simultaneous spectrophotometric determination of uranium and thorium by flow injection analysis using selective masking.
A flow injection system for the simultaneous determination of uranium and thorium has been developed by using selective masking and a spectrophotometric detector with two flow cells aligned with the same optical path. The injected sample solution was first mixed with a reagent solution containing Chromazurol S (CAS) and cetyltrimethylammonium chloride (CTMAC), and the total absorbance of uranium- and thorium-CAS complexes was measured in the first flow cell at 620 nm. The sample stream was then mixed with an EDTA solution in order to convert the thorium-CAS complex to a thorium-EDTA complex, and the absorbance of the uranium-CAS complex was measured in the second flow cell. The detection limits were 10 microg dm(-3) for uranium and 7 microg dm(-3) for thorium. The calibration graphs were linear (r < 0.9998) at least over the ranges of 0.1 to 10 mg dm(-3) for uranium and 0.08 to 8 mg dm(-3) for thorium. The RSDs were less than 1.5% (n = 3) in the calibration range. Uranium and thorium of up to the 6-fold concentration to each other could be determined in admixtures with relative errors of less than 3.3%. The sample throughput was 24 per hour. The proposed system was successfully applied to the analysis of a uranium-thorium ore mock solution by coupling with anion-exchange in a magnesium nitrate medium to eliminate interference from coexisting elements.
Dynamic ion exchange chromatography for determination of number of fissions in thorium-uranium dioxide fuels
High-performance liquid chromatography and the use of /sup 138/La as a fission monitor have been examined for the determination of the number of fissions and burnup in (Th, U)O/sub 2/ fuels. The fission product /sup 139/La in a solution of irradiated fuel was separated on a reversed phase dynamically modified with 1-octanesulfonate, and the eluted metal ions were monitored by an ''on-line'' postcolumn reaction system. The relative standard deviation of the peak heights for lanthanum in 13 fuel solutions over a 1 month period was 0.96%, and the agreement between the HPLC burnup results and those obtained by standard mass spectrometric techniques was within 0.1%; the largest source of uncertainty for the determination of the number of fissions was that associated with fission yield values. Other uses of this chromatographic system were also examined briefly. 24 references, 3 figures, 1 table.