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.
Determination of trace amounts of nitrogen in uranium based samples by ion chromatography (IC) without Kjeldahl distillation.
A simple, sensitive and fast ion chromatographic (IC) method with suppressed conductivity detection is described for the determination of traces of nitrogen in uranium based fuel materials. Initially a method was developed to determine nitrogen as NH4(+) using cation exchange column after matrix separation by Kjeldahl distillation. The method was then improved by eliminating this distillation. Matrix separation after sample dissolution was done by hydrolyzing and filtering off the polyvalent cations. This had helped in reducing both the sample size and analysis time. Optimization of dissolution conditions for various kinds of uranium based samples was done to keep acid content minimum; a prerequisite chromatographic condition. The calibration plot for nitrogen was linear in the concentration range of 0.02-1 mg L(-1) with regression coefficient of 0.9999. The relative standard deviation (R.S.D.) obtained in this method (100 microL injected) was 3% and 2% in 9 replicates at nitrogen level of 28 and 55 ng g(-1), respectively. Detection limit based on S/N=3 (100 microL injected) as well as three times of variation in blank value was 4 ng g(-1). The developed method was authenticated by comparison with certified uranium-alloy standard as well as with independent indophenol photometry method. The developed method was applied to uranium-alloy, uranium-metal, sintered UO2 pellets and sintered UO2 microspheres samples.
Influence of the elemental composition of zircon and collophane minerals on their electrical conductivity
Abstract During high-tension electrostatic separation of zircon and collophane from other impurity minerals, it was noticed that different varieties of both minerals was separated at different conditions. Detailed electrical conductivity measurements had been carried out to elucidate the presence of the different varieties of these minerals. It was found that there are three varieties of zircon and collophane minerals having different conductivity values. Complete elemental analysis applying ED-XRF technique ensured the difference in the elemental composition of the varieties of both minerals. The variations in the behaviour is found to be a function of the type and concentration of the presented impurity elements. The presence of Zn, Fe, Si, Mn, Ti and Y in low concentration levels in collophane increases its conductivity. In case of zirconm it was noticed that the presence of these elements in addition to Ca, U, Th, Hf and Nd in high concentration levels improves its conductivity.