Determination of trace amounts of nitrogen in uranium based samples by ion chromatography (IC) without Kjeldahl distillation

Abstract

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 NH 4 + 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 μL 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 μL 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 UO 2 pellets and sintered UO 2 microspheres samples.