Analytical Sciences

Abstract − Analytical Sciences, 37(8), 1111 (2021).

A Direct Non-destructive Method for Determination of Sulfur in Ore Samples Using EDXRF Spectrometry
Buddhadev KANRAR,*,** S. Sanjay KUMAR,* S. MONDAL,*** N. L. MISHRA,* and Sangita DHARA*,**
*Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai, 400085, India
**Homi Bhabha National Institute, Anushakti Nagar, Mumbai, 400094, India
***Materials Processing and Corrosion Engineering Division, Bhabha Atomic Research Centre, Mumbai, 400085, India
A method has been developed for direct non-destructive energy dispersive X-ray fluorescence (EDXRF) determination of sulfur in solid uranium ores and intermediates, obtained from the alkaline recovery process for uranium from its ores. The method involves thorough grinding of a few mg of solid powder samples to fine particle size and mixing the fine powder thus obtained with a few drops of 10% collodion solution in amyl acetate to make a paste. A very small amount of this paste was transferred with the help of the pestle tip, spread uniformly in the form of thin slurry on Mylar films, and dried to make very thin sample specimens on thin Mylar film supports. These specimens were presented for EDXRF measurements. A calibration plot was made by plotting the intensity ratios of S Kα and Rayliegh scattered peak of the excitation source (Ge Kα) against sulphur percent in the certified reference materials (CRMs). It was found that the precision obtained using this methodology was within 5% (±1σ) and the deviation of the EDXRF analytical results from the expected values of CRM was within 7%. The developed method was successfully applied for the determination of sulfur in the samples obtained from the different stages of the uranium ore processing using alkaline based leaching method.