Abstract
A method was developed for rapid separation and determination of iron by employing capillary zone elec-trophoresis (CZE) technique with direct UV detection. Iron could be separated from matrix uranium by di-rect injection of dissolved sample solution into capillary using a mixture of 10 mM HCl and 65 mM KCl (pH = 2) as background electrolyte (BGE) at an applied voltage of 15 kV. The developed method has a very high tolerance for the matrix element U (100 mg/mL) and as such may not need prior separation of iron from the matrix. Iron could be separated with better than 95% recovery. The method showed a linear calibration over a concentration range 1-50 ppm of Fe. The migration times for the iron peak were reproducible within 1% for both pure Fe(III) and in presence of matrix uranium (80 mg/mL). The precision (RSD, n = 22) of peak area obtained for 1ppm of iron was 3.5%. The limit of detection (LOD) (3 ) was 0.1 ppm and the ab-solute LOD was 9 × 10-14 g considering the sample injection volume of 1.5 nL. The developed method has been validated by separating and determining iron in two certified reference materials of U3O8. The method was applied for the determination of iron in different uranium based nuclear materials. The CZE method is versatile for routine analysis as it is simple, rapid and has simple sample preparation procedure.
Highlights
A method was developed for rapid separation and determination of iron by employing capillary zone electrophoresis (CZE) technique with direct UV detection
Iron could be separated from matrix uranium by direct injection of dissolved sample solution into capillary using a mixture of 10 mM HCl and 65 mM KCl as background electrolyte (BGE) at an applied voltage of 15 kV
Separation and determination of trace elements in nuclear materials is important in nuclear industry as their performance in the reactor critically depends on their purity [1]
Summary
Separation and determination of trace elements in nuclear materials is important in nuclear industry as their performance in the reactor critically depends on their purity [1]. Analysis of a matrix-matched reference material every time along with samples is indispensable to confirm the quantitative recovery of iron This necessitates a simple, reliable, rapid and specific method to minimize the labour involved and to achieve maximum sample throughput. The second approach provides the complete pre-capillary or on- capillary conversion of metal ions into stable, charged complexes, which can move with different mobilities depending on their charge, size and stability [29]. It is worth mentioning that while separating the metal-aminocarboxylic acid anionic complexes, it would be difficult to achieve a large separation factor to overcome the problem of peak masking In these methods higher pH electrolyte media (typically pH 6-10) are used for the effective coating of CTAB on the capillary surface and subsequent formation of double layer necessary for reversing the EOF. Interferences from other metal cations can be eliminated due to the anionic complex formation with chloride ligand
Sign-in/Register to view highlights & summary Sign-in/Register to access full text options 
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
