Rapid Separation and Quantification of Iron in Uranium Nuclear Matrix by Capillary Zone Electrophoresis (CZE)

Abstract

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 (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(III). 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 1 ppm of iron was 3.5%. The limit of detection (LOD) (3) was 0.1 ppm and the absolute 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 U 3 O 8 . 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.

Online spectrophotometric determination of Fe(II) and Fe(III) by flow injection combined with low pressure ion chromatography

“…applied in Fe speciation, e.g. ICP-AES method [12], capillary electrophoresis with ultraviolet detection method [13], flame atomic absorption spectrometry [14], ion selective membrane potentiometric sensor [15], combination of sequential injection analysis and flame atomic absorption spectrometry [16,17], microcolumn ion chromatography with UV-Vis detection [18] as well as combination post-column derivatization HPLC or flow injection technique method and visible absorbance detection [3,13,16] were also reported. Regarding these spectrophotometric methods, iron has been determined using, e.g.…”

“…Regarding these spectrophotometric methods, iron has been determined using, e.g. phenanthroline [1], resorcylic acid [3], solochrome yellow 2GS [5], 8-hydoxyquinoline [6], di-2-pyridyl ketone benzoylhydrazone (DPKBH) [7], 1,10-phenanthroline [13], 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine (PDT) [10] or cetylpyridinium chloride [8] as reagents. Some of the proposed methods are based on determination of one form of the iron and/or the total iron, concentration of the other analyte is then calculated by subtracting the concentration of the concentration found for the total iron.…”

Spectrophotometric and Fluorometric Methods for the Determination of Fe(III) Ions in Water and Pharmaceutical Samples

“…2 As a result, Fe(III) detection or sensing is critical for biological and environmental issues. 3 Many traditional analytical techniques were used in Fe determination, e.g., ICP-AES method, 4 ion-selective membrane potentiometric sensor, 5 flame atomic absorption spectrometry, 6 and the combination of ultraviolet detection and capillary electrophoresis method, 7 Also, UV−vis detection and microcolumn ion chromatography, 8 as well as atomic absorption spectrometry after solid-phase extraction, 9 were also reported. When compared to alternative techniques like luminescence spectroscopy, these procedures are costly, are time-consuming, and need pretreatment or preconcentration.…”