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Detection of metal ions by liquid chromatographic separation of their 1,3-dimethyl-4-acetyl-2-pyrazolin-5-one chelates

Journal Article · · Anal. Chem.; (United States)
DOI:https://doi.org/10.1021/ac00171a017· OSTI ID:6481064

Metal ions are determined by adding 1,3-dimethyl-4-acetyl-2-pyrazolin-5-one (DMAP) to an aqueous sample and then separating the metal chelates by direct injection onto a liquid chromatographic column. Separations on a C-18 silica column and a polystyrene-divinylbenzene column are compared, with a better separation seen on the polymeric column. It is found that the most efficient separations are seen at pH 5 with an acetic acid buffer. Separations of metal-DMAP complexes using different organic modifiers are compared. Good separations using acetonitrile and tetrahydrofuran are seen, and an inversion of retention is seen in tetrahydrofuran. Several metal ions can be separated and quantified; separation conditions, linear calibration curve ranges, and detection limits are presented for Fe(III), U(VI), Ga(III), and Cu(II). Interferences due to the presence of other ions in solution are investigated. Finally a method for selectively determining uranium with postcolumn reactor detection using Arsenazo I is presented.

Research Organization:
Iowa State Univ., Ames (USA)
DOE Contract Number:
W-7405-ENG-82
OSTI ID:
6481064
Journal Information:
Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 60:20; ISSN ANCHA
Country of Publication:
United States
Language:
English