Publication Details

Category Text Publication
Reference Category Journals
DOI 10.1016/S0039-9140(03)00041-9
Title (Primary) Simultaneous determination of zirconium and hafnium as ternary complexes with 5-Br-PADAP and fluoride using solid-phase extraction and reversed-phase liquid chromatography
Author Oszwaldowski, S.; Jakubowska, J.
Source Titel Talanta
Year 2003
Department BOOEK
Volume 60
Issue 4
Page From 643
Page To 652
Language englisch
Keywords Determination of Hf(IV) and Zr(IV); 2-(5-Bromo-2-pyridylazo)-5-diethylamino-phenol; Solid-phase extraction; Liquid chromatography
Abstract

Solid-phase extraction (SPE) along with reversed-phase liquid chromatography (RP-LC) was used for the simultaneous determination of Zr(IV) and Hf(IV) by means of their ternary chelates with fluoride and 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP). The conditions of SPE sorption were examined in detail: type of SPE column, volume of the sample, volume of the eluent, concentrations of metal ions, fluoride salt, chromogenic reagent, organic phase, and pH. It was established that the sorption of Zr(IV) and Hf(IV), as their ternary chelates, on SPE Zorbax SPE C18 (EC) cartridge was the most efficient, when the sample containing metal ion (Zr(IV), Hf(IV), both, up to 2 mug), 5-Br-PADAP 1.5 x 10(-4), NaF 7.5 X 10(-5) Mol l(-1), methanol 40%, pH 4.5+/-1 was applied for the SPE sorption. The chelates were discarded from SPE cartridge using acetonitrile/water (99.75+0.25, v/v) eluent containing 3.8 x 10(-4)mol, l(-1) sodium fluoride and subsequently separated by RP-LC method. The RP-LC separation of both chelates was optimized and Zorbax SB-C18 analytical LC column along with acetonitrile/water (65+35, v/v) eluent containing the 1.5 X 10(-4) mol l(-1) sodium fluoride was used. The established SPE/LC conditions allow Zr(IV) 0.08-2.0 mug and Hf(IV) 0.04-2.0 mug determination in a sample volume up to 150 ml. The detection limits, 0.03 mug Hf(IV) and 0.05 mug Zr(IV), were obtained. Recoveries, (94+/-2)% for Hf(IV) chelate and (106+/-2)% for Zr(IV) chelate were obtained, when 1 mug of Zr(IV) and Hf(IV) ions were determined by the present SPE/LC method from the sample volume of 100 ml. The established, pre-concentration SPE conditions, along with the LC separation and determination allow the assay of Zr(IV) and Hf(IV) in complicated matrix materials. The present SPE/LC method was applied to the determination of Zr(IV) and Hf(IV) in tap water and reference geological material (rock, NCS DC 73303; certified content: Zr, 27.7 x 10(-3)% (w/w) and Hf, 6.5 x 10(-4)% (w/w)).
Persistent UFZ Identifier https://www.ufz.de/index.php?en=20939&ufzPublicationIdentifier=5110
Oszwaldowski, S., Jakubowska, J. (2003):
Simultaneous determination of zirconium and hafnium as ternary complexes with 5-Br-PADAP and fluoride using solid-phase extraction and reversed-phase liquid chromatography
Talanta 60 (4), 643 - 652 10.1016/S0039-9140(03)00041-9