Department of Analytical Chemistry, Faculty of Chemistry, Warsaw University of Technology, ul. Noakowskiego 3, 00-664 Warsaw, Poland.
Talanta. 2002 Oct 16;58(4):773-83.
The formation of Fe(III) and Fe(II) chelates with pyridylazo and thiazolylazo reagents was examined. Optimum conditions for the formation of Fe(III) and Fe(II) chelates with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) were in detail evaluated. The LC method for simultaneous separation of Fe(III) and Fe(II) ions as 5-Br-PADAP chelates was evaluated using the PEEK column with C18 e.c. stationary phase and acetonitrile+water (90:10, v/v) eluent containing the 1x10(-3) mol l(-1) C(12)H(25)SO(3)Na, the ion-pairing reagent, pH 3.4-3.6. The simultaneous determination of 20-500 mug l(-1) Fe(II) ions (detection at 555 nm) and 20-500 mug l(-1) Fe(III) ions (detection at 585 nm) as 5-Br-PADAP chelates (for both ions, detection limit, 18 mug l(-1) for 20 mul loop) was established. The chromatographic method was applied to the water analysis. Although the present method is able to determine both Fe(III) and Fe(II) ions, the Fe(III) ion was not detected in all water samples. The Fe(II) was detected only in fresh gathered oligocene water at the level of 135 mug l(-1). The present method was used to the investigation of the distribution of Fe(III)/Fe(II) ions in aqueous and micellar solutions after action of external, ultrasonic field.
研究了吡啶偶氮和噻唑偶氮试剂与 Fe(III)和 Fe(II)形成螯合物的情况。详细评价了 2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)与 Fe(III)和 Fe(II)形成螯合物的最佳条件。采用 PEEK 柱和 C18 e.c.固定相,以乙腈+水(90:10,v/v)为流动相,其中含有 1x10(-3)mol l(-1)C(12)H(25)SO(3)Na(离子对试剂),pH 3.4-3.6,评价了同时分离 Fe(III)和 Fe(II)离子作为 5-Br-PADAP 螯合物的 LC 方法。同时测定了 20-500µg l(-1)Fe(II)离子(555nm 检测)和 20-500µg l(-1)Fe(III)离子(585nm 检测)(均为 5-Br-PADAP 螯合物,检测限为 20µl 环时 18µg l(-1))。该色谱方法应用于水样分析。尽管该方法能够同时测定 Fe(III)和 Fe(II)离子,但在所有水样中均未检测到 Fe(III)离子。仅在新鲜采集的始新世水中检测到 Fe(II),浓度为 135µg l(-1)。本方法用于研究外加超声场作用下水溶液和胶束溶液中 Fe(III)/Fe(II)离子的分布。