Separation and determination of metallocyanide complexes of Fe(II), Ni(II) and Co(III) by ion-interaction chromatography with membrane suppressed conductivity detection applied to analysis of oil refinery streams (sour water)

A separation and determination method for the analysis of cyanometallic complexes of Fe(II), Ni(II) and Co(III) was developed to be applied to the analysis of petroleum refinery streams (sour water). Ion-interaction chromatography was used employing an analytical column IonPac NS1 10 microm and a chromatographic system ICS 2500 equipped with a membrane conductivity suppression ASRS ultra 4mm, both supplied by Dionex Corporation. The mobile phase was composed of 2 mmol l(-1) TBAOH, 1 mmol l(-1) Na(2)CO(3), 0.1 mol l(-1) NaCN and ACN (77:23, v/v), flowing at 0.7 ml min(-1). At the optimized conditions, detection limits estimated by the calibration curve parameters and relative standard deviation were: 0.002 mg CNl(-1) and 3.1% for Fe(CN)(6)(4-); 0.003 mg CNl(-1) and 2.5% for Ni(CN)(4)(2-) and 0.003 mg CNl(-1) and 2.8% for Co(CN)(6)(3-). Sour water samples without any pretreatment (except membrane filtration) from a petroleum refinery in Brazil were analyzed successfully by external calibration method.