High-performance liquid chromatographic-spectrophotometric determination of copper(II) and palladium(II) with 5,10,15,20-tetrakis(4N-pyridyl)porphinefollowing homogeneous liquid-liquid extraction in the water-acetic acid-chloroform ternary solvent system

The homogeneous liquid-liquid extraction method based on the pH dependent p hase-separation phenomenon was studied in the water-acetic acid-chloroform ternary solvent system. The optimum conditions were determined as follows, i.e. in order to obtain a water-immiscible small phase (approximately 50 mu l) of chloroform, sodium hydroxide ([NaOH](T) = 1.29 M) was added to a homo geneous aqueous solution which consisted of water, chloroform (0.2 ml, 0.57 vol.%) and acetic acid (2 ml, 5.71 vol.%), where the final total volume wa s 35 ml. During the extraction of the 5,10,15,20-tetrakis(4N-pyridyl)porphi ne (TPyP), Cu(II)- and Pd(II)-TPyP complexes, when the volume ratio (V-W/V- O) between the water phase and organic phase was 700, the distribution rati o (D) and extraction percentage (E%) were TPyP (5600, 88.9%), Cu(II)-TPyP ( 6000, 90%) and Pd(II)-TPyP (6700, 91%), respectively. This extraction metho d was applied to the HPLC system. The calibration graphs were linear and pa ss through the origin over the concentration range of 2 x 10(-8)-4 x 10(-7) M for Cu(II) and 5 x 10(-8)-8 x 10-7 M for Pd(II). The relative standard d eviations for the central value of the calibration graph were 3.2% for Cu(I I) and 3.7% for Pd(II) (10 determinations). Moreover, the detection limits (S/N = 3) were 5 x 10(-9) M for Cu(II) and 8 x 10(-9) M for Pd(II). (C) 200 0 Elsevier Science B.V. All rights reserved.