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A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of iron(II) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of iron(II) as 2,3-dichloro-6-(3-carboxy-2-hydroxy-1-naphthylazo)quinoxaline on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed iron(II) complex is measured directly at 743 and 830nm. Iron(III) was determined by difference measurements after reduction of iron(III) to iron(II) with hydroxylamine hydrochloride. Calibration is linear over the range 1.0–20μgL⁻¹ of Fe(II) with relative standard deviation (R.S.D.) of 1.65% (n=10.0). The detection and quantification limits for 100mL sample system are 280 and 950ngL⁻¹ using 0.5g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 2.86×10⁶Lmol⁻¹cm⁻¹ and 0.0196ngcm⁻² …