This paper outline a new, simple, selective and sensitive spectrophotometric procedure for the quantitative determination of iron. The bidentate ligand of 2- (1-Acetyl-2-oxopropyl)acrylonitrile has been synthesized ,and determined by elemental analysis and infrared spectroscopy. The compound reacts with Fe(III) to form a colored complex with an absorption maxima at 400nm and 490nm. The effect of pH, amount of reagent, time, temperature and the interference of many ions on the Fe (III) determination was also estimated. Beer's law is obeyed for iron concentration in the range (0.23- 4.48μg/ ml) for spectrophotometric method and (0.56-8.4) for extraction spectrophotometric method. The molar absorptivity was in the rang 2.70x104-3.46 x 104 L.mol-1cm-1. Sandall's sensitivity was found to be 1.61 x 10 -3 – 2.07 x 10-3 μg . cm-2. The RSDs for both spectrophotometric and extraction spectrophotometric methods were below 3%. The analytical error SD/√n was within 0.021. The technique has been applied to the determination of iron in alloys and in pharmaceutical preparations.