25 mL of the standard iron solutionwas transferred to a 100-mL volumetricflask, and 25 mL of distilled water to asecond 100-mL volumetric flask. To them, 1mL of hydroxylamine, 10 mL of sodiumacetate, and 10 mL of orthophenanthrolinewere added to each flask. The mixtures wereallowed to stand for 5 min; diluted to themark and mixed.A pair of matched cells for theinstrument was cleaned. Each cell wasrinsed with at least three portions of thesolution it is to contain. The absorbance of the standard was determined with respect tothe blank.This procedure was repeated withfive other volumes of the standard ironsolution (1, 5, 15, 35, and 45 mL).Determination of Iron10 mL of the unknown wastransferred to a 100-ml volumetric flask;treated in the exact same way as thestandards and the absorbance was measuredwith respect to the blank. The volume of unknown taken to obtain absorbancemeasurements for replicate samples arewithin the range of the calibration curve wasaltered.
Spectrophotometer is an instrumentused to measure the intensity of wavelengthsin a spectrum of light compared with theintensity of light from a standard source.
The red-orange complex that forms between iron (II) and 1,10-phenanthroline(orthophenanthroline) is useful indetermining iron in water supplies. Thereagent is a weak base that reacts to form phenanthrolinium ion, phenH
, in acidicmedia. Complex formation with iron is thus best described by the equation:Fe
Iron (II) is quantitatively complexedin the pH range between 3 and 9. A pH of about 3.5 is ordinarily recommended to prevent precipitation of iron salts, such as phosphates. An excess of a reducing reagent,such as hydroxylamine, was needed tomaintain iron in the +2 oxidation state. Thecomplex, once formed, is very stable.The determination was performedwith a spectrophotometer set at 508 nm andthe data were obtained as shown:
1 0.02805 0.073115 0.347825 0.440035 0.767945 0.9901Unknown 0.1299
The volume of the unknown sample# 4 was 7.0271 mL, computed by using themethod of linear regression.
Spectophotometers are a vital andnecessary instrument in quantitativeanalysis. In this experiment the volume of iron in the given solution was determinedusing this technology. The result obtainedusing the calibration curve was 7.0271 mL.Several reagent were added to the sample tomaintain its stable state throughout the procedure.
1. Christian, G.D., Analytical Chemistry, 6
edition. New Jersey. John Wiley, 2004.