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Spectrophotometric Determination of Iron

Spectrophotometric Determination of Iron

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Published by: Dozdi on Apr 13, 2010
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Analytical Chemistry Laboratory 2
Spectrophotometric Determination of Iron
 Mr. ***** 
 Department of Chemical Engineering and Chemistry, Mapua Institute of Technology
A complex of iron (II) in the water sample was formed with 1,10-phenanthroline,Fe(C
and the absorbance of this colored solution is measured with a spectrophotometer.The volume reading was recorded at 7.0271 mL. The spectrum was plotted to determine theabsorption maximum. Hydroxylamine (as the hydrochloride salt to increase solubility) was addedto reduce any Fe
to Fe
and to maintain it in that state.
The main purpose of thisexperiment is to determine the amount of iron in the given sample from reading itsabsorbance by using a spectrophotometer. Aseries of solutions with differentconcentration will be measured to establish acalibration curve.
The spectrophotometer is a simpleinstrument for measuring the amount of light transmitted through solutions. It has adiffraction grating that can be used to adjustthe wavelength of light transmitted. Ingeneral the light used should be thecomplimentary color of the solution beingtested. The amount of light at a givenwavelength that a sample absorbs is oftendirectly proportional to the concentration of the absorbing species in the sample and tothe distance (path length) the light musttravel through the sample.Iron is a stable ion. It forms anintense red colored compound withorthophenanthroline solution, and is the basis for its determination. Since thesolutions are reddish orange, a blue-greenwavelength of light (508) should be selectedfor the spectrophotometer.Chemically, iron is an active metal.It combines with the halogens (fluorine,chlorine, bromine, iodine, and astatine),sulfur, phosphorus, carbon, and silicon. Itdisplaces hydrogen from most dilute acids.It burns in oxygen to form ferrosoferricoxide, Fe3O4. When exposed to moist air,iron becomes corroded, forming a reddish- brown, flaky, hydrated ferric oxidecommonly known as rust. The formation of rust is an electrochemical phenomenon inwhich the impurities present in iron form anelectrical “couple” with the iron metal. Asmall current is set up, water from theatmosphere providing an electrolyticsolution. Water and soluble electrolytes suchas salt accelerate the reaction. In this processthe iron metal is decomposed and reactswith oxygen in the air to form rust. Thereaction proceeds faster in those placeswhere rust accumulates, and the surface of the metal becomes pitted
Preparation of the Calibration Curve
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
+ 3phenH
+ 3H
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:
V (mL)Absorbance
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.

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