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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(C12H8N2)32+ 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 the
absorption maximum. Hydroxylamine (as the hydrochloride salt to increase solubility) was added
to reduce any Fe3+ to Fe2+ and to maintain it in that state.

basis for its determination. Since the


Objective solutions are reddish orange, a blue-green

The main purpose of this wavelength of light (508) should be selected


experiment is to determine the amount of for the spectrophotometer.
iron in the given sample from reading its Chemically, iron is an active metal.
absorbance by using a spectrophotometer. A It combines with the halogens (fluorine,
series of solutions with different chlorine, bromine, iodine, and astatine),
concentration will be measured to establish a sulfur, phosphorus, carbon, and silicon. It
calibration curve. displaces hydrogen from most dilute acids.
It burns in oxygen to form ferrosoferric
Discussion oxide, Fe3O4. When exposed to moist air,
iron becomes corroded, forming a reddish-
Overview brown, flaky, hydrated ferric oxide
commonly known as rust. The formation of
The spectrophotometer is a simple rust is an electrochemical phenomenon in
instrument for measuring the amount of which the impurities present in iron form an
light transmitted through solutions. It has a electrical “couple” with the iron metal. A
diffraction grating that can be used to adjust small current is set up, water from the
the wavelength of light transmitted. In atmosphere providing an electrolytic
general the light used should be the solution. Water and soluble electrolytes such
complimentary color of the solution being as salt accelerate the reaction. In this process
tested. The amount of light at a given the iron metal is decomposed and reacts
wavelength that a sample absorbs is often with oxygen in the air to form rust. The
directly proportional to the concentration of reaction proceeds faster in those places
the absorbing species in the sample and to where rust accumulates, and the surface of
the distance (path length) the light must the metal becomes pitted
travel through the sample.
Iron is a stable ion. It forms an Methodology
intense red colored compound with
orthophenanthroline solution, and is the Preparation of the Calibration Curve
25 mL of the standard iron solution (orthophenanthroline) is useful in
was transferred to a 100-mL volumetric determining iron in water supplies. The
flask, and 25 mL of distilled water to a reagent is a weak base that reacts to form
second 100-mL volumetric flask. To them, 1 phenanthrolinium ion, phenH+, in acidic
mL of hydroxylamine, 10 mL of sodium media. Complex formation with iron is thus
acetate, and 10 mL of orthophenanthroline best described by the equation:
were added to each flask. The mixtures were
allowed to stand for 5 min; diluted to the Fe2+ + 3phenH+ ↔ Fe(phen)32+ + 3H+
mark and mixed.
A pair of matched cells for the Iron (II) is quantitatively complexed
instrument was cleaned. Each cell was in the pH range between 3 and 9. A pH of
rinsed with at least three portions of the about 3.5 is ordinarily recommended to
solution it is to contain. The absorbance of prevent precipitation of iron salts, such as
the standard was determined with respect to phosphates. An excess of a reducing reagent,
the blank. such as hydroxylamine, was needed to
This procedure was repeated with maintain iron in the +2 oxidation state. The
five other volumes of the standard iron complex, once formed, is very stable.
solution (1, 5, 15, 35, and 45 mL). The determination was performed
with a spectrophotometer set at 508 nm and
Determination of Iron the data were obtained as shown:
10 mL of the unknown was
transferred to a 100-ml volumetric flask; V (mL) Absorbance
treated in the exact same way as the 1 0.0280
standards and the absorbance was measured 5 0.0731
with respect to the blank. The volume of 15 0.3478
unknown taken to obtain absorbance 25 0.4400
measurements for replicate samples are 35 0.7679
within the range of the calibration curve was 45 0.9901
altered. Unknown 0.1299

Instrumentation The volume of the unknown sample


# 4 was 7.0271 mL, computed by using the
method of linear regression.

Conclusion

Spectophotometers are a vital and


necessary instrument in quantitative
analysis. In this experiment the volume of
iron in the given solution was determined
using this technology. The result obtained
using the calibration curve was 7.0271 mL.
Spectrophotometer is an instrument Several reagent were added to the sample to
used to measure the intensity of wavelengths maintain its stable state throughout the
in a spectrum of light compared with the procedure.
intensity of light from a standard source.
References
Interpretation
1. Christian, G.D., Analytical Chemistry, 6th
The red-orange complex that forms edition. New Jersey. John Wiley, 2004.
between iron (II) and 1,10-phenanthroline
2. Filby, G. “Spreadsheets for Chemists,”
VCH Publishers, New York, 1995, p. 210.

3. Schwartz, L.M. “Advances in Acid-Base


Gran Plot Technology,” J. Chem. Educ., 64,
947-950 (1987).