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SPECTROPHOTOMETRIC DETERMINATION OF IRON IN

AQUEOUS SOLUTIONS AS A COMPLEX OF 1,10PHENANTHROLINE


J.K.UY1 AND A.F.D. FIDELES2
1
DEPARTMENT OF MINING METALLURGICAL AND MATERIALS ENGINEERING, COLLEGE OF
ENGINEERING
2
DEPARTMENT OF FOOD SCIENCE AND NUTRITION, COLLEGE OF HOME ECONOMICS
UNIVERSITY OF THE PHILIPPINES, DILIMAN, QUEZON CITY, PHILIPPINES
DATE PERFORMED: NOVEMBER 30, 2014
INSTRUCTORS NAME: MARIEL CLORES

DISCUSSION
What are the basic principles of Beers law?
Beers law relates the absorbance of a species to its concentration and
absorptivity. Its general form is:
A=abc
where: A = absorbance
a = absorptivity constant
b = path length of radiation
c = concentration of the species
It is used to find out the concentration of an unknown species by utilizing a
spectrophotometer to measure the absorbance of the species. Normally, measuring
the absorbance of known concentrations and then using the information to find the
actual concentrations of the unknown solutions to create a calibration curve.
Why is Beers law expressed in terms of absorbance instead of transmittance?
Its simply because there is a linear relationship when it comes to the
absorbance and concentrations of species. This way, it is easier to use in
experiments.
What are the limitations of Beers law?
The relationship between the concentration and absorbance of species at
higher concentrations no longer exhibit a linear relationship. This makes it difficult
to create a relationship between them. Additionally, should the reactions of the
species not proceed to completion, the absorbance will be greatly affected.
What is the significance of spectral scanning?
Spectral scanning simply determines the wavelength at which the species
absorbs the most. This is important since certain substances react differently at
different wavelengths.
What is the reaction between iron and hydroxylamine hydrochloride?

4Fe3+ + 2NH2OHHCl 4Fe2+ + N2O + 4H+ + H2O

What is the absorbing species and the spectral region at which the complex
strongly absorbs?
The absorbing species is Fe(C12H8N2)32+. It strongly absorbs at around 510nm.
What is the significance of following the sequence of addition of reagents?
Adding the hydroxylamine hydrochloride first is important since it will be the
one to reduce the Fe3+ to Fe2+. Failure to do so will make less Fe2+ available to react
with the 1,10-phenanthroline.
What is the importance of the calibration procedure?
Creating the calibration curve shows the molar absorptivity of the species.
Additionally, using the solution with highest concentration will give us max which will
be the wavelength all the succeeding readings will be done at.
What is the importance of adding phenanthroline in excess?
This ensures that the reaction proceeds to completion, in that all the Fe 2+ will
create the absorbing species and only that will create the measured absorbance
reading.
What are the requirements for a species to be analyzed using the
spectrophotometric method?
First, the species must be colored. Second the concentrations of the species
must not be too high due to the limitations of Beers law. Third, that the
spectrophotometer used contains in its range the max of the species.
What is the importance of determining max and the baseline?
Measurements at max show minimal deviation from the linear relationship
between the concentration and absorbance. This in turn creates more accurate
measurements and calculations. The baseline is created by using a blank
reference cell. In this experiment, the blank reference cell used contained all the
substances added to the analyzed solution except the analyte. This acts as a base
cell to subtract all other absorbing species that may be formed aside from the
absorbing species in question.
What are the possible sources of error?
Since the preparation of solutions was done in a different room as the
measurement, the temperature difference may have played a role in the reaction
between the species. Also, an incomplete reaction between the Fe 2+ and
phenanthroline may have created a lower absorbance reading.
References:
[1]
Spectrophotometry.
http://www.chm.davidson.edu/vce/spectrophotometry/beerslaw.html (accessed

November 5, 2014)
[2]
Ultraviolet-Visible (UV-Vis) Spectroscopy Limitations and Deviations of BeerLambert Law.
http://pharmaxchange.info/press/2012/05/ultraviolet-visible-uv-vis-spectroscopy%E2%80%93-limitations-and-deviations-of-beer-lambert-law/ (accessed November
5, 2014)
[3]
Spectrophotometric Determination of Iron. http://httpserver.carleton.ca/~rburk/high_schools/speclab.pdf (accessed November 5, 2014)

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