Spectrophotometric Determination of Iron

Experiment No.
Spectrophotometric Determination of Iron
Chem 352 © Department of Chemistry, BUET

Objective
 Study the analytical technique such as spectrophotometric method to

analyze metals in different environmental samples.
 Understand the technique or method to observe and monitor the heavy and
toxic metals pollution in various environmental components such as water,
soil, and food chains.
 Obtain and interpret a Beer-Lambert Law Plot from prepared standard

solutions.
 Determine the concentration of iron in unknown samples.

Importance
 UV-Vis spectroscopy is one of the best methods for the determination
of impurities in organic molecules.
 Qualitative analysis
 Quantitative analysis
 Chemical kinetics
 Detection of functional groups
 Quantitative analysis of pharmaceutical substances
 Quantitative analysis of heavy and toxic metals in different

environmental samples: water, soil, sediments, and food chains.
Theoretical Background
UV-Visible Spectroscopy
♦ UV-vis spectroscopy measure the response of a sample/analyte to ultra violet

and visible range of electromagnetic radiations.
♦ An analytical technique which concerns with the measurement of

absorption of electromagnetic radiation [ UV: 180-400 nm; Visible: 400-800 nm].
♦ It is also known as electronic spectroscopy.

UV-Visible Spectroscopy
♦ Molecules have either n, π or σ electrons.

n electrons: in non bonded electrons
σ electrons: in saturated compounds
π electrons: in unsaturated compounds
♦ These electrons absorb UV and Visible part of electromagnetic

radiations and undergo a transition from ground state to excited state.
♦ Electronic transitions also occur in metallic species.
♦ d-d transitions, metal to ligand charge transfer (MLCT)

ligand to metal charge transfer (LMCT).

Generally, the most probable transition is from highest
occupied molecular orbital (HOMO) to lowest occupied
molecular orbital (LUMO).

Types of electronic transitions: d-d transition

Types of electronic transitions: charge transfer transitions

Types of electronic transitions: charge transfer transitions
Iron(III) Nitrate and Ammonium Thiocyanate Reaction
Fe(NO3)3 + 3NH4SCN Fe(SCN)3 + 3NH4NO3

UV-Visible Spectrophotometer
♦ Spectrophotometer or Spectrometer is an instrument design to measure the

spectrum of a compound.
♦ Spectrum is a graph of intensity of absorbed or emitted electromagnetic radiation

by sample/ analyte verses frequency or wavelength (ʎ)
♦ The amount of light absorbed at each wavelength of UV and Visible region of

electromagnetic radiation by samples is measured.

UV-Visible Spectrophotometer

UV-Visible Spectrophotometer : Experimental Set Up

UV-Visible Spectrophotometer : Instrumentation

UV-Visible Spectrophotometer : Instrumentation

Absorbance and the Beer – Lambert Law

Absorbance and the Beer – Lambert Law
According to the Beer-Lambert Law, absorbance is proportional to

concentration, and Absorbance versus concentration plot is a straight line.

Deviations of Beer – Lambert Law
Chemical Deviations:
Instrumental deviations.
Experimental deviations: Reflection, Scattering

Let Us Start the Experiment
Prepare seven solution of different

Prepare 100 ppm Fe3+ Stir the solutions well and
concentrations each with a volume
stock solution of 100 mL in volumetric flasks wait for 10 minutes
Get the blank solution in two

quartz cells and place it in the
spectrometer
Wipeout the water at the surface Place solutions of the rest six Fe3+ Place auto zero and base line.
Get a blank run to check the status
of quartz cell before placing in samples in another quartz cell
of the machine. Keep one quartz cell
spectrophotometer solutions and place it in sample in the reference sample chamber.
chamber
Record the absorbance of each sample Get a graph paper and prepare a calibration
at λmax = 480 nm of concentration and absorbance.
Let Us Start the Experiment

Data Collection and Calculation
0.8
Concentration(ppm)
1
2
0.6 3
Absorbance(a.u)
4
5
Unkonwn
0.4
0.2
0.0
300 400 500 600 700 800

Wave Length (nm)

Data Collection and Calculation
Data Table:
No. of Observations Fe3+ solutions (ppm) Wavlength (ʎ) Absorbance (A)
1 Blank
2 1
3 2
4 3
5 4
6 5
7 Unknown

Results
The concentration of Fe3+ in the unknown sample (from calibration curve) =
The concentration of Fe3+ in the unknown sample (from equation) =

Discussions
Discussion: Should be based on-

 Precautions taken to minimize error
 Justification of error (despite sufficient precautions)
 Justification of error should be based on reasons that are
beyond your control

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Experiment No.

Spectrophotometric Determination of Iron

Chem 352 © Department of Chemistry, BUET

 Study the analytical technique such as spectrophotometric method to

 Obtain and interpret a Beer-Lambert Law Plot from prepared standard

 Determine the concentration of iron in unknown samples.

Chem 352 © Department of Chemistry, BUET

 Detection of functional groups

 Quantitative analysis of pharmaceutical substances

 Quantitative analysis of heavy and toxic metals in different

♦ UV-vis spectroscopy measure the response of a sample/analyte to ultra violet

♦ An analytical technique which concerns with the measurement of

♦ It is also known as electronic spectroscopy.

Chem 352 © Department of Chemistry, BUET

♦ Molecules have either n, π or σ electrons.

♦ These electrons absorb UV and Visible part of electromagnetic

♦ Electronic transitions also occur in metallic species.

♦ d-d transitions, metal to ligand charge transfer (MLCT)

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Iron(III) Nitrate and Ammonium Thiocyanate Reaction

Fe(NO3)3 + 3NH4SCN Fe(SCN)3 + 3NH4NO3

Chem 352 © Department of Chemistry, BUET

♦ Spectrophotometer or Spectrometer is an instrument design to measure the

♦ Spectrum is a graph of intensity of absorbed or emitted electromagnetic radiation

♦ The amount of light absorbed at each wavelength of UV and Visible region of

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

According to the Beer-Lambert Law, absorbance is proportional to

Chem 352 © Department of Chemistry, BUET

Chem 352 © Department of Chemistry, BUET

Prepare seven solution of different

Get the blank solution in two

Chem 352 © Department of Chemistry, BUET

300 400 500 600 700 800

Chem 352 © Department of Chemistry, BUET

No. of Observations Fe3+ solutions (ppm) Wavlength (ʎ) Absorbance (A)

Chem 352 © Department of Chemistry, BUET

The concentration of Fe3+ in the unknown sample (from calibration curve) =

The concentration of Fe3+ in the unknown sample (from equation) =

Chem 352 © Department of Chemistry, BUET

Discussion: Should be based on-

Chem 352 © Department of Chemistry, BUET

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