Revised Jobs Method

Method of Continuous Variation: Determination of Molecular
Formula for an Iron (III) – Salicylic acid Complex by

spectrophotometry
Background:
Complexation reactions of the form:

xM + yL ↔ Mx Ly
are based on the reaction of a metal cation (M) and a ligand (L). These reactions are widely used
in analytical chemistry. Absorption spectroscopy is a powerful tool for exploring these
complexation reactions. In this experiment, one general approach to study the composition of
complexes (the metal to ligand ratio) by absorption measurement is being demonstrated, in order
to carefully evaluate the properties of a particular chemical system.
The method is called the Job’s method of continuous variation. Using this method, the molecular
formula of the ferric salicylate complex can be determined. Job’s method is only effective when
a single complex is formed. Job’s method is dependent on the validity of the Beer’s Law over the
region of study. Beer’s Law gives us the relation between absorbance (A) of a solution and
intensity of the light (I):
A = log I₀/I
where I₀ is the intensity of the incident light, and I is the intensity of the transmitted light.
Another relation, from Beer’s Law relating absorbance to concentration of the solution is:
A = έcl
where έ is the molar extinction coefficient and l is the optical path length. With these formulae,
we can find the spectra of the solutions of the two species, recorded over a range of
concentrations, each solution containing the same total reagent concentration. So, in this
experiment [Salicylic acid] + [Fe3+] = constant. By seeing the spectra, we pick a wavelength, at
which there is good absorbance and the absorbance of each solution is noted.
In this method, metal cation and ligand solutions with identical concentrations are mixed in
different amounts such that the total volume of the mixture solutions and the total moles of
reactants in each mixture is constant. This procedure causes the mole ratio of reactants to be
varied across the set of mixture solutions. The absorbance of each solution is then measured and
plotted vs. the volume fraction of one of the reactants (M or L). For example, the volume fraction
of the metal is
VM/(VM + VL)
1
where VM is the volume of the metal cation solution and V L is the volume of the ligand solution.
A plot of this type is reproduced above in Figure 1. Assuming the complex absorbs more than the
reactants, a maximum occurs at a volume ratio VM/VL corresponding to the combining ratio of
cation and ligand in the complex. At other volume ratios, one of the reactants is a limiting
reagent. In the plot in Figure 1, this maximum occurs at V M/VL = 0.33/0.66, suggesting a
complex of the formula ML2.
Figure 1: Continuous-variation plot for a 1:2 complex, ML2
Reagent:
1. 0.0025 M Iron (III) ammonium sulfate: A solution of 0.0025M Fe3+ is prepared by

dissolving 0.301g of ferric ammonium sulfate in 250 cm3 of 0.0025M sulfuric acid.
2. 0.0025 M salicylic acid: A solution of 0.0025M salicylic acid is prepared by dissolving
0.086g of salicylic acid in 250 cm3 0.0025M sulfuric acid.
3. 0.0025 M sulfuric acid: using 0.25 M H2SO4 solution, the working acid solution is
prepared by further dilution to get the required acid solution.
2
Procedure:
A: Find the wavelength of maximum absorbance:
1. 5 ml of 0.0025 M Fe (III) solution is added with 5 ml of 0.0025 M salicylic acid in 25 ml

volumetric flask and dilute up to the mark with distilled water. Mix well the contents and
keep for 10 min at room temperature.
2. Record the absorption spectrum between 400 nm and 650 nm. Since your measurements
are in the visible region, plastic cells can be used.
3. Note λmax and use that wavelength for all further absorption measurements.
B: Determine the mole ratio of the complex:
1. Transfer 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10 mL of the standard Fe3+ solution to separate 25

mL volumetric flasks.
2. To each flask, respectively, add 10, 9, 8, 7, 6, 5, 4, 3, 2, 1, and 0 mL of the 2.5 x 10 -3 M
Salicylic Acid solutions. Prepare similarly a blank solution except the addition of Fe (III)
solution.
3. Dilute to the mark with distilled water, and mix.
4. After ten minutes, Measure the absorbance of each mixture vs. the blank solution at the
chosen wavelength.
5. Plot absorbance vs. mole fraction of Fe3+.. Extrapolate the linear portions of the curve and
locate the intersection.
3
Results & Discussion:
Volume Fe3+: Salicylic acid Mole fraction of Absorbance

(ml) (Fe3+: Salicylic acid)
10 : 0
9:1
8:2
7: 3
6:4
5:5
4:6
3:7
2:8
1:9
0 : 10
I. Write the chemical equation for the reaction that will take place in the lab
4
II. What is the mole ratio of Fe+3 to salicylic acid for the equation
III. Attach the two graphs (wavelength of maximum absorbance & Continuous-variation
plot) together with your results.
IV. Conclusion:

Revised Jobs Method

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Method of Continuous Variation: Determination of Molecular

Formula for an Iron (III) – Salicylic acid Complex by

Complexation reactions of the form:

Figure 1: Continuous-variation plot for a 1:2 complex, ML2

1. 0.0025 M Iron (III) ammonium sulfate: A solution of 0.0025M Fe3+ is prepared by

A: Find the wavelength of maximum absorbance:

1. 5 ml of 0.0025 M Fe (III) solution is added with 5 ml of 0.0025 M salicylic acid in 25 ml

B: Determine the mole ratio of the complex:

1. Transfer 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10 mL of the standard Fe3+ solution to separate 25

Volume Fe3+: Salicylic acid Mole fraction of Absorbance

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