Separation of Cations by Paper Chromatography

Objective:
The separation of the cations Copper (II), Nickel (II), Iron (III) and an unknown
will be done by paper chromatography, by using filter paper, TLC paper, and a
hydrochloric acid/acetone mixture as the solvent. The chromatogram will develop
by observing the solvent front as it moves through the paper. The three
known/unknown ions used during the experiment will be determined by using a
dimethylglyoxime solution and ammonia to visually establish the ions based on
colour change. With the information gathered from the experiment the unknown
ions can be determined as well as the retention factor.
Method:

0.5M solutions of Copper II (Cu), Iron III (Fe), Nickel II (Ni)

Unknown solution #7
Solvent mixture: Hydrochloric acid and Acetone (HCL and C3H6O)
15M Ammonia (NH3)
1% Dimethylglyoxime (C4H8N2O2)
TLC Paper
12.5cm Filter Paper
Petri Dishes
100mL Beakers
25mL Graduated Cylinder
Capillary Pipette
Scissors
Ruler

Safety: Acetone is extremely flammable, as a liquid and as a vapour. Do not pour

down the sink.
For a full laboratory procedure, refer to; Chemistry II (CHEM 2131) Laboratory
Manual, pages 4-9.

Observations/Calculations:

Retention factor calculations from the filter paper chromatography:

Ni = a/x
= 1.1cm / 2.7cm
= 0.41cm
Cu = a/x
= 2.2cm / 2.7cm
= 0.81cm
Fe = a/x
= 2.6cm / 2.7cm
= 0.96cm
Unknown #7 (Fe) = a/x
= 1.8cm / 1.9cm
= 0.95cm
Unknown #7 (Cu) = a/x
= 1.3cm / 1.9cm
= 0.68cm
Retention factor calculations from the TLC paper chromatography:
Ni = a/x
= 3.7cm / 3.9cm
= 0.95cm
Cu = a/x
= 3.8cm / 3.9cm
= 0.97cm
Fe = a/x
= 4.1cm / 3.9cm
= 1.05cm

Unknown #7 (Fe) = a/x

= 3.6cm / 3.9cm
= 0.92cm

Unknown #7 (Cu) = a/x

= 3.4cm / 3.9cm
= 0.87cm
Table 1: Colour changes of ions with the presence of dimethylglyoxime and
ammonia.

Cations

Dimethylglyoxime

Ammonia

Copper (II)

No colour change
occurred
No colour change
occurred
Turned pink

Turned blue

Iron (III)
Nickel (II)
Unknown #7

No colour change
occurred

No colour change
occurred
No colour change
occurred
Yellow area did not
change, a blue colour
appeared.

Discussion:
The qualitative data found during the experiment allowed the determination
and location of the ions on the paper based off of the visual colours of the ions. As
the solvent moved, the ions did as well. The iron ion, which appeared as a yellow
colour on the wet paper, stayed that colour throughout the entire experiment and
no colour development was necessary. The colour intensity of the iron allowed for
the movement of the ion to be documented and observed throughout the entire
experiment. The copper ions react with water and ammonia gas to form Cu(NH3)4.
This compound forms a blue colour which is what appeared on the paper when it
was placed over the ammonia fumes. This blue colour shows that copper ions are
present.

When the

dimethylglyoxime was sprayed onto the paper, it reacted with the nickel ions to
form a red/pink colour. The colour changes that occurred during the experiment
allowed for the determination of the unknown ions. The unknown appeared yellow
on the paper, meaning that iron ions were present and no further colour change
would occur. When the paper was exposed to the dimethylglyoxime no colour
change occurred, meaning there were no nickel ions present. When the paper was
exposed to the ammonia fumes a blue colour appeared, meaning there was a
presence of copper ions. The unknown #7, based off of qualitative value can be
determined as iron and copper ions.

The retention factor of each ion on the

filter paper and the TLC paper was calculated. These calculations showed how far
each ion traveled in relation to the solvent front. A retention factor of <1 means
that it did not pass the solvent front, a retention factor of >1 means that the ion did
pass the solvent front. On both the filter and TLC paper the iron ion had the highest
retention factor, meaning it was the closest to the solvent front, with R f values of
0.96cm (filter paper) and 1.05cm (TLC paper). On the TLC paper the iron had a
retention factor of >1, therefore the ion traveled beyond the solvent front. The
copper ion was the second closest to the solvent front with R f values of 0.81cm
(filter paper) and 0.91cm (TLC paper). The nickel ion was the farthest from the
solvent front with Rf values of 0.41cm (filter paper) and 0.95cm (TLC paper). The
same showed for the unknown solution, the iron ion traveled farther than the
copper ion, keeping closer to the solvent front.
Conclusion:
From the information gathered from this experiment the unknown ion solution
#7 can be determined as iron and copper ions. The retention factor calculations for
both the filter and TLC paper proved that the iron had the highest retention factor,
copper the second highest, and nickel had the lowest R f value.