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Paper

Chromatography

October 2,
2014

Purpose: The purpose of this lab was to become familiar with


chromatography, a technique for separating the components of a
mixture, and to separate a mixture of transition metal cations by
paper chromatography.
Background Information: In this lab, we worked with mixtures which are
a physical combination of two or more pure substances. The components of
the mixture do not change in chemical composition. With paper
chromatography, extraction is used where a solvent was added that the
substance would be soluble in and thats how the effect of the colors
moving up the paper is apparent. Chromatography is separating the
components of a mixture on the basis of their differing adsorptive
tendencies on a stationary phase. The leading edge of the mobile phase in
the chromatogram is called the eluent front, the
eluent being the solvent. The solutions have two phases: the stationary
phase and the mobile phase (movement along the paper)
List of Materials:
-8 capillary tubes
-600 mL beaker
-chromatography paper
-rubber band
-6M HCl -NH3
- 5 separate solutions containing
2+
3+
2+
2+
these ions: Mn , Fe , Co , Ni , and Cu2+
-Ammonia Chamber
(already
prepared -unknown
by instructor)
-unknown
soln. 2
-unknown
-plastic
soln.
1
soln.
3
wrap
scissor
-ruler
-10 mL graduated cylinder
-funnel
Procedure: First take the ammonia and, using a funnel, measure out 9 mL
in the graduated cylinder. Pour this into the 600 mL beaker. Next measure
out 1 mL of hydrochloric acid the same way and pour that into the beaker
as well. This is called the developing chamber. Cover the beaker with
plastic wrap and put a rubber band around it to hold it tightly in place. Take
the chromatography paper, measure so that it is 10 X 20 cm and cut off
excess paper. Measuring 2 cm up from one of the sides that is 20 cm, make
a 20 cm line the whole way across. Then, mark the line every 2 cm so that
there are 8 marks in between the edges of the paper. After this, gather
each solution: Mn2+, Fe3+, Co2+, Ni2+, Cu2+, unknown 1, unknown 2, and
unknown 3. Place a capillary tubes in each of the solutions. When some of
the solution is present in the capillary tubes, assign one of the eight marks
on the chromatography paper for each solution and make a dot by using
the capillary tube. Allow to dry and add a dot to each mark for each
solution twice more. Make sure that each spot is dry then staple the
chromatography paper together. Place it inside the developing chamber,
place the plastic wrap over top tightly again, and wait about 20 minutes.
After completing this, take out the chromatography paper and draw a line

at the eluent front and let dry. Measure the height from the 2 inch line that
was drawn on the paper earlier. Observe the colors of the spots where the
8 solutions were and record them. Next, place the paper inside the
ammonia chamber and close it with the plastic wrap and rubber band. Wait
about 5 minutes and take out. Observe the colors and

record again. Measure up from the 2 cm line to the end of where each
color climbed to and record this as well. Determine which cation(s) that
each of the unknown solutions contain by comparing color changes after
the ammonia test.
Safety Considerations: While performing this lab, there were some
safety precautions that needed to be taken. Being that hydrochloric acid is
a strong acid, it can be very harmful to a persons skin and eyes. For this
reason safety goggles were worn, along with lab coats to prevent damage
to clothing. Another chemical used in the lab was ammonia, which can be
damaging if inhaled too much. Because of this, the ammonia chamber was
placed under the fume hood.
Data Tables:
Distance of eluent from origin, Deluent: 5.5 mm
Color
(original)

Color (with
NH3)
Tan

Distance
(mm)
Traveled,
Dion
1.00

Mn2+

Clear

Fe3+

.182

Orange

Brown

0.40

.0727

Co2+

Pink

Light brown

1.10

.200

Ni2+

Blue-green

Light blue

0.90

.164

Cu2+

Light blue

Blue

1.70

.309

Color

Rf

Unknown #1

Unknown #2

Unknown #3

tan

light blue

brown

Ni2+

Fe3+

Cations Present Mn2+

Observations: The results were brighter and more apparent when the
paper was placed in the ammonia chamber.
Results:
Ratio of Fronts
Rf=Distance from origin to final position of ion
Distance from origin to eluent front
Rf=Dion/ Dsolvent

Rf=1.00 mm/5.5 mm
Rf=.182
Discussion: The cation present in unknown solution 1 was manganese, in
unknown solution 2 was nickel (II), and in unknown 3 was iron (III). These
results were correct because they went along with the colors of those ions
in the known solutions after the tests. One source of error would be that
maybe the paper was not left in each of the chambers long enough which
would cause the distance the ion traveled to be less than what it should be
and therefore the ratio of fronts would be lower. Another source of error
would be that maybe the oils from our hands would have contaminated the
paper and affected the polarities of each of the solutions with the cations.
This would also cause the distance the ion travels to be less.
Questions:
1.)
a.) The developing chamber must be covered during the
development of the chromatogram so that the vapors can reach the
entire paper. This prevents the uneven saturation for each of the
different solutions.
b.) The Rf value will be less than what it should be if the developing
chamber is
not covered because the ammonia/hydrochloric acid solution wont be able
to reach all of the way up the paper.
2.) If the paper touches skin that it can get contaminated and change the
way each of the solutions separate.
3.) A pencil was used to mark the chromatogram instead of a pen
because the ink will spread out and cause an interference with the data
when it gets wet. Using a pencil would prevent this from happening
because its just a solid.
4.) The cation samples are repeatedly spotted and dried because they
need to be able to absorb into the paper and they take time to do this. It
also needs to spread out as well in order to absorb more of the solution.
5.) If the eluent were above the 1.5 cm line, then the distance from the
origin to the final position of the ion would be lower and therefore the
ratio of fronts value in the results would be lower.
6.) The center of the band is used to calculate the Rf value for a cation
because it has a higher concentration of the cations than the leading
edge does.
7.) If two cations have the same Rf value then the best option would be to
use a different type of chamber. Use a solvent that can dissolve only one
of the ions and not the other and the one that reaches highest on the
paper is the more soluble one.

Conclusion: The purpose of this lab was to see how chromatography


works as a method for separating a mixture and to use it to find the
cations present in an unknown solution.

In this lab, the paper chromatography technique was used and the cations
in the unknown solutions were found, therefore, the objectives were met.
From the results, it was concluded that Manganese ions were present in
unknown #1, Nickel (II) ions were present in unknown #2, and Iron (III) ions
were present in unknown #3. It was hard to say whether or not the solution
had more than one cation in it. One way to test for that would be to
conduct multiple experiments and combine it with solutions that each
cation could react with to produce a precipitate and using a centrifuge. If a
precipitate forms that that cation is present and this could be done to more
easily show the presence of 2
or more cations.