Iryna Belskaya

Partner: Katherine Belfer

Lab Instructor: Budimir Zdravkovic
September 26, 2018
Experiment 4. What is in my sample? “Let’s find the cations”

Introduction:
For the research purposes in the scientific world, in medical field, and for crime solving purposes
it is very often required to identify what elements are present in the mixture. There are different
ways and techniques of doing so. By adding different reagents to the solution and applying
techniques like centrifugation and decantation, a scientist can conclude presence or absence of
certain elements in the solution. In this lab we learnt how to separate and identify different
elements in the mixture given. In the first part of the lab we followed the steps of separation
scheme in order to do qualitative analysis of the mixture provided and confirm the presence of
the cations of group 1 (Ag+, Pb2+, Hg22+), group 2 (Cu2+, Bi3+) and group 3 (Fe3+). In the second
part of the lab we followed the same steps of qualitative analysis for the unknown mixture
provided for us, and identified cations present in our unknown sample.

Materials
Test tubes & test tube rack
Graduated cylinder
pH paper
Beaker
Centrifuge Machine
Hot plate
Pasteur pipette
Test tube holder
Safety goggles
Sharpie for labeling the test tubes
Cations solutions,
6M HCL, hot water, KI, 6M NH4OH, 6M HNO3, 1M solution thioacetamide, 3% H2O2
Observations and Experimental:
Part A. In this part our group performed certain manipulations with the cations mixture provided
to identify presence of particular cations in the mixture. The description of steps of procedure
and our observation provided below.
Step Procedure Observation
1
Dispense 4mL of the cations mixture
solution into a test tube. The top of the solution in a test tube turned
Add 4 drops of 6M HCl. Mix well. yellow, bottom stayed blue.
Centrifuge for 2-3 min.
Decant your solution in a new test Precipitate formed, solution turned into liquid
tube, label solid (AgCl, PbCl2, and solid parts.
Hg2Cl2) and the supernatant solution
(Cu2+, Bi3+, Fe3+).

2
Add 4mL of hot water in the test tube Color of the solution did not change, solid and
with precipitate. Mix well. Centrifuge liquid parts formed.
for 2-3 min.
Decant your solution in a new test
tube. Label solid (AgCl, Hg2Cl2) and
supernatant (Pb2+) solution.

3
Cool the test tube with supernatant The solution turned yellow and opaque. With
solution (Pb2+) and add 5-6 drops of time yellow precipitate collected at the bottom
KI, until the first yellow sign. Yellow of the test tube and the liquid part of the
precipitate confirms presence of Pb2+. solution turned clear and lighter yellow color
comparing to the color when we just added KI.
The procedure confirmed presence of Pb2+ in
our mixture.

4
Take solid (AgCl, Hg2Cl2) and add 25 6M NH3 solution was not available in the lab,
drops of 6M NH3. so we used 6M NH4OH instead for this step.
Mix well. Centrifuge for 2-3 min. After the procedure the dark grey precipitate
Decant your solution in a new test was formed, which confirmed the presence of
tube. The grey dark precipitate Hg2+ in the mixture.
(Hg+HgNH2Cl) formed confirms the
presence of Hg22+.
5
Add 30 drops of 6M HNO3 to the After adding 30 drops of 6M HNO3 the
supernatant (Ag+) until white solid mixture turned opaque. After some time the
will form. white solid was formed and it settled on the
That confirms the presence of Ag+. bottom of the test tube. This confirmed the
presence of Ag+.

6
Check the pH of the supernatant from When checked for pH, the paper turned
Step 1 with the pH paper to be about yellow-green color, which confirmed the pH
0.5. of 0.5.
Add 20 drops of 0.1M NH3 to the
supernatant from Step 1. We used 6M NH4OH instead of NH3 solution.
Add 40 drops of 1M thioacetamide,
mix well. Heat on a water bath for 5 We repeated the procedure of adding drops of
min. thioacetamide and warming of the mixture in
Add again 6 drops of 1M solution of water bath 3 times.
thioacetamide and heat on a water
bath for 5 min. Repeat until you see The solution was dark, with black precipitant
no more black precipitate formed on the bottom and on the walls of the test tube.
when you add additional drops of
thioacetamide solution.

7
Centrifuge the solution again. Decant The supernatant solution was clear and the
your solution in a new test tube, label precipitate was dark along the walls of the
solid (Bi2S3, CuS), and liquid (Fe3+). tube.

8
Add 10 drops of 3% H2O2 to the After adding hydrogen peroxide the top of the
supernatant and then 9 drops of 0.1M mixture turned red for some time. After a
KSCN until deep red color will minute the color on the top of the solution
appear. Red color indicates presence faded to light orange color. 0.1 M KSCN was
of Fe3+. not available in the lab, so we did not add it.
However, it did not make a problem, because
hydrogen peroxide turns the solution red (if
Fe3+ is present) temporarily, and KSCN
solution makes the red color stay. For our
purpose we confirmed the presence of Fe3+.
 9
Add 45 drops of 6M HNO3 to the
precipitate from Step 7and heat for 5
min on a boiling water bath.
Centrifuge and decant to remove any
excess of sulfur (yellow/black traces). We used 6M NH4OH solution instead of 6M
NH3 solution.
Add 50 drops of 6M NH3 to the
supernatant solution. Mix well. The solution “split up”. The top of the
Centrifuge and decant. The white solution was clear at first, then in the middle
precipitate confirms the presence of there were white flakes mixed with blue color
Bi3+. liquid, and the bottom was yellowish and
The supernatant blue solution clear.
confirms presence of Cu2+. After decantation we had white precipitate and
blue color supernatant solution, which
confirmed the presence of Bi3+, and Cu2+ in
our test tubes.

Part B. Our group was working with the unknow sample number 52.

In this part of the lab our group was given unknown mixture and we had to follow the same steps
as in part A in order to identify presence or absence of particular cations in our unknown sample.
The procedure we followed and our observations are described in the table below.
Step Procedure Observation
1
Dispense 4mL of the cations mixture
solution into a test tube.
Add 4 drops of 6M HCl. Mix well.
Centrifuge for 2-3 min. The solution precipitated right away, white
Decant your solution in a new test precipitant formed.
tube.
After centrifugation: baby blue-green liquid
and white precipitant were in our test tube.

2
Add 4mL of hot water in the test tube After centrifugation: amount of white
with precipitate. Mix well. Centrifuge precipitant became smaller.
for 2-3 min.
Decant your solution in a new test
tube.
3
Cool the test tube with supernatant After we added KI the liquid turned yellow,
solution (Pb2+) and add 5-6 drops of which confirmed the presence of Pb2+ in our
KI, until the first yellow sign. Yellow unknown sample.
precipitate confirms presence of Pb2+.

4
Take solid and add 25 drops of 6M After we performed the instructed actions for
NH3. this step there was no grey precipitant, which
Mix well. Centrifuge for 2-3 min. indicated absence of Hg2+ in our unknown
Decant your solution in a new test mixture.
tube. The grey dark precipitate
(Hg+HgNH2Cl) formed confirms the
presence of Hg22+.

5
Add 30 drops of 6M HNO3 to the After we added 6M HNO3 there was no white
supernatant (Ag+) until white solid precipitant formed, which confirmed the
will form. absence of Ag+ in our sample.
That confirms the presence of Ag+.

6 Check the pH of the supernatant from The pH paper did not change color (stayed
Step 1 with the pH paper to be about blue), which meant that our solution was basic
0.5. (weak base).
Add 20 drops of 0.1M HN3 to the We did not have NH3 available in the lab, so
supernatant from Step 1. we used NH4OH instead.
Add 40 drops of 1M thioacetamide, After adding 6M NH4OH to our sample, our
mix well. Heat on a water bath for 5 sample split into 2 phases. The top layer was
min. darker blue liquid, the bottom layer was light
Add again 6 drops of 1M solution of baby blue liquid, the sample had dark muggy
thioacetamide and heat on a water precipitant in the middle of two phases of
bath for 5 min. Repeat until you see liquid in our test tube.
no more black precipitate formed After adding 40 drops of thioacetamide the top
when you add additional drops of of the liquid in the tube turned dark.
thioacetamide solution. After water bath our sample had dark opaque
top of the mixture and baby blue clear liquid
on the bottom of the test tube.
After centrifuge the we had dark precipitant on
the walls of the tube, clear light blue liquid on
the top and muggy opaque yellowish liquid on
the bottom of the test tube.
 At the end of this step we had our sample
black, flakey, and muddy with lots of residue.

7
Centrifuge the solution again. Decant The supernatant solution was clear and the
your solution in a new test tube. precipitate was black along the tube.

8
Add 10 drops of 3% H2O2 to the Substance turned lighter, but not red, not
supernatant and then 9 drops of 0.1M orange.
KSCN until deep red color will
appear. Red color indicates presence
of Fe3+.

9
Add 45 drops of 6M HNO3 to the After adding 45 drops of nitric acid the
precipitate from Step 7 and heat for 5 solution started smoking a little bit.
min on a boiling water bath. After the water bath it became dark (blakish)
Centrifuge and decant to remove any liquid, opaque.
excess of sulfur (yellow/black traces). After the centrifugation we had our liquid in
the sample looking clear yellowish, with
Add 50 drops of 6M NH3 to the precipitant on the bottom.
supernatant solution. Mix well. There was black precipitant stuck on the walls
Centrifuge and decant. The white of the tube.
precipitate confirms the presence of
Bi3+.
The supernatant blue solution
confirms presence of Cu2+.

Discussion and conclusion:

In the first part of the lab we learnt what reagents can be used to identify
presence/absence of particular cations. We also found out about techniques like decantation,
centrifugation and heat application to the mixture, which help break the mixture down to the
collections of separate elements. This, in turn, enables the person working in the lab to identify
presence or absence of certain elements in the solution by adding specific reagents, and
analyzing the color and precipitate formed. We identified presence of cation Pb2+ in the step 3 of
part A by the fact that yellow precipitate was formed when we added KI solution to our sample.
In step 4 a grey precipitate was present after the decantation confirming the presence of Hg22+.
Step 5 identified the presence of Ag+ due to the formation of white precipitate. Red color of the
solution in step 8, which appeared when we added 10 drops of 3% H2O2 identified presence Fe3+.
In Step 9 two things were confirmed, the presence of Bi3+ due to white precipitate forming and
Cu2+ since the supernatant solution was blue.
In the part B of the lab we performed the same steps working on our unknown sample
number 52 in order to identify the presence/absence of cations Cu2+, Bi3+, Fe3+, Pb2+, Hg22+, Ag+.
Our solution turned yellow in the step 3 after adding KI, which confirmed the presence of Pb2+.
We did not see any grey precipitant formed in the step 4, which indicated that our unknown
sample number 52 did not have cation Hg2+. Our sample did not form any white precipitant in
the step 5 after adding 30 drops of 6M nitric acid to the supernatant from step 4, which indicated
absence of Ag+. Adding 10 drops of 3% H2O2 did only made our solution few shades lighter, but
it did not turn the solution red, which confirmed absence of Fe3+. Finally, after prescribed
manipulations in step 9 we indicated absence of Cu2+ due to color of the solution not being blue.
The presence of Bi3+ in our unknown sample was questionable. The precipitant of white color
indicates the presence of Bi3+. This precipitant forms when you add 50 drops of 6M NH3 to the
supernatant solution derived in steps 7,8,9. Our precipitate looked grey. The grey color of
precipitant can be explained two ways. First, it might have looked grey due to the original color
of the precipitate, and that means, we did not have Bi3+ in our unknown sample. Second, the
precipitant might have looked grey due to the walls of the test tubes being covered with dark
precipitate from previous steps.
Based on the cation we identified in our unknown sample, the separation scheme will
look approximately this way. First separation scheme is modeled for Pb2+, which we identified
with 100% of certainty. See separation scheme1 attached at the end of the report.
Second separation scheme is modeled for the Pb2+, and Bi+ (in case Bi+ was present in the
unknown sample). See separation scheme2 attached at the end of the report. The equations for
the steps where we identified, or possibly identified, cations are also attached to this lab report.
Possible chemical equations are on the page with separation scheme. Please, see attachements.
In all we were able to determine presence/absence of particular chemical elements in our
sample 1(known mixture) and sample 2(unknown mixture number 52). We were able to identify
the elements due to specific reaction (color change, solid formed) that cations have when mixed
with certain reagents. One of our test tubes from part B was taken by somebody else, which left
us with one test tube to experiment, leaving us no chance to compare the derived results between
two test tubes for higher degree of confidence about our conclusions. The fact that we used 6M
NH4OH instead of 6M NH3 could have resulted some errors. Some imperfections, affecting the
results of our procedures in part B could be addressed to instrumental issues (different size of
drops, not boiling water etc).

Focus Questions:
1. What is present in the known mixture? And how is it known?
In the known mixture are present following cations: Cu2+, Bi3+, Fe3+, Pb2+, Hg22+, Ag+.
The presence of Pb2+ is confirmed by solution with this cation turning yellow when KI was
added. The presence of Hg22+ was confirmed by the grey dark precipitate which formed after
adding 6M NH4OH to the solution and after this solution was centrifuged. The presence of Ag+
was indicated by white solid, which formed after adding 30 drops of 6M HNO3 to the solution.
The presence of Fe3+ was confirmed by red color of solution when added 10 drops of hydrogen
peroxide. The presence of Cu+ was indicated by blue color of the solution when 50 drops of 6M
NH4OH was added to the supernatant solution. And white precipitate formed after adding 50
drops of 6M NH4OH to the solution indicated the presence of Bi3+.
2. What number is your unknown sample and what cations are present in it?
Number of my unknown solution is 52. I identified presence of Pb2+ cation in it. There also
could have been Bi3+ in my sample. I am not sure about presence of Bi3+ in my mixture, because
the precipitate that formed at the end of step 9 was grey color, when it should have been white in
order to indicate the presence of Bi3+. However, the precipitant might have looked grey because I
was looking at it through the precipitant on the walls of my test tube, and the wall precipitant
was dark, which could have made the white precipitant of Bi3+ look grey instead of white.

References:
Smeureanu, Gabriela, and Stephanie Geggier. General Chemistry Lab Manual. N.p.: LAD
Custom, 2016. Print.
Post-Lab Assessment Questions:
1. Define the following terms:
a) Decantation- Decantation is the process of separation of liquid from solid and other non-
mixing liquids, by removing the liquid layer at the top from the layer of solid or liquid below.
b) Centrifugation- Centrifugation is a technique which involves the application of centrifugal
force to separate particles from a solution.
c) Supernatant- the liquid lying above a solid residue after crystallization, precipitation,
centrifugation, or other process.
d) Precipitate- a substance that is deposited in solid form from a solution.

2. What reagent(s) can be used to identify and confirm Ag+, Hg22+, and Pb2+ ions?
Ag+- 6M HNO3 (nitric acid)
Hg22+- 6M NH3 (ammonium), in our case it was 6M NH4OH
Pb2+- KI (potassium iodide)

3. List all the solid precipitates that you encounter during the experiment and their colors.
Yellow solid precipitate: Pbl2
White solid precipitate: AgCl, Bi(OH)3
Grey dark solid precipitate: Hg+HgNH2Cl

4. What is the precipitating reagent for silver ion in Step 1? Would a solution of NaCl work as
well? Why or why not?
HCl is the precipitating reagent for silver (Ag+). Solution of NaCl would work as well since Cl
has same quantity of negative charge for both NaCl and HCl. The equation for reaction with HCl
is Ag (+) + HCl(-) AgCl, and the equation for reaction with NaCl is Ag (+) + NaCl(-) AgCl.
Therefore, both solutions will work.

5. What was your assigned unknown color could you make an educated guess on what ions may
be present in your unknown solution based on its initial color? Justify your answer.
 The color of our sample was clear. It is possible to say if specific cations are present by
looking at the reaction of the solution with reagents, however, it is hard to say what is present by
only looking at the mixture.