Separation and Qualitative Determination of Cations and Anions

AP Chemistry lab #14

Introduction:
Separation and Qualitative Determination of Cations and Anions Lab focuses on
determining the composition of a sample solution in term of ions. To identify the cations and the
anions in solutions, we will use analysis scheme to determine the ions in solutions.
Concept:
Qualitative analysis and precipitation reactions.
Background:
Qualitative analysis is the procedure that used to identify what substances are present in a
mixture by chemical and physical means.
In this experiment, we will perform a series of semi-micro scale experiments to identify
the cations of one unknown" solution and the anions in another. First, we will try to isolate the
suspected ion, and then we will perform a confirmatory test to prove that is suspected ion is the
one we expected.
It is suggested that you perform the experiments more than one time to confirm result.
For the ease of keeping track of results, it is suggested to print out the Data Tables page
of this lab.
Things that you should know before doing this lab:
Keep Track of Everything
Label all the test tubes you are using, and keep track of what section of the lab you are
doing. Also, do not forget to fill in the Data Table after you performed a step.
Known Solution
Unknown Solution
Step
Procedure
Results
Conclusion
Results
Conclusion
+
1 Add HCl to known White ppt
Ag
solution in TT1.
forms, other
Centrifuge. Pour the ions present in
colored solution into solution in
TT2
TT2
TT = Test Tube ppt = precipitate
Fill out the Known Solution first, and then the Unknown Solution later when you are
analyzing it.
Be Organized and Safe
Put the chemicals in an organized order and within reach. Due to the present of corrosive
acids and relatively toxic chemicals, you should put them away if lab does not require further
use. Beral pipets, stirring rods, and test tubes should be rinsed carefully (at least twice) with
distilled water before you reuse them for another step to avoid contamination.

How to use a centrifuge

Centrifuge solutions so that the solid is packed at the bottom of the test tube. Dont forget
to counterbalance the test tubes in the centrifuge with similar test tubes holding equivalent
volumes of liquid (Figure 1). Let the centrifuge spin for about 30 seconds. Usually the
supernatant liquid (the liquid above the precipitate) can be poured off of the precipitate.
Sometimes precipitates tend to float on the surface of the solution. If this is the case, use a Beraltype pipette to draw off the supernatant liquid. It is better to leave a little liquid over the
precipitate than to transfer some of the precipitate.

Pre-Lab Questions:
Use the flow charts at the end of the experimental
procedure to answer the following questions. In
each question, a test is carried out to determine the
presence or absence of several ions. Only those listed
may be present. State if the tests indicate if each ion
is present, absent, or undetermined.

Only do pre-lab questions 1-5 for Procedures I and II The Cation Lab, and only do prelab questions 6-8 for Procedures III and IV, The Anion Lab.
1. Test for Ag+1, Cu2+, Fe3+
Some 6 M HCl is added to a solution that may contain the three ions. A white precipitate
forms.
Ions present: ___________ Ions absent: ___________ Ions undetermined: ____________
2. Test for Cu2+, Ag+1, and Zn+2
Some 6 M HCl is added to a solution that may contain the three ions. No precipitate forms. The
addition of 6 M NaOH until the solution is basic results in no formation of precipitate.
Ions present: ___________ Ions absent: ___________ Ions undetermined: ____________
3. Test for Cu+2, Fe+3, and Zn+2
6 M NaOH is added to a clear solution that may contain the three ions until the solution is
basic. A dark precipitate forms. The precipitate totally dissolves in 6 M H2SO4. The addition of 6
M NH3 to this acidic solution until it is basic results in a clear solution containing a dark
precipitate. The dark precipitate completely dissolves in 6 M H2SO4.
Ions present: ___________ Ions absent: ___________ Ions undetermined: ____________
Only one of each of the following pairs of reactants undergoes a reaction. Complete and balance
the equation for the reaction that occurs.
4. NaCl (aq) + BaCl2 (aq)
Na2SO4(aq) + BaCl2(aq)
5. K+1(aq) + Cl-1(aq)
Ag+1(aq) + Cl-1(aq)
6. Test for CO3-2 and Cl-1
Some 6 M HCl is added to the solution that may contain the above ions. Formation of bubbles is
noted as the solution is heated.
Ions present: ___________ Ions absent: ___________ Ions undetermined: ____________
7. Test for Cl-1, SO4-2, CO3-2 , and NO3-1
Addition of AgNO3 causes no precipitate to form. Addition of BaCl2 to fresh solution also causes
no precipitate to form.
Ions present: ___________ Ions absent: ___________ Ions undetermined: ____________
Only one of each of the following pairs of reactants undergoes a reaction. Complete and balance
the equation for the reaction that occurs.
8. H2O (l) + NO3(aq) + OH(aq) + Al(s)
CO3-2(aq) + OH-1(aq)

Materials:
Cation solution, 5 mL
Distilled H2O
6 M NaOH solution
6 M acetic acid solution
.1M KSCN solution
.1M AgNO3 solution
.1M BaCl2 solution
Test tubes, 13 x 100 mm, 6
Wire test tube holder
Spatula
Watch glass
Litmus paper
Centrifuge

6 M HCl solution
6 M NH3 solution
6 M H2SO4 solution
.1M K4Fe(CN)6 solution
6M HNO3 solution
0.05 M Ba(OH)2 solution, saturated
Beakers
Test tube rack
Stirring rods
Transfer Pipettes
Test tube stoppers
Hot plate
Anion solution, 5 mL

Safety Precautions:
Silver nitrate solution is mildly toxic and irritating to body tissue. It also stains skin and
clothing.
Cupric nitrate solution is mildly toxic. Zinc nitrate solution is mildly toxic and is irritating to
body
tissue. Ferric nitrate solution is irritating to body tissue. Barium hydroxide and barium chloride
solutions are toxic by ingestion. Potassium thiocyanate solution is slightly toxic by ingestion.
Avoid
contact with concentrated acids since toxic hydrogen cyanide gas may be liberated.
Concentrated
ammonia (ammonium hydroxide) solution and hydrochloric acid solutions are toxic by
inhalation,
ingestion, and are corrosive to all body tissues. Sulfuric acid solution and sodium hydroxide
solution are severely corrosive to eyes, skin, and other tissue. Nitric acid solution is severely
corrosive, a strong oxidant, and toxic by ingestion and inhalation. Acetic acid solution is a
corrosive liquid. Wear chemical splash goggles, chemical-resistant gloves, and a chemicalresistant apron. Wash hands thoroughly with soap and water before leaving the laboratory.

Qualitative Analysis of Cations:

The instruction below is written for a solution with all known species of ions. Your
unknown solution may or may not be the same. Therefore, you should write down any
differences while performing the steps in the Unknown Solution columns.
It is necessary to follow these steps.
1.
Separation of Ag+ from Fe2+, Cu2+, and Zn2+
Note: Solutions of silver and zinc salts are colorless while those of copper (II) and iron (III) are
blue and yellow, respectively.
Silver ions will react with chloride ions to produce solid silver chloride and precipitate at
the bottom of the test tube. Other ions, however, will not form solid precipitate. Therefore,
Ag+ can be separated from the solution by introducing chloride ions to the solution.
Ag+ (aq) + Cl- (aq) AgCl (s)
a. Add 8 drops of 6M HCl to the unknown solution and stir it. If Ag+ is present, a
white precipitate will form.
b. Centrifuge the solution. To make sure that all the precipitate has formed, add a
few (2-3) drops of HCl until no more solid form.
c. Centrifuge again. Either pour off or transfer (by using a Bural pipet) the liquid
into another TT, then use distilled water to wash the precipitate. Centrifuge and
discard the wash water
2.
Confirmation of Ag+
a. Add 1 mL 6M NH3 to the precipitate from procedure 1c
-Solid silver
dissolvedcomptely
by ammonia
solution and form a colorless complex
b. chloride
Stir untilcan
the be
precipitate
dissolves.
ion.
c. Add 15 drops of 6 M HCl to+the solution.
Students will observe smoke and heat
AgCl(s)
+ off
2NH
Ag(NH3between
)2 (aq) +strong
Cl- (aq)
3 (ap)
give
from
thereaction
acid and base. Be caution when holding
+
-Solution HCl(aq)
is
added
to
Ag(NH
)
(aq)
with
the
present
of Cl- (aq). A precipitate
3 2 may get very hot
the test tube due to the tube
AgCl(s) isd.observed
new pH
ironindicator
NH4+(aq)paper
formsor litmus paper to see if the solution is
Stir andand
testawith
+
+
Ag(NH
)
(aq)
+
Cl
(aq)
+
2H
(aq)

+ 2NH4+(aq)
3
2
acidic. If not acidic, add more HCl.AgCl(s)
White precipitate
in acid solution is the
presence of AgCl.
3.
Separation of Iron and Copper from Zinc.
-In a basic solution, amphoteric sinc will from colorless complex ion, while hydroxides of all
the other ions will precipitate. Iron will precipitate with the rust color Fe(OH)3(s) and copper as
blue Cu(OH)2.
Fe3+ (aq) + 3OH-(aq) Fe(OH)3(s)
Cu2+(aq) + 2OH-(Aq) Cu(OH)2(s)
ZN2+(Aq) +4 OH- (aq) ZN(OH)42-(aq)
a. Add while stirring 6M NaOH to the solution from procedure 1c until the solution
is basic and add 3 more drops.
b. Stir and place test tube in a hot water bath for 3 minutes. A formation will indicate
the presence of iron/copper.
c. Centrifuge the solution to separate the solid from solution, save the clear solution
Zn(OH)42-(aq) for procedure 6

4.

d. Wash the precipitate with 10 drops of 6M NaOH and 10 drops of distilled water.
e. Centrifuge to discard water. Save precipitate for procedure 4
Separation of Iron from Copper; Confirmation of Copper.

-Both cupric hydroxide, Cu(OH)2, and ferric hydroxide, Fe(OH)3 dissolve in acid solution
Cu(OH)2(s) + 2H+(aq) -> Cu2+(aq) + 3H2O(l)
Fe(OH)3(S) + 3H+(aq) -> Fe3+(aq) + 3H2O(l)
-When ammonia, is added to a Cu2+ solution, will cause the blue tetraamine copper(II)
complex ion to form. The blue color indicates the existence of copper. Meanwhile, the
hydroxide ions will precipitate from the basic ammonia solution.
Cu2+(aq) + 2H+(aq) Cu(NH3)42+(aq)
Fe3+(aq) + 3OH(aq) Fe3+(aq) + 3H2O(l)
-Another way to test for copper is to precipitate a red brown copper(II) hexacyanoferrate(II)
2+
a. Add](s),
5 drops
distilled
water to precipitate from step 3e.
Cu2[Fe(CN)
from of
a Cu
solution.
6
b. Slowly add 6M H2SO4 when the solution is acidic (confirm by litmus paper). Stir
to dissolve (take about 6 drops)
c. Add 6M NH3 to the solution until it is basic then add 1-mL extra.
d. Centrifuge and separate precipitate from liquid. Save precipitate for procedure 5.
The color blue of the solution will tell the existence of copper.
e. Dispose of copper solution as directed by instructor.
5.
Confirmation of Iron.
Ferric hydroxide will dissolve in sulfuric acid. The presence of iron can be tested by the
addition of thiocyanate ion, SCN-, which will form a wine-red color.
Fe(OH)3(s) + 3H+(aq) Fe3+(aq) + 3H2O(l)
Fe3+(aq) + SCN-(aq) FeSCN2+(aq)

6.

a. Wash the precipitate fo iron hydroxides from procedure 4d.

b. Add 6M H2SO4 utnill the precipitate dissolves.
c. Add 5 drops of 0.1 M KSCN solution. The red color of FeSCN2+ shows the
presence of iron.
d. Dispose the solution as directed by instructor.
Confirmation of Zinc.

The confirmatory test for zinc is the formation of a precipitate of potassium zinc hexacyano ferrate
(II). K2Zn3[Fe(CN)6]2. This precipitate is white if pure, and if iron present, it will be slightly green,
or blue-green
Zn(NH3)42+(aq) + 4H+(aq) Zn2+(aq) + NH4+(aq)
3ZN2+(aq) + 2K+(aq) + 2Fe(CN)64-(aq) K2Zn3[Fe(CN)6]2(s)
a. Add 6M HCl slowly to solution in procedure 3c until slightly acidic
b. Add 3 drops of 0.1 M KK4[Fe(CN)6] and stir.
c. Centrifuge to get precipitate K2Zn3[Fe(CN)6]2 which is white to light green or blue
green in color.
d. Dispose of zinc precipitate and solution as directed by instructor.

7.

Repeat steps 1-6 for cation unknown sample. Record the result for each step.

Qualitative Analysis of Anions

This part of lab does not require you to perform each experiment in order; you can pick a section
and perform that particular experiment.
This part also required the use of the hot water.
1. Separation of the Chloride (Cl-); Confirmation of Chloride.
Chloride ions form solid precipitate with silver ions in aqueous solution.
Cl- (aq) + Ag+ (aq) AgCl (s)
Solid silver chloride can be dissolved by ammonia solution and form a colorless complex ion.
AgCl(s) + 2NH3 (ap) Ag(NH3)2+ (aq) + Cl- (aq)
If nitric acid is added, the complex ion will break down, forming solid AgCl and aqueous NH4+
Ag(NH3)2+ (aq) + Cl- (aq) + 2H+ (aq ) AgCl (s) + 2 NH4+ (aq)
a.

Place 10 drops of the unknown solution of anions into a TT. Use a Beral pipet
and obtain a sample of the solution. Check for its pH level. IF the solution is not
acidic, add 6M acetic acid, CH3COOH, until it is acidic.
b.
Add 10 drops of 0.1M silver nitrate, AgNO3, and a white precipitate will form (if
Cl- present.)
c.
Centrifuge and discard the liquid, wash the precipitate with distilled water,
centrifuge again, and discard the wash water.
d.
Add 0.5mL 6M ammonia, NH3, to dissolve the precipitate. Stir.
e.
Centrifuge again, pour the liquid into another test tube, add 1 mL 6M nitric acid,
HNO3, to the liquid. Caution: the solution will get hot and smoke.
f.
Obtain a samplc of the liquid to check for pH. Add more HNO3 to make it acidic.
The appearance of white solid AgCl will confirm the presence of Cl2. Confirmation of Carbonate.
In acidic solutions, carbonate ions form carbon dioxide and water. The carbon dioxide gas will
bubble up when an acid is added to a carbonate solution.
CO32- (aq) + 2H+ (aq) CO2 (g) + H2O (l)
When carbon dioxide is passed through a saturated solution of barium hydroxide, Ba(OH)2, it
will form a white precipitate.
CO2 (g) + Ba2+ (aq) + 2OH- (aq) BaCO3 (s) + H2O (l)
a.

b.

c.

Obtain a strip of colored paper (can be paper from your notebook) and use a Beral
pipet to wet the strip with a saturated solution of barium hydroxide (add 5-6 drops
to the strip)
Place 1 mL of the unknown solution into a test tube and add 0.5 mL of 6M
HNO3
Place the test tube into a hot water bath and observe to see if any gas bubble form.

Place the strip of saturated Ba(OH)2 onto the top of the test tube (the wet part of
the strip should cover the mouth of the test tube.)
Observe for any white precipitate on the strip.
e.
3. Confirmation of Sulfate
d.

Sulfate ions will react with barium ions in aqueous solution to form white solid precipitate
which is insoluble even in acidic solutions.
SO42+ (g) + Ba2+ (aq) BaSO4 (s)
a. Place 0.5 mL of the unknown solution into a test tube.
b. Add HNO3 (drop by drop) until the solution is acidic.
c. Add 0.5 mL 0.2 BaCl2 and observe precipitate formation.
4. Confirmation of Nitrate
Nitrate ions reduce to ammonia as follow:
3NO3+ (aq) +8Al (s) + 5OH- (aq) + 18H2O (l) 3NH3 (g) + 8Al(OH)4- (aq)
Gaseous ammonia, NH3, can turn moist litmus paper from pink to blue.
a. Place 1 mL of the solution in a test tube and add 6M of NaOH until the solution is
basic then add 6 drops in excess.
b. Use a Beral pipet and transfer the solution to another test tube without getting the
walls of the new test tube wet with solution.
c. Add the tip of a spatula containing aluminum granules, careful not to splatter the
solution.
d. Wet one end of a long piece of litmus paper with distilled water. While holding
the dry end, put the wet end into the test tube. (the wet end can touch the wall)
e. Place the test tube in a hot water bath until the solution start to bubble strongly.
f. Let the solution cool down and observe the color change on the litmus paper.
5. Repeat steps 1-6 for anion unknown sample. Record the result for each step.

Post-lab questions
1. What is the precipitating reagent for silver (Ag+)? Would a solution of NaCl work as
well? Why or why not?
2. In the analysis scheme, Ag+ is precipitated as AgCl. The precipitate is then dissolved, and

then AgCl is precipitated again in the confirmatory step. Explain the chemistry of each of
these steps by showing a balanced net ionic equations for each of these steps.
3. When Fe3+ and Cu2+ react with NH3 solution they form two different types of products.
One is a precipitate and one is a complex ion in solution. Write net ionic equations for
these two reactions.
4. Fe+3 can be identified in solution by breaking apart the iron (III) hydroxide, putting Fe+3
back into solution, and then complexing it to form a blood-red solution. Write a net ionic
equation for this process.
5. The confirmatory test for chloride ion with silver ion is the same chemical reaction used
to confirm silver in the cation analysis scheme. Explain what the reaction is and how the
initial precipitate is dissolved and re-precipitated. Use net ionic equations in your
explanation.
6. Write separate oxidation and reduction half-reactions for the procedure used in the test
for nitrate ions.
7. In the nitrate test, why must care be taken to keep the moist litmus from coming in
contact with the cotton or the solution?
8. In step 3, Ba2+ is added to the solution containing all six of the anions and precipitates
BaSO4, but not BaCO3. However, in step 2, the precipitation of BaCO3 is the
confirmatory test for carbonate ion. Why doesnt BaCO3 precipitate in step 3 but does in
step 2?