CHM 361 LABORATORY REPORT

EXPERIMENT : 3
TITLE: QUALITATIVE ANALYSIS OF CATIONS ; Ag+, Fe3+, AND Co2+

NAME : 1) NUR ATHIRAH BINTI ABDUL TALIB

2) NUR ‘ AIN NASUHA BINTI AZHAR

STUDENT NO. : 1) 2020594787

2) 202491518

Class : A4AS120511

DATE OF REPORT : 1 DECEMBER 2022

SUBMISSION

LECTURER’S NAME :
OBJECTIVE
- To separate different cations in aqueous mixtures using selective precipitation and
identify the cations using suitable chemical tests.

INTRODUCTION

Qualitative analysis is the useful process to detect the presence of specific ions in
an aqueous solution. The procedure used to separate and identify more than 20
common metal cations from a single solution consists of selectively precipitating only a
few kinds of metal ions at a time under given sets of conditions (LibreTexts, 2022).
Characteristic colors of aqueous ions as well as solid compounds can be very useful in
identification. Unlike quantitative analysis, where the amount of a particular material is
measured, a qualitative analysis scheme simply confirms the presence or absence of
certain materials. A common analysis is the identification of aqueous ions. In such an
analysis, there are two distinct phases. First, a scheme must be developed to separate
the ions from each other. Then, a different test is performed to uniquely confirm the
identity of each separated ion.

In addition to analyzing the unknown for its component ions, the development of a
qualitative analysis scheme highlights some of the important chemical behavior of these
metal salts in aqueous solution. The principles of chemical equilibrium are emphasized,
as illustrated by precipitation reactions, acid-base reactions, complex-ion formation, and
oxidation-reduction reactions. Ions are often separated in solution by their different
solubilities as noted by Reger et al. (2010). A metal ion in a mixture may precipitate
which forms a solid in the presence of a specific anion, while the remaining metal ions
remain dissolved in aqueous form. The two ions may be separated by collecting the solid
at the bottom of a test tube in a centrifuge, a device that creates a centrifugal force by
rotation. After the precipitate is compacted,the liquid solution above the solid is carefully
poured off into a separate container. In a confirmatory test, each ion has a unique
response to an added chemical, such as a solution colour change or the formation of a
precipitate. This unique response confirms the presence of that particular ion

APPARATUS
- Small test tubes
- Test tube racks
- Test tube holders
- Litmus paper
- Hot plate
- Centrifuge
- Beakers
- Distilled water bottles
- Glass rod
- Dropping pipette
- Vial containing unknown solution

CHEMICALS
- 0.5 M aqueous solutions of Ag+, Fe3+ and Co2+
- 6 M hydrochloric acid solutions, HCl
- 6 M ammonia solution NH3
- 6 M nitric acid solution HNO3
- 0.1 M potassium thiocyanate solution, KSCN
- 0.1 M potassium ferrocyanide solution, K4[Fe(CN)6 ]
- 6 M potassium nitrite, KNO2
- 6 M acetic acid solution, CH3COOH

PROCEDURE
1. A table was created in our lab notebook before coming to the lab. All of our
observations were filled in this table.
2. 2 mL solution containing Ag + (toxic), Fe3+ and Co2+ ions was measured into a test
tube.
 3. 6 drops of 6 M HCl solution (corrosive) was added into ionic solution to bring
about precipitation. By using a clean stirring rod, the content of the test tube was
stirred well.
4. The test tube was centrifuged for 2 minutes. One drop of 6 M HCl was added to
the test tube and carefully observed the supernatant. If more precipitate was
formed upon this addition, few more drops (1-2 drops) of HCl was added and will
be centrifuged again. The solution was tested again to ensure a complete Ag
precipitation.
Confirming the presence of Ag+ ion
5. When the precipitation of silver(I) chloride is completed, the supernatant was
decanted into a clean test tube, it was labeled and set aside. The precipitate was
washed in the test tube by adding 10-15 drops of water to it. The precipitate was
stirred well and the test tube was centrifuged. The supernatant was decanted and
discarded. This procedure was repeated to wash the precipitate one more time.
6. In a fume hood, 8 drops of 6 M NH 3, solution (corrosive, irritant, strong fumes)
were added to the washed precipitate and it was stirred well. Our observations
were recorded.
7. 6 M HNO3, solution (corrosive, strong oxidant) was added while mixing, until the
solution was shown as acidic when tested with a litmus paper. Our observations
were recorded.
All precipitates and solutions that we suspected contained silver were discarded
into the chemical waste bottle labeled "Silver".

Separating and confirming the presence of Fe3+ ion

8. 16 drops of 6 M NH3 solution was added to the supernatant that was set aside earlier
until the solution was shown as basic when tested with the litmus paper. The solution
was stirred well and be sure the solution was strongly basic!
9. The test tube was centrifuged and tested for complete precipitation. When it has been
determined that the precipitation of iron(III) hydroxide was completed, the supernatant
was decanted into a clean test tube,and it was labeled and set aside.

10. The remaining precipitate was washed with water. 10 drops of 6 M HCI was added to
the clean precipitate. The mixture was heated in a boiling water bath to dissolve the
precipitate, if necessary. When the precipitate was dissolved, it was tested with a litmus
paper to be sure it was strongly acidic.

11. The solution was separated into two approximately equal portions.

12. To one portion, 3 drops of 0.1 M KSCN solution were added and our observations
were recorded.

13. To the other portion, 6 M NH3 was added until the solution, which was initially
strongly acidic, became weakly acidic. If the solution becomes basic, 6 M acetic acid
solution was added dropwise until it was weakly acidic. Three drops of 0.1 M
K4[Fe(CN)6 ] solution were added and our observations were recorded.

Confirming the presence of Co2+ ion

14. To the supernatant that was set aside, 6 M HCI was added until the solution became
acidic. In a fume hood (the gas generated is toxic!), six drops of 6 M KNO2 solution
(oxidizer, irritant) was added, the solution was mixed well and our observations were
recorded. When the evolution of gas has subsided (this may require several minutes),
the test tube was centrifuged and discarded the supernatant so that the precipitate and
its colour could be clearly observed. The appearance of a yellow precipitate confirmed
the presence of Co2+.
15. An unknown solution containing one or more cations (Ag +, Fe3+, and Co2+) was
obtained. The above procedure was repeated by using 15 drops of this solution. All of
our observations were recorded and then filled in the data sheet.

RESULTS
DATA SHEET

EXPERIMENT 3
Qualitative Analysis of Cations : Ag+, Fe3+, and Co2+

Name : 1.NUR ATHIRAH BINTI ABDUL TALIB

2.NUR’ AIN NASUHA BINTI AZHAR
Student ID : 1.2020594787
2.2020491518
Date of Experiment : 10 NOVEMBER 2022
 RESULTS
Table 1 : Known solution containing Ag+, Fe3+ and Co2+ ions

Steps Substance Reagent Observation Conclusion

Got silver
1 Known solution 6 M HCl, 3 drops White precipitate precipitates silver(I)
(clear, colourless) presence chloride

Confirmation the
White precipitate presence of Ag+ ion
2 Known solution 6 M NH3, presence in cloudy
(ppt) 8 drops

The solution is in
Litmus paper color basic and
3 Known solution 6 M HNO3, change from blue confirmation the
(ppt) 3 drops to red presence of Ag+ ion

Precipitate is formed
Red ppt and litmus of Fe(OH)3 and the
4 Supernatant 6 M NH3, 16 drops paper change from solution is in acidic
+ 6 M HCl,10 drops red to blue

Confirmation the
0.1 M KSCN, Red brick colour presence of Fe3+
5 ppt dissolved 3 drops solution ion

6 M NH3, 6 M acetic Confirmation the

6 ppt dissolved Deep blue color presence of Fe3+
acid, solution ion
0.1 M K4[Fe(CN)6],3
drops
 Table 2: Unknown solution containing Ag+, Fe3+ and Co2+ ions

Steps Substance Reagent Observation Conclusion

Got silver
1 Unknown solution 6 M HCl, 6 drops White precipitate precipitates silver(I)
(clear, colourless) presence chloride

6 M NH3, Confirmation the

2 Unknown solution White precipitate
presence of Ag+ ion
(ppt) 8 drops presence in cloudy

The solution is in
Litmus paper colour basic and
3 Unknown solution 6 M HNO3, change from blue confirmation the
(ppt) 3 drops to red presence of Ag+ ion

Precipitate is formed
Red ppt and litmus of Fe(OH)3 and the
4 Supernatant 6 M NH3, 16 drops paper change from solution is in acidic
+ 6 M HCl, 10 blue to red
drops

Confirmation the
0.1 M KSCN, Red brick colour presence of Fe3+
5 ppt dissolved 3 drops solution ion

6 M NH3, 6 M acetic Confirmation the

6 ppt dissolved Deep blue colour presence of Fe3+
acid, solution ion
0.1 M K4[Fe(CN)6],3
drops

Identification of unknown solution :

Cations found in the solution : Ag+ and Fe3+
DATA ANALYSIS / JUSTIFICATION / VALIDATION /CALCULATION

From the result, in steps 1 and 2, both known and unknown solutions showed the
presence of Ag+ ion. This can be confirmed by the observation of the white precipitation
of the silver ion as it is known as an insoluble silver chloride, AgCl salt. This precipitation
is accomplished simply through the addition of hydrochloric acid, HCl In step 1. The
reaction for this reaction is Ag +(aq) + HCl (aq) → AgCl (s) + H+ (aq). Then, iron (III) and
cobalt (II) cations not showing observations that form insoluble chloride salts, but for
silver in the form of a precipitate was then separated from the supernatant into another
test tube. Next, to confirm the presence of silver in the precipitate, ammonia, NH 3 is
added, as in the step 2 which results in the dissolution of the silver(I) compound, where
white precipitate presence in cloudy form. AgCl(s) + 2NH 3(aq) → Ag(NH3)2+(aq) + Cl–(aq).
Then, nitric acid was added which will shift the equilibrium to the left as the acid reacts
with the ammonia, NH3, that causes the silver ion to re-precipitate as silver chloride and
turn litmus paper color change from blue to red as in step 3.

Then, for step 4 of known and unknown solutions, the supernatant that was
decanted and ammonia were added to this solution causes the iron (III) ion to form an
insoluble and precipitate ferum(III) hydroxide, Fe(OH) 3. So, when tested, using the litmus
paper will change color from red to blue as a strong basic solution. The equation for this
reaction is Fe3+(aq) + 3 NH3(aq) + 3 H2O(l) → Fe(OH)3(s) + 3 NH4+(aq).
Centrifugation and decantation leaves Fe(OH) 3 solid, which can be dissolved in hot
hydrochloric acid, HCl. Then two tests were done for confirmation iron (III), Fe 3+ ion. First
is in step 5 by addition of potassium thiocyanate solution, KSCN. This reaction produced
a red-brick colour solution as Fe 3+ was present and the equation of this reaction is Fe 3+
(aq) + SCN–(aq) → Fe(SCN)2+ (aq). For the second test, ammonia, NH 3 is first added until
the solution is only weakly acidic, and this is followed by the addition of potassium
ferrocyanide, K4[Fe(CN)6], solution. Then, deep blue solution will appeared when iron
(III), Fe3+ is present as the equation for this reaction is 4Fe 3+(aq) + 3 K4[Fe(CN)6](aq) →
Fe4[Fe(CN)6]3 (s) + 12 K+.

QUESTION

1. If potassium ferrocyanide, K 4 [Fe( CN ¿¿ 6], is added to a strongly acidic solution,

toxic hydrogen cyanide, HCN, gas is produced. Balance the following equation,
which represents this reaction:
K 4 [Fe( CN ¿¿ 6] + HCl → HCN + KCl + FeCl 2

Balance equation = K 4 [Fe( CN ¿¿ 6 ¿ + 6HCl → 6HCN + 4KCl + FeCl 2

2. In the confirmation test that you performed for A g+¿¿ ion, addition of nitric acid, HN
O3, to a solution containing Ag+ produced a white precipitate of AgCl. Where did
the chloride ion come from?

= It came from adding HCl solution to the silver cation. During the confirmation
test of silver (Ag+ ), we have to take a little amount of salt of Ag+ and add some
HCl reagent to it, then all the silver present will precipitate out as AgCl.
Ag + Cl−¿ ¿ (HCI) → AgCl

After that we will have to centrifuge this solution to get centrifugation. This will be
dissolved in NH3 to form a clear solution. Then, if we add HNO 3 reagent, it will
form a white ppt again. Hence, the chloride ion comes from 6 M HCL that was
added to clean the precipitate.
DISCUSSION

Qualitative analysis is an analytical procedure in which to observed what is

present in the compound. In a systematic qualitative analysis, each substance present is
separated from the other substances. Then a confirmatory is used to prove that the
isolated substances is the expected result for each substance. The objective of this
experiment was achieved. The silver cation (Ag+) reacts with the chlorine anion (Cl-) in
the presence of soluble chlorides such as hydrochloric acid, and silver(I) chloride forms
as a white precipitate. The precipitate of silver (I) chloride (AgCl) was then added with
6M NH3 and the solution turns to cloudy white precipitate which shows the presence of
Ag+ ion. Other than that,

In order to show the presence of Fe3+ ion, the solution of known and unknown was
tested with two different reagents. Firstly, when KSCN was added to the solutions, it will
turn the orange solution to red brick. This is because iron III thiocyanate is formed thus
this shows that fe3+ iron is present. Besides when 0.1M of K4[FE(CN)6] was added, the
solution change from orange to dark blue. This is due to formation of iron (III)
hexacyanidoferrate that will prove the presence of ion Fe3+.

For this experiment, the presence of the cobalt ion, Co 2+ which remains in the decanted
supernatant solution in step 14, can be confirmed by a simple test. The basic solution is
made strongly acidic with the addition of hydrochloric acid, HCl. Then, addition of a
solution of potassium nitrite, KNO2, will produce an insoluble yellow compound,
potassium hexanitritocobaltate, K3[Co(NO2)6] and the equation for this reaction is
Co2+(aq) + 7NO2(aq) + 3 K+(aq) + 2H+(aq) → NO(g) + H2O(l) + K3[Co(NO2)6]
The reaction produces nitric oxide, NO, which is a colorless gas. Nitric oxide reacts with
oxygen in the air to produce nitrogen dioxide, NO 2, which may be visible as a red-brown
gas.Reaction : 2 NO(g) + O2(g) → 2 NO2 (g).
One source of error was the unsanitary pipets used. Many consisted of other solutions
that were not washed that could have affected the results. Test tubes were also at times
dirty and not washed thoroughly. Some of the solution was also accidentally spilled,
causing the accuracy of the test to be fatal. At times, the solution was not stirred
thoroughly and could have disrupted the solution’s results.

CONCLUSION
In conclusion, our objective is achieved to separate different cations in aqueous mixtures
using selective precipitation and identify the cations using suitable chemical tests. In this
experiment, Ag+ , Fe3+, Co2+ cations were tested to know if these cations are present in
known and unknown solutions. Chemical tests by using HCL and NH 3 solutions can be
used to identify the presence of Ag + ions when white precipitate presence in cloudy.
Then, for Fe3+ ions can be identified by using KSCN because it will show a red brick
colour solution if the solution consist of Fe 3+ ions . Other than that, Fe 3+ ions can be
shown if there is K4[Fe(CN)6] solutions too because if the observation shows deep blue
color solution, it will prove the presence of Fe 3+ ions. Last for Co2+ cation, can be
identified by using HCl and KNO 2 solution. The presence of Co 2+ ions can be shown by
the appearance of a yellow precipitate when the solution that contains Co 2+ ion is added
with KNO2 solution . Thus,this shows that our known solution consists of Ag + , Fe3+, Co2+
cations meanwhile The unknown solution consists of the ions Ag+ and Fe3+ since the
presence of Co2+ ion is not confirmed due to no confirmation test of this ion was made.

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