SEM OCTOBER 2022 - FEBRUARY 2023

LABORATORY REPORT
CHM361
QUALITATIVE ANALYSIS OF CATIONS: Ag+,
Fe3+ AND CO2+
NAME : MUHAMMAD AIMAN BIN ZAIZILAN/

MOHAMMAD SHUKRI MOHAMMAD SUIB

STUDENT ID : 2020494552 / 2020824588

GROUP : AS1205D
CRITERIA FULL OBTAINED

Procedure 2%

Results / Data / Observation (Datasheet) 2%

Data Analysis / Justification / Validation 4%

Question 2%

Discussion 2%

Conclusion 1%

Format 2%

Data Sheet EXP 3 5%

Total 20%
OBJECTIVE

• To separate different cations in aqueous mixtures using selective precipitation

• To identify the cations using suitable chemical tests.

INTRODUCTION

Qualitative analysis is the process of separating and identifying components of mixtures. Differ
than quantitative analysis, which measures the amount of a specific element, a qualitative
analysis just verifies the existence or absence of various components. Then, a different test is
run to establish the identification of each isolated ion. In this experiment, we implement a
qualitative analysis method to separate and identify the components of a chemical mixture to
determine the presence of cations which is silver(I), iron (III) and cobalt (II) ions.

The elemental component of inorganic salts is determined using qualitative analysis, an

analytical chemistry technique. It mainly focuses on ion detection in an aqueous salt solution.
During qualitative analysis, the ions in a mixture are separated using selective precipitation.
When a carefully chosen, reagent is added to an aqueous mixture of ions, one or more of the
ions precipitate while the others remain in solution. This is referred to as selective precipitation.
Each ion can be separated, and then its identity can be confirmed using a chemical reaction
specific to that ion.

Cations are present in various salts and have variable solubilities in water. The differential
in solubility of these salts can be used to separate the cations. Consider the characteristics of
calcium (Ca2+) and sodium (Na+) cations. Calcium chloride is easily soluble in water, but
calcium hydroxide is almost completely insoluble. In contrast, sodium chloride and sodium
hydroxide are both very soluble in water. An aqueous solution containing a combination of
calcium chloride and sodium chloride can be treated with an aqueous solution containing
hydroxide ions.

A solid precipitate of insoluble calcium hydroxide will occur because of this treatment. In
contrast, the sodium hydroxide remains dissolved in water. Filtration can be used to separate
the solid carrying calcium ions from the aqueous solution containing sodium ions.
APPARATUS

• Small test tubes

• Test tube rack
• 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 solution, 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. Table was created in lab notebook before coming to lab. All observations were entered
in this table.
2. 2 mL solution containing Ag+(toxic) Fe3+, and Co2+ ions were measured into a test tube.
3. 6 drops of 6 M HCl solution (corrosive) were added to ionic solutions to bring about
precipitation. The contents of the test tube were sure to be stirred (with a clean stirring
rod).
4. The test tube was centrifuged for 2 minutes. One drop of 6 M HCl was added to the test
tube and the supernatant was observed carefully. If more precipitate was formed upon
this addition, a few more drops (1-2 drops) of HCl were added and 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 was completed, the supernatant was
decanted into a clean test tube, labelled, and set it 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 one more time.
6. In a fume hood, 8 drops of 6 M NH3 solution were added to the washed precipitate and
stirred well. Observations were recorded.
7. 6 M HNO3 solution was added while mixing until the solution is acidic when tested
with a litmus paper. Observations were recorded.

Separating and confirming the presence of Fe3+ ion.

8. Sufficient amount of 6M NH3 solution was added to the supernatant that was set aside
earlier until the solution is basic when tested with the litmus paper. The solution is
stirred well and be sure that it 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, labelled it and set it aside.
10. The remaining precipitate was washed with water. 10 drops of 6 M HCl were added to
the clean precipitate. The mixture was heated in a boiling water bath to dissolve the
precipitate, if necessary. When the precipitate has 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 the observations were
recorded.
13. To the other portion, 6 M NH3 was added until the solution, which was initially strongly
acidic, to be weakly acidic. 6 M acetic acid solution was added dropwise until it is
weakly acidic if the solution becomes basic. Three drops of 0.1 M K4[Fe(CN)6]
solution were added and observations were recorded.
 DATA SHEET

EXPERIMENT 3

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

Date of Experiment : 15 November 2022

RESULTS
Steps Substances Reagent Observation Conclusion
1 Ag+, Fe3+ 6 M HCl, 3 drops Pale orange solution is Fe3+ ions were
(clear, colourless) formed with white dissolved in the
precipitate solution and Ag+
ions were present
6 Ag+ ion 6 M NH3, 8 drops Milky yellow solution Ag+ ions were
(clear, colourless) present

7 Ag+ ion 6 M HNO3, 7 drops Blue litmus paper turn Solution is acidic
(clear, colourless) red

8 Fe3+ ion 6 M NH3, 20 drops Red litmus paper turn Solution is basic
(clear, colourless) blue

12 Fe3+ ion 0.1 M KSCN, Yellow solution turns Fe3+ is present

3 drops brown
(clear, colourless)

13 Fe3+ ion 0.1 M K4[Fe(CN)6], Brown solution turns Fe3+ is present

3 drops dark blue
(yellow colour)

Identification of unknown solution: Ag+ and Fe3+

Cations found in the solution: Ag+ and Fe3+
QUESTIONS

1. If potassium ferrocyanide, K4[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:

K4[Fe(CN)6] + HCl → HCN + KCl + FeCl2

K4[Fe(CN)6] + 6HCl → 6HCN + 4KCl + 2FeCl2

2. In the confirmation test that you performed for Ag+ ion, addition of nitric acid, HNO3 , to a
solution containing Ag+ produced a white precipitate of AgCl. Where did the chloride ion
come from?

Nitric acid (HNO3) will react with ammonia (NH3), ammonium nitrate (NH4No3), and
other substances to change the equilibrium to the left. This reaction results in the formation
of silver chloride, a white precipitate, rather than Ag+.

AgCl(s) + 2NH3(aq) → [Ag(NH3)2](aq) + Cl- (aq)

DISCUSSION

Qualitative analysis is a branch of science that investigates the substance or chemical

composition of a sample. It describes the presence or absence of various chemical components
in an unknown sample. In qualitative analysis, only the identity of metal ions is determined,
not the amount. To validate the results, a confirmatory test of the separated material and its
impurities is performed. Only a minor amount of ingredients is used to carry out this
experiment.

Firstly, 3 drops of the hydrochloric solution are added to the known solution. A white
precipitate formed at the bottom of the test tube for the known solution which shows that the
solution contains the silver ion Ag+. At the same time, the solution turns pale orange, indicating
that Fe3+ ions were dissolved. However, after the application of the unknown substance, there
are no changes that would indicate the presence of Ag+.

Additional confirmation testing is done to determine whether Ag+ is present in the

sample. Using the AgCl precipitate left from the prior reaction, 8 drops of NH3 are added to
the solution. As a result, the solution turns milky yellow. However, the unknown solution does
not undergo any changes when the same reagent is applied which indicates that there is no
presence of Ag+ in the solution. Then, 7 drops of 6M HNO3 solution are added to both known
and unknown solution. Both of the solutions are proven acidic as blue litmus paper turns red.
It indicates that Ag+ is present.

In the next step, the previously set aside supernatant is mixed with 20 drops of a 6M
NH3 solution. It is tested with litmus paper to prove that it is strongly basic. As a result, the red
litmus paper turns blue which indicates that it is strongly basic. The result is also applicable to
the unknown supernatant. Then, the first portion of the separated solution is added with 3 drops
of 0.1 M KSCN solution which turns the yellow solution to brown.

Next, 10 drops of 6M NH3 are added to the previous solution. As a result, the brown
solution turns to dark blue. Apart from that, it is also proven that the solution which was initially
strongly basic, has become weakly basic. Thus, it is confirmed that there is a presence of Fe3+
ions in both unknown and known solutions.
CONCLUSION
Test using HCL and NH3 solution can be used to identify the presence of Ag+ ion. KSCN and
K4 [Fe(CN)6] solutions can be used to detect Fe3+ ions. Using litmus paper, one may determine
the acidic and the basic solutions.
REFERENCES

• Vedantu. (2022, November 29). Qualitative chemical analysis. VEDANTU. Retrieved

January 7, 2023, from https://www.vedantu.com/chemistry/qualitative-chemical-
analysis
• Qualitative Analysis of Cations (Theory): Class 11: Chemistry: Amrita Online Lab.
Retrieved 3 January 2023 from:
https://amrita.olabs.edu.in/?sub=73&brch=7&sim=180&cnt=1