CHM361 LABORATORY REPORT

EXPERIMENT 2

QUALITATIVE ANALYSIS OF CATIONS: Ag+, Fe3+, Cu2+, and Ni2+

Name: Nurul Azwa binti Mansur

Student No: 2016747873

Lab group: 5A

Date of Report Submission: 31 MARCH 2019

Lab Partner’s Name:

1) Norafifa binti Anjam@Ampau
2) Nur Izzatie binti Zainorin

Lecturer’s Name: Mdm Rabuyah Binti Ni

OBJECTIVES:

1. To understand the rationale and the procedure behind the separation for various
cations.
2. To determine cation present in the unknown solution using established schemes.

INTRODUCTION:

Qualitative analysis is the process by which components of mixtures are

separated and identified. 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 this lab, we develop
a qualitative analysis scheme to separate and identify the components of a chemical
mixture. The mixture will be composed of the iron (III) ion (Fe 3+), the barium ion
(Ba2+), and the silver ion (Ag+).

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. A metal ion in
a mixture may precipitate (form 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 supernatant (the liquid solution above the solid) is decanted (carefully poured off)
into a separate container. The soluble ion is in the liquid supernatant while the
insoluble ion is in the solid precipitate. Thus they are physically separated from each
other when the liquid is poured off, leaving the solid behind. The solid precipitate is
typically washed with water to help remove any traces of the soluble ions that remain.
This prevents "false positive" test results later on.
Once the ions in a mixture have been separated, their identity can be further
verified by a confirmatory test. In a confirmatory test, each ion has a unique response
to an added chemical, such as a solution color change or the formation of a
precipitate. This unique response confirms the presence of that particular ion.

APPARATUS:

 Small test tubes

 Test tube rack
 Small test tube stoppers
 Test-tube holders
 Hot plate
 Centrifuge
 250 mL beakers
 Spatula
 Stirring rod
 Distilled water bottle
 Glass rod
 Dropping pipette
 Litmus paper
 Vial containing unknown solution

CHEMICALS:

Unknown Cationic Solutions

 0.05 M silver nitrate AgNO3 (aq)

 0.05 M copper (II) nitrate Cu(NO3)2 (aq)
 0.05 M nickel nitrate Ni(NO3)2 (aq)
 0.05 M iron (III) nitrate Fe(NO3)2 (aq)
 6 M HCl (aq)
 6 M HNO3 (aq)
 6 M NH3 (aq)
 6 M H2SO4 (aq)
 6 M NaOH (aq)
 6 M CH3COOH (aq)
 0.1 M K4[Fe(CN)6]
 0.1 M KSCN
 Unknown solution

EXPERIMENTAL PROCEDURE:

Qualitative Analysis of Cations

1. Separation of the silver from iron, copper, and nickel ions.

a) 8 drops of 6 M HCl was added to the solution to be analyzed and it was stirred. A
white precipitate indicates that the Ag+ was presented.
b) The solution was centrifuged and it was tested with one drop of 6 M HCl to make
sure that precipitation is complete and no additional precipitate formed. More
precipitate does form, so that 6 M HCl was added until precipitation is complete.
c) The clear solution was centrifuged, decanted (poured off), and saved into a
second test tube for procedure 3.
d) The precipitate was washed by adding 1 ml distilled water and stirred. The wash
water was centrifuge and discarded.

2. Confirmation of silver.

a) 1 mL of 6 M NH3 was added to the precipitate from procedure 1d, which is AgCl.
b) It was stirred until the precipitate completely dissolves.
c) 15 drops of 6 M HCl was added to the solution. The solution was fumed and the
reaction between the strong acid and the base were given off heat and silver was
presented. The test tube may get very warm.
d) It was stirred and tested with litmus paper to ensure the solution is acidic. More
HCl was added if it is not acidic. The appearance of the white AgCl precipitate in
the acidic solution confirms the presence of silver.
e) The silver compound was disposed as directed by the instructor.

3. Separation of iron and copper from nickel.

a) 6 M NaOH was added with stirred to the solution saved from procedure 1c until
the solution is basic and then 3 more drops was added.
b) The test tube was stirred and placed in a hot water bath for 3 minutes. The
formation of a precipitate indicates the presence of either copper or iron or both.
c) The solution was centrifuge and the clear solution was separated from the solid.
The clear solution was saved for procedure 6.
d) The precipitate was washed with a mixture of 10 drops of 6 M NaOH and 10
drops of water.
e) The wash water was centrifuge and discarded. The precipitate was saved for
procedure 4.

4. Separation of iron from copper; confirmation of copper.

a) 5 drops of water was added to the precipitate from procedure 3.

b) About six drops of 6 M H2SO4 dropwise was added until the solution is acidic
when tested with litmus paper. It was stirred to dissolved the precipitate.
c) 6 M aqueous NH3 was added to the solution until the solution is basic to litmus,
and then 1 mL extra was added.
d) The supernatant liquid was centrifuged and separated from the precipitate. The
precipitate was kept for procedure 5. The presence of the blue Cu(NH 3)42+ ion is
the confirmatory test for copper.
e) For an additional confirmatory test, 6 M CH 3COOH, acetic acid was added to the
solution containing the Cu(NH3)42+ until the blue colour fades and the solution
becomes acidic. Then, 2 drops of 0.1 M K4[Fe(CN)6] was added. A red-brown
precipitate of Cu2[Fe(CN)6] reconfirms the presence of copper.
f) The copper solution was disposed as directed by the instructor.
5. Confirmation of iron.

a) The precipitate of iron hydroxide from procedure 4d has been washed.

b) 6 M H2SO4 dropwise was added until the precipitate dissolves.
c) 5 drops of 0.1 M KSCN solution was added to the solution. The deep red
[FeSCN]2+ ion confirms the presence of iron.
d) The iron solution was disposed as directed by the instructor.

6. Steps 1-5 was repeated for the cation unknown sample. The results of each step was
recorded.

OBSERVATION:

Qualitative Analysis of Cations

Step Procedure Known solution Unknown

solution
Results Concl Results
usion
1 Add HCl to known solution in White precipitate White
TT1. centrifuge. Pour coloured forms precipitate
solution into TT2. forms
2 Add NH3 to precipitate TT1. Precipitate dissolve Ag+ Precipitate
Dissolve precipitate. Add HCl. in NH3 white prese dissolve in
Precipitate forms. precipitate with nt. NH3
HCl. white
precipitate
with HCl.
3 To solution in TT2, add NaOH. Precipitate forms. Cu2+ Precipitate
Solution basic. Heat. Precipitate and forms
forms. Pour solution in TT3. add Fe3+
NaOH and water to precipitate in may
TT2. Centrifuge. Discard be
solution. prese
nt.
4 To TT2, add H2SO4 until Basic solution blue Cu2+ Basic
solution is acidic. Stir to dissolve prese solution
ppt. Add NH3. Precipitate forms. nt blue
Solution blue. Centrifuge,
discard blue solution.

5 Wash ppt in TT2. Add H2SO4 Acidic solution Zn2+ Acidic

until precipitate dissolves. Add 5 turns deep red. prese solution
drops KSCN. Solution turns nt. turns deep
deep red. red.

ANALYSIS:

Identify the cations present in the unknown cationic solution.

Ag+, Fe3+, and Ba2+.

QUESTIONS:

1. Write out the balanced net ionic equations for all the observations in the analysis
of the known cationic solution. Indicate the color of the ions and precipitate
underneath the chemical species.
Step Cation Colour Balanced chemical equation
1 Ag+ Colorless Ag+(aq) + Cl-(aq) → AgCl (s)
2 Fe3+ Pale violet Fe3+(aq) + OH- (aq) → Fe(OH) 3 (s)
or brown
2+
3 Cu Pale blue Cu2+(aq) + OH- (aq) → Cu(OH) 2 (s)

4 Ni2+ Pale green Ni2+ (aq) + 6 NH3 (aq) → Ni(NH3)62+ (aq)

5 Ba2+ Green Ba2+(aq) + SO42_ (aq) → BaSO4 (s)

2. What is the precipitating reagent for silver (Ag +)? Would a solution of NaCl
work as well? Why or why not?
HCl is the 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 solution will work.

DATA/RESULT:

Table 2.1: Qualitative Analysis of Cations

Step Procedure Known solution Unknown

(Be specific) solution
Results Conclusion Results
1 6 M HCl White Ag2+ ion is No precipitate
precipitate present
formed
2 6 M NH3 White Ag2+ ion is No precipitate
precipitate present
formed

3 6 M NaOH Clear solution Ni2+ ion is Blue green

obtain present precipitate is
present

4 6 M H2SO4 Red-brown Cu2+ ion is No precipitate

 precipitate present
formed
5 6 M H2SO4 Deep red Fe3+ ion is Deep red ion
precipitate present was present
formed

DISCUSSION:

Qualitative analysis is the analytical procedure to discover the things present. A

systematic qualitative analysis scheme is used to find the substances present and
alienated from other substances. Then a confirmatory test is used to prove the results
of the separated substance and its containments. This experiment is used in small
quantities of reagents on a semi-micro scale. Thus, experimental errors can be
exposed greatly if cleanliness and care are ignored.

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:

The unknown solution consists of the ions Ag+ and Cu2+.

REFERENCES:
1. Electrolysis of Sodium Chloride | Introduction to Chemistry. (n.d.). Retrieved
from https://courses.lumenlearning.com/introchem/chapter/electrolysis-of-
sodium-chloride/
2. F., V. (n.d.). Why doesn't NaCl and HCl have the same effect on an equilibrium
reaction. Retrieved from
https://www.wyzant.com/resources/answers/242847/why_doesn_39_t_nacl_and
_hcl_have_the_same_effect_on_an_equilibrium_reaction
3. the qualitative analysis of Ag+, Cu+ and Zn2+. (n.d.). Retrieved from
https://www.academia.edu/17108134/the_qualitative_analysis_of_Ag_Cu_and_
Zn2_
4. What is the precipitating reagent for the silver group (Ag+, Hg2 2+, Pb2+)?
(n.d.). Retrieved from https://answers.yahoo.com/question/index?
qid=20090607172833AAzeIoC