CHM 475: Inorganic Chemistry

NO. OF
EXPERIMENT
TITLE

Experiment 1 & 2
Qualitative Analysis for Identification of Metal ions

NAME

Siti Farah Wahida binti Ismail

ID NUMBER
PARTNERS
NAME
GROUP
LECTURERS
NAME
LAB
INSTRUCTOR
DATE OF
EXPERIMENT
DATE OF
SUBMISSION

2014773321
Syahirah binti Bakri
ED2474A
Dr. Amalina Tajuddin
Puan Nurul Izza Taib
27th September & 4th October 2016
18th October 2016

Introduction
Cation is an ion that consists of positive charge which come from the loses of
electrons. Among the elements in the periodic table, the alkali metals (Group 1) and alkalineearth metals (Group 2) are the most reactive metals, having one and two valence electrons,
respectively. Therefore, metals lose that electrons and form cations. For example, Zn2+,
Mg2+and Fe2+.
For covalent compound, which involved reactions between non-metals and nonmetals can be identified by using the physical properties like testing on the boiling or melting
point, refractive index or solubility in the solution but for ionic compound which involved the
metal cations, qualitative analysis was used. Qualitative analysis will determine the chemical
properties of an unknown by taking the end result of several reactions with numbers of
reagent. Before conducting the qualitative analysis, the predetermine step should be done first
as to know what particular reaction will take place if a specific ion is present. By knowing the
reaction later on the ions in the unknown can be determined. For example, if a reaction is
known to produce a precipitate if ion A is present and a precipitate is formed when the
reaction is run, then ion A may be present in solution. If no precipitate is formed when the
reaction is run, then ion A is clearly not present in the unknown solution and a different
reaction will have to be run to determine what ions are present.
There are two general situations in which qualitative analysis is used which is in the
identification of a simple salt, or the identification of multiple cations in a solution. For
experiment 1 and 2, we are using a mixture and unknown and getting to identify the multiple
cations in a solution.
Objectives
Experiment 1: To identify the metal cations present in the mixture,
unknown 1 and unknown 2 by using qualitative analysis
Experiment 2: To have the confirmation on the present of ions, Ag +, Cu2+
and Zn2+ by conducting the confirmation test.

EXPERIMENT 1: Qualitative Analysis for Identification of Metal Cations

Materials and Apparatus

Materials
- Unknown 1
- Unknown 2
- Mixture
- Distilled water
- 6M HCl
- 6M NH3
- Thioacetamide
- (NH4)2CO3
- 1M K2CrO4
- 1M K2C2O4

Apparatus
- Test tubes
- Measuring cylinder
- Dropper
- Centrifuge

Methods
Procedure A
1. 2 drops of 6M HCl were dropped to 1ml of the mixture of the metal
cation
2. The suspension was centrifuged for 1 minute when the ppt of
chloride is formed.
3. 1 additional drop of 6M HCl was added to the clear supernatant to
check for complete precipitation
4. The suspension was centrifuged again for one minute when the ppt
is observed
5. The supernatant was decanted in a clean test tube
6. The supernatant was saved for procedure B
Procedure B
1. 6M NH3 was added dropwise to the solution until it is basic.
2. The sample was put in the boiling water bath for 2-3 minutes to
remove the excess NH3
3. The volume of the solution was adjusted to 2mL with distilled water
and 10 drops of 6M HCl was added.
4. 12 drops of thioacetamide were added to the solution and stirred
wisely
5. The sample was heated in the boiling water bath for 10 minutes to
allow the hydrolysis of thioacetamide producing H2S

6. The sample was centrifuged for 2 minutes after the ppt of sulphide
is formed and the supernatant was decanted to a clean test tube
7. The supernatant was saved for procedure C
Procedure C
1. 3 additional drop of thioacetamide was added to the supernatant
and was reheated for five more minutes to test for complete
precipitation
2. The solution was centrifuged after the ppt was formed and the
supernatant was decanted into a clean test tube and the ppt was
discarded
3. The volume of the solution was adjusted to 3mL with distilled
water and 10 drops of 6M HCl and 10 drops of 6M NH 3 were
added
4. 6M NH3 was added dropwise until the solution is basic.
5. 5 additional drop of 6M NH3 and 12 drops of thioacetamide were
added and the mixture was stirred thoroughly.
6. The sample was heated in the boiling water bath for 10 minutes
7. The sample was centrifuged when the ppt of sulphide is formed
and the supernatant was decanted.
8. The supernatant was saved for procedure D.
Procedure D
1. 6M NH3was added dropwise to the sample until it changed basic
2. 10-15 drops of NH3were added to the buffer solution
3. 20-30 drops of (NH4)CO3 were added to the sample and stirred to
mix
4. The test tube containing ppt of carbonate was transferred to the
warm water bath of 70-80oC for 2-3 minutes.
5. The warmed mixture was centrifuged and the supernatant was
decanted which containing either Na+ or K+
6. The ppt was saved for procedure D(i)

Procedure D (i)
1. The ppt was washed with 2mL of distilled water. The sample was
centrifuged and the wash water was decanted
2. 6M of acetic acid was added dropwise and stirred to dissolved the
ppt
3. A few more drops of 6M acetic acid were added until it became
acidic.
4. 6 drops of 1M K2CrO4 was added to the solution and stirred
5. The sample was centrifuged after the ppt of chromate is formed
6. The supernatant was saved for procedure D(ii)

Procedure D(ii)
1. 10 drops of 1M K2C2O4 were added to the solution and stirred
about 10 minutes
2. The solution was centrifuge after the ppt of oxalate is formed.

Results and Observations

Observation

Balanced chemical equation

1. On adding HCl to the initial sample

Unknown 1: clear supernatant
Unknown 1: Unknown 2: formed white

Unknown 2: Ag+(aq) + Cl-(aq)

precipitate

Mixture: Ag+(aq) + Cl-(aq) AgCl(s)

AgCl(s)

Mixture: formed white precipitate

2. On adding H2S under acidic condition
Unknown 1: clear supernatant

Unknown 1:

Unknown 2: formed white

Unknown 2: Cu2+(aq) + S2-

precipitate

Mixture: Cu2+(aq) + S2-

CuS
CuS

(s)

(s)

Mixture: formed white precipitate

3. On adding H2S under basic condition
Unknown 1: clear supernatant
Unknown 1: Unknown 2: formed white

Unknown 2: Zn2+ (aq) + S2-(aq)

precipitate

Mixture: Zn2+ (aq) + S2-(aq)

ZnS
ZnS

(s)

Mixture: supernatant change to

brown
4. On adding CO32Unknown 1: clear supernatant

Unknown 1:

Unknown 2: formed white

Unknown 2: Ba2+(aq) + CO32-

precipitate

Mixture: Ba2+(aq) + CO32-

BaCO3
BaCO3

Mixture: white precipitate formed

in blue supernatant
5. On adding CrO42Unknown 1: clear supernatant
Unknown 1: Unknown 2: yellowish precipitate

Unknown 2: Ba2+(aq) + CrO42 (aq)-

formed

BaCrO4

Mixture: yellowish white

Mixture: Ba2+(aq) + CrO42-

BaCrO4

precipitate formed
6. On adding C2O42Unknown 1: clear supernatant
Unknown 1: Unknown 2: yellowish precipitate

Unknown 2: Ba2+(aq) + CO32-(aq)

formed

BaCO3

(s)

Mixture: yellowish precipitate

Mixture: Ba2+(aq) + CO32-(aq)

formed
Unknown Number 2 contains Zn2+, Na+ or K+

BaCO3

EXPERIMENT 2: Qualitative Analysis of Transition Metal Cations: Ag+, Cu2+ and Zn2+
Materials and Apparatus
Materials
- Unknown 2
- Mixture
- Distilled water
- 6M HCl
- 6M NH3
- Thioacetamide
- 6M HNO3
- 6M CH3COOH
- 0.1M K4 Fe(CN)6

Apparatus
- Test tubes
- Measuring cylinder
- Dropper
- Centrifuge

Methods
Procedure A
1. 2 drops of 6M HCl were dropped to 1ml of the mixture of the metal
cation
2. The suspension was centrifuged for 1 minute when the ppt of
chloride is formed.
3. 1 additional drop of 6M HCl was added to the clear supernatant to
check for complete precipitation
4. The suspension was centrifuged again for one minute when the ppt
is observed
5. The supernatant was decanted in a clean test tube
6. The supernatant was saved for procedure B and the ppt was
continued with the confirmation test for cation (Ag+)
Confirmation Test for Cation (Ag+)
1.
2.
3.
4.
5.

The ppt was washed

10 drops of 6M NH3 were added
The mixture was stirred to dissolved
6M HNO3 was added to the mixture dropwise
The presence of Ag+ was confirmed when the ppt formed

Procedure B
1. 6M NH3 was added dropwise to the solution until it is basic.
2. The sample was put in the boiling water bath for 2-3 minutes to
remove the excess NH3
3. The volume of the solution was adjusted to 2mL with distilled water
and 10 drops of 6M HCl was added.
4. 12 drops of thioacetamide were added to the solution and stirred
wisely
5. The sample was heated in the boiling water bath for 10 minutes to
allow the hydrolysis of thioacetamide producing H2S
6. The sample was centrifuged for 2 minutes after the ppt of sulphide
is formed and the supernatant was decanted to a clean test tube
7. The supernatant was saved for procedure C and the ppt was
continued with the confirmation test for cation (Cu2+)
Confirmation Test for Cation (Cu2+)
1. The ppt was washed
2. The ppt was centrifuged. The supernatant was discarded and the
3.
4.
5.
6.
7.
8.
9.

ppt was saved.

20 drops of 6M HNO3 was added
The solution was boiled for several minutes with stirring occasionally
Then the solution was centrifuged and the ppt was discarded.
Drops of 6M NH3 were added until the solution become basic
Drops of 6M HNO3 were added until the solution become acidic
10 drops of 0.1M K4Fe(CN)6 were added
The solution was centrifuged and the presence of ppt confirmed the
presence of Cu2+

Procedure C
1. 3 more drops of 1M of thioacetamide were added to the supernatant
and was reheated for five more minutes in the water bath
2. The solution was centrifuged when ppt is formed and the ppt was
discarded
3. The volume of the solution was adjusted to 3mL with distilled water
and 10 drops of 6M HCl and 10 drops of 6M NH3 were added
4. 6M NH3 was added dropwise until the solution is basic.
5. 5 additional drop of 6M NH3 and 12 drops of thioacetamide were
added and the mixture was stirred thoroughly.
6. The sample was heated in the boiling water bath for 10 minutes
7. The sample was centrifuged when the ppt was formed
8. The supernatant was discarded
9. The ppt was washed
10.
1 drop of 6M NH3 was added
11.
The solution was centrifuged and the supernatant was
discarded
12.
20 drops of 6M HNO3 were added to the ppt
13.
The mixture was heated in boiling water bath for several
minutes with stirring
14.
The mixture was centrifuged and the supernatant was
discarded and the ppt was used in the confirmation test for cation
(Zn2+)
Confirmation Test for Cation (Zn2+)
1.
2.
3.
4.

Drops of 6M NH3 was added to the ppt until basic

Drops of 6M CH3COOH was added until acidic
10 drops of 0.1M K4Fe(CN)6 were added and mixed thoroughly
The solution was centrifuged when the ppt formed which confirmed
the presence of Zn2+

5.

Results and Observations

Observation

Balanced chemical equation

1. On adding HCl to the initial sample

Unknown 2: clear supernatant
Unknown 2: Mixture: white precipitate formed in
Mixture: Ag+(aq) + Cl-(aq) AgCl(s)
blue supernatant
Confirmatory test for the cation
Unknown 2: clear supernatant
Unknown 2: Mixture: white precipitate formed in

Mixture: Ag+(aq) + Cl-(aq) AgCl(s)

blue supernatant
2. On adding H2S under acidic condition
Unknown 2: White precipitate was

Unknown 2: Cu+(aq) + S2-(aq)

formed

AgCl(s)

Mixture: dark green precipitate

Mixture: Cu+(aq) + S2-(aq) AgCl(s)
Confirmatory test for the cation
Unknown 2: White precipitate in
Unknown 2: 2Cu2+(aq) + S2-(aq)
green supernatant

Cu2[Fe(CN)6(s)

Mixture: brick red precipitate was

Mixture: Cu+(aq) + Fe(CN)64--(aq)

formed

Cu2[Fe(CN)6(s)
3. On adding H2S under basic condition
Unknown 2: formed white precipitate Unknown 2: Zn2+ (aq) + S2-(aq)
in light blue supernatant

ZnS

Mixture: supernatant change to

Mixture: Zn2+ (aq) + S2-(aq)

(s)

ZnS

brown with precipitate

Confirmatory test for the cation
Unknown 2: formed white precipitate Unknown 2: 3Zn2+ (aq) + 2Fe(CN)64in light blue supernatant

Zn3[Fe(CN)6]2(s)

Mixture: darker brown supernatant

Mixture: 3Zn2+ (aq) + 2Fe(CN)64Zn3[Fe(CN)6]2(s)

with precipitate
Unknown Number 2 contains Cu2+, Zn2+

(aq)

(s)

(aq)

Discussion:
In these two experiments, which was used the qualitative analysis,
there are two principle that important while using it. The first principle is
confirmatory test. The confirmatory test will determine the presence of
certain ions in the solution by removing the interfering ion before the
confirmatory test is done using the second principle that is separation.
These are procedures that separate groups of ions from other groups, or
individual ions in a mixture of ions.
For these experiments, there are five analytical group of cation that
have the possibilities present in the mixture and unknown solution. The
analytical group I cation which consist Ag +, Hg2+ and Pb2+ can be easily
separated as the ions will form slightly soluble chloride with the addition
of hydrochloric acid. This will separate the ions from the other group ions
which still remain in the solution. The group I chloride precipitates was
removed for further tested. In experiment 1, the mixture and unknown 2
formed white precipitate when HCl was added. This shown that the
present of the group I ions. The precipitate was discarded from the
supernatant. In experiment 2, the precipitate that was discarded later
were further tested in conformation test for Ag + ions. To distinguish
between silver and mercury chloride was by using advantage of the
tendency transition metal ion, Ag+ to form water soluble complex ion with
ammonia, HN3. When the present of HN3 in a larger amount, it makes the
AgCl ion completely dissolves. In this way, the silver ion is separated from
the mercury ion. For experiment 2, mixture and unknown 2 shown a
positive result of Ag+.
For group II cation which consists of As 3+, Bi3+, Cd3+, Cu2+, Hg2+, Pb2+,
Sn4+ ions, the positive result also shown in the mixture and unknown 2 for
experiment 1 and 2. In experiment 1 the positive result shown by the
present of white precipitate while in experiment 2, the confirmatory test
helps in the confirmation of the Cu 2+ presence. The Group II cations are
chloride soluble ions and consequently they are readily separated from
the slightly soluble Group I chloride insoluble cations. They can be further

separated into groups through selective precipitation of a number of

sulfides. HgS, Bi2S3, CuS, SnS and SnS2 precipitate from reaction with
H2S in 0.3M H+. Because any of the Group I cations have already been
removed with the Group I precipitation. There will be also no precipitation
out from H2S at 0.3M H+ of the other sulfides as they have high
equilibrium constants. The precipitation should have a black colour but
during the experiment, the pH might affect the experiment which turn out
to be white colour precipitation. For confirmation test for copper ion 6M
acetic acid was added dropwise until the solution becomes acidic which
turn the red litmus paper into blue. Once it is acidic, a few drops of 0.1M
potassium ferrocyanide (K4Fe(CN)6) were added and result in a maroon
precipitate of Cu2Fe(CN)6 which automatically indicate the present of
copper ions.
The group III cations consists of Co 3+, Fe2+, Mn2+, Ni2+, Zn2+, Al3+,
Cr3+. The ions of Group III are precipitated as their sulfides, or as their
hydroxides, from a basic solution of hydrogen sulfide. The sulfides of the
ions of Group III are not sufficiently insoluble to be precipitated in the
acidic solution of hydrogen sulfide of Group II but will be precipitated by
basic solutions of hydrogen sulfide. A basic hydrogen sulfide solution also
contains a concentration of hydroxide ions. Although this is very small, it
is sufficient to precipitate the very insoluble hydroxides of aluminium and
chromium (III) ions. In experiment 1, the mixture give out the white
precipitate and for unknown 2, the solution turn into brown which might
affected by the present copper which is not totally being separated in the
previous step.
The analytical group IV cations consist of Ba+, Ca2+, Mg2+, Sr2+. All
these ions can form chlorides, sulphides, and hydroxides that is soluble
under the precipitation process for group I, II and III. The carbonates of
these ions will form precipitation in aqueous ammonia solution containing
ammonium carbonate except for MgCO3. In experiment 1, the precipitate
form in mixture and unknown 2 was yellowish precipitate which indicate
the present of Ba2+ ions.

The last group is analytical group V which consists of Na + and K+. For
this group the supernatant that left from previous steps which determining
the analytical group IV cation consists all the analytical group V ions. By
adding the K2C2O4 will separate between Ca 2+ and Mg2+. The precipitate
that form after addition of K2C2O4 indicate the present of Calcium ion as
stated in the flow charts of predetermine steps.
In these experiments, there are lots of precaution steps that need to
be taken care of. This is because most of the steps requiring the students
to use a high molarity of acid and base which can give a bad impact when
spilled on the skin directly which requiring the students to wear gloves
while conducting these experiments. Besides that, the students also use
mask as some of the chemical gave out pungent smell which sometimes
might affect the smell.
There are several errors occurred in these experiments which affect
the colour solution and the present of the precipitate. One of the errors is
during turning the solution into acidic or basic, the pH is not accurately
measure which affect the colour of copper. Besides that, the technical
error which was during washing and decantation process might affect the
precipitate to form and the ions are not well separated.

Conclusion:
Metal cation can be determined by using qualitative analysis which
involved the predetermine steps, separation steps and the confirmation
test which give out the ions for experiment 1 and 2. The metal cations in
mixture and unknown II solution in experiment was Zn2+ and Na+ or K+
while the unknown II and mixture in experiment 2 contained Cu2+ and
Zn2+.
References:
1. Hadariah

Bahron,

Kamariah

Muda,

Sharifah

Rohaiza

Syed

Omar, Karimah

Kassim/2015/Inorgani Chemistry: Experiment for Undergraduates/UiTM PRESS.

2. C. Raymond, CHEMISTRY, 2010, 10th edition, Mc Graw Hill Higher Education