TITLE: Identification of ions

AIM: To identify the cation(s) and anion(s) present in an unknown sample.

APPARATUS/MATERIALS: test tube rack, test tubes, test tube holder, test tube brush,
droppers, glass rod, filter, funnel, filter paper, spatula, small beakers
Labels A-F

Reagents: diluted NaOH(aq), diluted NH3(aq), AgNO3(aq)

Q – unknown sample.

PROCEDURE:
1. Clean apparatus and set up the workstation.
2. Add 5ml of distilled water to substance Q and stir with a glass rod for…
3. Filter the emerging mixture into a test tube.
4. Place the residue aside and add equal amounts of the filtrate to test tubes labeled A, B
and C and place aside.
5. Wash and filter the residue multiple times then add it to a test tube labeled D.
6. Add 5ml of dilute HNO3 to that test tube and stir with a glass rod until dissolved.
7. Add equal amounts of that mixture to test tubes labeled D, E and F and place aside.
8. Add a few drops of diluted NaOH(aq) to A, then in excess.
9. Observe the changes and record your results in a suitable table.
10. Add a few drops of NH3 (aq) to test tube B, then in excess.
11. Observe the changes and record your results.
12. Add a few drops of silver nitrate to test tube C, then in excess.
13. Observe the changes and record your results.
14. Add NH3 aq in excess to test tube C.
15. Observe the changes and record your results.
16. Using test tubes D, E and F instead of A, B and C repeat steps 7-10.
17. Analyze the results collected.

RESULTS:
 Procedure Observation Inference

Filtrate Residue Filtrate Residue

Addition of NaOH aq White ppt No ppt Mg2+ ions Ba2+ ions

dropwise then in excess formed formed possibly possibly
Insoluble in present present
excess

Addition of NH3 aq White ppt No ppt Mg2+ ions Ba2+ ions

dropwise then in excess formed formed definitively definitively
Insoluble in present present
excess

Addition of silver nitrate White ppt N/A Halide ion N/A

dropwise then in excess formed present
Cl-, Br- or I-

Addition of NH3 aq in White ppt N/A Cl- ion N/A

excess dissolves present

The two compounds were found to be 1. MgCl2 and 2. BaSO4

DISCUSSION:
 Qualitative chemical analysis is a branch of chemistry that deals with the identification
of elements or grouping of elements present in a sample. Identifying ions is an important
laboratory exercise in chemistry because it is used to determine the presence of specific cations
and anions in a given sample or compound. A compound is a substance made up of two or more
different chemical elements combined in a fixed ratio. An anion may be defined as an atom or
molecule that is negatively charged and a cation may be defined as an atom or molecule that is
positively charged. This lab aims to identify the cation(s) and anion(s) present in an unknown
sample, Q by performing a series of tests on it to identify its ions based on their characteristic
reactions, first the Indicative test which tells what ions could be present and the confirmatory test
which specifies which ion is present.
It was noted that solution Q was a mixture of two compounds one insoluble in water, and
one that is soluble in water. One cannot test for multiple anions and cations simultaneously
hence these two compounds were separated based on their differences in solubility. Hence after
having dissolved the first compound, the second was retrieved by filtration.The filtrate is the
liquid which passes through the filter paper and the residue is the solid left on the filter paper. In
order to test for cations specifically, each compound must be in solution. Therefore the insoluble
compound was dissolved in nitric acid to facilitate the future tests. This insoluble salt dissolves
in nitric acid due to the acid's ability to react with the salt's anion and convert it into a soluble
nitrate salt. The resulting nitrate salt is soluble in water, allowing the salt to dissolve in the nitric
acid solution.
The indicative test for cations was executed on the filtrate. Dilute sodium hydroxide
solution was added and a white precipitate formed which was insoluble in excess. This evoked
the deduction that Mg2+ ions may be present. This result was obtained because when Sodium
hydroxide (NaOH) being a strong base that dissociates in water to form hydroxide ions (OH-)
and sodium ions (Na+) which chemical equation;
● NaOH → Na+ + OH-
is added to a solution containing magnesium ions (Mg2+), the hydroxide ions react with the
magnesium ions to form insoluble magnesium hydroxide, a white insoluble precipitate,
represented by the following equation;
● Mg2+ + 2OH- → Mg(OH)2
 Next, the confirmatory test for cations was carried out on the filtrate. Dilute aqueous
ammonia solution was added to the filtrate. A white precipitate formed which was insoluble in
excess. This confirmed that Mg2+ ions were definitely present in the filtrate. Similar reactions
took place which explains the nature of the results obtained. Ammonia can act as a weak base
and can undergo the following reaction with water:
● NH3 + H2O ⇌ NH4+ + OH-
The OH- formed then goes on to react with Mg2+ ions in the same way aq NaOH did previously.
Secondly, the indicative test for anions was carried out on the filtrate. Aqueous silver
nitrate was added to the solution and a white precipitate was formed. This indicates the possible
presence of a halide ion, be it Cl-, Br- or I- because, when silver nitrate (AgNO3) is added to a
solution containing halide ions, a white insoluble precipitate of silver halide forms due to a
chemical reaction that occurs between the silver ions and the halide ions.
To pinpoint exactly which halide was present, the confirmatory test for anions, addition
of aqueous ammonia, was performed on the filtrate. The white precipitate dissolved and this
hereby confirmed that Cl- ions were present. The addition of aqueous ammonia to a solution
containing AgCl results in the formation of [Ag(NH3)2]+. This is represented in this equation;
● AgCl + 2NH3 → [Ag(NH3)2]+ + Cl-
The complex ion [Ag(NH3)2]+ is soluble in water because the ammonia molecules act as ligands
and form coordinate covalent bonds with the silver ion. This reduces the concentration of free
silver ions in the solution, which reduces the tendency of the silver chloride to precipitate.
Hence the filtrate was determined to be MgCl.
The indicative test for cations was executed on the residue. Dilute sodium hydroxide
solution was added and no precipitate was formed. This indicated the presence of Ba2+ ions
because when NaOH is added to Ba2+ ions the following reaction occurs;
BaX+ NaOH→Ba(OH)2+NaX
Barium hydroxide is soluble in water when low in concentration, hence will dissociate and not
precipitate when in contact with sodium hydroxide solution.
The confirmatory test was executed on the residue by adding aqueous ammonia but
still no precipitate emerged. This confirmed the presence of Ba2+ because Barium hydroxide
also forms but it is more soluble in aqueous ammonia due to the formation of a complex ion,
Ba(NH3)6]2+ it dissolves in ammonia. Hence no precipitate forms.
This is represented by the equation;
● Ba(OH)2 + 6NH3 → [Ba(NH3)6]2+ + 2OH-
The residual compound was determined to be BaSO4 because the only barium salts which are
insoluble in water are sulfate and carbonate. In the reaction of the barium carbonate and nitric
acid, products carbon dioxide, water and barium nitrate are formed. The evolution of carbon
dioxide gas would cause bubbles to form. Since no bubbles were observed during the reaction, it
was deduced that the anion present with Ba2+ ion was SO42-.