 Chemistry Qualitative Analysis:-

 Analysis of group I (Silver Group)

This group includes Pb2+, Ag+ and Hg22+. But in the present context, we shall study only Pb 2+. Group
reagent for this group is dil. hydrochloric acid.

 Procedure

1. To the original solution add dil. hydrochloric acid. If a white precipitate is formed, first group (Pb 2+) is
present.
2. Filter and wash the ppt. with cold water and examine as in Table 12.12.
 Chemical Reactions Involved in Group I Analysis

 Analysis of group II (copper group)

This group includes Pb2+ and Cu2+ in IIA group and As3+ in IIB Group. But in the present context, we
shall study only Pb2+ and Cu2+. These are precipitated as their sulphides. If group I is absent, the tests
for radicals of group II are carried out. Group reagent for this group is H 2Sgas in the presence of dil.
HCl.

 Procedure

Take about 2 ml of the original solution in a test tube’. Make it acidic with dil. HCl and warm the
contents. Through this solution pass H 2S gas from the Kipp’s apparatus by turning
the stop cock as shown in Fig. 12.10, Formation of the black or yellow precipitates indicates the
presence of group II radical. If this is observed, pass more of H 2S gas to ensure complete
precipitation of the radical sulphide.

Identification of IIA Groups. Note the colour of the precipitate. If the precipitate is black in colour, it
indicates Pb2+ or Cu2+. Draw as an inference in table no. 12.13.
Confirmation test of Cu2+:- Dissolve the ppt in 50% HNO3 and then proceed for confirmation test as shown
in table no. 12.12.

Procedure Observation Inference

1. K4Fe(CN)6 test – To the

solution add potassium Chocolate brown ppt formed Confirmation of Cu2+.
ferrocyanide.

 Chemical Reactions Involved in the Analysis of Group II

 Analysis of group III (iron group)

The cations present in this group are Fe 2+, Fe3+, Cr3+ and Al3+. Only Fe2+/Fe3+ and Al3+ are included in
the syllabus of this class. These cations are precipitated as hydroxides by adding ammonium
hydroxide in presence of ammonium chloride. Thus, group reagent for this group is NH4OH in the
presence of NH4Cl.

 Procedure

In case, first and second groups are absent proceed for group III with the original solution. Take about
5 ml of the original solution and add 4-5 drops of cone, nitric acid. Boil the solution for sometime. Add
to it about 2 g of solid NH4Cl and boil again. Cool the solution under tap water. Add excess of
ammonium hydroxide to it and shake. A ppt. shows the presence of some cation of group III. Filter the
ppt. and wash with water. Note the colour of the ppt. If the ppt. is reddish brown in colour, it indicates
the presence of Fe3+ and if the colour is white, it indicates the presence of Al 3+. Analyse the ppt. and
draw inferences as in Table 12.14.
 Chemical Reactions Involved in the Analysis of Group III

 Analysis of group IV (Zinc group)

The radicals present in this group are CO 2+, Ni2+, Mn2+ and Zn2+. But in the present context, we shall
study only Zn2+. These are precipitated as sulphides by passing H2S gas through the ammonical
solution of the salt.
The group reagent for this group is H2S gas in the presence of NH4Cl and NH4OH.

 Procedure

If there is no ppt. in the third group, then use the same ammonical solution for the fourth group. Pass
H2S gas through the solution. If some ppt. is formed, presence of some radical of group IV is
 indicated. Filter the ppt. and wash it with water. Note the colour of the ppt. and analyse the ppt
according to the table no. 12.15.

 Confirmation test of Zn 2+ :- Dissolve the ppt in dil. HCl and then divided into two parts as shown in
Table no. 12.15.

Procedure Observation Inference

2. NaOH test - To one part of

soution add sodium hydroxide White ppt formed. Confirmation of Zn2+.
solution.

3. K4Fe(CN)6 test – To
another part add Bluish green ppt formed Confirmation of Zn2+.
potassium ferrocyanide.

 Chemical Reactions Involved in the Analysis of Group IV

Passing of H2S gas through the group III solution will precipitate the radicals Zn 2+ as their sulphides.
Formation of dirty white ppt. (ZnS) indictes zinc.
  Analysis of group V (calcium group)

Group V consists of three radicals: Ba2+, Sr2+ and Ca2+. These cations are precipitated as their
carbonates.
Group reagent for this group is (NH4)2CO3 in the presence ofNH4Cl and NH4OH.

 Procedure

If the fourth group is absent, then proceed for radicals of group V.

To the O.S. add 2-3 gins of solid NH4Cl, boil, cool and add NH4OH till the solution smells of ammonia.
Then add (NH4)2CO3 solution. Appearance of white ppt. indicates the presence of group V cation.
Filter and wash the ppt. with water. Dissolve the ppt. in hot dil. acetic acid. Divide the solution into
three parts and proceed as in Table 12.16.

Note:

1. Proceed to test for group V cations in the order, Ba2+, Sr2+ and Ca2+. If Ba2+ is confirmed, do not test for
Sr2+ or Ca2+ Similarly if Sr2+ is confirmed, do not test for Ca2+.
2. Original solution can be preferably used for testing Sr 2+ and Ca2+.

 Chemical Reactions Involved in the Analysis of Group V Radicals

 Analysis of group VI (Magnesium group)

 Chemical Reactions Involved in Confirmation of Mg 2+

nal
  Aim:- To determine the Molarity and strength of KMnO 4 Solution by
titrating with standard solution of Mohr’s salt solution(M/20).

 Chemical Equations

 Indicator

KMnO4 is a self-indicator.

 End Point

Colourless to permanent pink colour (KMnO4 in burette).

 Procedure

1. Wash the burette and then Rinse and fill the burette with the given KMn04 solution.
2. Add Mohr’s salt solution exactly 10 ml to the conical flask by mouth pipetting using volumetric
pipette.
3. Add one test-tube (~ 20 ml) full of dilute sulphuric acid to the solution into the same conical
flask.
4. Note the initial reading of the burette.
5. Now add KMnO4 solution from the burette till a permanent light pink colour is imparted to the
solution in the titration flask on addition of last single drop of KMnO4 solution.
6. Note the final reading of the burette.
7. Repeat the above steps 3 times to get a set of three concordant readings.
 Observations

Initial burette Final burette Volume used of

SL NO. Mean volume
reading (in ml) reading (in m) KMNO4 (in ml)

1.
------ ------ ------ ------
2.
------ ------ ------ ------

3.
------ ------ ------ ------

 Calculations

(a) Molarity of the KMnO4 solution.

From the overall balanced chemical equation, it is clear that 2 moles of KMnO 4 reacts with 10
moles of Mohr’s salt.

(b) Strength of KMnO4 solution = Molarity of KMnO4 X Molar mass of KMnO4.

[Where, Molar mass of KMnO4 = 158 g]

 Aim:- To determine the Molarity and strength of KMnO 4 Solution by
titrating with standard solution of oxalic salt solution(M/40).

 Chemical Equations

 Indicator

KMnO4 is a self-indicator.

 End Point

Colourless to permanent pink colour (KMnO4 in burette).

 Procedure

1. Wash the burette and then Rinse and fill the burette with the given KMn04 solution.
2. Add oxalicacid salt solution exactly 10 ml to the conical flask by mouth pipetting using
volumetric pipette.
3. After that add one test-tube (~ 20 ml) full of dilute sulphuric acid to the solution in conical flask
followed by adding about 100 ml of hot water into the same conical flask.
4. Note the initial reading of the burette.
5. Now add KMnO4 solution from the burette till a permanent light pink colour is imparted to the
solution in the titration flask on addition of last single drop of KMnO 4 solution.
6. Note the final reading of the burette.

 Repeat the above steps 3 times to get a set of three concordant readings.

 Observations

Initial burette Final burette Volume used of

SL NO. Mean volume
reading (in ml) reading (in m) KMNO4 (in ml)

1.
------ ------ ------ ------
2.
------ ------ ------ ------
3.
------ ------ ------ ------

 Calculations

(a) Molarity of the KMnO4 solution

From the overall balanced chemical equation it is clear that 2 moles of KMnO 4 react with 5
moles of oxalic acid.

(b) Strength of KMnO4 solution = Molarity of KMnO4 X Molar mass of KMnO4.

[Where, Molar mass of KMnO4 = 158 g]

1. Tests for aldehydes group.

Aim:
To identify the presence of aldehydes functional group in the given organic
compound.

1. Tollen’s Test (Silver mirror test)

Procedure

Place 1 ml of silver nitrate solution in a clean test-tube and add 2-3 ml of dilute
NaOH solution. A brown precipitate forms. Now add dilute ammonia solution drop
wise until the brown precipitate of silver oxide just dissolves. To this add 3-4 drops
of the given liquid (or 0.1 g if solid) and warm the test-tube on a water-bath for
about 5 minutes.

A shining mirror confirms the presence of the aldehyde group.

2. Fehling’s Test

Procedure

Take 1 ml each of Fehling’s solution A and B in a test-tube. Add 4-5 drops (or 0.2 g)
of the given organic compound and warm the test-tube in hot water bath for 4-5
minutes.
2. Tests for phenol group.

Aim:
To identify the presence of phenol functional group in the given organic
compound.

1. Ferric Chloride Test

Phenols react with ferric ions to form coloured complexes. Many other types of
organic compounds also react with ferric chloride solution.

Procedure

Take 1 ml of neutral ferric chloride solution in a clean test-tube and 2-3 drops of
the liquid compound (or 1 crystal if solid). A change in colour indicates the
phenolic group. Phenol produces violet colouration.

3. Tests for carboxylic group.

Aim:
To identify the presence of carboxylic acid functional group in the given organic
compound.

1. Sodium Hydrogen carbonate Test

Carboxylic acids react with sodium hydrogen carbonate to give carbon dioxide
gas which is identified by the effervescence produced.
To 1 ml of organic liquid in a test-tube, add a pinch of sodium bicarbonate
(NaHCO3). A brisk effervescence indicates the presence of carboxylic group in the
organic compound.

2. Ester Test

A carboxylic acid reacts with an alcohol in presence of a little sulphuric acid to

form an ester which is recognized by its fruity smell.

4. To Prepare colloidal solution of starch.

Aim:
To prepare lyophilic sol of starch.

Theory:
When water is used as a dispersion medium, starch has the ability to form sol.
This formation is enhanced with the help of heating. To prepare sol the mixture of
water and starch is heated to about 100° C.

Materials Required:
1. Tripod stand
2. Beaker of about 50 to 250 mL
3. Funnel
4. Distilled water
5. Wire gauze
 6. Glass rod
7. Mortar and pestle
8. Burner
9. Filter paper
10. 500 mg starch

Procedure:
1. Take a mortar and add 500 mg of starch to it.
2. Pour a few drops of distilled water and pestle the starch
into a thin paste.
3. Transfer the grounded paste to a 50 ml beaker.
4. Take a 250 mL beaker and pour 100 mL of distilled water to
it and heat the water to boiling.
5. Slowly pour the paste into the boiling water and
constantly keep stirring with the help of a glass rod.
6. Let it boil for 10 minutes after you have transferred all the
paste into the beaker.
7. Allow it to cool.
8. With the help of a filter paper attached to a funnel, you
can filter out the contents.
9. Label the filtrate as starch sol.

Precautions:
▪
▪ The apparatus used for the experiment should be washed
with distilled water and dried before conducting the
experiment.
▪ Use distilled water to prepare starch sol.
▪ Make sure to convert starch into a smooth paste before
adding to the boiling water beaker.
▪ Keep constantly stirring the mixture while preparing starch
sol.