FIRST YEAR PUC

PRACTICALS SYLLABUS
Basic Laboratory Techniques

1. cutting glass tube and glass rod

2. Bending a glass tube
3. Drawing out a glass jet
4. Boring a cork
Characterization and purification
of chemical substances
1. Determination of melting point of an
organic compound
2. Determination of boiling point of an
organic compound
3. crystallization of impure sample of
anyone of the following:
Alum, Copper sulphate,
sulphate, Benzoic acid.
 Experiments related to pH change
• Any one of the following experiments:
* Determination of pH of some solution
obtained from Fruit juice, varied concentration
of acid, base and salts using pH paper or
universal indicator.
* Comparing the pH of solution of strong and
weak acid of same concentration
* Study the pH change in the titration of a
strong base using universal indicator.
• Study the pH change by common ion effect in
case of weak acid and weak base.
 Chemical equilibrium
• Study the shift in equilibrium
between ferric ions and thiocyanate
ion by increasing/ decreasing the
concentration of either ions.
• Study the shift in equilibrium
between [Co(H2O)6]2+ and chloride
ions by changing the concentration
of either of the ions.
 Quantitative estimation:
• Using a chemical balance.
• Preparation of standard solution of oxalic
acid.
• Determination of strength of a given
solution of NaOH by titrating it against
standard solution of oxalic acid.
• Preparation of standard solution of sodium
carbonate.
• Determination of strength of a given
solution of HCl by titrating it against
standard Na2CO3 solution.
Qualitative analysis of inorganic salt
Determination of anion and cat ion in a
given salt.
Anions:--
Anions:
CO33-, S-2, SO33-, SO44-, NO3-, Cl-, Br-,

I-, PO43-, C2O42-, CH3COO-.

Cat ions:-
ions:-
Pb2+, Cu2+, As3+, Al3+, Fe3+, Mn2+, Ni2+,

Zn2+, Ca2+, Sr2+, Ba2+.

• Detection of nitrogen, sulphur,
sulphur, chlorine.
Common apparatus use
in Laboratory

and their uses

Conical flask
Burette
Measuring cylinder/ volumetric flask
Burette
Lower meniscus of solution in burette
Beaker
Test tubes and test stand
Separating funnel
Bunsen burner
Bunsen Flame
Round bottom flask
Tripod stand
Crucible tongs
Graduated/ measuring cylinders
Droppers
Test tube holders
Measuring cylinders
Watch Glass
Volumetric Measuring flask
Funnel
Reagent bottles
Wash bottle ( water bottle)
Wire gauze
Chemical Balance
Thiele’s Tube
Spatulla
Kipp’s apparatus
TEST TUBE BRUSH
 Preparation of
Standard Solution of Sodium Carbonate
QUALITATIV ANALYSIS OF
INORGANIC SALT

Preliminary Examination of Salt.

Colour
Soluility
 ANALYSIS OF ACIDIC RADICALS
Preliminary test with dilute Sulphuric Acid
Test Observation Inference
0.1g of 1)A colourless ,
Odourless gas Carbonate
Salt +dil
of CO2 is (CO32-) is
H2SO4
evolved with present
warm
brisk
effervescence,
which turns lime
water milky
 2)Colourless gas of
H2S with smell of Sulphide
rotten egg is (S2-) is
evolved which turns present
lead acetate paper
black

3)Colourless gas SO2 with Sulphite

a pungent smell which (SO32-) is
turns acidified K 2Cr2O7 present
Solution green
4)Brown gas which
turns acidified KI
Nitrite
solution containing
(NO2-) is
starch solution blue
present

5)Colourless vapour Acetate

with smell of (CH3COO-)
vinegar, vapour is present
turns blue litmus
red
 Confirmatory test for CO32- S2- SO32- NO3-
and CH3COO-
A) 0.1g of salt + dilute H4SO4
Carbonate CO2 gas evolved with
ion (CO32-) bricsk effervescence
which turn s lime water
milky.

D) Nitrite ion. 1 mL of water extract + few

(NO3-) drop of KI solution and add
few drop of starch solution
acidify with acetic acid. Blue
colour appears.
B) Sulphide 1mL of water extract +
ion (S2-) ammonium hydroxide add
a drop of sodium
nitroprusside solution.
Purple or violet
colouration appears.

C) Sulphite 1 mL of ate extract + BaCl2

ion (SO32-) solution. A white ppt is
formed which dissolves in dil.
HCl.
E) Acetate 0.1g of salt in a china dish
ion add 1mL of ethanol and
(CH3COO-) 0.2mL conc. Sulphuric acid
and heat, Fruity odour
evolved.

If no positive result obtained in step I then go

for Step II
Step II: Preliminary test with conc Sulphuric acid:
Test Observation Inference

0.1 g of 1) Colourless gas with Chlorid ion

salt + 3-4 pungent which gives (Cl-) is
dense white fumes present
drop of
when a rod dipped in
Conc. NH4OH is brought near
Sulphuric mouth of the test tube.
acid and
Warm 2) Reddish brown gas
with pungent smell Bromide
heating. After adding of ion(Br-) is
solid MnO2, solution Present
acquires red colour
3) Violet vapour which Iodide ion(I-)
turns starch Paper blue is Present
and a layer of violet
sublimate is formed on
side of test tube
fumes become dense
on adding MnO2.

4) Brown fumes evolved Nitrite ion

which become dense by (NO -) is
3
heating with cu- turning
and solution turn blue
Present
colour.
5) Colourless gas, Oxalate ion
odourless gas evolved (C2O42-) is
which turns lime Present
water milky an gas
coming out of lime
water burns with
a blue flame if ignite.
Confirmatory test for Cl-,Br-, I-, NO3-, and
c2O42-. Radicals
A) Chloride a) 0.1g of salt + pich of MnO2
ion.(Cl-) and 3-4 drop conc. H2SO4 heat
the mixture
Greenish yellow chlorine gas is
evolved which gives pungent
odour.
b) 1mL of sodium carbonate
extract acidify with dil. HNO3 or
take water extract and add
silver nitrate solution . A curdy
white ppt. is obtained which
soluble in NH4OH solution
B) Bromide a) 0.1 g of salt + pinch of
ion. (Br-) MnO2 add 3-4 drop conc.
H2SO4 heat the mixture .
Intense brown fumes
evolved.
b) 1mL of sodium extract
acidified with dil. HNO3 or
take water extract and add
silver nitrate solution. A
pale yellow ppt which is
slowly soluble in NH4OH
solution.
C) Iodide a) 1 mL of salt solution
Ion. (I-) neutrilization with Hcl & add
1 mL CHCl3 or CCl4, now add
an excess of chlorine water
drop by drop and shake TT. A
violet colour appears in the
organic layer.
b) 1 mL of sodium carbonate
extract acidify with dil HNO3
or takes water extract, add
AgNo3 solution A yellow ppt
in soluble in NH4OH solution
is obtained.
D) Nitrate 1 mL Water extract add 2 mL
Ion (NO3-) conc. H2SO4 mix through cool
the mixture under the tap.
Add freshly prepared FeSO4
solution along the side of TT
without shaking A dark
brown ring is formed at the
junction of the two solution.
E) Oxalate 1 mL of water extract
ion (C2O42- acidified with acetic acid
) and add calcium chloride
solution. A white ppt
insoluble in ammonium
oxalate and oxalic acid but
soluble in dil Hcl & dil
HNO3.
if no positive test is obtained in step I & II
then go for step III
 III Test for SO42- and PO43-

Confirmatory test for Sulphate & Phosphate ion

•
Sulphate 1 mL water extract + dil
(SO4-2) HCl +Bacl2 solution white
ppt insoluble in conc. HCl is
obtained.
 Phosphate 1 mL water extract + conc.
Ion (PO4-3) HNO3 and add ammonium
molubidate solution & boil
A canary yellow ppt is
formed.
 SYSTEMATIC QUALITATIVE
ANALYSIS OF INORGANIC SALT

Preliminary examination of the salt for cation

Test Observation
Inference
Colour
Light green, yellow, brown Fe2+,Fe3+
Blue Cu2+
Bright green Ni2+
Blue, red, Violet, pink Co2+
Light pink Mn2+
• Dry heating test:
0.1g of salt is heated in dry test tube and observe
the colour of salt in hot and also when it become
cold.
Colour when cold Colour when hot Inference
Blue White
Cu2+
Green Dirty white or yellow Fe2+
White yellow Zn2+
Pink Blue Co2+
• Flame test:
Platinum loop is dip in the paste of salt and held in the
non--luminous flame. Observe the colour of flame first
non
with nicked eye and then through a blue glass.
• Color of flame observed by Colour of flame observed by
Inference
Naked eye through blue glass

• Green flame with blue center no change Cu2+

• Crimson red Purple Sr2+
• Apple green Bluish green Ba2+
• Brick red Green Ca2+
Preparation of Original
solution(O.S.)

Salt is dissolved in distilled water if not

soluble then heat, if even insoluble then
salt dissolved in dil. HCl or Conc. HCl or
dil. HNO3 or a mixture of conc. HCl and
COnc. HNO3 in the ratio of 3:1 this
mixture is called Aqua regia.
regia. A salt not
soluble in aqua regia is considered to be
an insoluble salt.
Analysis of Zero group cat ion (NH4+
ion)

• 0.1 g of a salt and add 1-

1-2mL of NaOH solution and heat
If there is a smell of ammonia this indicate the presence
of ammonium ions. Ring the glass rod dipped in HCl near
the mouth of the test tube. White fumes are observed.
observed.

• Pass the gas through Nessler’s reagent. Brown ppt. is

obtained
ANALYSIS OF BASIC RADICALS

Test observation Inference

• O.S. + dil. HCl White ppt I-group Pb2+ is present
No ppt II-
II-group is absent

• O.S. + dil. HCl + pass H2S gas. Black PPt. II-group Cu2+, Pb2+
II-
Yellowppt As3+ is present
No ppt. II-
II-group is absent

• O.S. + Solid NH4Cl Brown ppt. III-group Fe3+

III-
+ excess NH4OH White gelatinous ppt. Al3+ is present
No ppt. III-
III-group is absent
 Test observation Inference

• O.S
O.S.. +solid NH4Cl White PPt.
PPt. IV--group Zn2+
IV
+ excessNH4OH Flesh colour ppt Mn2+
+passH2S. Black ppt. Ni2+, Co2+is presnt
No ppt. IV- group is absent

• o.s
o.s.. + solid NH4Cl White ppt. V-group
Ba2+,Ca2+,Sr2+
+ excess NH4OH is present
+ solid (NH4)2CO3
No ppt. VI-- group Mg2+ is
VI
present
Analysis of Group I cation:
cation:
(Pb2+)

• Dissolve the ppt in hot water and divide

into two parts.

Part 1 + KI solution yellow ppt Pb2+ is confirmed

Part 2 + potassium chromate Yellow ppt which is Pb2+ is

confirmed
solution soluble In NaOH solution
 cation: (Pb2+, Cu2+ ,
Analysis of Group II cation:
As3+ )

• II group PPt + yellow ammonium PPt is insoluble Pb2+, Cu2+ is present

Sulphide solution and shake PPt is soluble As3+ is present

• Confirmatory test for Pb2+ and Cu2+ ions

• II group ppt boil with White ppt. Pb2+ is confirmed

dil HNO3and add few drop of
alcohol and dil. H2-SO4 .

• This White ppt is dissolved in

ammoniumAcetate + acetic acid+ KI yellow ppt Pb2+is confirmed
Solution

• If no white ppt add excess of Chocolate brown ppt Cu2+ is confirmed

NH4OH solution + acetic acid
+ potassium ferro cyanide solution.
Analysis of Group III cations:
cations:
(Fe3+, Al3+)

• Brown ppt dissolve in dil HCl and divide the solution into two part.
• Part I + potassium Blue ppt. or Fe3+ is confirmed
ferrocyanide Solution colour appears

• Part 2+ potassium thiocyanate Blood red Fe3+ is confirmed.

coloration appears

• White gelatinous ppt dissolve

• in dil. HCl + NaOH solution White gelatinous Al3+ is confirmed.
ppt soluble in excess
 cations: (Zn2+, Mn2+,Ni2+, and
Analysis of Group IV cations:
Co2+)

• Dissolve the white ppt in White PPt soluble Zn2+ is confirmed.

dil. HCl and boil in excess
+ NaOH solution.

• Dissolved the flesh ppt in White ppt Mn2+ is confirmed.

dil. HCl and boil which turns brown
+ excess NaOH solution.

• Dissolve the black ppt in aqua regia heat the solution to dryness and cool. Dissolve the residue in water and
divide the solution into two Parts.

• To first part + NH4OH more +

few drop of dimethyl glyoxime
(DMG)shake Bright red ppt Ni2+is confirmed.
• To second part+ NH4OH +
actic acid+ solid KNO2. Yellow ppt Co2+ is confirmed.
 cations: (Ba2+, Sr2+
Analysis of Group V cations:
and Ca2+)
• Dissolve the ppt by boiling with dil. Acetic acid and divide the solution into three parts.
• First part + potassium
Chromatesolution yellow ppt Ba2+is confirmed.
• FLAME TEST
Paste of salt in conc. HCl is held
on the Bunsen flame grassy green flame Ba2+ is confirmed.
• second part + (NH4)2SO4 solution White ppt Sr2+ is confirmed
Heat and scratch the side of the
Tes t tube with glass rod.
• FLAME TEST
• Paste of salt in conc. HCl is held
on the Bunsen flame Crimson red flame Sr2+ is confirmed.
• Third part + ammonium oxalate
Solution shake well White ppt Ca2+ is present.
• FLAME TEST
• Paste of salt in conc. HCl is held
on the Bunsen flame Brick red flame Ca2+ is confirmed.
Analysis of Group VI cation
+2
(Mg )
• If Group V is absent then perform the test
for Mg+2+ ions.

• OS+NH4OH White ppt Mg+2 is

+Na2HPO4 Solution
confirmed
Titrimetric analysis
Aim:- Preparation of 250 mL of 0.1M Standard
Aim:-
solution of Oxalic acid.

• Theory:

• Hydrated oxalic acid is dibasic weak acid and its molar mass is 126 g. If
126g of oxalic acid is present in one liter of the solution It is known as one
molar (1.0M) solution. There for preparing 250mL of 0.1M oxalic acid
solution, we required: 126g x 0.1M x 250mL/ 1000mL =3.1500g of
hydrated oxalic acid.

• In general for preparing a solution of required molarity,

molarity, the amount of
substance to be weighed can be calculated by using the formula given
below:

Mass of solute in grams(m) x 1000

Molarity (M) = --------------------------------------------------------------------------------
-----
Molar mass of solute x vol. of solution to be prepared in mL
mL(v)
(v)
Procedure:
• Weigh an empty watch glass accurately. Then
weigh 3.1500g oxalic acid on the above watch
glass. Transfer oxalic acid carefully from the
watch glass into a clean measuring flask using
a funnel. Weigh the empty watch glass again
and find out the mass of oxalic acid
transferred to the measuring flask. Wash
funnel several times with distilled water by
using a wash bottle to transfer the sticking
particles. Swirl the measuring flask till solid
oxalic acid is completely dissolved Add more
distilled water to make up the volume with
distilled water up to the mark by adding last
few mL drop wise. Stopper the flask and shake
it thoroughly to make the solution
Aim:- Determination of the concentration( strength) of a
Aim:-
given sodium hydroxide solution by tritrating it against a
standard solution of oxalic acid.

• Reaction:
COOH COONa
COOH + 2NaOH ---

---
COONa + 2H2O.

• Procedure:
Wash the burette with distilled water and rinse the burette with sodium
hydroxide solution. Then fill sodium hydroxide solution into the burette through a
funnel above the zero mark.
Remove the air gap, if any from the nozzle of the burette and remove the
funnel Note the initial reading by keeping the eye exactly at the same level as the
lower meniscus of the solution.
Pipette out 10mL of oxalic acid solution in a clean conical flask. Add 1-
1-2 drops
of phenolphthalein indicator to the conical flask. Titrate the acid with sodium
hydroxide solution till a very faint permanent pink colour is obtained. Read the lower
meniscus of the solution in the burette and note down.
Repeat the procedure until three concordant readings are obtained.
• Table

• Calcuation:
• Molarity of NaOH solution can be calculated by using the equation:
Oxalic aid Sodium hydroxide
a1M1V1 = a2M2V2

Where, M1 and V1 are the molarity and volume of the oxalic acid, a1 is basicity of oxalic
acid =2
M2 and V2 are the molarity and volume of the sodium hydroxide solutio0n ,a2 is
acidity of sodium hydroxide solution =1

Calculate the concentrqatiuon of sodium hydroxide solution in g/L.

Concentration (strength) in g/L = Molartity x Molar mass.

Result:

The concentration of the given NaOH solution is ________ g/L

Aim:- preparation of 0.1M slandered
Aim:-
solution of sodium carbonate.

• Theory:

• Molar mass of dry sodium carbonate is 106g. To prepare

0.1M Na2CO3 solution, 10.6000g of sodium carbonate
should be dissolved per liter of the solution.

• There fore to prepare 100 mL of 0.1M Na2CO3 solution

1.0600g of sodium carbonate is dissolved in minimum
quantity of water and the solution id diluted exactly
100 mL by adding water.
Procedure:

• Weigh an empty watch glass accurately. Then weigh

1.0600g Sodium carbonate on the above watch glass.
Transfer Sodium carbonate carefully from the watch
glass into a clean measuring flask using a funnel. Weigh
the empty watch glass again and find out the mass of
Sodium carbonate transferred to the measuring flask.
Wash funnel several times with distilled water by using a
wash bottle to transfer the sticking particles. Swirl the
measuring flask till solid Sodium carbonate is completely
dissolved Add more distilled water to make up the
volume with distilled water up to the mark by adding last
few mL drop wise. Stopper the flask and shake it
thoroughly to make the solution.
Aim:- Determination of the strength of a given solution of
Aim:-
dilute hydrochloric acid by titrating it against a standard
solution of sodium carbonate.

• Reaction:
Na2 CO3 + 2HCl -
2 NaCl + H2O + CO2

• Procedure:
Wash the burette with distilled water and rinse the burette with
hydrochloric acid solution. Then fill hydrochloric acid solution into the
burette through a funnel above the zero mark.
Remove the air gap, if any from the nozzle of the burette and remove
the funnel Note the initial reading by keeping the eye exactly at the same
level as the lower meniscus of the solution.
Pipette out 10mL of Sodium carbonate solution in a clean conical
flask. Add 1-
1-2 drops of Methyl orange indicator to the conical flask. Titrate
the Base with hydrochloric acid solution till Colour changes from yellow to
pinkish--red colour is obtained. Read the lower meniscus of the solution in
pinkish
the burette and note down.
Repeat the procedure until three concordant readings are obtained.
• Table

• Calculation:
• Molarity of HCl solution can be calculated by using the equation:

HCl solution Na2CO3 solution

a1 M1 V1 = a2 M2 V2

Where, M1 and V1 are the molarity and volume of the HCl solution, a1 is basicity of HCl = 1
M2 and V2 are the molarity and volume of the sodium carbonate solution ,a2 is acidity
Of sodium carbonate solution = 2

• Calculate the concentration of hydrochloric acid solution in g/L.

Molar mass of hydrochloric acid is 35.5 g mol-1
Concentration (strength) of HCl solution in g/L = Molartity x Molar mass.

Result:

The concentration of the given HCl solution is ________ g/L