GRAVIMETRIC ANALYSIS
ESTIMATION OF LEAD AS LEAD SULPHATE
AIM:
To estimate gravimetrically the weight of lead present in the whole
of the given solution.
PRINCIPLE:
The lead present in a soluble salt solution is precipitated as lead
sulphate by the addition of dilute sulphuric acid. The precipitate is
filtered washed and weighed after it has been dried and ignited along
with the filter paper in a weighed ignited along with the filter paper in a
weighed silica crucible and weighed as lead sulphate.
(CH3COO)2 Pb + H2SO4 → PbSO4↓ + 2CH3COOH.
PROCEDURE:
The given solution is made up to 100ml in a standard flask using distilled water.
20 ml of this is pipette out into a clean 400ml beaker provided with a watch glass
rod and is diluted to about 50ml. This solution is heated to boiling and to this hot
solution 20ml of dilute sulphuric acid is added in drops with constant stirring and
then 40ml of alcohol. The precipitate is allowed to settle and filtered through
Whatman 41 filter paper using 10% dilute alcohol as wash solution. The
precipitate is dried. After drying the precipitate is carefully removed from, the
filter paper and kept in a safe p[lace. The filter paper alo0ne is then incinerated in
a preheated and weighed silica crucible. The crucible is cooled a drop of
concentrated sulphuric acid is added and heated again. It is cooled in a
desiccators and then weighed along with the precipitate already removed from
a filter paper. A duplicate experiment is performed.
RESULT:
The amount of lead present in the whole of the given solution is
A = ______d______g
B = ______f______g.
S.N OBJECT TO BE WEIGHED WEIGHT IN GRAMS
O CRUCIBLE A CRUCIBLE B
1 Empty silica crucible
2 Silica crucible + lead sulphate
3 Lead sulphate
Weight of lead sulphate a b
CALCULATION:
Molecular weight of lead sulphate = 303.25
Atomic weight of lead = 207.19
CRUCIBLE A:
303.25g of lead sulphate contains 207.19g of lead.
a g of lead sulphate contains = 207.19× a /303.25
= c g of lead
20 ml of the given solution contains = c g of lead
Therefore 100 ml of the given lead solution contains = c × 100 / 20
= d g of lead.
CRUCIBLE B:
303.25 g of lead sulphate contains 207.19 g of lead.
b g of lead sulphate contains = 207.19× b /303.25
= e g of lead
20 ml of the given solution contains = e g of lead
Therefore 100 ml of the given lead solution contains = e ×100 / 20
= f g of lead
ESTIMATION OF LEAD A S LEAD CHROMATE
AIM:
To estimate gravimetrically the weight of lead present in the whole of the given
solution.
PRINCIPLE :
Lead is precipitated as lead chromate in dil.CH3COOH medium by the addition
of potassium chromate solution. The precipitated lead chromate is filtered in a
sintered crucible, washed dried at 120° c and weighed.
Pb(CH3COO)2 + K2CrO4 → PbCrO4 ↓ + 2CH3COOK
Pb(NO3) + K2CrO4 → PbCrO4 ↓ + 2KNO3.
PROCEDURE :
The given solution is made upto 100ml in a standard flask with distilled water.
20 ml of this solution is pipette out into a clean 400ml beaker provided with a
watch glass and glass rod. The solution is diluted to about 50ml and is heated to
boiling. To the hot solution 10ml of 4% potassium chromate solution is added
drop by drop with constant stirring. The precipitate is digested over a water bath
for half an hour and allowed to settle. The precipitate is then filtered through a
preheated and weighed sintered glass crucible using hot water as wash solution.
The precipitate is dried in an electric oven at 120°C for 45 minutes, cooled and
weighed. Heating cooling and weighing are repeated to attain constant weight. A
duplicate experiment is performed.
Result:
The amount of lead present in the whole of the given solution is
A = _______d_______ g.
B = _______f_______ g.
S.N WEIGHT IN GRAMS
OBJECT TO BE WEIGHED
O CRUCIBLE A CRUCIBLE B
1 Empty sintered glass crucible
2 sintered glass crucible + lead
chromate
3 Lead chromate
Weight of lead chromate a b
CALCULATION:
Molecular weight of lead chromate = 323.19
Atomic weight of lead = 207.19
CRUCIBLE A:
303.25g of lead chromate contains 207.19g of lead.
a g of lead chromate contains = 207.19× a /323.19
= c g of lead
20 ml of the given solution contains = c g of lead
Therefore 100 ml of the given lead solution contains = c × 100 / 20
= d g of lead.
CRUCIBLE B:
323.19 g of lead chromate contains 207.19 g of lead.
b g of lead sulphate contains = 207.19× b /323.19
= e g of lead
20 ml of the given solution contains = e g of lead
Therefore 100 ml of the given lead solution contains = e ×100 / 20
= f g of lead
ESTIMATION OF BARIUM AS BARUIUM CHROMATE
AIM:
To estimate gravimetrically the weight if barium present in the whole of the
given solution.
PRINCIPLE :
Barium is precipitated as barium chromate in acetic acid medium by addition of
potassium chromate. The precipitate barium chromate is filtered in a sintered
crucible, washed, dried at 120°c and weighed as barium chromate.
BaCl2 + k2CrO4 → BaCrO4 ↓ + 2KCl
PROCEDURE :
The given solution of barium chloride is made upto 100ml in a standard flask
with distilled water. 20ml of this is pipette out into a 400ml beaker provided with
a watch glass and glass rod. The solution is diluted to 50ml and heated to boiling.
About 5g of ammonium acetate crystals and 10ml of 1N acetic acid are added to
the hot solution. 20ml of 4% potassium chromate is then added drop by drop
with constant stirring. The precipitate of barium chromate formed is digested
over a steam bath and allowed to settle and tested for complete precipitation by
adding a few more drops of potassium chromate to the supernatant liquid. The
precipitate is filtered through a preheated and weighed sintered glass crucible
using cold water as wash so9lution. The precipitate is dried in an electrical oven
at 100°C, cooled and weighed. Heating cooling and weighing are repeated to
attain constant weight. A duplicate experiment is also performed.
Result:
The amount of barium present in the whole of the given solution is
A = _______d________ g.
B = _______f________ g.
S.N OBJECT TO BE WEIGHED WEIGHT IN GRAMS
O CRUCIBLE A CRUCIBLE B
1 Empty sintered glass crucible
2 sintered glass crucible + barium
chromate
3 barium chromate
Weight of barium chromate a b
CALCULATION:
Molecular weight of barium chromate = 253.34
Atomic weight of barium = 137.34
CRUCIBLE A:
253.34g of barium chromate contains 137.34g of Ba.
a g of barium chromate contains = 207.19× a /253.34
= c g of Ba
20 ml of the given barium solution contains = c g of Ba
Therefore 100 ml of the given barium solution contains = c × 100 / 20
= d g of Ba.
CRUCIBLE B:
253.34 g of barium chromate contains 137.34 g of Ba.
b g of barium sulphate contains = 207.19× b /253.34
= e g of Ba
20 ml of the given solution contains = e g of Ba
Therefore 100 ml of the given barium solution contains = e ×100 / 20
= f g of Ba.
ESTIMATION OF BARIUM AS BARIUM SULPHATE
AIM:
To estimate gravimetrically the weight of barium present in the whole of the
given solution.
PRINCIPLE :
Barium is precipitated as barium sulphate in hydrochloric acid medium, using
sulphuric acid as the precipitant. The precipitated barium sulphate is filtered,
washing and weighed after it has been dried and ignited along with the filter
paper in a weighed crucible as barium sulphate.
BaCl2 + H2SO4 → BaSO4↓ + 2HCl.
PROCEDURE :
The given solution of barium chloride is made upto 100ml in a standard flask
with distilled water. 20ml of made up solution is pipetted out into a clean 400ml
beaker provided with a watch glass and a glass rod. The solution is diluted to
50ml with distilled water and acidified with 2ml of dilute hydrochloric acid and
heated to boiling. To the hot solution added about 20ml of hot 5N H 2SO4 over
slowly with constant stirring. The precipitated barium sulphate is digested over a
steam bath for half an hour and allowed to settle. Tested for complete
precipitation by adding 2 drops of 5N sulphuric acid to the supernatant liquid in
the beaker. Then the precipitate is filtered through Whatmann No.40 filter paper
using hot water as wash solution. The filter paper along with the preci8pitate is
incinerated in a preheated and weighed silica crucible. It is cooled and weighed.
Heating, cooling and weighing arte repeated to attain constant weight. A
duplicate is also performed.
RESULT:
The amount of barium present in the whole of the given solution is
A = _______d________ g
B = ________f_______ g.
S.N OBJECT TO BE WEIGHED WEIGHT IN GRAMS
O CRUCIBLE A CRUCIBLE B
1 Empty silica crucible
2 silica crucible + barium sulphate
3 barium chromate
Weight of barium sulphate a b
CALCULATION:
Molecular weight of barium sulphate = 233.34
Atomic weight of barium = 137.34
CRUCIBLE A:
233.34g of barium sulphate contains 137.34g of Ba.
a g of barium sulphate contains = 137.34× a /233.34
= c g of Ba
20 ml of the given solution contains = c g of Ba
Therefore 100 ml of the given barium solution contains = c × 100 / 20
= d g of Ba.
CRUCIBLE B:
233.40 g of barium sulphate contains 137.34g of Ba.
b g of barium sulphate contains = 207.19× b /253.34
= e g of Ba
20 ml of the given sulphate solution contains = e g of Ba
Therefore 100 ml of the given barium solution contains = e ×100 / 20
= f g of Ba.
DETERMINATION OF BOILING POINT OF A LIQUID
AIM:
To determinate the boiling point of a given liquid.
PRINCIPLE :
A small amount of the liquid is taken in a round bottomed flask with a side tube
and fitted with a thermometer. The liquid in the round bottomed flask is heated
slowly and the temperature at which the liquid boils is noted.
APPARATUS
i. Round bottomed flask with a side tube
ii. Thermometer (110°C)
iii. Adapter
iv. Receiver
v. Stand
vi. Condenser
PROCEDURE :
The given liquid is taken to about one third of a round bottomed flask with side
tube. To promote uniform heating, some porcelain pieces are introduced into it.
The mouth of the flask is closed with mercury seal carrying the thermometer. The
mercury seal is so arranged that the bottom of it is in level with the side tube of
the round bottomed flask. The side tube of the apparatus is connected to a
condenser. The condenser is attached to the adapter which in turn is introduced
into a receiver. The flask is then slowly heated on a wire guaze. The temperature
rises gradually and finally the liquid boils and the vapour escapes through the side
tube and collects in the receiver in drops. The constant temperature at which the
liquid distills steadily is the boiling point of the liquid. When two third of the
liquid has been distilled away, heating is stopped. The apparatus is cooled the
experiment is repeated with the collected liquid to get concordant results.
RESULT:
The boiling point of the given liquid = __________°C.
PREPARATION OF ORGANIC COMPOUND
HYDROLYSIS
PREPARATION OF SALICYLIC ACID FROM METHYL SALICYLATE
AIM:
To prepare a pre sample of salicylic acid from methyl salicylate.
PRINCIPLE :
Methyl salicylate is easily hydrolyzed by sodium hydroxide solution and the
acid is precipitated out by adding hydrochloric acid.
REACTION :
CHEMICAL REQUIRED :
i. Methyl salicylate = 2.5ml
ii. 10% sodium hydroxide = 15ml
PROCEDURE :
Methyl salicylate (2.5ml). 15ml of 10% sodium hydroxide and a few porcelain
bits are taken in a round bottom flask. The flask is fitted with water condenser
and the contents are boiled till the oily drops are not seen. The contents are
cooled and transferred into a beaker. Concentrated hydrochloric acid is added to
the solution in small quantities with vigorous stirring till the solution is acidic. The
precipitate is filtered and washed with water. A portion of the sample is
recrystallised from hot water.
RECRYSTALLISATION :
About 1g of the benzoic acid is dissolved in boiling water and recrystallized.
White crystals of salicylic acid are separated and dried.
RESULT :
The yield of salicylic acid = __________g.
BENZOYLATION
PREPARATION OF BENZANILIDE FROM ANILINE
AIM:
To prepare a pure sample of crystals of benzanilide from aniline.
PRINCIPLE :
Aromatic amines, in general react with benzoyl chloride in aqueous medium
to yield the respective benzanilides. In the Schotten - Baumann method of
benzoylatic, the amino compounds is treated with a slight excess of sodium
hydroxide solution and benzoyl chloride. On vigorous shaking, benzoylation takes
place readily and the product separates solid.
REACTION :
CHEMICALS REQUIRED :
i. Aniline = 5ml
ii. Benzoyl chloride = 5ml
iii. 10% sodium hydroxide = 50ml
PROCEDURE :
Aniline (5ml) is taken in a conical flask fitted with a cork. About 5ml of
sodium hydroxide and 5ml of benzoyl chloride are added to the flask. The flask is
corked well and the contents are shaken vigorously. After cooling, again 5ml of
sodium hydroxide and 0.5ml of benzoylchloride are add4ee and shaken well. The
process is repeated till all the benzoyl chloride is added. If the mixture smells that
of benzoylchloride, some more sodium hydroxide must be added. The white
precipitate of benzanilide formed is filtered and dried. A portion of the sample is
recrystallised from alcohol.
RECRYSTALLISATION :
About 1g of the benzoic acid is dissolved in boiling water and recrystallised.
White crystals of salicylic acid are separated and dried.
RESULT :
The yield of benzanilide =___________g.
HYDROLYSIS
PREPARATION OF BENZOIC ACID FROM ETHYL BENZOATE
AIM:
To prepare a pure sample of benzoic acid from ethyl benzoate.
PRINCIPLE :
Esters are readily hydrolyzed by a strong solution of alkali. Sodium salt of the
acid obtained is neutralized with a mineral acid like Conc.HCl. When benzoic acid
is precipitated as white crystals.
REACTION :
CHEMICAL REQUIRED :
i. Ethyl benzoate = 5ml
ii. 10% sodium hydroxide solution = 30ml
PROCEDURE :
About 5ml of ethyl benzoate and 30ml of 10% sodium hydroxide solution
are placed in a R.B.flask. A few porcelain chips or a glass bead is introduced
into it. It is heated ion a wire guaze until no oily drops of ethyl benzoate
are seen in the R.B.flask. The heating is then discontinued and the flask is
cooled. The contents are poured into a beaker containing 200ml water and
stirred well. About 10ml of 1:1 HCl solution is added in small quantity at a
timer till the solution is slightly acidic. It is tested by placed a drop of the
solution on a blue litmus paper which turns red. A white precipitate of
benzoic acid crystals is readily formed in the beaker on cooling. It is filtered
off using Buchner funnel, washed well with water dried. A small portion of
the sample is recrystallized using hot water.
RECRYSTALLISATION :
About 1g of the benzoic acid is dissolved in boiling water and recrystallised.
White crystals of benzoic acid are separated and dried.
RESULT :
The yield of benzanilide =___________g.
OSAZONE REACTION
PREPARATION OF GLUCOSAZONE FROM GLUCOSE
AIM:
To prepare pure crystals of glucosazone from glucose.
PRINCIPLE :
Glucose undergoes addition as well as oxidation reaction when treated with
phenyl hydrazine in slightly acid medium.
REACTION :
CHEMICALS REQUIRED :
i. Glucose
ii. Phenyl hydrazine
iii. Glacial acetic acid
iv. Sodium acetate crystals
PROCEDURE :
In a large hard glass boiling tube or in a 100 R.B.flask 2g of glucose is dissolve in
20ml of wter. 4ml of phenyl hydrazine liquid or mostly available from phenyl
hydrazine as its hydrochloride is introduced into flask. Of it 4ml of acetic acid
followed by 2g of sodium acetate crystals are added. Calculated quantity of acetic
acid and sodium acetate crystals added to maintain a moderate acidic
mediumneither excess nor inadequate addition of CH3COOH and CH3COONa is
desired, since it may lead to dissolution of the precipitate. The flask is then
heated on a water-bath for thirty minutes. The yellow precipitate of glucosazone
is filtered the pump, washed with water and dried.
RECRYSTALLISATION :
About 1g of sample is recrystallised from alcohol. Pure yellow crystals of
glucosazone are separated and dried.
REPORT :
The yield of glucosazone =___________g.
