RECORD OF CHEMISTRY

BY
AMRUTH SHRI S NAIR
10A
 INDEX
S.No: TOPIC Pg.no:
| LABORATORYPREPARATIONS 1
1. Hydrogen chloride gas 2-5
2. Hydrochloric acid 6-8
3. Nitric acid 9-11
4. Ammonia 12-15
|| MANUFACTURUNG METHOD 16

1. Nitric acid 17-20

2. Sulphuric acid 21-23
3. Ammonia 24-28
||| IDENTIFICATION TESTS 29
1. Sulphuric acid 30-31
2. HCL gas and acid 32
3. Ammonia 33
4. Carbon dioxide 34
1.

Laboratory preparation
. 2.

Preparationofhydrogenchloridegasfromcommonsalt
3.
.LABORATORY PREPARATION OF HYDROGEN CHLORIDE GAS
In the laboratory, hydrogen chloride gas can be prepared by the
action of concentrated sulphuric acid on sodium chloride.

Reactants:Sodium chloride and concentrated sulphuric acid.

Procedure : Set up the apparatus as shown in Figure.

Place some common salt in a flask and pour concentrated sulphuric
acid through the thistle funnel. The reaction proceeds slowly in the
cold. On heating the mixture gently there is effervescence and HCl
gas is evolved in a controlled manner.
The gas is dried by passing through a washer bottle containing
concentrated sulphuric acid.
It is collected by upward displacement of air in a gas jar.

Reaction:
<200°C
NaCl+H₂SO₄-------------NaHSO₄ + HCI↑

Though it is a reversible reaction, yet it ges to completion as

hydrogen chloride continuously escapes as a gas.
The reaction can occur upto the stage of formation of sodium
sulphate on heating above 200°C.

4.
The reaction can occur upto the stage of formation of sodium
sulphate on heating above 200°C.
>200°C
NaHSO₄ + NaCl----------- Na₂SO4 ₄+ HCI↑
Or
>200°C
2NaCl+H₂SO₄------------Na₂SO₄ + 2HCI
(Conc.)

Note:
(i) Sodium chloride is cheap and therefore it is preferred for
preparation of HCl over other metal chlorides.
(ii)Conc. Nitric acid is not used during the preparation of HCI because
it is volatile and may volatilize out alongwith hydrogen chloride.

Purification of HCI gas:

It is dried by passing through conc. Sulphuric acid.
The other drying agents like phosphorus pentoxide (P₂O₅) and quick
lime (CaO) cannot be used, since they react with hydrogen chloride.
2P₂O₅+ 3HCl → POC1₃ + 3HPO₃
CaO + 2HCl → CaCl₂ + H₂O
5.
Collection:

1 . Hydrogen chloride gas is collected by the downward delivery

(upward displacement of air) as it is 1.28 times heavier than air.
2 . It is not collected over water, since it is highly soluble in water.

Precautions :
(a)The lower end of the thistle funnel must be dipped in conc.
Sulphuric acid.
(b)Delivery tube should be dipped in drying agent i.e., conc. H₂SO₄
(c) temparature maintained at nearly 200°C

At higher temperature i.e., above 200°C:

(i) The apparatus which is made of glass may crack.
(ii) Fuel is wasted.
(iii)sodium sulphate formed, forms a hard crust which sticks to the
glass and is difficult to remove.
6.
Funnelarrangement

7.

.LABORATORY METHOD OF PREPARATION OF

HYDROCHLORIC ACID

The aqueous solution of HCl gas is known as Hydrochloric

acid.
It is prepared by dissolving hydrogen chloride gas in water.
The gas is passed into water until no more gas is absorbed.
The product is concentrated and contains about 36% of
hydrogen chloride by mass.
Procedure:
An inverted funnel, connected to the hydrogen chloride gas
supply, is placed in the beaker in such a way that it just
touches the water taken in the trough.
Since HCl gas is highly soluble in water, the water rises up in
the funnel, back-suction occurs and in turn, the level outside
the funnel falls creating an air gap between the rim of the
funnel and the surface of water.
The pressure outside and inside then becomes equal and the
water which had risen in the funnel falls down again.
This process continues till the water in the trough is
saturated with hydrogen chloride gas resulting in the
formation of hydrochloric acid.

.8.
.
Mechanism by which back suction is avoided or minimized
The funnel arrangement –

(a) prevents or minimizes back-suction of water.

(b) provides a large surface area for absorption of HCl gas.
Precaution: To prevent such an accident, an empty flask
(anti-suction device) is put between the generative flask and
the water trough. In case, the back suction occurs, the water
will collect in it and will not reach the generating flask.
A dilute aqueous solution of hydrochloric acid gets gradually
concentrated on distillation, till the concentration of the acid
reaches 22.2% HCl by weight and 77.8% water by weight
which boils at 110 °C. No further increase in concentration is
possible on boiling, as molecules of HCl (g) get mixed with
water vapours.
9.

Laboratory preparation of nitric acid

10.

LABORATORY PREPARATION OF NITRIC ACID

Reactants : it is obtained by distilling conc.sulphuric acid with

potassium nitrate KNO₃ (nitre) or sodium nitrate NaNO₃ (Chile
saltpetre).

Procedure: A mixture of equal parts, by weight, of

potassium/sodium nitrate and concentrated sulphuric acid is heated
gently to 180°C-200°C in a glass retort . Sulphuric acid is a non-
volatile acid and produces volatile nitric acid on reacting with
potassium nitrate or sodium nitrate.

Collection: The vapours of nitric acid are ondensed to a light yellow

liquid by chilling the receiver with running cold water.

Note:Pure acid is colourless but the acid obtained in the laboratory is

slightly yellow. The yellow colour is due to dissolution of reddish
brown coloured nitrogen dioxide gas in the acid. This gas is produced
due to the thermal decomposition of a portion of nitric acid.

4HNO₃---- 2H₂O+ 4NO₂ + O₂

11.
The yellow colour of the acid is removed: (i)If dry air or CO₂ is
bubbled through the yellow acid, the latter turns colourless because
it drives out NO₂ from warm acid which is further oxidised to nitric
acid.
(ii)By addition of excess of water, nitrogen dioxide gas dissolves in
water and thus the yellow colour of the acid is removed. The
reaction is the reverse of the decomposition of nitric acid.
Precautions:
(1) All glass apparatus is used because nitric acid vapours attack
rubber and cork.
(2) Conc. HCI is not used in place of conc. H₂SO₄ because HCI is
volatile and hence nitric acid vapours will carry HCI vapours.
(3) The temperature of the reaction should not exceed 200°C,
because sodium sulphate formed at higher temperature forms a
hard crust which sticks to the walls of the retort and is difficult to
remove, although the yield of HNO₃ is higher.
>200°C
NaNO₃+NaHSO₄--------Na₂SO₄ +HNO₃
>200°C
2NaNO₃+H₂SO₄--------Na₂SO₄+2HNO₃

The higher temperature:

(i) May damage the glass apparatus,
(ii) Decomposition of nitric acid can also occur
(iii) Wastage of fuel
12.

Laboratory preparation of Ammonia

. 13.
LABORATORY PREPARATION OF AMMONIA

(1)From ammonium chloride

Reactants: Ammonium chloride (NH4₄Cl) and calcium hydroxide

[Ca(OH)₂]. (Excess of calcium hydroxide is mixed well with
ammonium chloride).

Reaction:
2NH₃Cl + Ca(OH)₂→ CaCl₂ + 2H₂O + 2NH₃↑

Procedure:Reactants (ammonium chloride and calcium hydroxide in

excess) are finely grindedand taken in a round-bottom flask fitted in
a position, mouth downwards On heating the mixture, ammonia gas
is evolved.

Precautions:The flask is tilted in such a way that the water formed in

the reaction does not trickle back into the heated flask and thus
break it.

Drying of ammonia gas:In order to get dry ammonia, the gas is

passed through a drying tower containing lumps of quicklime (CaO).
14.
Unsuitability of other drying agents:Other drying agents like conc.
Sulphuric acid, phosphorous pentoxide and anhydrous calcium
chloride are not used, as ammonia being basic, reacts with them.
2NH₃+ H₂SO₄------(NH₄)2SO₄
6NH₃+ P₂O₅+ 3H₂O---2 (NH₄)₃PO₄ (ammonium phosphate)
CaCl₂ + 4NH,→ CaCl₂.4NH₃(addi on compound)

Collection:
Ammonia gas is collected in inverted gas jars by the downward
displacement of air because it is:
(i) Lighter than air (V.D. of NH₃ 8.5; that of air,14.4).
(ii) Highly soluble in water and therefore, it cannotbe collected
over water.

Note:
1. Higher ratio by weight of the alkali is used it may
counteract the loss by sublimation of NH₄Cl.
2. Calcium hydroxide is used, as it is cheap and not
deliquescent like other alkalies.
3. Though all ammonium salts, on heating with alkalies give
NH₃, yet NH₄NO₃ (explosive in nature) and NH₄NO₂on
warming with alkalies do not produce ammonia because
they decompose on heating.
15.
ꕔ
NH₄NO₃ ----N₂O+ 2H₂O
ꕔ
NH₄NO₂----N₂+2H₂O
(2)From metal nitrides
Ammonia can also be obtained by the actionof warm water on
nitrides of metals like magnesium or Aluminium. (This method is
costly)
Reaction:
Mg₃N₂+6H₂O-- 3Mg(OH)₂+ 2NH₃↑
Or
AIN+3H₂O AI(OH)₃+ NH₃↑

Procedure: Magnesium nitride or Aluminium nitride is kept in a

round bottomed flask fitted with a thistle funnel and a delivery tube ,
Warm water is added very slowly.
Ammonia gas is liberated and magnesium hydroxide or aluminium
hydroxide is also formed, but it remains in the flask and the liberated
ammonia gas escapes through the delivery tube.
The ammonia gas formed is collected by holding the jar with its
mouth downwards over the delivery tube.The gas can be dried by
passing it through quicklime packed in a drying tower.
16.

MANUFACTURING METHOD
17.

Manufacture of nitric acid by Oswald process

18.
MANUFACTURE OF NITRIC ACID
A German chemist Ostwald, in 1914, developed Ostwald process.
The process is explained in three steps:

Step 1:Catalytic oxidation of ammonia

A mixture of dry air (free from carbon dioxide and dust particles) and
dry ammonia in the ratio of 10:1 by volume, is first compressed and
then passed into the catalytic chamber containing platinum gauze as
catalyst at about 800°C

This results in the oxidation of ammonia into nitrogen monoxide

(Nitric oxide).
Pt
4NH₃+5O₂-------- 4NO + 6H₃O + Heat
800°C
The reaction is exothermic and the heat evolved maintains the
temperature of the catalytic chamber.

The hot gases are then passed through a heat exchanger (cooling
chamber), and then they are mixed with air and passed into another
chamber called oxidising chamber.
19.
Step II: Oxidation of nitric oxide in oxidation chamber

In this chamber, nitric oxide combines with oxygen to form nitrogen

dioxide at about 50°C.
50°C
2NO(g) + O₂(g)------- 2NO₂(g)

Step III: Absorption of nitrogen dioxide in water

The nitrogen dioxide together with the remaining air (sometimes

more air is added at this stage) is passed through the absorption
tower (a steel tower filled with quartz stone packed in layers), from
the top of which warm water trickles.
The nitrogen dioxide and oxygen present in the air react with water
to form nitric acid.

4NO₂(g) + 2H₂O(l) + O₂(g) · → 4HNO₃ (aq.).

The nitric acid obtained at the bottom of the tower is concentrated

above 50%.
The above acid on further distillation gives 68% nitric acid. This acid
is concentrated nitric acid which is used in laboratories.
20.
Concentration of nitric acid

Nitric acid up to 98% (fuming nitric acid) is obtained by distilling 68%

HNO3₃ over conc. Sulphuric acid.

Pure 100% nitric acid is obtained by strongly cooling the 98% acid,
when colourless crystals of pure nitric acid get separated at – 42°C.

Note: In the manufacture of nitric acid,

(i) Higher ratio of air is used because oxygen is only 1/5th in air
and it is required in all the three chambers.

(ii) Quartz is acid resistant and when packed in layers it helps in

dissolving nitrogen dioxide uniformly in water.
21.

Contact processsfor the manufacture of sulphuric acid

22.

MANUFACTURINGOFSULPHURIC ACID (CONTACT PROCESS)

The various step in the contact process are as follows:

1.production of Sulphur dioxide: Sulphur dioxide is produced by

roasting metallic sulphides in air
Equation:
4FeS₂+11.O2------2Fe₂O₃+8SO₂
Or
By burning louisiana sulfur(95.5% pure) in purified air
Equation:
• S+O₂--- SO₂
2 verification of gases:
The mixture of Sulphur dioxide and air contains various impurities
which must be removed otherwise the catalyst losses its efficiency.
The mixture is passed through a purifier called *electric precipitator*
consisting of a chamber with wires at high electric potential. The
electric charge attracted solid particles which are removed. The
mixture is then held to a *water scrubber* where it is completely
free from the dust particles. It is then dried by a prayer of
concentrated sulphuric acid in another chamber it then goes into the
arsenic purifier were everytime of arsenic oxide is removed
23.

3.catalytic oxidation of Sulphur: the clean dried gaseous mixture of

Sulphur dioxide and pass through *contact tower* loosely packed
with vanadium pendoxide or Platinum on perforated shelves. The
catalyst is placed in vertical iron pipe inside a cylindrical iron Tower
called the *converter* here the preheated mixture of Sulphur
dioxide and air(oxygen) on passing through catalyst pipes form
sulphur trioxide
V₂O₅
2SO₂+O₂ ⇋ 2SO₂+ꕔ
450°C
Since the reaction is highly exothermic, the catalyst is heated only in
the beginning to about 450°C. This temperature is maintain by the
heat evolved during the reaction

4.absorption of sulphur trioxide in sulphuric acid: the gases called in

a heat exchanger and is then absord in absorption tower in
concentrated sulphuric acid (98%).
SO₃+H₂SO₄ --- H₂S₂O₇(OLEUM)

5.Dilutionm to obtain sulphuric acid: it is diluted in dilution time by

adding calculator amount of water to obtain sulphuric acid of the
decide strength
H₂S2₂O₇ + H₂O ---- 2H₂SO₄ (oleum)
24.

Manufacture of Ammonia by Habers process

.25.

MANUFACTURE OF AMMONIA (HABER’S PROCESS)

Reactants: Nitrogen and hydrogen in the ratio of 1:3 by volume.

Sources of reactants :

Nitrogen gas is obtained by fractional distillation of liquid air.

Hydrogen gas is obtained from water gas (Bosch process) or from

natural gas.

Reaction :

N₂+ 3H₂⇌ 2NH₃+ heat.

The reaction is reversible, exothermic and proceeds with a decrease
in volume.

Favourable conditions:

Temperature: Optimum temperature is 450-500 °C.

Pressure: Above 200 atm..
26.
Catalyst: Finely divided iron*.

Promoter: Traces of molybdenum or Al2O3.

Rate of conversion : About 15% of the reacting gases get converted

to ammonia.
Recovery of ammonia :
Ammonia is separated from the unreacted nitrogen and hydrogen
by:

1. Liquefaction- -Ammonia is liquified easily as compared to

nitrogen and hydrogen.

2. Absorbing in water because NH, is highly soluble in water, while

N2 and H2 are very slightly soluble.

Process: Nitrogen and hydrogen are dried, purified and then mixed in
the ratio of 1: 3 respectively, at a relatively high pressure. This
mixture is passed in an electrically heated catalytic chamber
containing finely divided iron with aluminium oxide or a little amount
of molybdenum at a temperature of 500°C. Mixture of ammonia
formed along with residual nitrogen and hydrogen exchanges their
heat with the incoming unreacted nitrogen and hydrogen mixture.
27.
The hot mixture of the outgoing gases contains nearly 15% ammonia.
The mixture is passed through the cooling pipes (condenser).

Ammonia liquefies first, whereas nitrogen and hydrogen do not

liquefy easily.

The unchanged nitrogen and hydrogen are recirculated through the

plant to get more ammonia. By re-circulating in this way, an eventual
yield of 98% can be achieved. The ammonia produced is stored as
liquid under pressure.
:

(i) The reaction is exothermic, hence low temperature will

favour the synthesis. However, at low temperature, the
reaction proceeds slowly. In practice, the optimum
temperature has been found to be in the range of 450°C to
500°C.

(ii) Four volumes of reactants produce two volumes of product,

hence high pressure favours the formation of ammonia.

The optimum pressure is found to be 200 to 900 atm. Practically, a

pressure of about 250 atm. Is used.
28.
(iii)Catalyst and promoter: The speed of the reaction can be
improved by using a catalyst, which is finely divided iron, obtained by
the reduction of iron oxide.

A promoter molybdenum or Al₂O₃ is used to increase the efficiency

of the catalyst.

(iii) Since the reaction is exothermic, the heat evolved further

maintains the temperature. External heating is, therefore,
not required after the reactants are initially heated.

Note: The purification of nitrogen and hydrogen is necessary as

impurities like carbon dioxide, carbon monoxide and traces of
sulphur compounds (H₂S) poison the catalyst. The removal of these
catalytic poisons from nitrogen and hydrogen is very essential.
29.

IDENTIFICATION TESTS
30.
TESTS FOR SULPHURIC ACID AND SULPHATES

(1)When barium chloride solution is added to sulphuric acid or any

soluble metal sulphate, white precipitate of barium sulphate is
formed.

BaCl₂ + H₂SO₄ → BaSO₄ + 2HCI

BaCl₂+ MgSO₄→ BaSO₄ + MgCl₂

The white precipitate of barium sulphate is insoluble in any mineral

acid like hydrochloric acid or nitric acid.

Note: Precipitates of both barium sulphate and barium sulphite are

white in colour but barium sulphite precipitate dissolves in mineral
acids while barium sulphate precipitate does not.

(2)Conc. Sulphuric acid on heating with copper evolves sulphur

dioxide.
Cu + 2H₂SO₄→ CuSO₄+ 2H₂O + SO₂ ↑
(Conc.)
31.
Sulphur dioxide turns acidified potassium dichromate solution
green(Reducing property of SO₂).

K₂Cr₂O₇+H₂SO₄+3SO₂→Cr2(SO₄)3+K₂SO₄+ H₂O
(Orange). (Green)

(3)Conc. Sulphuric acid on heating with NaCl evolves pungent

fumes of HCl gas.
Δ
NaCl+H₂SO₄------NaHSO4 + HCl ↑
(Conc.)

HCl gas gives dense white fumes of ammonium chloride, with a glass
rod dipped in ammonium hydroxide.

HCI + NH4₄OH ⇌ NH₄Cl + H₂O

(dense white fumes)
32.
IDENTIFICATION TEST FOR HYDROGEN CHLORIDE AND
HYDROCHLORIC ACID

(1)HCI gas possesses a characteristic irritating smell.

(2)HCl gas gives thick white fumes of ammonium chloride, when a

glass rod dipped in ammonia solution is held near the vapours
of the acid.

NH₃+ HCl → NH₄CI

(3)With silver nitrate solution, both the gas and the acid give a
white precipitate of silver chloride.

AgNO₃ + HCl → AgCl↓+ HNO₃

The precipitate is insoluble in nitric acid but soluble in ammonium
hydroxide.

(4)A greenish-yellow gas, i.e. chlorine, is liberated when

concentrated hydro-chloric acid is heated with an oxidising
agent like manganese dioxide.
MnO2+4HCl-----MnCl2+2H2O+Cl2
The gas liberated turns moist starch iodide paper blue black.
33.
IDENTIFICATION TEST FOR AMMONIA

Ammonia gas can easily be recognised by the following

characteristics:
1. Has a sharp characteristic odour.
2. It turns
● moist red litmus blue
● moist turmeric paper brown
● phenolphthalein solu on pink.

3. It gives dense white fumes with concentrated hydrochloric acid.

NH₃+HCl -NH₄Cl
4. When NH3 gas is passed through copper sulphate solution blue
precipitate is formed which changes to Deep Blue solution on
passing the gas in access.

5. Ammonium salt generally produce Ammonia gas which

warmed with alkali like sodium hydroxide

6. Ammonium salt gives brown colour or precipitate with

Nessler’s solution K₂Hgl₄
34.
IDENTIFICATION TEST FOR CO₂GAS
(a) The gas is colourless and odourless.

(b)It turns moist blue litmus faint red.

© When the gas is passed through the lime water, it turns milky due
to the formation of white precipitate of calcium carbonate.

Ca(OH)₂ + CO₂ → CaCO₃ +H₂O

The milkiness disappears on passing excess of CO₂

CaCO₃ + CO₂+ H→ Ca(HCO₃)₂

Ppt (soluble)

(d)The gas has no effect on filter paper dipped in acidified

K₂Cr₂O₇orKMnO₄.
___________________________________________