3

CHAPTER

DETERMINATION OF MELTING PoINT

The melting point of a substance may be defined as the temperature at which the
substance
changes from the solid state to the liquid state. It is a very useful physicalconstant
a pure substance melts at a definite temperature and has a sharp because
melting point while an
impure substance has a lower melting point and melts over a wide range.
determination of melting point is a very convenient method to check the purityTherefore,
of a solid
substance. Moreover, melting point determination can be used to identify a
comparing its melting point with the melting points of known substances. substance by

EXPERIMENT 3.1
To determine the melting pointof the given solid
substance.
REQUIREMENTS
100 ml beaker, thermometer, iron stand, clamp, tripod stand,
tube 8to 10 cm long and 1 to 2 mm diameter, spatula. Liquid stirrer, thin-walled capillary
paraffin.
PROCEDURE
1. Powder the crystalline substance. Take a capillary tube and seal its
one end by heat
ing (Fig. 3.1). For filling the substance make a heap of the powdered substance on
the porous plate. Push the open end of the capillary tube into the heap.Some substance

Inverted
Heap of porous
sample plate Tap

Sealed capillary
Push

Fig. 3.1. Sealing one end of the Fig. 3.2. Charging the capillary tube
capillary tube.
16
DETERMINATION OF MELTING POINT
17
will enter into it. Now tap the sealed end of the cap1illary tuhe on
the no
plate gently. Fill the capillary tube up to 2-3 mm.
2. Attach the capilary tube to athermometer which isimmersediin abath of
liquid paraffin.
Thesurface tension of the bath liquid is suflicient to lhold the capillary tube
in position.

Thomometor

Boakor

-Liquid paraffin
Capillary

Burner
Substance

Fig. 3.3. Taking the melting point.

3. Heat the beaker slowly and go on stirring the liquid in the beaker so that the
temperature remains uniform throughout. For this, a glass loop stirrer is moved up
and down. When the temperature is within 15° of the melting point of the pure
substance, the flame is lowered. Now, the temperature is allowed to rise slowly.
4. The temperature is noted when the substance starts melting. The
temperature is
noted again when it is completely melted. The average of the two readings gives the
melting point of the substance.
PRECAUTIONS
1. Use dry and powdered sample for the deternmination of melting point.
2. Keep the lower end of the capillary tube and the thermometer at the same level.
3. Packing of the powder should be uniform without any big air gaps in between the
solid particles.
4. Heating should be gradual and the bath should be stirred regularly to maintain
uniform temperature.
5. The bulb of the thermometer and the capillary sticking to it should not touch the
side or the bottom of the beaker.
6. Do not use rubber band for attaching the capillary tube to the thermometer.
OBSERVATIONS
Temperature at which the unknown substance begins to melt = t,°C
Temperature at which the substance completely melts = t,'C.
t, + t
Melting point of the unknown substance =
2 C=t°C.
RESULTS
The melting point of the given substance = t °C
 4
CHAPTER

DETERMINATION OF BoILING PoINT

temperature at which the vanour
The boiling point of a liquid may be defined a8 the
liguid
pressure of the liquid is equal to the atmospheric pres8ure exerted upon the
Surface. sur
The boiling point of the liquid depends upon the pressure exerted upon the liquid
different
therefore a liquid has
face. Since atmospheric pressure is different at different place,
boiling points. The
boiling points at different places. For the sakeof comparison we use normal
normal boiling point of a liquid may be defined as the temperature at which vapour
pressure (760 mm).
pressure of the liquid is equal to one standard atmospheric
it.
Theboiling point of a liquid increases if non-volatile impurities are present in

EXPERIMENT 4.1

Todetermine the boiling point of the liguid.

REQUIREMENTS
thermometer, a capillary tube, a
100 ml corning glass beaker, asmnall thin walled test tube,
or conc. sulphuric acid
tripod stand, wire gauze, stirrer, iron stand with clamp, liquid paraffin
and the given liquid.
PROCEDURE
boiling point
1. Take a small test tube and fill it two-third with the given liguid whose The rubber
with a rubber band.
is to be determined. Fix this tube to the thermometer
outside the liquid
band should be fixed near the mouth of thetube so that it remains
somewhere at the
paraffin bath. Adjust the tube so that the bottom of the tube is
middle of the thermometer bulb.
through a cork. Lower
2. Clamp the thermometer carrying test tube in an iron stand
Adjust the ther
the thermometer along with the tube into a liquid paraffin bath. tube with the
mometer so that its bulb is well under the acid and open end of the
rubber band is suficiently outside the acid bath.
about one cm from one end by
O. Take a capillary tube 5-6 cm in length and seal it at
the test tube so
neating it in flamne and giving a slight twist. Place this capillary in
that sealed part of it stands in the liquid.
19
20
PRACTICAL CHEMISTRY-XI
4. Start heating the liquid paraffin bath slowly and stir the bath gently. Keep an eye on
the liquid and the test tube and also on the thread of the mercury in the thermn
meter. At first, a bubble or two will be seen escaping at the end of the capillary
dipping in the liquid, but soon a rapid and continuous stream of air bubbles escapes
from it.This is the stage when the vapour pressure of the liquid in the sealed canil.
lary just exceeds the atmosphericpressure. Note the temnperature when continuous
stream of bubbles starts coming out. Remove the flame and note the temperature
when the evolution of bubbles from the end of the capillary tube just stops. The
mean of these twotemperatures gives the boiling point of the liquid.

Capillary
Stirrer

Rubber band

Liquid

Liquid paraffin

Bubbles Capillary
tube

Liquid

Fig. 4.. Determination of the boiling point.

5. Allow the temperature fall by 10°C and repeat the heating and again note the boiling
point.
PRECAUTIONS
1. Keep the lower end of the ignition tube and the thermometer bulb at the same leve
2. Record the temperature as the boiling point at which brisk and continuous evolu organic
of the bubbles starts from the lower end of the capillary dipped in the liquid
compound. inthe
3. If on placing the sealed capillary tube in the test tube, the liguid is seen rising this
capillary tube, it indicates that the capillary tube is not properly sealed. Reject
capillary tube and use a sealed new one.
4. The sealed point of the capillary tube should be well within the liquid.
5. The paraffin bath must be heated very slowly and the paraffin stirred to e
uniform heating.
DETERMINATION OF BOILING POINT 21

OBSERVATIONS
Boiling point

Mean boiling point = = t°C.

2

RESULTS
The boiling point of thegiven liquid = t°C
Table 4.1. Boiling Points of Some Organic Compounds
Compound Boiling point (°C) Compound Boiling point (°C)
Benzyl alcohol 205 Ethyl benzoate 212
Glvcerol 290 Methyl salicylate 223
Ethylene glycol 197 Nitrobenzene 211
Phenol 182 Aniline 184
o-Cresol 190 o-Toluidine 200
Benzaldehyde 179 Chlorobenzene 132
Acetophenone 202 Bromobenzene 157
Phenyl acetate 196 Benzoyl chloride 197

Note. Paraffin can be safely heated upto 220°C while conc. H,SO, can be heated upto 280°C.
For finding the melting points of solids, having lower melting points, liquid paraffin may be
used while for solids having melting points greater than 200°C conc. H,S0, may be used.

VIVA QUESTIONS WITH ANSWERS

1. Define boiling point.
Ans. Boiling point may be defined as the temperature at which the
becomes equal to the atmospheric pressure. vapour pressure of the liquid
2. What is the effect of
increase of pressure on the boiling point ?
Ans. On increasing the outside pressure the boiling point of liquid
3 What is the effect of increases.
deerease of pressure on the boiling point ?
Ans. On decreasing the outside pressure the boiling point of
liquid
4 What
will happen to the boiling point of the liquid if some decreases.
to it ? non-volatile liquid is added
Ans. The boiling point of the liquid will
5. Why do different liquids have increase.
different boiling points ?
Ans. Boiling point depends upon intermolecular forces existing in
have intermolecular forces of different the liquid. Since different liquids
6.
Why is food cooked more quickly in a strength therefore their boiling points are different.
pressure
Ans. In a pressure cooker water boils at a higher cooker ?
higher temperature. temperature and hence cooking takes place at a
(. SupPpose boiling point of a liguid is 100°C in Delhi. Ata hill
different ? Give reasons. station will it be the same or
Ans. The boiling point of the liquid will be less than 100°C at the
with decrease in atmospheric pressure. At hill bill station. Boiling point decreases
in plains. stations the atmospheric pressure is less than tnà.
 EXPERIMENT 5.1

To prepare crystals ofpure copper sulphate (CuSO, 5H,0) from a given impure
sample of the blue vilriol.
THEORY
added to it in
The given sample is shaken with water. A few drops of dilute sulphuric acid are
order to prevent hydrolysis of copper sulphate. Copper sulphate present in the sample gets
dissolved while the insoluble impurities are left behind. The solution is filtered. The filtrate is
concentrated to the crystallisation point and then cooled. On cooling, crystals of copper sulphate
(CuSO,.5H,0) separate out.
REQUIREMENTS
Crude sample of copper sulphate, a 400 ml beaker, a china dish, a funnel, an evaporating dish
and a policeman (glass rod).
PROCEDURE
it smal
I. Preparation of Solution. Take about 25-30 ml of water and add to
quantities of the powdered crude copper sulphate. Stir well to dissolve it. Make several
 CRYSTALLISATION
PURIFICATION OF CHEMICAL SUBSTANCES BY 27

additions of the powdered sample till a little of it remains undissolved even if it is

stirred for sometime. Now add 2-3 ml of dilute sulphuric acid to make the solution
clear. This prevents hydrolysis of the copper sulphate.
9 Bltration of the Solution and Concentration of the Filtrate to Crystallisation
noint, Filter the solution and collect the filtrate in a china dish. The insoluble
impurities are left as residue on the filter paper.
reduced
Heat the china dish on a sand bath till the solution is
toabout one-third of itsoriginal volume. As the solution gets
heated up, it is stirred well with a glass rod to avoid crust Roll
formation on the side of the dish. If the crust is formed, it is No.
dissolved into the solution by removing it with glass rod. Don't
allow the solution in the dish to boil.
Remove a drop of the solution at the end of a glass rod and
cool it by blowing. The appearance of a crust or tiny crystals
on the glass rod shows that the crystallisation point has Fig, 5.12. Preserving
reached. Now turn off the burner and stop heating. Transfer of crystals.
the hot saturated solution in a crystallising dish.
containing
3. Cooling the Hot Saturated Solution. Place the crystallisation dish
allow it to
hot saturated solution on a beaker containing water filled to the brim and
cool slowly for sometime. Deep blue crystals of copper sulphate will appear. After
about half an hour, the crystallisation is complete.
4. Separation of Crystals and Drying. Decant off the mother liquor carefully. Wash
water. Re
the crystals with a little ethyl alcohol containing small amount of cold
move the crystals on a filter paper which soaks the solution.Transfer the crystals on
another filter paper and dry them by pressing gently between the folds of the filter
and
papers or by spreading on a porous plate. Transfer the crystals to a dry test tube
cork it (Fig. 5.12).
The crystals of pure copper sulphate (CusO,.51,0) are triclinic, transparent
and blue.

PRECAUTIONS
1. The filtrate should be evaporated slowly by gently heating during concentration.
2. The filtrate is to be evaporated only up to the crystallisation point. It should never be
heated to dryness. Avoid overheating of the solution.
3. The solution should be cooled slowly without disturbing it. It should never be cooled
rapidly.
4. Wash the crystals with the washing liquid 3-4 times using very small amount of the
liquid each time.
b. In case the crystals obtained are very small, it means that the solution has been
concentrated more than that required at the crystallisation stage.
10.1. DETECTION OF NITROGEN, SULPHUR, CHLORINE, BROMINE AND
IODINE BY. LASSAIGNE'S TEST
 Table10.1. Detection ofN, S,CL Br and Iby
Lassaigne's Test
Experiment
Observations Inference
Preparation of Lassa
igne's extract
Fuse a small piece of sodium
in a fusion tube. Add a little
organic compound to it and heat.
Plunge it in a china dish
containing distilled water. Boil
the contents and filter. The
fltrate is called Lassaigne's
extract.

1.Test for Nitrogen :

Prussian blue colour Nitrogen present
To 2 ml of Lassaigne's extract
add 2 ml of freshly prepared
|FeSO,,
4 boil and add a few drops
of FeCl, solution and concen
trated hydrochloric acid.
 PRÁCTICAL CHEMISTRY-

138

Sulphur present
2. Test for Sulphur: ex
Black ppt.
(a)To 2 mlof Lassaigne'sacid
acetic
tract add 2-3 drops of
acetate
and 1 ml of lead
solution. Purplecolour Sulphur present
(b) To2 ml of Lassaigne'sex
tract add a few drops of sodium
nitroprusside solution.
3. Test for Halogens :
(a)Silver nitrate test
ppt. solu Chlorine present
Acidifv a little of Lassaigne's (i) Acurdy whiteNH,OH.
extract with concentrated HNO, ble in excess of
boil, cooled and add silver nitrate (iü) Apale yellow ppt. spar Bromine present
solution. ingly soluble in NH,OH.
(üi) A bright yellow ppt. Lodine present
insoluble in NH,OH.
(6) Carbon disulphide test
Acidify another portion of (i) Orange colour in CS, Bromine present
Lassaigne'sextract with dil. HCI layer.
and add l ml of CS, and two drops (iü) Violet colour in CS, Iodine present
of chlorine water and shake.
layer.

VIVA QUESTIONS WITH ANSWERS

1. Why is sodium metal kept under kerosene oil?
Ans. Sodium metal reacts with oxygen and moisture
contact of air and sodium and thus protects it from the present in air. Kerosene oil prevents the
2. action of moisture and oxygen.
Why an organic compound is fused with
extract ? sodium metal for preparing Lassaigne s
Ans. When the organic compound is
and halogens, if present in heated with sodium, the elements such as
the
water. The aqueous solution is then compound, are converted into sodium salts whichnitrogen,soluble
suip in
used to identify these are
3.
Can we use elements.
potassium
Ans. No. Potassium
in place of
sodium in
4. In the
is too
reactive metal and henceLassaigne's test ?
Ans.It isLassaigne' s test for nitrogen
what is
dangerous to use.
due to the the bluish green colour due to?
5. During
the formation of ferric
ferrocyanide,
due to ? detection of nitrogen,
Ans. The sometimes Fe,[(FeCN)3
a blood
red colour is obtained. Whatisthis
the organicformation of blood red colour with
6. Why is fr compound. It is due to FeCL,