EXPERIMENT1

AIM:Detemine molecular mass of naphthalene by Rast method using

camphor as solvent
Introduction: When one mole of a solute is contained in 1 kg of solvent, the melting point of that mixture is
lowered by a characteristic amount. That amount is called the molal freezing point depressio n constant, Kf.

This can be written as a formula: Kf = Molecular depression constant for camphor (39.7)
w = Weight (mass) of unknown compound (solute)
W = Weight (mass) of camphor (solvent)
T = Depression of melting point
M = gram molecular weight of solute
In this simulation you will be asked to find the molecular weight of an unknown solid by measuring the
depression of the melting point of camphor when the solid is mixed with it.
Procedure:
Put a little pure camphor onto a clean watch glass. Now take a melting point tube sealed at one end, and tamp it
into the solid – open end down. Now invert the tube and tap it lightly on the bench to get the solid to the end of
the tube. While this method works with most dry solids, camphor has a peculiar tenacity and it may have to be
poked to the bottom of the tube with a wire.

The tube is now attached to a thermometer with a rubber band. The assembly is put into a thiele tube full of oil.
The tube is designed so that the hot oil will circulate evenly.

At the melting point the solid will become clear liquid. Record the melting point of the pure solvent (camphor).
record the temperature when the last crystal melts.

measure the melting point of a mixture of camphor and your unknown sample. a homogeneous solution of the
unknown and camphor in known concentration. weigh some camphor and some unknown, melt them together
and find the melting point of the mixture.

Measure the mass of an empty test tube. Add about 1 gram of camphor and record its mass. Add about 0.1 gram of
the unknown solute and record its mass. The contents of the test tube are melted by placing it in an oil bath
preciously heated to 180-185 degrees. The liquid must not be heated more than one minute or the camphor will sublime
from the solution.

The tube is taken from the bath, propped up in another beaker and allowed to cool. Some of the solid is scraped
from the tube and powdered on a watch glass. It is convenient to use the bottom of a test tube as a pestle.
A little of the solid is put into a melting point tube as before. The tube is attached to the thermometer and the
melting point is obtained. Record the melting point of the mixture.
Data:
Melting Point of pure camphor: T1
Melting Point of mixture: T2
Depression in freezing point
T=T2-T1

Mass of empty test tube: _______

Mass of t.t. + camphor: _______
Mass of t.t. + camphor + unknown: _______

Calculations:
Weight of camphor, W, = _______
Weight of unknown, w, = _______

K f  w 1000
M T W
 EXPERIMENT 2
Aim- To Prepare Coppertetraamine complex [Cu(NH3)4]SO4.H2O.

Theory- Tetraamine complex is prepared by the action of ammonia on

copper suplahte.

Requiremants- Copper sulphate=5g

Concentrated ammonia=10ml

Ethyl alcohol= 15ml

Procedure-

1. Take 5g of finely powdered Copper sulphate and dissolve in minimum

amount of water in a 200ml beaker. Add Few drops of dil.H2SO4 to
get a clear solution\
2. Add 10ml of concentrated ammonia solution to copper sulphate
solution slowly with constant stirring until the blue ppt.of Cupric
hydroxide initially formed dissolve to give a deep blue solution
having ammonical smell.
3. Add 15ml of ethyl alcohol slowly to the beaker with constant stirring
so that blue colour is discharged and the purple coloured ppt of
tetraamine copper(II) sulphate separates out.
4. Heat the reaction mixture to 60-700C on a water bath for 10-15min.
5. Allow the solution to cool. Needle shaped blue coloured crystals of
tetraammine copper(II) sulphate separates out.
6. Decant off the supernatant liquid.
7. Separate the crystals of filtration on an Buchner funnel under
sunction. Wash the crystals with ethyl alcohol.
8. Remove the filter paper alongwith crystals from the Buchner funnel
and place it on the folda of the filter paper.
9. Dry the crystals in the folds of filter paper and record the yield.

Result- Deep blue in colour and needle shaped crystals are formed.

Expected yield-5g.
 EXPERIMENT 3
Aim- To prepare Sodium trioxalatoferrate (III) Na3[Fe(C2O4)3].9H2O

Theory- Sodium trioxalatoferrate (III) is prepared by the action of sodium

oxalate on hydrated ferric oxide ( Fe2O3.3H2O) which is prepared by the
reaction of ferric chloride with sodium hydroxide.

Requirements- Ferric chloride =10.0g

Sodium hydroxide=11.5g

Oxalic acid= 12.0g

Procedure-

1. Dissolve 10.0g of ferric chloride in 50ml of water.

2. Dissolve 7.5g of sodium hydroxide in 50ml of water.
3. Add Sodium hydroxide to ferric chloride solution in small lots with
stirring to get precipitate of ferric hydroxide.
4. Allow the precipitate to stand and settle down.
5. Filter through a Buchner and wash the ppt. with hot water.
6. Dissolve 12g of oxalic acid in 50ml of water in beaker and it to 4g of
sodium hydroxide pellets to get sodium oxalate solution.
7. Add ferric hydroxide ppt. to hot sodium oxalate solution with stirring.
8. Filter the solution to remove any insoluble impurities. Collect the
filtrate in a china dish.
9. Heat the solution and concentrate it to the crystallization point.
10. Allow the concentrated solution to cool slowly and green coloured are
obtained.
11. Wash the crystals with cold water and then with ethyl alcohol.
12. Dry the crystals and note the weight.

Result

The green coloured ppt are obtained and expected yield=15g

 EXPERIMENT 4
AIM: Determination of the strength of a solution

of hydrochloric acid by a standard solution of sodium hydroxide

conductometrically
Theory:
When hydrochloric acid solution (HCl) is titrated with sodium hydroxide solution
° + –1 –1
(NaOH), the highly mobile hydrogen ions ( H = 350 ohm cm ) are progressively
° + –1 –1
replaced by slower moving sodium ions ( Na = 50 ohm cm ) and the conductance of

the solution decreases. After the end point, the conductance of the solution rises sharply due
° – –1 –1
to the presence of excess, highly mobile hydroxide ion ( OH = 198 ohm cm ). Thus the
neutralization of a strong acid by addition of a strong base leads to a minimum conductance
+
at the end points. This is due to the disappearance of H ions and their
 +
replacement by slower moving Na ions of the base followed by the presence of highly
–
mobile OH ions after the end point.
Therefore the nature of the plot (conductance of the solution versus volume of base
added) will be as given below:

Figure 1

The conductivity cell used for this titration should permit stirring by shaking and to which
the reagent can be added from burette. A large increase in volume during titration should
be avoided.

Apparatus: Conductometer, conductivity cell, beaker, pipette, burette, conical flask.

Chemicals: Hydrochloric acid (HCl), sodium hydroxide (NaOH), conductivity water.
Procedure:
1. HCl solution of unknown strength is provided.
2. 0.1 (N) NaOH solution is provided.
3. Calibration of the instrument done at room temperature.
 4. Conductometric Titration:
i) Rinse the conductivity cell a number of times with conductivity water or double
distilled water.
ii) Pipette out 20 mL of HCl in a beaker and dip the conductivity cell in it, so that the
cell should dip completely in solution.
iii) Note the temperature of the sample solution and accordingly set the temperature
control or keep the cell in a thermostat at room temperature.
iv) Add NaOH solution (few drops) from burette into HCl in lots of 0.5 ml,after each
addition stir it and measure the conductance after each addition.
v) Note the conductance till 10 ml of NaOH solution has been added
Observation and Calculation:
Table 1:- Conductometric Titration

s.no Volume of 0.1 N NaOH conductance

added(ml)
1 0.0
2 0.50
3 1.00
4 1.50
5 2.00
6 2.50
7 3.00
8 3.50
9 4.00
10 4.50
11 5.00
12 5.50
13 6.00
14 6.50
15 7.00
16 7.50
17 8.00
18 8.50

Plot a graph between conductance and volume of titrant (NaOH solution). Two
intersecting lines will be obtained (as given in the Figure 1) and the points of
intersection of these lines represent the equivalent point.
 Let, V2 be the volume of NaOH at the equivalent point (from graph) for 20 ml 0.1
NHCl
Then (HCl) N1 V1 = N2V2(NaOH)
 N1 = ()V2/200 (N) 
Strength= normality × equivalent bond
= (V2/200) × 36.5 g/L

Precautions:
i) Electrical connection should be made carefully.
ii) Temperature during the experiment should be kept constant as conductance depends
on temperature.
iii) Stirring should be done after each addition of titrant.
iv) To avoid the dilution effect, the concentration of the titrant should be 5-10 times more
than that of the solution to be titrated.
 EXPERIMENT 5

AIM:To find refractive index of the given liquid samples and find Molar
refraction and specific refraction.

APPARATUS:Abbe’s refractometer, temperature controller, light

source and samples.

THEORY:

Abbe’s
Refractometer:The
Abbe instrument is the
most convenient and
widely used
refractometer, Fig(1)
shows a schematic
diagram of its optical
system. The sample is
contained as a thin
layer (~0.1mm)
between two prisms.
The upper prism is
firmly mounted on a
bearing that allows its
rotation by means of
the side arm shown in
dotted lines. The lower
prism is hinged to the
upper to permit
separation for cleaning
and for introduction of
the sample. The lower prism face is rough-ground: when light is
reflected into the prism, this surface effectively becomes the source for
an infinite number of rays that pass through the sample at all angels.
The radiation is refracted at the interface of the sample and the
smooth-ground face of the upper prism. After this it passes into the
fixed telescope. Two Amici prisms that can be rotated with respect to
another serve to collect the divergent critical angle rays of different
colors into a single white beam, that corresponds in path to that of the
sodium D ray. The eyepiece of the telescope is provided with
crosshairs: in making a measurement, the prism angle is changed until
the light-dark interface just coincides with the crosshairs. The position
of the prism is then established from the fixed scale (which is normally
graduates in units of nD). Thermosetting is accomplished by circulation
of water through the jackets surrounding the prism.

The refractive index of a substance is ordinarily determined by

measuring the change in direction of colliminated radiation as it passes
from one medium to another.

(1)

Where v1 is the velocity of propagation in the less dense medium M1

and v2 is the velocity in medium M2; n1 and n2 are the corresponding
refractive indices and θ1 and θ2 are the angles of incidence and
refraction, respectively Fig 2.

When M1 is a vacuum, n1 is unity because v1 becomes equal to c in

equation (1). Thus,

(2)

Where nvac is the absolute refractive index of M2. Thus nvac can be
obtained by measuring the two angles θ1 and θ2Abbe's refractometer
is used to measure the refractive index of the given organic liquid.
Using a particular monochromatic light source, the apparatus is
calibrated with water as the liquid. Adjust the micrometer screw to
focus the boundary between the bright and dark regions. Adjust the
refractometer scale to place the cross wire of the telescope exactly on
the boundary between the bright and dark regions. Repeat the same
process for different organic liquids after the equipment is calibrated.

PROCEDURE:

1. Clean the surface of prism first with alcohol and then with
avetone using cotton and allow it to dry.
 2. Using a dropper put 2-3 drops of given liquid b/w prisms and
press them together
3. Allow the light to fall on mirror.
4. Adjust the mirror to reflect maximum light into the prism box
5. Rotate the prism box by moving lever until the boundary b/w
shaded and bright parts appear in the field of view.
6. If a band of colors appear in the light shade boundary make it
sharp by rotating the compensator.
7. Adjust the lever so that light shade boundary passes exactly
through the centre of cross wire
8. Read the refractive index directly on the scale
9. Take 3 set of readings and find the average of all the readings.

OBSERVATIONS:

Room temp. =_degrees

Sr.No. LIQUID REFRACTIVE INDEX

1.
2.
3.
i

Specific refraction, R = (n2 _ 1)/(n2 + 2) × 1/d

Molar refraction, Rm= R ×M( molecular mass of liquid)