EXPERIMENT 6

TITLE: GAS ABSORPTION-VALIDATION OF LIQUID PHASE ANALYSIS

AIM: To analyze the composition of ammonia (NH3) in air by, (1) Acid-base titration of the liquid
phase, (2) Specific gravity method.

THEORY: Set out a suitable theory for this experiment.

APPARATUS

250 ml volumetric flasks, 100 ml measuring cylinder, suitable hygrometer, 50 ml burette, pipette,
wash bottle.

REAGENTS

Concentrated Ammonia solution (commercial grade), phenolphthalein indicator, distilled water,

concentrated hydrochloric acid.

METHOD

Step 1: Sample preparation.

Sample 1

 Transfer 100 ml aliquot from the stock solution of Ammonia(commercial grade) whose
concentration has been predetermined and dilute it with distilled water in the ratio 1:1 by volume
in a 250 ml volumetric flask and label it sample 1.

Sample 2

 Transfer 100 ml aliquot from sample 1 and dilute it with distilled water in the ratio 1:1 by volume
in a 250 ml volumetric flask and label it sample 2.

Sample 3

 Transfer 100ml aliquot from sample 2 and dilute it with distilled water in the ratio 1:1 by volume
in a 250ml volumetric flask and label it sample 3.

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 Sample 4

 Transfer an aliquot of 100 ml from sample 3 and dilute it with distilled water in the ratio
1:1 by volume in a 250 ml volumetric flask and label it sample 4.

Sample 5

 Transfer 100 ml aliquot from sample 4 and dilute it with distilled water in the ratio 1:1 by
volume in a 250 ml volumetric flask and label it sample 5.

Sample 6

 Transfer 100 ml aliquot from sample 5 and dilute it with distilled water in the ratio 1:1 by
volume in a 250 ml volumetric flask and label it sample 6.

Sample 7

 Transfer 100 ml aliquot from sample 6 and dilute it with distilled water in the ratio 1:1 by
volume in a 250 ml volumetric flask and label it sample 7.

Sample 8

 Transfer 100 ml aliquot from sample 7 and dilute it with distilled water in the ratio 1:1 by
volume in a 250 ml volumetric flask and label it sample 8.

Sample 9

 Transfer 100 ml aliquot from sample 8 and dilute it with distilled water in the ratio 1:1 by
volume in a 250 ml volumetric flask and label it sample 9.

Procedure

(a) Firstly, determine the concentration of the solutions from sample 3 to 9 by acid-base
titration with standard HCl using the experimental set up as shown above.

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Experimental set up 2

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(b) Secondly, determine the specific gravity of the solutions from sample 3 to 9 by
hygrometer method using the hygrometer as shown in the experimental set up as shown
above.

Step 2: Determination of ammonia concentration and specific gravity.

 Determine the concentration of the solutions from sample 3 to 9 by acid-base titration

with standard HCl (Either 0.2M, 0.5M or 1.0M of HCl).
 Determine the specific gravity of the solutions from sample 3 to 9 by hygrometer
method using the hygrometer.

Assume that, as a student, you have performed this experiment and you have collected
experimental data as shown in the table below.

Experimental data:

Titration of NH3 solution with 0.8456 M HCl solution

Sample Volume of NH3 solution used Volume of HCl used Conc of NH3 Specific
Number (cm3) (cm3) (mol/dm3) gravity
1 62.8 20 0.976
2 31.0 20 0.987
3 16.3 20 0.992
4 15.5 20 0.995
5 7.8 20 0.996
6 4.1 20 0.996
7 4.5 20 0.997
8 2.3 20 0.996
9 1.1 20 0.997

Calculate and fill in the concentrations of NH3 solution in the table

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WRITE UP:

 Plot the graph of Concentration against Dilution and Specific gravity against Dilution.

Note that Dilution must be on the x-axis.

EXERCISE:

 From the two graphs obtained, compare and explain the similarities in the two methods
for determining the amount of ammonia (NH3)
 Which method between the two seems to be a better method for determining the amount
of NH3?
 Advise on which other solution the hygrometer can be used for analysis.

EXPERIMENT 8

TITLE: RAYLEIGH’S DIFFERENTIAL DISTILLATION

AIM: To determine the relative volatility of a wide boiling mixture by differential distillation.

APPARATUS
Quick-fit distillation kit, measuring cylinders, thermometer, pipette, burette, beakers, wash
bottle, conical flask.

REAGENTS
Sulphuric acid, distilled water, methyl orange indicator, 0.1M sodium carbonate.

PRINCIPLE
The depletion of the liquid feed mixture in a still pot is given by:
wdx = (y-x) dw
Where y = kx,
k = proportionality constant called the VLE constant. The integration of equation above
through definition of y gives:

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 In w/w0 =- 1/k-1 In x/x0
Where W0 is initial feed amount
x0 is initial composition
w is residue amount
x is distillate amount
k = f (α), α= relative volatility.

PROCEDURE

 Prepare 0.001 M sodium carbonate.

 Add 50 ml of distilled water, followed by 2.5 ml concentrated sulphuric acid in a double
necked round bottomed flask.
 Carefully assemble the quick-fit full set with the thermometer component in its right
place.
 Connect the condenser to the cooling-water tubing and place a measuring cylinder
under the condenser tube outlet.
 Heat up the contents and commence the distillation.
 Collect the distillate (D) every after five milliliters (5 ml).
 Measure the residue amount (w) in ml by subtracting the distillate (D) from the initial
feed (w0)
 Measure the concentration of x (distillate amount) by titrating it against 0.001M sodium
carbonate
 Continue distilling until you obtain about 8-9 measuring cylinders for the distillate.

Assume that, as a student, you have performed this experiment and you have collected experimental data
as shown in the table below.

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Experimental data: w0 = x0=

TIME (min) TEMP (OC) w x

5 98 50 3.26
10 98 45 3.62
15 98 40 4.07
20 98 35 4.66
25 98 30 5.43
30 98 25 6.52
35 98 10 8.15
40 98 15 10.85
45 105 10 16.25

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WRITE UP:

 Plot graph of In w/w0 vs. In x/x0 for the acid or base

 Plot a graph of In w/w0 vs. In x/x0 for water

EXERCISE:
 Determine α
 Calculate the absolute, relative and relative percentage errors in the experiment