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EXPERIMENT NO.

5
Abstract
Determine the amount of salicylic acid in acetyl salicylic acid, trade named as Aspirin.
For this we would know the actual amount of salicylic used for each tablet of Aspirin.
The following are the reagents & requirements for the experiment; standard solution of
NaOH & HCl, solution of Aspirin, burette, pipette, conductometer & volumetric flasks.
Here we used conductometric titration between NaOH & Aspirin solution, where NaOH
solution is standardized by HCl of 0.1M.

Theory
Conductometry [1] is the technique by which quantitative analysis has been made for
analysis of different species using the electrical conductance between the two electrodes.
This basically based on ability of conductances of different solutions by their respective
ions in the solvents.

The volume of titration which is required to react completely with the analyzed substance
in the titrand is called Equivalence Point. The measure of ability of a solution to conduct
electricity is called its conductance[2].
Water is a very poor conductor of electricity. The presence of ionic species (electrolytes)
in water increases the conductance considerably. Solutions of electrolytes, like metallic
conductors, obey Ohm's law. Thus, the current I passing through a solution of a particular
electrolyte is proportional to the applied potential difference V as given by the equation:
V
I=
R
Here R is the resistance offered by the solution in ohms (W)
V
R=
Or I
The resistance is directly proportional to the length  , of liquid through which the current
passes, and inversely proportional to its area of cross-section A. It therefore follows that:
ρ ×
R=
A
Here r is the constant of proportionality and is called the specific resistivity[2]. It is a
constant for an aqueous solution of a given electrolyte of fixed concentration at a
particular temperature. In SI units, resistivity has the units of ohm meter (W m). If area of
cross-section is increased, more ions will be able to flow and resistance will decrease.
The conductance L is defined as the reciprocal of the resistance expressed in units of W –1
or Siemens (S).
1
L=
R
Thus, the conductance of a homogenous body of uniform cross-section is proportional to
the cross-sectional area A and inversely proportional to the length  , given by:
A A
L= =κ ×
ρ × 
Here the reciprocal of resistivity r is replaced by another constantk, which is called the
specific conductivity with units W –1m –1 or S m –1 which can be expressed as:
 1 k  
κ= = = ∴ k =
RA ρ R A 
Here k is called the cell constant. [2]

The conductivity of a solution of an electrolyte increases as the temperature is raised. The
conductivity of a particular electrolyte at a fixed temperature depends upon:
a) the number of ions present in unit volume of solution
b) the speed at which the ions oscillate in step with the applied alternating voltage
c) ionizability of the electrolyte [2]

Conductivity does not solely depend upon the number of ions present in unit volume of
the solution. Concentrated solutions of very soluble electrolytes show a maximum
conductivity value which then decreases on further concentration of the solution. The
reason lies in the fact that ionic distances becomes less as concentration increases. This
results in a greater attraction between positive and negative ions, and with a greater
reduction in ionic speeds. The phenomenon is called "ionic interference". [2]

As the concentration of weak electrolyte is increased, there is an increase in the number
of molecules, but a small proportion of them are ionized. By increasing the concentration
of a weak electrolyte, the conductivity reaches a maximum value followed by a steady
decrease. This is the same effect as was observed for strong electrolyte but in this case,
ionic interference is not responsible as a weak electrolyte produces very few ions and few
ions can not interfere to a considerable extent.[2]

The addition of an electrolyte to a solution of another electrolyte under conditions
producing no appreciable change in volume will affect the conductance of the solution
according to whether or not ionic reactions occurs, the conductometric conductance may
either increase or decrease; thus in addition of base to a strong acid, the conductance
decreases owing to the replacement of hydrogen of high conductivity by another cation of
lower conductivity. This is the principle underlying conductometric titrations; i.e. the
substitution of ions of one conductivity by ions of another conductivity.[1]

Aspirin, or acetylsalicylic acid is a salicylate drug often used as an analgesic (to relieve
minor aches and pains), antipyretic (to reduce fever), and as an anti-inflammatory. It also
has an anti-clotting effect and is used in long-term, low doses to prevent heart attacks and
blood clot formation in people at high risk for developing blood clots. High doses of
aspirin may also be given immediately after an acute heart attack; these doses may inhibit
the synthesis of prothrombin and therefore produce a second and different anticoagulant
effect, although this is not well understood.
Aspirin is one of the most frequently used drugs in the treatment of mild to moderate
pain, including that of migraines, and fever. It is often combined with other analgesics,
even though this has never been shown to be more effective or less toxic than aspirin
alone. Aspirin has been used in addition to other non-steroidal anti-inflammatory drugs
and opioid analgesics in the treatment of pain associated with cancer. Aspirin can cause
blood loss. It can also cause heartburn.

Results
Weight of Aspirin = 0.5293 gm

· Standardization of NaOH Against 0.1M HCl

Initial Final
Serial Difference
Volume of Volume of
No. (ml)
NaOH (ml) NaOH (ml)
1 0 4.5 4.5
2 4.5 8.9 4.4
3 8.9 13.3 4.4

Titration Reaction
NaOH + HCl ® NaCl + H2O

Concentration of NaOH
Concentration of HCl = M1 = 0.1 M
Volume of HCl solution = V1 = 5 ml
Volume of NaOH solution = V2 = 4.4 ml (from table)
Concentration of NaOH = M2 =?

Formula
M 1V1 M 2V M 1V1 n2
= M2 =
n1 n2 Þ V2 n1
Here n1 = n2 = 1
5 × 0.1 × 1
M2 = = 0.1136M
1 × 4.4

· Conductometric Titration Between NaOH And Aspirin
Cell constant = 0.01 cm-1
→Addition of 3 ml of NaOH into Aspirin Solution
Volume of NaOH Conductance (µS) Specific Conductance
added (ml) (µS/cm)
0 4.59 0.0459
3 15.20 0.1520
6 20.90 0.2090
9 54.80 0.2480
12 30.80 0.3080
15 35.30 0.3530
18 41.20 0.4120
21 48.10 0.4810
24 52.23 0.5223
27 57.19 0.5719
30 60.09 0.6009
33 63.34 0.6334
36 59.30 0.5930
End Point
Volume of NaOH consumed concluded by graph = 2.5 ml

→Addition of 2 ml of NaOH into Aspirin Solution
Volume of NaOH Conductance (µS) Specific Conductance
added (ml) (µS/cm)
0 4.81 0.0481
2 6.20 0.0620
4 18.20 0.1820
6 22.24 0.2224
8 24.31 0.2431
10 29.90 0.2990
12 34.60 0.3460
14 36.50 0.3650
16 38.29 0.3829
18 39.67 0.3967
20 40.23 0.4023
22 43.80 0.4380
24 43.80 0.4380
26 43.80 0.4380
28 43.80 0.4380
30 43.80 0.4380
End Point
Volume of NaOH consumed concluded by graph = 2.0 ml

→Addition of 1 ml of NaOH into Aspirin Solution
Volume of NaOH Conductance (µS) Specific Conductance
added (ml) (µS/cm)
0 4.97 0.0497
1 5.09 0.0509
2 20.35 0.2035
3 22.12 0.2212
4 24.65 0.2465
5 27.79 0.2779
6 29.30 0.2930
7 32.33 0.3233
8 35.60 0.3560
9 37.99 0.3799
10 40.10 0.4010
11 40.55 0.4055
12 41.77 0.4177
13 45.36 0.4536
14 48.29 0.4829
15 50.67 0.5067
16 54.72 0.5472
17 59.80 0.5980
18 61.33 0.6133
19 65.44 0.6544
20 59.50 0.5950
21 64.95 0.6495
22 68.60 0.6860
23 67.66 0.6766
24 67.66 0.6766
25 67.95 0.6795
26 67.95 0.6795
End Point
Volume of NaOH consumed concluded by graph = 1.5 ml

→Addition of 0.5 ml of NaOH into Aspirin Solution
Volume of NaOH added Conductance (µS) Specific Conductance
(ml) (µS/cm)
0 4.91 0.0491
0.5 5.10 0.0510
1.0 5.44 0.0544
1.5 5.38 0.0539
2.0 15.36 0.1536
2.5 16.10 0.1610
3.0 17.50 0.1750
3.5 18.70 0.1870
4.0 21.90 0.2190
4.5 25.70 0.2570
5.0 26.80 0.2680
5.5 27.80 0.2780
6.0 28.65 0.2865
6.5 29.95 0.2995
7.0 31.45 0.3145
7.5 32.02 0.3202
8.0 33.59 0.3359
8.5 34.72 0.3472
9.0 35.51 0.3551
9.5 36.44 0.3644
10.0 38.20 0.3820
10.5 39.65 0.3965
11.0 40.09 0.4009
11.5 41.22 0.4122
12.0 42.25 0.4225
12.5 43.54 0.4354
13.0 44.70 0.4470
13.5 45.70 0.4570
14.0 45.49 0.4549
14.5 46.29 0.4629
15.0 47.01 0.4701
15.5 47.53 0.4753
16.0 48.73 0.4873
16.5 49.21 0.4921
17.0 50.01 0.5001
17.5 51.22 0.5122
18.0 51.65 0.5165
18.5 52.10 0.5210
19.0 53.72 0.5372
19.5 53.72 0.5372
20.0 53.98 0.5398
End Point The end point from the graph = V4 = 1.5 ml

· Average Volume required of NaOH
V1 + V2 + V3 + V4 2.5 + 2.0 + 1.5 + 1.5
V = = = 1.875ml
4 4

· Concentration of NaOH while titrating with Aspirin Solution

Concentration of NaOH = M1 = 0.1136 M
Volume of NaOH = V1 = 1.875 ml
Concentration of Aspirin = M2 =?
Volume of Aspirin = V2 = 30 ml

Titration Reaction

H O O O C N a O OO C

C C C C 3H
3H + NaOH ¾¾¾® + H2O

Sodiumoacetoxy
Aspirin
benzoic acid

Formula
M 1V1 M 2V M 1V1n2
= M2 =
n1 n2 Þ V2 n1
Here n1 = n2 = 1
0.1136 × 1.875 × 1
M2 = = 7.11 × 10 −3 M
1 × 30

· Amount of Aspirin (Acetyl Salicylic Acid) in the Given Tablet
Concentration of aspirin is found to be 7.11×10-3 M. Therefore,

M × Mol.Wt. × V 7.11 × 10 −3 × 164.1604 × 250
=
Amount= 1000 1000 = 0.29138 gm
The amount of Aspirin is found to be 291.38 mg.

· Percentage of Aspirin
0.29138
×100 = 55.05%
% weight = 0.5293

· Percentage Error
The standard value of the amount of aspirin estimated on the label for a single tablet is
300mg.

300 − 291.38
× 100 = 2.873%
% error = 300

Hence,
The amount of ascorbic acid is found to be 291.38mg in a single given tablet with an
error of 2.873%.

Discussion [1]

The variation in the conductivity of a solution as the concentration of the solution is
varied is best represented by plotting conductivity values against the dilution of the
solution. The dilution of a solution is the reciprocal of its concentration, and is generally
defined as the number of liters of solution containing 1 gm. equivalent of solute.
Some substances, such as mineral acids, salt solutions, have much higher specific
conductivities than others, such as acetic acid & alcohols. The difference is shown by
plotting the results for each type of substance on conductivity-dilution graphs. Those
substances with high specific conductivities are known as strong electrolytes; they
include most mineral acids, alkalis and most salts. Substances with comparatively small
specific conductivities are known as weak electrolytes; they include most organic bases
and acids.
As a solution gets more and more dilute there are fewer and fewer solute particles in a
given volume of the solution. Because it is the solute that causes electrical conductivity
(pure water, and other solvents are very poor conductors), on this account, be expected
that conductivity would fall with increasing dilution.
a) For Weak Electrolyte
For a weak electrolyte, the degree of ionization increases with increasing dilution. The
maximum in the conductivity-dilution curves is due to the composite effect of decrease in
the total number of solute particles and increase in the degree of ionization. As dilution
increases, there are fewer molecules, but a higher proportion of them split up into ions.
b) For Strong Electrolyte
For a strong electrolyte the other factor is the decrease in ionic interference as the dilution
increases. A strong electrolyte is almost fully ionized at all dilutions. At low dilution, the
ions will interfere with each other so that their freedom of movement and their speed is
restricted. As a solution is diluted, the ionic interference decreases and the ionic speed
increases. For a strong electrolyte, increasing dilution gives fewer ions, in a fixed volume
of solution, but the ions that are present interfere less with each other, which gives higher
ionic speeds.

As mentioned earlier the purity of water is critical for the accuracy of our results.
Ordinary distilled water is not preferred. Specially pure water, known as conductance
water or conductivity water should be used for the preparation of solutions. The purest
water referred to as "ultra-pure" has a specific conductance of 0.05 mS / cm at 18°C. Air
must be rigidly excluded when it is being employed.
The water we utilized was not pure. It is most probable that it contained impurities
and stray electrolytes, which could cause variations in conductance by two ways:
a. Contribute the effects of their conductance directly
b. Cause ionic interference [2]

Conclusion
We conclude that the conductometric method is the best way to determine the
equivalence point, if there is a change in conductance is present in titrand solution.
Conductomertric titrations are useful for acid-base, precipitation, and complexation
titrations.

.
1 R.D. BRAUN, "Introduction to Chemical Analysis"
2
Chemical Process Principles

→Addition of 3 ml of NaOH into Aspirin Solution

V olume v/s S p. C onductance

0.7
0.6
Specific Conductance (us/cm)

0.5
0.4
0.3
0.2
0.1
0
0 5 10 15 20 25 30 35 40
V olum e of Na OH a dde d (m l)

→Addition of 2 ml of NaOH into Aspirin Solution
Volume v/s S p.C onductance

0.5
0.45
Specific Conductance (us/cm)

0.4
0.35
0.3
0.25
0.2
0.15
0.1
0.05
0
0 5 10 15 20 25 30 35
Volum e of Na OH a dde d (m l)

→Addition of 1 ml of NaOH into Aspirin Solution

Volume v/s Sp.Conductance

0.8

0.7
Specific Conductance (us/cm)

0.6

0.5

0.4
0.3

0.2

0.1

0
0 5 10 15 20 25 30
Volum e of NaOH adde d (m l)
→Addition of 0.5 ml of NaOH into Aspirin Solution
V o lu m e v /s S p .C o n d u c ta n c e

0.6

0.5
Specific Conductance (us/cm)

0.4

0.3

0.2

0.1

0
0 5 10 15 20 25
V o lu m e o f N a O H a d d e d (m l)