Instrumental Analytical Methods

Lab Report 2013

Anastazija Ristovska
Experiment 10
Conductometric Titration of a Mixture of Sulfuric and Acetic Acid with Sodium Base

900
800

Conductance (S/cm)

700
600
500
400
300

4,55ml;
283S/cm

200
100
0
0

10

12

14

Volume 0.1M NaOH added

Graph 1: Conductance
In this post-lab analysis we will try to find the best method of determining the
concentrations of sulfuric acid and acetic acid in a mixture based on conductometric titration
data. The purpose of the experiment was to titrate a mixture of weak and strong acid with a
strong base while measuring the conductance of the solution, then construct graphs showing the
titration curves, and eventually perform a regressional analysis to determine the titration end
points of sulfuric acid and acetic acid separately.
The conductance curve showed in Graph 1 is properly analyzed at the end of this report,
and prior to that analysis several other methods of potentially determining the sulfuric acid and
acetic acid concentrations through derivative analysis are examined. Derivative analysis seemed
particularly suitable since we were interested in detecting changes in slope, as well as speed of
change of increase and decrease in conductance.
From Graph 1 we can see that the point when all the sulfuric acid was reacted with
NaOH was reached when 4.55ml were added to the sulfuric acid acetic acid mixture solution.
1

This volume could be determined by finding the point when the conductance of the
solution stopped decreasing and began increasing.
The sulfuric acid, being the stronger acid, was the first one to be reacting with NaOH,
and while this was happening, the solution experienced a neutralization reaction in which four
charged ions combined to form two charged ions and a neutral water molecule.
Since the total number of charged species in the solution was decreasing, the
conductance was likewise decreasing. When the sulfuric acid has already reacted, the NaOH
began neutralizing the acetic acid. However, acetic acid being a weak acid, and the sodium
acetate salt formed being one that easily dissociates into ions, by adding NaOH to the solution
the concentration of sodium acetate was increased, and therefore the number of dissociated
positively and negatively charged species was increasing.
On the graph that shows the derivative dG/dV, i.e. change in conductance over change
in volume, it can be seen that when 4.55ml NaOH (1M) were added the derivative crossed over
to the negative. Beyond that point it is the absolute value of the derivatives that we are interested
in. We therefore constructed a |dG/dV| vs. volume NaOH added curve shown in Graph 4.
The point at which |dG/dV| reached a maximum value was the end of titration of
acetic acid. Therefore all the acetic acid was neutralized when 10.5ml 0.1M NaOH was added.
The sulfuric acid ions react much faster with NaOH than the acetic acid molecules (who are
likewise floating in the solution but are predominantly not dissociated into ions), and therefore
while the sulfuric acid is still reacting with NaOH the amount of acetic acid thats also reacting is
infinitesimally small and can be neglected.
The mass of sulfuric acid in the volumetric flask according to this method seemed to be
0.0045*0.1*98.08*5=0.22068g=220.7mg.

70

60

50

dG/dV

40

30

20

10

4,55ml; 2,2

-10

Volume 0.1M NaOH added (ml)

Graph 2: First Derivative

-1,5
4

10

12

14

-2

dG/dV

-2,5

-3

-3,5

-4

-4,5

Volume 0.1M NaOH added (ml)

Graph 3: First Derivative, Acetic Acid

3

|dG/dV|
4,5

10,5ml

dG/dV

3,5
3
2,5
2
1,5
1
0,5
0
4

10

12

14

Graph 4: Absolute Value of First Derivative

30
8,5
25

9,5

20

d2G/dV

15
10

d2G/dV2

5
0
-5
-10

6
9
8

Volume 0.1M NaOH added (ml)

Graph 5: Second Derivative

Based on Graph 2 and Graph 4, the volume spent to neutralize the acetic acid alone was
10.5-4.55=5.95ml. Therefore, the mass of acetic acid in the volumetric flask is
0.00595*0.1*98.08*5=0.2918g=291.8mg.
The masses found were 220.7mg H2SO4, and 291.8mg CH3COOH. These results,
however, were not quite too accurate. We therefore turn to another calculation method. The
final method of finding the exact masses is by analyzing the following plot given in graph 6. :
900
800

Conductance (S/cm)

700

y = 87,642x - 380,59
R = 0,9993

600
Series1

500

Series2
y = 34,512x + 110,53
R = 0,9761

400

Series3
Linear (Series1)
Linear (Series2)

300

Linear (Series3)

y = -114,93x + 748,98
R = 0,9754
200
100
0
0

10

12

14

Volume 0.1M NaOH added

Graph 6
If we set the equations of the first and second linear fit lines equal we will find the
volume of titrant spent to neutralize the sulfuric acid, and if we set the equations of the second
and third linear fit lines we will find the volume of the titrant spent to neutralize the acetic acid.

Mass in 100ml

Sulfuric Acid
-114,9x+749=34,51x+110,5
749-110,5=(34,51+114,9)x
x=(749-110,5)/(34,51+114,9)
x=4,27ml
0.00427*0.1*98.08*5=0,209g

in mg

209mg

Calculations

Acetic Acid
34,51x+110,5=87,64x-380,6
110,5+380,6=(87,64-34,51)x
x=(110,5+380,6)/(87,64-34,51)
x=9,24ml
(9,244,27)*0.1*98.08*0,005=0,244
244mg