Analytical Chemistry Lab CH

ANALYTICAL CHEMISTRY LAB CH-292
ZOHA MUSTAHSON
04061813008
BS CHEMISTRY 4TH
EXPERIMENT#1:
To calibrate the given volumetric apparatus and to investigate
errors in volume measurement.
OBSERVATIONS AND CALCULATIONS:

DISCUSSION:
This experiment was done to calibrate different volumetric apparatus and to
check the errors that are generated in the measurements involving these
apparatuses. In this experiment we observed three concordant readings for each
apparatus. The errors that were generated depicted that these were related to
height and radius of the glassware. When the height increased the chance of error
increased while the increase of radius decreased the chance of error. These errors
can be systematic as well as random. The difference in the weight of 100ML
beaker was due to random errors during the measurement of its weight. The eye
position while checking the liquid in the glassware should be perpendicular to the
reading scale so that personal errors can be avoided. Therefore, calibration
helped us to increase the chances of producing accurate measurements.
EXPERIMENT#2:
To find out the exact weight of a given watch glass and to
analyze the replicate measurements statistically.
RESULT:
The mean weight of watch glass is 13.194 with a standard deviation of 0.0258.
The range error for this measurement was found out to be 0.2728%.
DISCUSSION:
The experiment was performed to find out the exact weight of a given watch
glass. The weight was found in 10 concordant readings. The readings were
repeated to avoid the chances of errors and to increase the probability of finding
true value. Mean of these readings was used to obtain other statistical
parameters. Standard deviation as well as range error were found out to be of
small values which indicates high precision of the data.
EXPERIMENT#3:
To estimate Ca +2 concentration in drinking water by EDTA
complexometric titration.

DISCUSSION:
Ethylene diamine tetra acetate forms are complex with metal lines such as Ca +2.
The structure of complex is as follows:
The murexide Indicator used in the experiment has an end point at pH 11 when
the complex is formed. Concentration of calcium ions in tap water is higher than
its concentration in drinking water. Thus, the tap water is hard as compared to
drinking water. During this volumetric analysis systematic or random error may
have been generated altering the values.
EXPERIMENT#4:
To establish the constancy of solubility product.
DISCUSSION:
The equilibrium constant for the dissolution of a sparingly soluble salt is the
solubility product of that salt. In this experiment solubility product of calcium
hydroxide were found in different media such as distilled water and different
molar concentrations of sodium hydroxide. It was observed that the value of K SP
decreases with the decrease in molarity of sodium hydroxide. There might have
occurred a few fluctuations in the measurements due to errors that result due to
inappropriate measurement of endpoint, leaking or dirty equipment, or the
wrong amount of indicator.
EXPERIMENT#5:
To determine the concentration of the given strong acid
solution by conductometric titration.
Conductance Volume Conductance Volume Conductance Volume

of NaOH of NaOH of NaOH
added(ml) added(ml) added(ml)
8.95 0.0 4.88 16 2.56 32

8.51 2.0 4.40 18 2.83 34
7.95 4.0 3.93 20 3.06 36
7.44 6 3.44 22 3.30 38
6.87 8 3.05 24 3.52 40
6.30 10 2.62 26 3.73 42
5.83 12 2.21 28 3.93 44
5.82 14 2.31 30 4.0 46
GRAPH:
Y-Values
10
9
8
7
Conductance
6
5
4
3
2
1
0
0 5 10 15 20 25 30 35 40 45 50
Volume of NaOH
HCl +NaOH → NaCl+ H2O

M1V1/N1= M2V2/N2
M1= Molarity of HCl= unknown
V1= volume of HCl solution = 25mL
N1= coefficient of HCl in balanced chemical equation
M2= Molarity of NaOH= 0.1 M
V2= volume of NaOH (at equivalence point) = 28 mL
N2= coefficient of NaOH in balanced chemical equation
M1 x 25 /1 = 0.1 x 28/ 1
M1 =0.1 x 28/25 = 0.112 M
RESULT:
The above shown graph indicates that the equivalence point lies at (28, 2.21) i.e.
at 2.21 value of conductance and 28 mL of NaOH utilized. The molarity of HCl
solution being used is found to be 0.112 M approx. ~ 0.1M.
DISCUSSION:
Conductometric titration is a type of electroanalytical technique which is used to

determine the rate of change of an electrolyte solution as a function of added
titrant used to determine the equivalence point. The equivalence point is the
point at which the conductivity undergoes a sudden change This experiment
involves the titration of strong acid HCl with strong base NaOH. Before NaOH is
added, the conductance of H+ is high. When the base is added, the conductance
falls due to the neutralization of H+ with OH- to form water. This is indicated by
negatively sloped straight line in the graph. This decrease in the conductance
continues till the equivalence point. At the equivalence point, the solution
contains only NaCl and water. After the equivalence point, the conductance
increases because of the presence of unreacted OH- ions which is indicated by
positively slopped linear line. However, the increase is gradual only because H3O+
have a higher conductance value than OH-.
EXPERIMENT#6:
To determine the concentration of the given strong acid solution potentiometrically using
first and second derivative method.
OBSERVATION:
Volume of NaOH added (mL) pH First Derivative Second Derivative

10 2.48 0 0
12 2.52 0.02 0.01
14 2.56 0.02 0
16 2.68 0.06 0.02
18 2.77 0.45 -0.0075
20 2.98 0.105 0.03
22 3.27 0.145 0.02
24 10.27 3.5 1.6775
26 11.20 0.465 -1.5175
30 11.37 0.0425 -0.010563
32 11.48 0.055 0.00625
34 11.54 0.3 -0.0125
GRAPH:
1. pH vs. Volume curve
Y-Values
14
12
10
8
pH
0
0 5 10 15 20 25 30 35 40
Volume of HCl
2. First derivative curve:
1st derivative
4
3.5
2.5
1.5
0.5
0
0 5 10 15 20 25 30 35 40
-0.5
3. Second Derivative:
2nd derivative
2
1.5
0.5
0
0 5 10 15 20 25 30 35 40
-0.5
-1
-1.5
-2
The equivalence point lies somewhere between the initial and final inflection points. Initial
inflection point at 22 mL NaOH gives pH value of 3.27 while the final inflection point at 24 mL
NaOH gives pH value of 10.27, while the equivalence point lies at the value of 7pH. It is found
by adding the two inflection points and dividing by 2 to find the middle value.
Equivalence point= 22+24/2 = 23 mL
Thus, the equivalence point as shown by the three graphs is at 23mL.
NaOH + HCl → NaCl + H2O

M1V1/N1 =M2V2N2
M1= molarity of HCl=?
V1= Volume of HCl = 25 mL
M2= molarity of NaOH= 0.1 M
V2= Volume of NaOH used (at equivalent point) = 23 mL
M1V1/N1=M2V2/N2
M1 x 25= 0.1 x 23
M1= (0.1 x 23)/ 25
M1= 0.092M
Molarity of HCl= 0.096M
Amount/ L of HCl= molarity x molar weight = 0.092 x 36.5
= 3.358 g/ L
RESULT:
The molarity of HCl found by using the volume of NaOH at equivalence point and
the above-mentioned equation is 0.092 M approx. 0.1 M. Amount of HCl per dm3
is found to be 3.358 g/L.
DISCUSSION:
By using the potentiometric titration, the concentration of HCl is found out. A plot
of pH vs. volume of titrant (NaOH) gives a characteristic S-shaped curve. The two
inflection points as indicated in the normal titration curves are at 22 mL NaOH
and 24 mL NaOH, the middle of which is 23 mL NaOH which gives the equivalent
point (the point with maximum slope). Equivalent point is that where the H+ of
acid are completely neutralized by OH- because of continuous addition of base
NaOH. At this point the pH of solution is approximately 7 because of complete
neutralization. At equivalent point, minor addition of the titrant leads to a drastic
change in pH of the solution. For a more accurate value of equivalent point, first
derivative curve ∆pH/∆V is plotted, and the peak of this curve shows the
equivalent point to be 23mL. The x-intercept of the second derivative curve
∆pH2/∆V2 also indicates the equivalence point to be 23mL.
NUMERICAL:
What is the pKa value of chloroacetic acid. Suppose pH of the solution is 2.54.
SOLUTION:
The original molar concentration of chloroacetic acid is 0.1 M.
pH of solution= 2.54
-log [H+] = 2.54
[H+] = 10(-2.54)
[H+] = 0.0029 moles/dm3
EQUATION: ClCH2COOH + H2O → ClCH2COO- + H3O+
Initial conc: 0.1 M 0 0
Equilibrium conc: (0.1-0.0029) 0.0029 0.0029
Ka = [H3O+] [ClCH2COO-]
[ClCH2COOH]
Ka = (0.0029) (0.0029)
(0.1-0.0029)
Ka= 0.00000841
0.0971
Ka= 0.0000866
pKa= -log (0.0000866)
= 4.0624
The pKa of 0.1 molar chloroacetic acid is 4.0624.

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ANALYTICAL CHEMISTRY LAB CH-292

OBSERVATIONS AND CALCULATIONS:

OBSERVATIONS AND CALCULATIONS:

Conductance Volume Conductance Volume Conductance Volume

8.95 0.0 4.88 16 2.56 32

HCl +NaOH → NaCl+ H2O

Conductometric titration is a type of electroanalytical technique which is used to

Volume of NaOH added (mL) pH First Derivative Second Derivative

1. pH vs. Volume curve

NaOH + HCl → NaCl + H2O

pKa= -log (0.0000866)

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