CERTIFICATE IN PROCESS OPERATIONS

CHEMISTRY/CORROSION CHEM 1003 SF 18

LABORATORY EXPERIMENT 5: determination of the
concentration of an unknown alkali solution by a ph
monitored acid/base titration
DATE SUBMITTED: 27/02/14


DONE BY:
ANDERSON RAMSROOP
DEVAUGHNTE GERMIA
NIKOLAI JOHNSOn
Nicholas abraham
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AIM:
Determination of the concentration of an unknown alkali solution by a pH monitored Acid/Base
titration

APPARATUS AND MATERIALS
150 ml conical flasks
100 ml beakers
Small funnel
50 ml burette
25 ml pipette
Pipette bulb
Retort stand with clamps
White tile
pH meter and electrode
Stirring device and magnetic stir bar
Wash bottle with distilled water
Unknown NaOH solution
0.2 Molar HCl solution


PROCEDURE: 1
st
Titration
1. An unknown solution of NaOH was collected
2. The pipette was thoroughly rinsed with NaOH
3. The pipette bulb was used to transfer 25 ml of the unknown solution into a conical flask
4. 3 drops of phenolphthalein indicator was added to the unknown solution
5. 100 ml of the 0.2 Molar HCL solution was collected
6. The burette was mounted on the retort stand
7. A small amount of HCl solution was added to the burette using a funnel
8. The burette was rinsed with the small amount of HCl
9. The burette was completely filled with HCl to the 50 ml level and all bubbles removed
from the tip
10. The initial burette reading was recorded
11. The conical flask containing the unknown solution was placed under the burette and
carefully titrated until the first colour change occurred in the conical flask
12. The burette reading for this colour change was recorded as the final reading
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2
nd
Titration
1. The pH meter was assembled and calibrated
2. 25 ml of the unknown base was pipetted into a 100 ml beaker. Sufficient distilled
water was added to the base so that the pH electrode and magnetic stirring bar are
free to function without the stir bar hitting the electrode
3. The burette was zeroed and positioned directly above the beaker containing the
unknown base
4. The initial pH and voltage of the unknown base solution was recored on the data
sheet.
5. Acid was added continuously until 10 ml before the endpoint recorded I th first
titration and the pH and voltage readings taken
6. pH and voltage readings were recorded at 1 ml intervals until within 2 ml of the
endpoint recorded in the first titration.
7. The pH and voltage readings were recorded at 0.5 ml increments until within 1 ml
of the endpoint recorded in the first titration
8. Standardized HCl was added drop by drop, taking pH and voltage readings at each
addition until you are 0.5 ml after the neutralization point
9. The pH and voltage readings were taken at 0.5 ml intervals for the next 1.5 ml
addition. pH and voltage readings were taken after the addition of another 4 ml and
10 ml of standardized HCl
10. All the information was recorded in the data sheet required.
11. The beaker and burette was emptied and all equipment used were thoroughly
washed with distilled water















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OBERSERVATIONS AND RESULTS

Initial pH of Unknown is 12.83
Volume reading at which indicator turned colour in 1
st
titration is 25.15 ml
2
nd
titration results:
pH Vol. HCl (ml) Voltage (mV) Temperature (
o
C)
12.82 0 -333.8 23.1
12.20 15.15 -297.5 22.8
12.15 16.15 -294.2 22.8
12.08 17.15 -290.5 22.8
12.01 18.15 -286.0 22.8
11.93 19.15 -281.4 22.7
11.84 20.15 -276.0 22.7
11.72 21.15 -268.9 22.6
11.53 22.15 -257.5 22.6
11.23 23.15 -290.2 22.5
7.43 24.15 -16.8 21.7
7.32 24.20 -10.3 21.4
6.84 24.25 11.4 21.3
6.82 24.30 17.6 21.3
6.59 24.35 32.2 21.3
6.56 24.40 34.0 21.3
6.44 24.45 40.7 21.3
6.34 24.50 46.6 21.2
6.23 24.55 53.3 21.2
5.95 24.65 69.4 21.2
5.93 24.70 70.6 21.2
5.83 24.75 76.7 21.2
5.44 24.80 99.3 21.2
5.22 24.85 111.7 21.2
4.64 24.90 145.7 21.2
4.00 25.00 183.5 21.2
3.63 25.05 205.0 21.2
3.42 25.10 216.9 21.2
3.39 25.15 218.8 21.1
2.75 25.65 256.4 21.1
2.51 26.15 270.2 21.1
2.37 26.65 278.3 21.1
2.18 27.65 289.4 21.1
2.06 28.65 269.4 21.1
1.95 29.65 302.7 21.1
1.88 30.65 307.1 21.1
1.72 34.65 316.5 21.1
1.49 44.65 329.8 21.1
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CALCULATIONS
1. Volume of acid required to neutralize 25 ml of NaOH is 25.15 ml
2. Number of moles of acid of used to neutralize NaOH is 1 mole
3. + +
2

It can be seen that 1 mole of HCl reacts with 1 mole of NaOH. Therefore:
1000 ml of HCl contains 0.2 mols,
25.15 ml of HCl contains (0.2/1000) x 25.15 = 0.00503 moles
The number of moles in 25 ml of NaOH is therefore 0.00503
4. If 25 ml of NaOH has 0.00503, then 1000ml has (0.00503/25) x 1000 = 0.2012 moles
5. The concentration of NaOH is given by:
MHCl x VOLUMEHCl = MNaOH x VOLUMENaOH

(0.2 25.15)
25
= 0.201

6. The level of variation is about 0.75 ml between the first titration and the second
titration















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DISCUSSIONS:
2. () + () () +
2
()
3.





0
2
4
6
8
10
12
14
0 5 10 15 20 25 30 35 40 45 50
p
H
Volume of HCl
Graph of pH vs Volume of HCl
0
2
4
6
8
10
12
14
-400 -300 -200 -100 0 100 200 300 400
p
H
Voltage (mV)
Graph of pH vs Voltage (mV)
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4.
5. The concentration of NaOH is given by:
MHCl x VOLUMEHCl = MNaOH x VOLUMENaOH

(0.2 25.15)
25
= 0.201

6. 1) It is important to calibrate the meter and the electrode against buffers to ensure the
highest efficiency since buffers have fixed pH values across the pH range however these
values are temperature dependent

2) The actual pH of the sample would be 2.34

3) 1 mole of H
+
ions has a mass of 1g. Therefore 0.629 g of hydrogen ions contains
0.629/1 = 0.629 moles. The molarity is therefore (0.629/0.25) = 2.516 M. The pH of
this solution is = -log10 [H
+
] = -log10 [2.516] = -0.4007

4) Failure to rinse and wipe the electrode between readings of different samples will
cause contamination of the next sample whose pH is measured.

5) Adding distilled water to the base solution increases the concentration of H
+
ions in
solution and so decreases the pH. This can be seen the lower volume of acid used to
neutralize the base in the second titration

6) The end point volume of acid given by the indicator was almost 1ml more than the
volume of acid used using the pH meter. The concentration of the base used in the
second titration was reduced since distilled water had to be added to cover the electrode
and therefore the concentration of the base decreased, OR, the concentration of
hydrogen ions increased upon dilution and so decreased the pH of the base making it
weaker.

7) The solution in the beaker should be stirred continuously to ensure adequate and
intimate mixing of acid molecules with the alkali molecules





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ERRORS
There were errors of parallax in taking measurements in the burette readings and pipette
readings. In the second titration, one of the incremental additions of acid was overshot,
affecting the measurements taken.
Misjudging the colour of the endpoint may be difficult as some people have different sensitivity
to various colours
Contamination can be in issue if the glassware used was not clean or rinsed with the solution
it is supposed to hold. Also lack of care in transferring liquids can lead to contamination.
There was an observed leak in the burette that led to the acid dripping into the solution.
PRECAUTIONS
Care should be taken in handling acids and bases since they are both toxic and harmful to the
skin. Also all burette and pipette readings should be done at eye level to avoid parallax. All
instruments being used should be cleaned.

CONCLUSION
The first titration carried out with the use of an indicator gave an endpoint which was higher
than that of the second titration done with the use of the pH meter.