INTRODUCTION

There are several ways to measure the pH of a solution such as by using litmus
paper, indicators however, a glass electrode and a pH meter is used to obtained an
accurate results. The potentiometric tiltration is an experiment which uses an indicator
not only to identify the tiltration endpoint but also the entire progress of the tiltration
is monitored through a potential measurement. In potentiometric tiltration, the
collected data can be easily used to plot tiltration curve (pH against the volume of
tiltrant). The point at which the inflection point (curvature changes from positive to
negative ) is known as equivalence point. The equivalence point is used to indicate
the complete chemical conversion of the analyte by the tiltrant.
The pH meter is used to obtain a more precise readings to 0.01 pH unit. It is
measured on a scale of 0 to 14. A pH meter is a modified form of potentiometer which
is used to measure the concentration of H 3O+ ion in solution. The measurement of an
electric potential depends on differences of voltage between a reference electrode and
glass electrode which is sensitive to the concentration of H3O+ ion in solution.
Normally, two buffer solutions (one with the pH higher than the solution and another
with a pH lower than the solution) are sufficient enough for calibration. However,
multiple point calibration using three to four calibration solutions is used to provide
data with high accuracy. The pH values of 4, 7 and 10 are the most widely used pH
calibration buffers. The temperature compensation control on the meter should be
adjust to temperature of the solution being measured. The pH of the solution are
measured once the meter had been standardised and readings are stable. Errors in pH
measurement arises due to the presence of high concentration of sodium ion at high
ionic strength.
In this experiment, the exact concentration of hydrochloric acid is obtained from
the tiltration of hydrochloric acid with a standard solution of NaOH. The pH meter is
used in this experiment as the desired concentration measurement is determine
through analytical pH formulae.

OBJECTIVE
To determine the exact concentration of the given hydrochloric acid, HCl solution by
tiltration with a standard sodium hydroxide, NaOH solution by using a pH meter.
APPARATUS
 pH meter
 Burette
 Pipette
 Conical flask
 Standard volumetric flask
 Beakers
CHEMICALS
 Sample HCl solution
 Sodium hydroxide, NaOH
 Oxalic acid
 Phenolphthalein
 Buffer solutions of pH 4, 7 and 10.

METHODS

PART A(I): To prepare an approximately 0.1N Sodium Hydroxide (NaOH)

1) 10ml of 1M NaOH was pipetted into a volumetric flask.

2) A small amount of distilled water was added into the volumetric flask until it
reaches the mark of 100ml.

PART A(ii): To prepare an approximately 0.1N Oxalic Acid

1) 0.63g of oxalic acid (0.1 mol) powder is weighed out by using analytical balance.
2) The oxalic acid powder is completely dissolve in distill water till no more residue
is seen.
3) 10 ml of 1M oxalic acid was pipetted into another volumetric flask.
4) A small amount of distilled water was added into the volumetric flask until it
reaches the mark of 100ml.

PART B : Standardization of approximately 0.1M Sodium Hydroxide (NaOH)

1) The burette was cleaned and rinsed with distilled water to remove impurities.
2) The burette was preconditioned by rinsing it with NaOH solution for two to three
times.
3) The burette was filled with prepared 0.1M NaOH to exact measurement using filter
funnel.
4) All gas bubbles in the liqiud column of burette was removed if there is any and was
attached to the retort stand and clamp.
5) The initial volume of NaOH was read by recording the position of mark that line up
with the meniscus of the liqiud column.
6) Three Erlenmeyer flasks was prepared.
7) 10ml of standard oxalic acid is pipetted into the three separated Erlenmeyer flasks.
8) Two to three drops of phenolphathalein indicator was added into each Erlenmeyer
flasks containing standard oxalic acid by using a dropper.
9) The Erlenmeyer flask was placed under the burette and the stopcock was opened
slowly to allow the NaOH solution to be added into the Erlenmeyer flask drop by
drop till the solution turns pale pink which indicate the reaction has reached the end
point.
10) The final volume of NaOH required to turn the solution pink was recorded.
11) Step 12 to 13 was repeated for another two Erlenmeyer flasks.

PART C : Tiltration of Hydrochloric acid, HCl with Standardized NaOH

solution
1) A known volume of 10ml of hydrochloric acid, HCl solution is pipetted out into a
100ml beaker.
2) The burette was cleaned and rinsed with distilled water to remove impurities.
3) The burette was preconditioned by rinsing it with NaOH solution for two to three
times.
4) The burette was filled with prepared 0.1M NaOH to exact measurement using filter
funnel.
5) All gas bubbles in the liqiud column of burette was removed if there is any and was
attached to the retort stand and clamp.
6) The pH electrode of the pH meter was rinse thoroughly with distill water and was
gently wiped with a clean tissue paper.
7) The pH meter was immersed into the 100ml beaker containing 10ml of
hydrochloric acid and the pH of the solution was noted down.
8) A small increment of the NaOH solution is added from the burette and the solution
was stirred before immersing the pH meter. The pH of the solution was noted down.
9) Step 2 was repeated with small increments of NaOH solution until the the pH reads
10) The pH electrode of the pH meter was rinse thoroughly with distill water and was
gently wiped with a clean tissue paper each time before immersing it into the beaker
after the addition of NaOH.
11) An increment of drop by drop of NaOH solution was added into the beaker
containing hydrochloric acid solution and the pH of the solution was noted down.
12) A steep rise was seen in its value around pH 7.
13) There was only slight increase in pH value above pH 8.
14) The tiltration was stopped when the 5 to 6 readings was obtained is above pH 7.
15) A plot of pH versus volume of the standardized NaOH solution was plotted and
the equivalence point corresponding to pH 7 was located.
16) The normality of the hydrochloric acid solution was calculated using the formula
N1V1= N2V2.

RESULTS
Part B : Tiltration of standard oxalic acid solution with NaOH solution
First reading Second reading Third reading
Initial burette reading (ml) 0.0 11.2 22.5
Final burette reading (ml) 11.2 22.5 33.6
Volume of NaOH used (ml) 11.2 11.3 11.1

Indicator used : Phenolphthalein

Observation : The colourless solution turns to pink.

1st 2nd 3rd

reading reading reading
.Average volume of NaOH used = 11.2 ml + 11.3ml+ 11.1ml
3
= 11.2ml

The strength of the NaOH solution in terms of normality:

N1V1 = N2V2
( 0.1 ) (10) = N2 (11.2)
N2 = 0.0893N

Part C : Tiltration of Hydrochloric acid, HCl solution with Standardized NaOH

solution

Initial burette Final burette Volume of Cumulative pH

reading (ml) reading (ml) NaOH used volume of
(ml) NaOH used
(ml)
0.0 0.0 0.0 0.0 0.87
0.0 2.0 2.0 2.0 1.20
2.0 4.1 2.1 4.1 1.30
4.1 6.1 2.0 6.1 1.38
6.1 7.1 1.0 7.1 1.46
7.1 7.6 0.5 7.6 1.53
7.6 7.9 0.3 7.9 1.59
7.9 8.2 0.3 8.2 1.63
8.2 8.5 0.3 8.5 1.70
8.5 8.8 0.3 8.8 1.72
8.8 9.1 0.3 9.1 1.79
9.1 9.4 0.3 9.4 1.85
9.4 9.6 0.2 9.6 1.90
9.6 9.7 0.1 9.7 1.92
9.7 9.9 0.2 9.9 1.95
9.9 10.1 0.2 10.1 2.02
10.1 10.3 0.2 10.3 2.13
10.3 10.5 0.2 10.5 2.23
10.5 10.7 0.2 10.7 2.41
10.7 10.9 0.2 10.9 2.83
10.9 11.1 0.2 11.1 9.85
11.1 11.3 0.2 11.3 11.14
11.3 11.4 0.1 11.4 11.30
11.4 11.5 0.1 11.5 11.42