INTRODUCTION

Standardization is defined as the process of finding out the exact concentration or

molarity of a solution. One type of analytical procedure which is often used in
standardization is tiltration. Tiltration is the laboratory method that was used in this
experiment. Tiltration is a method used in measuring the amount of an analytical
reagent that is necessary to react quantitatively with the sample. In short, it means a
standard solution of known concentration is “tiltrated against” or reacted with a
solution of unknown concentration. The completion of the tiltration reaction can be
indicate by the indicator used (show color changes) and concentration of the unknown
solution can be found. The theoretical end point is the point at which the equivalence
point has been reached. In tiltration, the reaction between an acid and a base involves
the neutralisation process whereby the hydrogen ions or hydronium ions from the acid
reacts with hydroxide ions from the base to form water molecule. The equations
involved are:

H+ + OH- → H2O or H3O+ + OH- →2 H2O

The indicator used in this experiment is phenolphathalein. Phenolphathalein is an

organic compound which is colourless in acidic solution and pink in basic solutions.
During tiltrations, one to two drops of phenolphathalein indicator is sufficient enough
to produce result. Upon addition of phenolphathalein, the solution turns to pale pink
indicating the reaction has reached the endpoint.

The experiment involves two separate acid-base standardization procedures. The

molarity of sodium hydroxide (NaOH) solution will be determined by tiltrating
standard oxalic acid solution with NaOH in the first standardization procedure while
the second procedure involve tiltration of potassium acid phthalate solution with
NaOH.

APPARATUS AND CHEMICALS

 50 ml burette
 Measuring cylinder
 Beakers ( 1-L)(100ml)
 Droppers
 Filter funnel
 Glass rod
 Conical flask
 Erlenmeyer flask
 Retort stand and clamp
 10ml pipette
 Distilled water
 100ml volumetric flask
 Weighing balance
 Spatula
 Weighing bottle
 1M Standard oxalic acid solution
 Solid potassium acid phthlate
 1M Sodium hydroxide solution
 Phenolphthalein

METHODS

PART A : To prepare an approximately 0.1M 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 B(I) : Standardization of approximately 0.1M Sodium Hydroxide (NaOH)

1) 0.1M Standard oxalic acid was first prepared.
2) 10ml of 1M Standard oxalic acid was pippeted into another volumetric flask.
3) A small amount of distilled water was added into the volumetric flask until it
reaches the mark of 100ml.
4) The burette was cleaned and rinsed with distilled water to remove impurities.
5) The burette was preconditioned by rinsing it with NaOH solution for two to three
times.
6) The burette was filled with prepared 0.1M NaOH to exact measurement using filter
funnel.
7) All gas bubbles in the liqiud column of burette was removed if there is any and was
attached to the retort stand and clamp.
8) The initial volume of NaOH was read by recording the position of mark that line up
with the meniscus of the liqiud column.
9) Three Erlenmeyer flasks was prepared.
10) 10ml of standard oxalic acid is poured into the three separated Erlenmeyer flasks.
11) Two to three drops of phenolphathalein indicator was added into each Erlenmeyer
flasks containing standard oxalic acid by using a dropper.
12) 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.
13) The final volume of NaOH required to turn the solution pink was recorded.
14) Step 12 to 13 was repeated for another two Erlenmeyer flasks.
PART B(II) : Standardization with Potassium Acid Phthalate Solution
1) About 5g of pure potassium acid phthalate (standardization grade) was placed in a
weighing bottle and was dried in the oven for an hour at 110oC.
2) It was then cooled in the desiccator.
3) Samples of 0.70g, 0.80g and 0.90g of pure potassium acid phthalate was measured
using weighing balance and was placed into three clean, dry and numbered
Erlenmeyer flasks. The weight of each samples was recorded to the nearest 0.1mg.
4) 50ml of boiled and cooled distilled water was added into each Erlenmeyer flask
and followed by the addition of two drops of phenolphathalein indicator solution
(0.1% in 80% alcohol).
5) A clean 50ml burette was rinsed with NaOH solution to be standardized and the
burette was filled with NaOH solution using filter funnel.
6) The first solution is tiltrated to the first permanent pink color ( color must persists
for 30s). The volume of NaOH required was recorded to the nearest 0.01ml.
7) The remaining two solutions was tiltrated in the same way and the volume of
NaOH required was recorded.
8) The molarity (normality) of the NaOH solution for each tiltration was calculated.

RESULTS
Part B(I) :
First reading Second reading Third reading
Initial burette reading (ml) 0.0 0.0 0.0
Final burette reading (ml) 40.0 40.0 40.0
Volume of NaOH used (ml) 10.0 10.0 10.0

Part B(II) :
Weight of pure potassium 0.70 0.80 0.90
acid phthalate (g)
Initial burette reading (ml) 0.0 0.0 0.0
Final burette reading (ml) 9.4 3.5
Volume of NaOH used (ml) 40.6 46.5 51.6