Experiment 5.

AIM To prepare 250 ml. of Oxalic acid solution from crystalline Oxalic acid.
APPARATUS
Watch glass, analytical balance, weight
box, 250 ml measuring flask, wash bottle, a 250 ml
beaker and a glass rod.
CHEMICALS REQUIRED
Crystals of oxalic acid and distilled water.
THEORY :
Molecular mass of (COOH)2.2H20
= (12 + 16 + 16 + I) x 2 2 (18)
= 90 +36
= 126 gm/mol
1
Molarity
10
We know Molarity = 1000
x
1 1000
x
10 126 250
126
= = 3.15 gm
40
To prepare oxalic acid, 12.6 gms of oxalic acid should be dissolved in per litre water.

Hence to prepare 250 ml of — oxalic acid, 126 = 3.15 gms of oxalic acid
10 4 crystals are required.

OBSERVATIONS AND CALCULATIONS :

Weight of empty watch glass = WI gm
Weight of watch glass + weight of Oxalic acid = WI + 3.150 gm
Volume of solution to be prepared = 250 ml
PROCEDURE •
1. Weigh a clean and dry watch glass on an analytical balance.
'20Put the weights of the watch glass + 3.15 gms in the right pan and the watch glass and oxalic
acid on the left pan and weigh accurately.
3• Transfer the oxalic acid from the watch glass into a clean beaker. Wash the watch glass with
distilled water with the help of a wash bottle to transfer the particles sticking to the watch
glassinto the beaker.
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 Air Air
c

c cc

Fig. 5.3 : Washing of watch glass to Fig. 5.4 : Transferring Fig •5.5 : Transferring last traces
transfer sticking particles to beaker. solution to measuring flask. of
solution of measuring flask.

Use pipette to add last

drop of water to make
the volume upto the
mark.

Fig. 5.6 : Washing last traces of solution Fig. 5.7 : Using pipetteto add last drop of
from funnel to the measuring flask. water to make the volume upto the mark.
4. Dissolve the oxalic acid crystals in the beaker by stirring gently with a clean
glass rod.
5. Now transfer this solution carefully from the beaker into a 250 ml measuring
help of a funnel. flask with the
6. Wash the beaker with distilled water and transfer the washings to the measuring
flask.
7. Wash the funnel with distilled water.
8. Make up the solution upto the marked point with distilled water and shake it
by closingthe
stopper of the flask.
9. Lebel the solution as — oxalic acid.
10

PRECAUTIONS •
1. Apparatus should be clean.
2. Observe lower meniscus for colourless solutions.
3. Never heat measuring flask.
4. Use rider for weighing less than 10 mg.
5. Use distilled water for preparing standard solutions.
6. Add last drops of water through pipette to make volume upto the mark.
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 Experiment 5.3
Todetermine the molarity and strength
AIM (Na0H) by of the given solution of Sodium Hydroxide
titrating it against standard acid solution.
solution of 0.1 M Oxalic
APPARATUS
Burette, pipette, conical flask, burette stand, funnel and white glazed tile.
CHEMICAL REQUIRED •
Sodiumhydroxide solution and 0.1 M oxalic acid solution.
INDICATOR
Phenolphthalein
END POINT :
Colourlessto pink colour.
THEORY :
Thisis Acid-basetitration. Sincethis titration is used to determinethe strength of a base by
titrating it against a standard acid solution. It is called alkalimetry.
Oxalicacid is a weak acid and sodium hydroxide is a strong base. The indicator used therefore
is phenolphthalein. The end point is when the colour changes from colourless to pink.
COOH COONa
(aq.) + 2NaOH(aq.) (aq.) + 2H20(1)
COOH COONa
The solution to be taken in burette is Alkali i.e. given NaOH whose strength is to be determined.
PROCEDURE :
1. Wash the burette with water and rinse it with NaOH solution. Antiparallax
2. Fill the burette with NaOH solution and clamp it to the card
burette stand.
3. Rinse the pipette with 0.1 M oxalic acid and pipette out
10 ml. of oxalic acid solution in a titration flask. — Burette
4. Add 1-2 drops of phenolphthaleinindicatorin the titration
flask and place it on a white glazed tile.
5. Note down the lower meniscus of the solution in the burette
and record it as the initial burette reading. Stopcock
6. Now run the sodium hydroxide solution slowlyfrom the
Flask
burette in the titration flask. Continously stir the flask gently.
Plane tile
Add the sodium hydroxide solution dropwise till a faint
permanent pink colour appears on the addition of one more
drop. Read the lower meniscus of the solution again in the
burette and record it as the final burette reading.
Repeat the procedure and take three concordant readings. Fig. 5.8 : Titrationprocess

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OBSERVATION
Molarity of oxalic acid = 0.1 M
Volume of oxalic acid taken = 10 ml [Volumetaken in pipette].
Initial burette Final burette Volume of NaOH
No. reading (VI) (in ml) reading (V2) (in ml) used (V2 —VI)

1. 10.5 10.5 ml.

2. 10.5 21 10.5 ml.
3. 21 31.5 10.5 ml.
4. 31.5 42 10.5 ml.
Concordant reading = 10.5 ml (say)

CALCULATIONS :
MIVI M2V2
al a2
acid base

Where
20
VI = 10 ml. Oxalic acid —10.5 ml. NaOH
1

2Moxalic acid oxalic acid NaOH NaOH

N oxalic acid X V oxalicacid
-
NaOH NaOH

-
NaOH = 0.19 M
10.5
Molecular weight of NaOH = 40
Strength of NaOH = Molecular weight of NaOH x Molarity of NaOH
= 40 x 0.095= 3.8g/1.
RESULT :
Molarity of the given solution of NaOH = 0.19 M
Strength of the solution of NaOH = 3.8 g/l

PRECAUTIONS :
1. Do not rinse the titration flask with the solution.
2. Parallax-error while reading the burette or pipette should be avoided. Read the lower meniscus
3. If a drop of liquid falls on the walls of the conical flask while titrating, wash it into the liquid
with distilledwater.
4. Titration should be carried out very slowly dropwise towards the end point.

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