Topic : Volumetric Analysis – Stoichiometry

Purpose : To determine the exact concentration of monobasic acid, HX.

Materials : 0.3 mol dm^(-3) sodium hydroxide, NaOH solution, monobasic acid, HX (Unknown
Concentration), phenolphthalein indicator and distilled water.

Apparatus : 50.00 cm^3 burette, 25cm^3 pipette, 250cm^3 conical flask, 250 cm^3 volumetric flask,
50cm^3 beaker, dropper, glass rod, spatula white tile and retort stand with clamp.

Theory :

HX (aq) + NaOH (aq)  NaX (aq) + H2O (l)

Relative Molecular Mass of sodium hydroxide : 40.00 g mol^(-1)

Mass of sodium hydroxide, NaOH : 0.30 mol × 40.00 g mol^(-1)

= 12.0 g

Mass of NaOH required for 250cm^3 of sodium hydroxide = 12.0g × (250/1000)

= 3.0g

[NaOH] = (3.0g / 40.00 g mol^(-1)) × (1000 / 250) = 0.30 mol dm^(-3)

Procedure :

Part A

1. The mass of sodium hydroxide, NaOH needed to prepare 250cm^3 of 0.30 mol dm^(-3) of
sodium hydroxide, NaOH solution is calculated.
2. A clean 50cm^3 beaker is weighed using a weighing scale. sodium hydroxide powder is
added little by little using a spatula into the beaker until there is an increase in exactly 3.0 g in
the reading of the weighing scale.
3. Both the readings of the empty beaker as well as the beaker containing sodium hydroxide
powder are recorded in table 1.1.
4. The inner wall of the beaker is rinsed with distilled water to dissolve all the sodium
hydroxide, NaOH powder.
5. The solution is stirred with a glass rod to ensure there are no undissolved powder of sodium
hydroxide, NaOH.
 6. The sodium hydroxide, NaOH solution from the beaker is then transferred into a 250 cm^3
volumetric flask by using a filter funnel.
7. The beaker and glass rod are rinsed with distilled water, and the solution is poured into the
250 cm^3 volumetric flask to ensure there is no original solution remaining in the beaker.
This procedure is repeated 2 to 3 times.
8. The inner wall of the filter funnel is rinsed thoroughly to ensure there are no remaining
droplets of the original solution on the filter funnel. This procedure is repeated 2 to 3 times.
The filter funnel is removed.
9. A stopper is placed into the volumetric flask. The solution is then gently shaken.
10. Distilled water is added into the volumetric flask until the meniscus of the solution touches
the calibration line.
11. A stopper is placed into the volumetric flask. The flask is then inverted and gently shaken
several times to ensure the solution is homogeneous.
12. The volumetric flask is then labelled and stored.

Part B

1. A pipette is rinsed with a little 0.3 mol dm^-3 sodium hydroxide, NaOH solution. The solution is
then discarded from the pipette.
2. A burette and beaker are rinsed with a little monobasic acid, HX. The acid is then discarded from
the beaker and burette.
3. A 250cm^3 beaker is rinsed with a little 0.30 mol dm^(-3) of sodium hydroxide, NaOH solution.
The solution is then discarded.
4. 100cm^3 of 0.30 mol dm^(-3) sodium hydroxide, NaOH solution is poured into the beaker.
5. The apparatus is set up as in Figure 1.1.
6. The 50.00 cm^3 burette is filled with monobasic acid, HX with the aid of a filter funnel. The filter
funnel is removed. The initial reading of the burette is recorded.
7. 25 cm^3 of 0.30 mol dm^-3 sodium hydroxide, NaOH solution is pipetted from the beaker
containing sodium hydroxide, NaOH solution and released into a clean 250 cm^3 conical flask.
8. 2 to 3 drops of phenolphthalein indicator are added into the 250 cm^3 conical flask containing
sodium hydroxide, NaOH solution. The solution is swirled until the colour of the solution
changes completely from colourless to pink.
9. The 250 cm^3 conical flask is placed on the white tile below the burette.
10. HX is slowly dripped into the 250 cm^3 conical flask while swirled.
11. As soon as the solution changes from pink to colorless, the stopcock of the burette is closed. The
final reading of the burette is recorded. The difference in initial reading of the burette and final
reading of burette is labelled as V.
12. Steps 6 to 9 are repeated.
13. Monobasic Acid, HX is flowed into the 250 cm^3 conical flask until (V - 5). The flow is stopped.
14. HX is added drop by drop into the flask while swirling.
15. As soon as the solution turns colorless, the titration is stopped. The final burette reading is
recorded.
16. Steps 12 to 15 are repeated twice more.
17. The difference in volume of each set of readings are calculated.
18. The average volume of Monobasic Acid required to neutralise the 25cm^3 of 0.30 mol dm^(-3) is
calculated.

Figure 1.1
Results :

Mass of Beaker + sodium hydroxide powder / g 69.90

Mass of Empty Beaker / g 66.58
Mass of sodium hydroxide, NaOH used / g 3.32

Rough Volume, Accurate

Titration Number
V/cm^3 1 2 3
Final Reading/cm^3 14.90 28.30 13.30 26.60
Initial Reading/cm^3 1.00 14.90 0.00 13.30
Volume of Monobasic Acid, HX used/cm^3 13.90 13.40 13.30 13.30

Interpreting Data :

Average volume of Monobasic Acid used for titration : (13.30 + 13.30) / 2

= 13.30 cm^3

MaVa = MbVb

Ma(13.30) = 0.332(25)

Ma = 0.624 mol dm^(-3)

Conclusion :

- The exact volume of Monobasic Acid, HX used in this reaction is 0.624 mol dm^(-3)

Precaution :

1. Eye must be perpendicular to the calibration line, scale of the beaker, and scale of the burette.
2. The pipe of the distilled water bottle should not touch the Sodium hydroxide, NaOH solution.
3. There must not be any spills of the standard solution.
4. Use dropper towards the end to make sure the solution does not pass the calibration line when
adding distilled water to volumetric flask or pipetting sodium hydroxide, NaOH solution.