Chapter 2

DESIGN AND METHODOLOGY

Given that most of the apparatus needed for this experiment were in the groups locker,

only three separatory funnels with rubber bulbs were requested from the custodian which were

rinsed with distilled water and let to dry after securing the rubber bulbs covering the tip. A total

of three different concentration of HAc solution namely; 1N, O.5N, 0.25N were needed for the

experiment. The group made use of the 0.5N HAc solution left from the previous experiment

(Experiment 5; The Study of an Adsorption Isotherm: Acetic Acid solutions on Activated

Carbon) seeing that the solution is more than 25 mL in volume and that it has already been

standardized. With no time to waste, 25 mL of 0.5N HAc solution was displaced into a

separatory funnel labeled with 0.5N HAc eventually adding 25 mL of carbon tetrachloride

putting on its lid. The separatory funnel was submerged into a water trough almost full with

water of maintained temperature 25C. The tub of water was put together by letting tap water

take half of the trough soon after reading the waters temperature then gradually adding warm

water asked from the laboratory custodian. Using a phones stopwatch, the submerged solution

was under water for a total of 20 minutes with occasional swirling of the solution after every

three minutes.

Now, the members only needed to prepare 1N and 0.25N HAc solution by

simultaneously drawing out using pipette and pipetol ___ mL for 1N HAc then discharging to a

100 mL volumetric flask and again doing the same for 0.25 mL HAc only instead of ___ mL

___ mL was taken. The HAc solution were diluted to 100 mL by adding distilled water unto

their flasks until the mark later labeling the flasks with each respective concentration, capping
then shaking the solution by pressing the pointer finger on top of each of the flasks cap and

letting the remaining fingers and the palm take hold of the neck of the flasks then tipping the

flask downwards then back up until the solution has been thoroughly mixed. Like the 0.5N HAc

solution, 25 ml from each of the 0.25N and 1N HAc was suctioned and discharged into separate

separatory funnel labeled with the respective concentrations. Carbon tetrachloride of which is 25

mL was added unto each of the separatory funnel followed by immersing into the water trough

for 20 minutes. Throughout the submersion process, a thermometer was pitched into the water

for convenient monitoring of its temperature. The remaining volume of the 0.25N HAc in the

volumetric flask was poured into an acid burette to titrate 0.1N NaOH left from the previous

experiment. For the standardization of 0.25N HAc, 4 mL of the 0.1N NaOH was put into an

Erlenmeyer flask adding two drops of phenolphthalein then titrated with the 0.25N HAc in the

burette until the NaOH solution appeared colorless. The exact procedure and same volume of

the 0.1N NaOH were followed in the standardization of 1N HAc solution. The exact normality

of the HAc solution was computed by:

. ( )
= ( Eqn 2.1 )

The mean of the calculated normality from the equation above was used as the final

normality of the HAc solution which was computed by:

1 + 2
= ( Eqn 2.2 )
2

___ grams of NaOH pellets was dissolved into distilled water eventually pouring the

mixture into a 500 mL volumetric flask then further diluting to the mark, covering the flask with

its lid, and shaking the solution. To standardize this solution in order to obtain its true normality,

0.0248 grams of potassium hydrogen phthalate (KHP) was dissolved into 15 mL distilled water
later added with two drops of phenolphthalein and was titrated with 0.01N NaOH solution

recording the volume of NaOH used for the KHP mixture to reach its endpoint. A second

standardization was done by weighing 0.0358 grams of KHP then diluting with water and, just

like the first KHP solution, added with two drops of phenolphthalein afterwhich was titrated with

0.01N NaOH solution also recording the volume of NaOH for the KHP solution to attain

endpoint. The titration set-up was assembled just like in the figure by screwing in a double

burette clamp into an iron stand later attaching the base burette on the

left side while an acid burette was hooked on the right. The base burette

was filled with 0.01N NaOH past the 0 mL mark but by allowing the

solution to be run through, the solution was leveled with the liquid

reading mark. For computation of the normality of the NaOH solution,

the group used the formula:

1000
= ( Eqn 2.3 )

The mean of the calculated normality from the equation above was used as the final

normality of the NaOH solution.

1 + 2
= ( Eqn 2.4 )
2

After 20 minutes of submerging the 0.5N HAc with 25 mL CCl4, the separatory funnel

containing this solution was fixed into an iron stand and left for another 20 minutes before

extracting 20 mL of the CCl4 layer on the bottom of the funnel. The instructors attention, Engr.

Katelyn Gabon, was called to start and supervise the extraction process. First, the rubber bulb of
the medicine dropper was removed from the tip of the funnel followed by wiping the outside of

the funnel with a dry cloth. The stopcock was turned to a vertical position

to allow the CCl4 to flow into the Erlenmeyer flask as shown in the figure

occasionally adjusting the position of the stopcock to almost horizontal

when the flow of CCl4 is too rapid. The extraction was deemed to be

complete when all of the CCl4 on the bottom of the flask has been wringed

out into the Erlenmeyer flask. From the volume of the extracted CCl4

contained in the Erlenmeyer flask, 20 mL was taken and transferred into

another Erlenmeyer flask adding two drops of phenolphthalein and titrated

with the prepared 0.01N NaOH until endpoint was reached. The volume of

the NaOH consumed was recorded. The same was done with the remaining

separatory funnels filled with 0.25N and 1N HAc solution each having an added 25 mL CCl4.

After titrating all three of the extracted 20 mL CCl4, the 0.01N NaOH in the burette was changed

with 0.1N NaOH left from the previous experiment was used to titrate the removed 10 mL on the

water layer from separatory funnel of the different concentrations. The volume of the basic

solution needed for each of the three 10 mL water layer to reach their endpoint was recorded.

Further computation of the concentration of HAc was done by substituting the acquired values to

the following formulae:

0.01 ( )
= 4
(Eqn 2.5)

0.01 ( )
=
(Eqn 2.6)