Chapter 2

DESIGN AND METHODOLOGY

The experiment started with assembling the distillation set-up as shown in the figure

below. A few boiling chips were placed inside the distilling flask later filled with the

measured 100 mL of glacial acetic acid using a 100 mL graduated cylinder as measuring

apparatus and 2 mL of distilled water drawn out of the water bottle with a 10 mL pipette. A

single-holed cork equipped with a 150C thermometer was used to cap the opening of the

distilling flask. An iron clamp was attached to the neck of the distilling flask and the clamp

fixed into an iron stand while

making sure that the bottom of the

distilling flask is just above the iron

ring and the Bunsen burner below it.

Wire gauze was placed on top of the

iron ring to prevent direct contact of

Fig.2-1. Distillation set-up
the burners flame and the flasks bottom. The arm of the flask was attached to the open end

of the condenser that is clamped to a separate iron stand. An adapter was connected to the

other end of the condenser followed by laying a 50 mL graduated cylinder at the adapters

end to catch the distillate. The rubber tubing of the condenser was check and tightened to

prevent leakage before opening the water inlet.

Simultaneously, a 1000 mL of 1N NaOH solution was being prepared by another

member. The weight of the NaOH pellets to be dissolved to obtain 1N NaOH was calculated

by the equation:
 ( Normality of NaOH )( Volume of NaOH ) (Molar mass of NaOH )
weight of NaOH =
(factor of NaOH )(k )

(Eqn 2.1)

where normality is 1 normal

volume is 1000 mL liter

molar mass is 40 grams per mol

factor is 1

k is 1000 milliequivalence per equivalence

The calculated weight of the NaOH was used as basis for the grams of NaOH pellets

weighed using analytical balance. The weighed NaOH pellets which amounted to ____

was dissolved into a 100 mL distilled water contained in a beaker. The NaOH solution was

transferred into a 1000 mL volumetric flask and further diluted to 1000 mL indicated by the

mark on the neck of the volumetric flask. The flask was then capped, shook, labeled with 1N

NaOH and let to stand for a few minutes. A base burette was held by a member to chest level

while another gently poured the 1N NaOH into the burette having an attached funnel. Once

the burette was full, the solution was run to reduce the solution level to 0 mL mark and to

wash the inside of the glass below the stopcock. The burette was then fixed into a double

burette clamp on an iron stand and adjusted to a vertically straight position for correct

reading of solutions volume level. The NaOH solution was standardized to obtain its exact

normality which was done by dissolving ____ grams of potassium hydrogen phthalate

(KHP) into a volume of distilled water then adding two drops of phenolphthalein and titrated

with 1N NaOH solution in the burette and the volume of the NaOH solution used was

recorded. The standardization process was performed twice and in the second trial the

weight of KHP used was____ grams and both of which process was stopped when the KHP
solution turned light pink, an indication that the solution has reached its endpoint. The exact

normality of the NaOH solution was computed by the equation:

g KHP f 1000
Normality of NaOH= (Eqn 2.2)
Molar mass of KHP Volume of NaOH

Prior to heating, the group called the attention of the instructor, Engr. Katelyn

Gabon, to assess the experiment set-up and permit the group to carry out the activity after

taking a sample of 1 mL from the solution in the distilling flask then placed in an Erlenmeyer

flask labeled as L-1. The Bunsen burner was lit to a medium blue flame which was reduced

to low at the latter part of the procedure to minimize the sudden uncontrollable burst of the

solution inside the distilling flask. This phenomenon must be prevented as much as possible

as the solution when bursting can reach the arm of the distilling flask connected to the

condenser and contaminate the distillate as well as touch the tip of the thermometer leading

to an inaccurate reading of the temperature of the vapor solution. Another reason to keep the

flame to a minimum is to maintain the desired 2-3 drops per second of distillate.

The 50 mL graduated cylinder was replaced with a 10 mL cylinder for better

gauging of the first 2 mL distillate to be discarded and because the 10 mL graduated cylinder

is shorter than the 50 mL one stacking blocks were placed underneath the former to raise it

and prevent spilling of the distillate. After collecting 2 mL of the distillate, the 10 mL

graduated cylinder was replaced with the 50 mL while moving the stacking blocks to the side

for later use.

After collecting 5 mL of distillate, a member noted the temperature of the solution

in the distilling flask by reading the thermometer on the flask while another student took the

temperature of the distillate using another thermometer. The Bunsen burner was removed

after a volume of 10 mL distillate was gathered. From the solution in the distilling flask, 1
mL was drawn out and added into the Erlenmeyer flask tagged as L-1 and also 2 mL was

taken from the collected 10 mL distillate and placed into another Erlenmeyer flask tagged as

V-1. Both L-1 and V-1 were added with two drops of phenolphthalein then titrated with the

prepared 1N NaOH solution in the burette.

For the second distillation process, 5 mL of distilled water was added to the solution

in the distilling flask afterwhich 1 mL of this solution was drawn out and placed into another

Erlenmeyer flask marked as L-2. The solution was again heated and like the first distillation

process, the first 2 mL distillate gathered by the 10 mL graduated cylinder was discarded.

Temperature reading of both the solution in the distilling flask and the distillate was recorded

upon obtaining 5 mL of the distillate. With 10 mL distillate collected, the process was

stopped and 2 mL of the distillate was placed into an Erlenmeyer flask marked as V-2 and 1

mL of the solution in the distilling flask was added to the flask marked as L-2. Both L-2 and

V-2 were also titrated with the 1N NaOH solution with phenolphthalein as indicator. The

distillation process was repeated for another three times, the only difference is the amount of

distilled water added before the next distillation run increased to 10, 20, and 30 mL

respectively and that the labels L-2, V-2 changed into Ls 3,4,5 and Vs 3,4,5.