CHAPTER THREE

MATERIALS AND METHODS

3.1 Materials

1. Palm kernel fruits

2. Palm kernel nuts

3. Olive oil

4. Mortar l

5. Pestle

6. Bowl

7. Gas cooker

8. Rubber basin

9. Round bottom button flask (250 cm3)

10. Pipette

11. Burette

12. Retort stand

13. Beakers – state their capacities

14. Crucible

15. pH meter

16. Analytical balance – give its make or model scale

17. Measuring cylinders – glass or plastic, and of what capacities?

18. Refluxing set up

19. pPlastic silicon mold

3.1.1 Reagents

1. Potasium Hydroxide (KOH)

3. Sodium Hydroxide (NaOH)

4. Distilled water

5. Sodium Chloride (NaOH)

6. Potasium Chloride (KOH)

7. Ammonium Chloride (NH4Cl)

8. Calcium Chloride (CaCl2)

9. Magnesium Chloride (MgCl2)

10. Iron Chloride (FeCl3)

3.2 Methods

3.2.1 Sample Collection

Fresh palm fruits and palm kernel were obtained from Buruku township market and taken to

Chemistry Department, Benue State University, Makurdi for the purpose of this study.

Olive oil was bought from a supermarket in Wurukum market, Makurdi, for the experiment.

3.2.2 Sample Pre-treatment

The palm kernel fruits and nuts were washed thoroughly to get rid of impurities and sun-dried

for thirty minutes.

3.2.3 3.3.3 Extraction of the Crude Palm Oil

The treated palm kernel fruits were boiled using a gas cooker until cracks were seen on

their peels, indicating that the fruits were properly cooked. The hot water in the boiling

pot was then separated from the boiled fruits, which were then pound to obtain the desired

content in the fruits. After pounding, the nuts and peels were separated from the mixture

using a basket, where the crushed (pounded) mixture was washed in the hot water (which
was initially poured out after boiling), leaving out the chaff. After separation, the chaff

and nuts were sun-dried while the desired fraction was boiled again at very high

temperature. After a while, fractions of oil were noticed to appear on the surface of the

boiling liquid. The oil was scooped into another container until the desired fraction of oil

was realized. The boiling mixture was discarded. The oil that was scooped into a fresh

container, which contained some amount of water, and was boiled again so to separate the

oil from the small amount of water left therein. Finally, and with care, the clean oil was

again scooped out using a cooking spoon into a clean container as palm oil.

3.2.4 Extraction of the Crude Palm Kernel Oil

The pre-treated palm kernel was ground into very fine particles using a grinding machine.

The pulverized sample was boiled water at a very high temperature until oil started

floating on top of the boiling mixture, and was carefully scooped out into a container. The

scooped oil, containing some amounts of water was again boiled while the final fraction

of clear oil was scooped out into a container as palm kernel oil.

3.2.5 Determination of the Saponification Value (SV)

250 cm3 capacity round bottom flask was weighed and 1 g of warm palm kernel oil was

introduced into the flask. 25 cm3 of 0.5 M KOH solution was also added. The mixture was

refluxed for one hour after which the heating was stopped and 5 drops of phenolphthalein

indicator were was added. The resultant hot soap was titrated against 0.5 M HCl. The process

was repeated three times and the average titre value was taken. A blank titration was equally

done out by titrating 25 cm3 of 0.5 M potassium hydroxide against 0.5 M HCl.

The Saponification Value (SV) was determined using the following formula:

S.V = [(B - A)25] / Weight of sample (g)

refluxed mixture in cm3

B = Titre value of sample B i.e. volume of the HCl solution used for the blank run in cm3

In order to calculate the amount of lye needed to make bar soap, KOH values of

saponification can be converted to NaOH values by dividing KOH values by the ratio of

molecular

weights of KOH and NaOH (1.403) (Muhammed et al., 2022).

Where is 3.2.6?

3.3 7 Formulation of Soaps

The cold method of production was used for the production of the soaps.

For the first brand of soap containing 70% palm kernel oil (PKO), 20% palm oil (PO) and

10% olive oil (OO). 42 g, 12 g and 6 g of palm kernel oil, palm oil and olive oil respectively

were blended together. To the blended oil, the cooled solution of 10.03 g NaOH (lye) with

22.42 g distilled water was transferred to the oil blends with continuous stirring and in one

direction until a homogenous paste was formed. The paste was stirred continuously until the

thickness of the paste increased and a trace-mark began to appear. The paste was then

transferred into a plastic silicon mold and allowed to cure at ambient temperature into a solid

bar soap.

For the second brand of soap containing 70% palm oil, 20% palm kernel oil and 10% olive

oil. 42 g, 12 g and 6 g of Pxalm Kxernel Oxil, Pxalm Oxil and Oxlive oil respectively were

blended together into a homogenous oil mixture. To the oil blend, a cooled solution of 9.01 g

of NaOH and 20.14 g distilled water was added with continuous stirring in one direction,
until a homogenous paste was made. The paste in then transferred into a plastic silicon mold

and allowed to cure at ambient temperature into a solid bar soap.

The third brand of soap containing 50% palm kernel oil, 30% palm oil and 20% olive oil was

prepared by blending together 30 g, 18 g and 12 g of palm kernel oil, palm oil and olive oil

respectively. To the blended oil, the cooled solution of 9.58 g NaOH and 21.41 g distilled

water was added with continuous stirring in one direction, until a homogenous paste was

made. The paste was then transferred into a soap mold and kept for the curing cure time to be

completed.

3.4 8 Determination of Moisture Content

Moisture content was determined by drying 10 g of the sample to a constant weight at 105 ºC

in an oven. It was allowed to cool and then reweighed. The moisture content was determined

by from the following formula:

Moisture content (%) = (Cs - Ch / Cs - Cw) × 100

Where;

Cw = weight of crucible

Cs = weight of crucible + sample

Ch = weight of crucible + sample after heating

3.5 9 Determination of Foamability

About 2.0 g of each soap (shavings) was added to a 500 cm 3 measuring cylinder containing

100 cm3 of distilled water. The mixture was shaken vigorously so as to generate foams. After

shaking for about 2 minutes, the cylinder was allowed to stand for about 10 minutes. The

height of the foam in the solution was measured and recorded (Muhammed et al., 2022).

3.6 10 Determination of pH
The pH was checked using a pH meter. 10 g of the sample was measured and dissolved in

deionized water in a 100 cm 3 volumetric flask. The electrode of the pH meter was put into the

solution and reading was taken for the soap sample. The same procedure was done for all the

prepared samples (Muhammed et al., 2022).

3.7 11 Reaction of Soap with Metals

To 5 xmlx of each soap in test tubes, 2 cm3 of 4% NaCl, KCl, NH4Cl, CaCl2, MgCl2 and

FeCl3 were added, each of the test tube were shaken and precipitate formation were observed

(Atiku et al., 2014).

You must diligently address all the queries. 29/5/2024.