Analytical and Organic Chemistry CLB 10803

1.0 SUMMARY

The purpose of this experiment is to produce a sample of hard soap and test them.
The experiment started with the preparation of Sodium Hydroxide (NaOH) solution. Then,
a certain amount of fat is added to the conical flask together with prepared Sodium
Hydroxide. The mixture is then heated in water bath of 100°C. Before submerging the flask
is wrap with aluminium foil to reduced loss of ethanol. Flask was swirled using tongs. The
maximum time heating the soap is 25 minutes but the soap can be seen during the 20
minutes. Observe the presence of alcohol and water , add 0.4 ml of 50% water/alcohol
mixture if the flask was dried. Next, 4 ml of Sodium Chloride (NaCl) solution was placed
in a beaker and mix it with soap in the flask. The new mixture was placed in an ice-water
bath while stirring it. A simple test to determine the pH value of the soap was conducted
by using the pH strip. The prepared soap was then collected by filtering it with Hirsch
funnel of ice-cold distilled water to remove excess Sodium Hydroxide (NaOH). The filter
was allowed to rest for a few minutes to partially dry the soap formed. The soap was then
tested by using three solutions; distilled water, Calcium Chloride and Trisodium
Phosphate. Throughout the test with the three solutions, it shows positive reaction towards
the soap. When distilled water was added to the soap and shaked, a thick foam was formed
on the surface of the clear solution. This proved that the soap formed in this experiment
was succeed. Next, as Calcium Chloride was added, white precipitate began to form in the
surface of the clear solution. In theory, Calcium Chloride was used to prevent soap product
from dissolving in water. Thus, the white precipitate formed on the surface of clear solution
when Calcium Chloride was added is clarified as soap scum.When Trisodium Phosphate
was added to the solution, a cloudy solution with white precipitate was observed.
Theoretically, Trisodium Phosphate was used to prevent Calcium ions; Ca2+ from react
with soap. There were few possible errors while conducting this experiment. Firstly,
apparatus used throughout the experiment might be contaminated as the solution used was
exposed to open surrounding in a period of time. Secondly, measurement of solutions taken
for this experiment might be not accurate as there were few minor mistakes. Third,
aluminium foil used in the experiment to cover the flask might be defect as we get reused
aluminium foil and it does not covers the flask well which caused evaporation to take place.
Analytical and Organic Chemistry CLB 10803

2.0 OBJECTIVE

The objectives of this experiment are:

I. To synthesize a sample of hard soap
II. To test the soap produced
Analytical and Organic Chemistry CLB 10803

3.0 RESULT

In this experiment, the data are analyzed using classical method. By classical
method, we make observations base on the changes that happens on the soap.

Classical method
Figure 4.1 below shows the table consist of the data analyzed by classical method
Analysis of data Results
Addition of distilled water Level of foam is at 2.4 ml
Level of foam is at 0.4 ml and precipitate
Addition of CaCl
form.
Level of foam is at 1 ml the solution is
Addition trisodium phosphate
cloudy and precipitate is formed
Analytical and Organic Chemistry CLB 10803

4.0 DISCUSSION

In this experiment, many steps are taken to ensure the production of soap is
achievable. Sodium hydroxide, NaOH and fat are used to produce soap by saponification.

Figure 5.1 shows the chemical equation for saponification

In the experiment, ethanol was added to the mixture of distilled water and sodium
hydroxide, NaOH to allow the saponification process between fat and NaOH to take place
at medium heat. Then, the mixture is heated in the water-bath of 100℃ because direct
heating from the Bunsen burner will cause the mixture to evaporate faster. Swirling the
flask that contain the mixture will slowdown the evaporation process of the mixture. Next,
sodium chloride, NaCl solution is added to remove glycerol from the mixture. This process
is called ‘salting out’. By adding water to the mixture to make it more liquid in texture and
then by adding a saturated solution of salt water. The glycerol is more soluble in the salt
water than the soap and, therefore, allows these two chemicals to be separated. Glycerol
can be removed by adding NaOH because glycerol is more soluble in salt water than in
soap. Therefore, allowing these two mixtures to become two layers or precipitate. Then,
the saponified mixture is transferred in an ice water-bath so that the saponified mixture can
be solidified. Then, the saponified mixture is filtered to obtain the solid soap.
Analytical and Organic Chemistry CLB 10803

Distilled water is also added to remove excess NaOH. In a classical method

analysis, the soap is added with distilled water to measure the foam level generated. The
foam level rises about 2.4 ml in this experiment. The foam generated shows that the soap
cleansing ability is affective than it is in soft water. Then, the soap is added with calcium
chloride, CaCl. The level of foam of the soap will drop because calcium ions are common
substance in forming water hardness. The calcium ions react with soap anions to form soap
scum.

Figure 5.2 shows the reaction of calcium ions with soap anions.

In the experiment, greater quantity of Ca2+ ions contains in the hard water. The
reaction of soap with the earth alkali ions produces precipitates which create an insoluble
residue on fabrics. Soap is less effective in hard water. The amount of soap needed for the
complete precipitation of Ca 2+ cannot be used in the washing process. Moreover extra soap
is required to disperse the precipitates in the suds. The harder the water, the more soap it
takes to disperse the precipitates in the washing liquor. Then, the trisodium phosphate is
added to the soap. The phosphate keeps Ca 2+ ions in solution by forming a soluble complex
with them, thus softening the water and preventing the formation of insoluble soap scum.
Analytical and Organic Chemistry CLB 10803

5.0 CONCLUSION AND RECOMMENDATIONS

From the results and the data analyzed, we can synthesize soap and can perform
classical and instrumental method of analysis on the soap. From the experiment that we
carried out, the cleansing ability of the soap are more efficient in soft water compare to the
cleansing ability in hard water that commonly consist of Ca2+ and Mg2+ ions. Some of the
analysis carried out are not achievable as there were errors done in the experiment.

For recommendation, a few steps that can be taken to prevent these types of errors
from occurring. The students need to stay focus and patient for readings to stabilize before
recording any data to prevent the physical errors which caused by experiments. Next, the
student also need to work together with other member when conduct the experiment.
Besides that, the students should take the three times of data reading and get the average to
get the exact value of data. To avoid the slow process when conduct the experiment, the
students should to read lab manual to understand what experiment is all about. Finally,
conductivity rod must be clean where it is supposed to be wiped every time a sample being
tested using the conductivity rod to get the accurate reading.
Analytical and Organic Chemistry CLB 10803

6.0 REFFERENCE

1. Paula Yurkanis Bruice, Organic Chemistry Fourth Edition.

2. Annick Rouessac, Francis Rouessac, Chemical Analysis: Modern Instrumentation
Method and Technique, John Wiley & Sons.Ltd.
3. Mohan, Jag, Organic Analytical Chemistry: Theory and Practice, Alpha Science
International, Ltd, 2004.
4. Retrieve from http://chemistry.about.com/library/glossary/bldef825.html
5. Retrieve from http://www.unir.de/Fakultaeten/nat_Fak_IV/Organische_Chemie
/Didaktik/Keusch/D-hard_water-e.htm
Analytical and Organic Chemistry CLB 10803

7.0 APPENDIX

PRE LAB QUESTIONS

1) Give the definition of saponification

A process by which triglycerides are reacted with sodium or potassium hydroxide

to produce glycerol and a fatty acid salt, called 'soap'.

2) Explain how soap can function as soap remover

Soap has a cleansing ability because of the non polar oil molecules, which carry
dirt, dissolve in the non polar interior of the micelle and are carried away with the
soap during rinsing. The micelle is made of long chain carboxylate ions that
arrange themselves in spherical clusters.

3) Synthetic detergent functions in the same way as soaps. Give the advantages of
synthetic detergent over soaps

The advantages of synthetic detergents over soap are that they have excellent
resistance to hard water. They contain "builders" which minimize the effects of hard
water. The most common "builder" used to be sodium trimetaphosphate. The
2+ 2+
phosphate keeps Ca and Mg ions in solution by forming a soluble complex
with them, thus softening the water and preventing the formation of insoluble
calcium soaps.
Analytical and Organic Chemistry CLB 10803

POST LAB QUESTIONS

1) Reaction of fat with NaOH will produce long chain carboxylic acid (soap) in form
of Bar. What would happen if sodium hydroxide, NaOH is replaced by potassium
hydroxide, KOH?
Since NaOH is a caustic base, using it to react with fat will produce a hard soap.
When we use potassium hydroxide instead of sodium hydroxide, soft soap will be
produced.