In the Laboratory

Making Usable, Quality Opaque or Transparent Soap W

Suzanne T. Mabrouk
Department of Chemistry, The Citadel, The Military College of South Carolina, Charleston, SC 29409;

Over the years this Journal has featured articles on the
history (1, 2) of soap, the industrial process of saponifica-
tion (35), and laboratory-ready experiments (613). The ex-
periments and those in organic laboratory textbooks have
described the hot (610, 1416) and cold (10, 11) processes
for making opaque soap, eq 1,
O
O Fats and Oils
+
R O M
R O HO
+ reduce the harshness of soap, to produce a dense creamy
O O
MOH
R O R
+
O M + HO
M = Na, K + component contributes different properties. These proper-
O ties are determined by the type and percentage of the fatty
O acids in each fat or oil (1923) (see Tables 1 and 2 in the
R O + HO
R O M
(1)
fats and oils soap glycerin
(triacylglycerols) (carboxylates)
and the conversion of commercially-available, opaque soaps
into transparent (12) or solid potassium soaps (13).
In the experiments, typically one fat or oil (79, 11, 14
16) is saponified with a stoichiometric excess of sodium hy-
droxide (7, 8, 10, 1416). In the hot process, excess base is
usually removed by filtration and rinsing of the soap precipi-
tated by the addition of aqueous sodium chloride (68, 14,
15). Alternatively, Evans suggests adding coconut oil or di-
lute hydrochloric acid to the melted soap, exposing thin pieces
of solid soap to air, or beating the melted soap (10) to re-
move the excess base. In the latter two methods the base
reacts with the CO2 in the air, eq 2:
2NaOH(aq) + CO2(g) Na2CO3(s) + H2O(l)
Hill (9) and Lehman (16) rinse the filtered soap with water.
As soap containing excess base will irritate the skin (10), stu-
dents have been prohibited from using the prepared soap.
Students will be able to use soaps from this experiment as
they contain 5% excess fat.
This experiment introduces students to the industrial
method of making opaque (formulas 18) or transparent soap
(formulas 10 and 11) and formulations chemistry (formula
9). It can accompany lectures on personal care products or
lipids in a first-year or organic chemistry course. The proce-
dures can be used independently or, as one reviewer noted,
as a multiweek project. Over three weeks, students can make
opaque soap in one two-hour period or transparent soap in
one three-hour period, and formulate a soap and test its ef-
fectiveness alongside commercial surfactants.
Opaque and transparent soaps are made using the cold
and semiboiled processes, respectively. In both processes,
premelted fats and oils are combined with base. In the
semiboiled process, heat is applied. Complete saponification
occurs in one week in the cold process, and a couple hours in
the semiboiled process. The byproduct glycerin is retained
in both methods. As some individuals find soap dehydrates
the skin, the presence of the humectant glycerin in the fin-
ished soap is advantageous.
Soap Formulation
Commercial manufacturers use 17% excess fat (17) to
lather, and to leave the skin feeling smooth and soft (18).
The formulations in this article use 5% excess fat. Effective
soaps are made from a mixture of fats and oils because each
Supplemental MaterialW). For example lauric acid, the pre-
dominant fatty acid in coconut oil (48.0%), produces a hard
and effective cleanser with a fluffy lather. Unfortunately, lauric
acid does not condition the skin nor provide a stable lather;
therefore other fatty acids are warranted. Table 3 in the
Supplemental MaterialW gives the percent maximum recom-
mended usage of fats and oils based on therapeutic benefits
(24), cost, and fatty acid content. Beeswax (25) and coconut
and palm oils (19) harden an otherwise soft soap. Manufac-
turers preferentially use coconut and palm oils because they
are cheap and they produce an effective cleanser with fluffy
lather (19).
Base, Water, and Scent
After selecting the fats and oils, the mass of required so-
dium hydroxide is determined from the saponification (SAP)
value of the soap (26, 27). The SAP value of the soap is cal-
culated from the sum of the product of the SAP value of each
(2)
fat or oil and the percent of this component in the soap (see
Table 3 in the Supplemental MaterialW) (20, 22, 23, 28).
Because SAP values are defined as the number of milligrams
of potassium hydroxide per one gram fat or oil (29), the SAP
value of the soap is converted to mass of potassium hydrox-
ide per gram fat or oil and subsequently multiplied by the
total mass of fats and oils. Since potassium hydroxide is typi-
cally used to make liquid soap while sodium hydroxide is used
to make solid soap, the required mass of potassium hydrox-
ide is converted to mass of sodium hydroxide. Because com-
mercial soap contains excess fats and oils to moisturize the
skin, the mass of sodium hydroxide is multiplied by 0.95.
The mass of deionized water and scent are determined by
multiplying the total mass of fats and oils by 0.375 and
0.0125, respectively; if the manufacturer of the scent pro-
vides a usage rate, then this value should be used instead.
Additional Ingredients
Deionized water is used to make soap because it pre-
vents the reaction of newly formed soap with hard water ions

1534 Journal of Chemical Education Vol. 82 No. 10 October 2005 www.JCE.DivCHED.org

 In the Laboratory

(17, 30); this unwanted reaction would lower the yield.
Deionized water also minimizes discoloration caused by im-
purities.
Milk in soap moisturizes the skin and produces a mild,
creamy, and rich consistency (31). Based on fat content,
whole milk (4%), half-and-half (10.518%), light cream (18
30%), light whipping cream (3036%), and heavy whipping
cream (3640%) are commonly used (32). In this article,
whipping cream is used for its high fat content. When re-
placing all water with milk, the milk must be frozen prior to
the addition of base (31), otherwise proteins in the milk de-
nature causing a tan-to-brown-colored soap (33). When us-
ing small quantities of milk, as in formulas 2, 4, 6, and 8,
the milk is added following saponification.
To reduce the formation of fibrous crystals and to make
transparent soap, castor oil, ethanol, glycerin, and sugar are
added to the hot soap solution (34). The molded soap is also
cooled slowly in the open.
Surfactant Tests
The prepared soap and commercial surfactants are tested
for pH, feel, and effectiveness (ability to lather) in hard and
soft water. The transparency of formulas 10 and 11 is con-
firmed by reading text written with a 14-point font through
a 1/4 in. slice of soap (35, 36).
Experimental Procedure
Chemicals
Majestic Mountain Sage (37) and From Nature With
Love (38) supply most fats and oils. Craft stores sell beeswax
and stearic acid. Supermarkets sell canola, corn, olive, saf-
flower, and sunflower oils, lard, sugar, and whipping cream.
Note that the coconut and palm oils should be melted prior
to use, as they separate on cooling. Replace any fats and oils
that burn on melting.
Cold-Process Soap (Formulas 18)
Combine and stir the deionized water and half of the
sodium hydroxide (Table 1) in a 250-mL beaker on a mag-
netic stirring plate. After the solid has dissolved, add the re-
maining sodium hydroxide. Stir and heat all fats and oils until
melted in a 400-mL beaker on a magnetic stirring hot plate.
Slowly pour the base solution into the beaker of fats and oils
and stir until trace is observed. To test for trace, dip a stir-
ring rod into the mixture and wave it over the surface. If the
drizzled material leaves a pattern on the surface before sink-
ing, the soap has traced. Add scent and cream and stir the
mixture until trace is reached again. Pour the soap into molds
or weighing boats (either four, 3 in. 3 in.-square boats or
six, 2 5/8 in. 3 in.-hexagonal boats). Place the molds in an
insulated chest for one week so that the evolving heat will
harden the soap.
Student-Formulated Cold-Process Soap (Formula 9)
After selecting the fats and oils and performing the nec-
essary calculations, prepare the soap as described in cold-pro-
cess soap.
Transparent Soap (Formulas 10 and 11)
Combine the fats, oils, and alcohol in a 500-mL three-
necked round-bottom flask equipped with a condenser and
two ground-glass stoppers. Place the flask on a heating mantle

Table 1. Required Ingredients for the Cold-Processed Soaps

Formula
Ingredients
1 2 3 4 5 6 7 8
Base Solution
Deionized water 75.00 40.00 75.00 40.00 75.00 40.00 75.00 40.00
Sodium hydroxide 24.70 24.70 29.60 29.60 29.20 29.20 29.50 29.50
Fats and Oils
Beeswax 10.00 10.00
Canola oil 18.00 18.00 60.00 60.00
Castor oil 18.00 18.00 20.00 20.00 40.00 40.00
Coconut oil 80.00 80.00 80.00 80.00
Corn oil 18.00 18.00 40.00 40.00
Lard 80.00 80.00
Olive oil 100.00 100.00 40.00 40.00
Palm oil 80.00 80.00
Stearic acid 20.00 20.00
Safflower oil 18.00 18.00
Sunflower oil 18.00 18.00 20.00 20.00 40.00 40.00
Other
Scent 02.50 02.50 02.50 02.50 02.50 02.50 02.50 02.50
Whipping Cream 35.00 35.00 35.00 35.00
NOTE: All quantities are in units of grams.

www.JCE.DivCHED.org Vol. 82 No. 10 October 2005 Journal of Chemical Education 1535

 In the Laboratory

on a magnetic stirring plate. Stir and heat the mixture until To make the sugar solution, stir and heat the deionized
the fats have melted (Table 2). water and sugar in a 250-mL beaker on a magnetic stirring
To make the base solution, stir the deionized water and hot plate until the sugar dissolves. Cover the beaker with a
half of the sodium hydroxide in a 250-mL beaker on a mag- watch glass to minimize evaporation. Following reflux, pour
netic stirring plate. Following dissolution, add the remain- the sugar solution through the condenser into the round-bot-
ing sodium hydroxide. Slowly pour the base solution through tom flask. Add glycerin through a neck on the flask. Stir the
the condenser into the round-bottom flask. Using a perma- solution at reflux an additional ten minutes and then allow
nent marker, draw a line on the outside of the flask to indi- it to cool to 60 C. Add scent and food coloring (drop by
cate the level of liquid. If the level drops, add more ethanol drop to desired shade) through a neck on the flask. Stir the
slowly through the condenser to bring the level to the line. solution a few minutes and pour it into molds or weighing
Stir the mixture at reflux for two hours. boats (six 3 in. 3 in. square boats). To promote transpar-
ency, leave the molds in the open. Within a few hours the
Table 2. Required Ingredients for the Transparent Soaps soap will harden.
Formula Surfactant Tests
Ingredients
10 11 Measure the pH of the prepared soap, commercial sur-
Fats and Oils factants, the students skin, and deionized water with
Castor oil 30.00 30.00 pHydrion paper. Wash hands with a bar of each prepared
Coconut oil 45.00 45.00 formulation and compare the quantity of lather, the size of
Olive oil 15.00 15.00
the bubbles, and the feel. Test the effectiveness of the pre-
pared soap and commercial surfactants1 in hard and soft wa-
Palm oil 45.00 60.00
ter with 4% aqueous calcium chloride and 9% aqueous
Shea butter 15.00 sodium phosphate tribasic, respectively. Test for transparency.
Base Solution
Deionized water 50.00 50.00 Hazards
Sodium hydroxide 22.48 22.68
Sugar Solution
Sodium hydroxide is caustic and can cause serious burns.
On contact, flush the affected area with water. Because hot
Deionized water 24.52 24.10
oils will burn, avoid contact. Since ethanol and essential and
Sugar 27.94 27.79 fragrance oils are flammable, keep away from flames. People
Other who are sensitive to coconut oil should not prepare formulas
Absolute ethyl alcohol 60.37 60.37 36, 10, or 11.
Glycerin 37.26 37.05
Scent 03.73 03.73
Results and Discussion
NOTE: All quantities are in units of grams. Since soaps are alkali salts of fatty acids, they were found
to be basic. The skin and deionized water were found to be
slightly acidic. None of the soaps lathered in hard water,
whereas the combars did. Combars are combination bars
composed of soap and synthetic detergent. All surfactants
lathered in soft water. Formulations 10 and 11 produced
transparent soap (Figure 1). Generally students liked the feel
of the prepared soap. In one organic section, where students
devised their own formulation, the majority of the students
preferred a soap made from 20% almond, 20% avocado, 35%
coconut, and 25% olive oils.

Figure 1. Student-prepared transparent soaps. (This image is shown
in color on p 1427.)
Conclusion
According to anonymous surveys, students enjoyed mak-
ing and testing the soap. From this experiment they learned
the chemistry of soap, which helped them in the lecture
course: I learned how soap actually works and how it is
chemically formed. Another student learned that it takes
many oils to be combined together to get soap. I learned
what transparent soaps are actually made of, and how easy it
is to make it. The students appreciated the freedom to se-
lect the scent for their soap and for those who devised a
unique formulation, enjoyed the experience and opportunity
to create something of their own: I enjoy making something
using chemistry that I can actually use. The students were
especially glad to take their finished soap home and to use

1536 Journal of Chemical Education Vol. 82 No. 10 October 2005 www.JCE.DivCHED.org


it. Any time you can use or take home what you make in
class you will be more interested in it.
In formulas 19, some students had difficulty recogniz-
ing trace. With all formulations, students wished the soap
would trace faster. Trace is reached in five to twenty min-
utes with formulas 19 whereas two hours are needed for for-
mulas 10 and 11.
Acknowledgments
I thank the students who tested the formulations; the
Chemistry Department, which provided funds; the spring
2004 organic chemistry students whose soaps appear in the
photographs; Russell K. Pace who took the photograph; and
Kevin Metzger who designed Figure 1.
W
Supplemental Material
Detailed instructions for students and notes for the in-
structor are available in this issue of JCE Online.
Note
1. Commercial surfactants used in this experiment will be clas-
sified as soaps, syndets, or combars based on the ingredients: soaps
are alkali salts of long chain fatty acids; syndets, or synthetic deter-
gents, are long alkane chains containing at least one functional
group; and combars or combination bars contain both soaps and
syndets.
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Journal of Chemical Education 1537