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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 occurs in one week in the cold process, and a couple hours in
history (1, 2) of soap, the industrial process of saponifica- the semiboiled process. The byproduct glycerin is retained
tion (35), and laboratory-ready experiments (613). The ex- in both methods. As some individuals find soap dehydrates
periments and those in organic laboratory textbooks have the skin, the presence of the humectant glycerin in the fin-
described the hot (610, 1416) and cold (10, 11) processes ished soap is advantageous.
for making opaque soap, eq 1,
Soap Formulation
O
O Fats and Oils
+
R O M
R O HO Commercial manufacturers use 17% excess fat (17) to
+ reduce the harshness of soap, to produce a dense creamy
O O lather, and to leave the skin feeling smooth and soft (18).
MOH
The formulations in this article use 5% excess fat. Effective
R O R
+
O M + HO soaps are made from a mixture of fats and oils because each
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 Supplemental MaterialW). For example lauric acid, the pre-
R O M dominant fatty acid in coconut oil (48.0%), produces a hard
(1)
fats and oils soap glycerin and effective cleanser with a fluffy lather. Unfortunately, lauric
(triacylglycerols) (carboxylates) acid does not condition the skin nor provide a stable lather;
therefore other fatty acids are warranted. Table 3 in the
and the conversion of commercially-available, opaque soaps Supplemental MaterialW gives the percent maximum recom-
into transparent (12) or solid potassium soaps (13). mended usage of fats and oils based on therapeutic benefits
In the experiments, typically one fat or oil (79, 11, 14 (24), cost, and fatty acid content. Beeswax (25) and coconut
16) is saponified with a stoichiometric excess of sodium hy- and palm oils (19) harden an otherwise soft soap. Manufac-
droxide (7, 8, 10, 1416). In the hot process, excess base is turers preferentially use coconut and palm oils because they
usually removed by filtration and rinsing of the soap precipi- are cheap and they produce an effective cleanser with fluffy
tated by the addition of aqueous sodium chloride (68, 14, lather (19).
15). Alternatively, Evans suggests adding coconut oil or di-
lute hydrochloric acid to the melted soap, exposing thin pieces Base, Water, and Scent
of solid soap to air, or beating the melted soap (10) to re- After selecting the fats and oils, the mass of required so-
move the excess base. In the latter two methods the base dium hydroxide is determined from the saponification (SAP)
reacts with the CO2 in the air, eq 2: 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
2NaOH(aq) + CO2(g) Na2CO3(s) + H2O(l) (2)
fat or oil and the percent of this component in the soap (see
Hill (9) and Lehman (16) rinse the filtered soap with water. Table 3 in the Supplemental MaterialW) (20, 22, 23, 28).
As soap containing excess base will irritate the skin (10), stu- Because SAP values are defined as the number of milligrams
dents have been prohibited from using the prepared soap. of potassium hydroxide per one gram fat or oil (29), the SAP
Students will be able to use soaps from this experiment as value of the soap is converted to mass of potassium hydrox-
they contain 5% excess fat. ide per gram fat or oil and subsequently multiplied by the
This experiment introduces students to the industrial total mass of fats and oils. Since potassium hydroxide is typi-
method of making opaque (formulas 18) or transparent soap cally used to make liquid soap while sodium hydroxide is used
(formulas 10 and 11) and formulations chemistry (formula to make solid soap, the required mass of potassium hydrox-
9). It can accompany lectures on personal care products or ide is converted to mass of sodium hydroxide. Because com-
lipids in a first-year or organic chemistry course. The proce- mercial soap contains excess fats and oils to moisturize the
dures can be used independently or, as one reviewer noted, skin, the mass of sodium hydroxide is multiplied by 0.95.
as a multiweek project. Over three weeks, students can make The mass of deionized water and scent are determined by
opaque soap in one two-hour period or transparent soap in multiplying the total mass of fats and oils by 0.375 and
one three-hour period, and formulate a soap and test its ef- 0.0125, respectively; if the manufacturer of the scent pro-
fectiveness alongside commercial surfactants. vides a usage rate, then this value should be used instead.
Opaque and transparent soaps are made using the cold
and semiboiled processes, respectively. In both processes, Additional Ingredients
premelted fats and oils are combined with base. In the Deionized water is used to make soap because it pre-
semiboiled process, heat is applied. Complete saponification 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. and stearic acid. Supermarkets sell canola, corn, olive, saf-
Deionized water also minimizes discoloration caused by im- flower, and sunflower oils, lard, sugar, and whipping cream.
purities. Note that the coconut and palm oils should be melted prior
Milk in soap moisturizes the skin and produces a mild, to use, as they separate on cooling. Replace any fats and oils
creamy, and rich consistency (31). Based on fat content, that burn on melting.
whole milk (4%), half-and-half (10.518%), light cream (18
30%), light whipping cream (3036%), and heavy whipping Cold-Process Soap (Formulas 18)
cream (3640%) are commonly used (32). In this article, Combine and stir the deionized water and half of the
whipping cream is used for its high fat content. When re- sodium hydroxide (Table 1) in a 250-mL beaker on a mag-
placing all water with milk, the milk must be frozen prior to netic stirring plate. After the solid has dissolved, add the re-
the addition of base (31), otherwise proteins in the milk de- maining sodium hydroxide. Stir and heat all fats and oils until
nature causing a tan-to-brown-colored soap (33). When us- melted in a 400-mL beaker on a magnetic stirring hot plate.
ing small quantities of milk, as in formulas 2, 4, 6, and 8, Slowly pour the base solution into the beaker of fats and oils
the milk is added following saponification. and stir until trace is observed. To test for trace, dip a stir-
To reduce the formation of fibrous crystals and to make ring rod into the mixture and wave it over the surface. If the
transparent soap, castor oil, ethanol, glycerin, and sugar are drizzled material leaves a pattern on the surface before sink-
added to the hot soap solution (34). The molded soap is also ing, the soap has traced. Add scent and cream and stir the
cooled slowly in the open. mixture until trace is reached again. Pour the soap into molds
or weighing boats (either four, 3 in. 3 in.-square boats or
Surfactant Tests 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
The prepared soap and commercial surfactants are tested harden the soap.
for pH, feel, and effectiveness (ability to lather) in hard and
soft water. The transparency of formulas 10 and 11 is con- Student-Formulated Cold-Process Soap (Formula 9)
firmed by reading text written with a 14-point font through After selecting the fats and oils and performing the nec-
a 1/4 in. slice of soap (35, 36). essary calculations, prepare the soap as described in cold-pro-
cess soap.
Experimental Procedure
Transparent Soap (Formulas 10 and 11)
Chemicals Combine the fats, oils, and alcohol in a 500-mL three-
Majestic Mountain Sage (37) and From Nature With necked round-bottom flask equipped with a condenser and
Love (38) supply most fats and oils. Craft stores sell beeswax 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.

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
Figure 1. Student-prepared transparent soaps. (This image is shown using chemistry that I can actually use. The students were
in color on p 1427.) especially glad to take their finished soap home and to use

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In the Laboratory

it. Any time you can use or take home what you make in Maibach, H. I., Eds.; Marcel Dekker: New York, 2001; p
class you will be more interested in it. 493.
In formulas 19, some students had difficulty recogniz- 18. Piso, Z.; Winder, C. A. Soap, Syndet and Soap/Syndet Bar
ing trace. With all formulations, students wished the soap Formulations. In Soap Technology For The 1990s; Spitz, L.,
would trace faster. Trace is reached in five to twenty min- Ed.; American Oil Chemists Society: Champaign, IL, 1990;
utes with formulas 19 whereas two hours are needed for for- p 217.
mulas 10 and 11. 19. Cavitch, S. M. The Chemistry of Soapmaking. In The
Soapmakers Companion; Storey: Pownal, VT, 1997; p 238.
Acknowledgments 20. Davidsohn, J.; Better, E. J.; Davidsohn, A. The Fatty Raw
Materials: Introduction. In Soap Manufacture; Interscience
I thank the students who tested the formulations; the Publishers: New York, 1953; Vol. I, pp 206211.
Chemistry Department, which provided funds; the spring 21. Use of Natural Fats and Oils in Cosmetics. In Baileys Indus-
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photographs; Russell K. Pace who took the photograph; and Sons: New York, 1996; Vol. 5, pp 366367.
Kevin Metzger who designed Figure 1. 22. Altman, P. L.; Dittmer, D. S. Fats and Oils: Properties and
Composition. In Biology Data Book, 2nd ed.; Federation of
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Supplemental Material American Societies for Experimental Biology: Bethesda, MD,
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Note 24. Cavitch, S. M. An Overview of Soapmaking Oils. In The
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1. Commercial surfactants used in this experiment will be clas- 118.
sified as soaps, syndets, or combars based on the ingredients: soaps 25. Cavitch, S. M. Answers to Soapmakers Most-Asked Ques-
are alkali salts of long chain fatty acids; syndets, or synthetic deter- tions. In The Soapmakers Companion; Storey: Pownal, VT,
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