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Cold- Process Synthesis and Properties of Soaps Prepared from Different

Triacylglycerol Sources

Article · January 2010

DOI: 10.4314/njbas.v18i2.64350

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 Available online at http://ajol.info/index.php/njbas/index ISSN 0794-5698
Nigerian Journal of Basic and Applied Science (2010), 18(2): 315-321

Cold- Process Synthesis and Properties of Soaps Prepared from Different Triacylglycerol
Sources

A.A. Warra1*, L.G. Hassan2, S.Y. Gunu1 and S.A. Jega1

1
Department of Biochemistry, Kebbi State University of Science and Technology, P.M.B 1144,
Aliero, Nigeria.
2
Department of Pure and Applied Chemistry, Usmanu Danfodiyo University, P.M.B 2346,
Sokoto, Nigeria.
[Author of Correspondence: aliyuwarra@yahoo.com]

ABSTRACT: This study was conducted to find out how different fats and oils produce soaps of
different characteristics. It describes cold-process saponification using different fats and oils. Shea nut
oil (SAP value:183.9mgKOH/g), groundnut oil (SAP value:187.7mgKOH/g) and Tallow (SAP value:
140.3mgKOH/g) were used. Colour, texture, lathering and cleansing power of the prepared soaps
were analyzed. shea butter soap had the best lathering capacity. The groundnut oil soap had the most
effective cleaning power .The soaps were also recommended for household use .This activity was also
provided to share a delight in chemistry with senior school students and to actively engage them in
hands-on-active learning.
Key words: cold-process, saponification, triacylglycerols and properties

INTRODUCTION harshness of soap, to produce a dense creamy

Soap is a mixture of sodium or potassium salts lather, and to leave the skin feeling smooth and
of various naturally occurring fatty acids. Soap soft (Mabrouk, 2005).The formulation in this
is a substance of ancient origin, the paper uses 10% excess fat and oils.
manufacture of which according to Gunstone et This paper describes the cold-process
al,(1986)has evolved from primitive beginnings saponification and use hands-on-active learning
into a sophisticated chemical process. Evidence approach. This strategy is vital in teaching
of soap making dates back to the Egyptian and students laboratory techniques and inquiry
Babylonians. Several millennia ago crude skills. Laboratory exercises should be used
mixture of animal fats and the alkaline plant ash frequently throughout a science course to
were found to generate crude soaps which promote science learning (Chiappetta and
lathered and cleaned effectively (Phansteil et al, Koballa, 2006). Therefore activities of this kind
1998). Through the centuries, there have been should be encouraged in schools. This project
other times when people were able to make was carried out in the Chemistry Laboratory of
soap using sodium or potassium salts as is done Haliru Abdu senior Arabic Secondary School,
recently. When the Germans tribesmen of Jega, Kebbi State, Nigeria.The fats and oils
Caesar’s time boiled goat tallow with potash used were obtained from Jega central market.
leached from the ashes of wood fires, they were While the sodium hydroxide (analytical grade)
carrying out the same chemical reaction as one used as the alkali in the hydrolysis of the fats
carried out on a tremendous scales by modern and oils were obtained from laboratory store in
soap manufacture by hydrolysis of glycerides the department of chemistry, Haliru Abdu
(acylglycerols) (Morrison and Boyd, 2004). Senior Arabic secondary School, Jega.
The commonest oils used in soap making are
lard and tallow from animal sources, coconut, MATERIALS AND METHODS
palm and olive oil from vegetable source Preparation of Tallow from Animal Fat: The
(Pavila et al,1982).The Commercial preparation of fats for soap making consist of
manufacturers use 1-7% excess fat to reduce the cleaning the fats to be free from impurities
315
 Warra et al.; Cold- Process Synthesis and Properties of Soaps Prepared from Different Triacylglycerol Sources

contained in it. This is called rendering. To titrated with 0.5 M HCl until a pink colour
render the fat, all meat tissues were removed. indicated the end point.
The fat was then placed in a stainless steel pot The expression for saponification value (S.V.)
containing 500cm3 of distilled water. The is given by: S.V = 56.1N (V0-V1)/M, where V0
mixtures were boiled until the fat melted. The = the volume of the solution used for blank test;
solution was allowed to cool down and left VI = the volume of the solution used for
overnight. The next day the fat had solidified determination; N = actual normality of the HCl
and floated to the top forming a layer of clean used; M = Mass of the sample.
fat. All the impurities being denser as the fat Iodine value: 0.4g of the sample was weighed
remained in water underneath the fat. into a conical flask and 20ml of carbon tetra
Saponification Procedure: For each soap chloride was added to dissolve the oil. Then
formulation 200g/dm3 NaOH solution was 25ml of Dam’s reagent was added to the flask
poured directly into the stainless steel container using a safety pipette in fume chamber. Stopper
(pot) containing the fat and oil in the ratio 1:1 was then inserted and the content of the flask
(v/v). When the mixture of tallow and was vigorously swirled. The flask was then
groundnut oil was used the fat/oil mixture placed in the dark for 2 hours 30 minutes. At
contains 3:2 (v/v). The fats/oil was warmed the end of this period, 20ml of 10% aqueous
gently and was poured into the stainless steel potassium iodide and 125ml of water were
soap making pot followed by the alkali solution added using a measuring cylinder. The content
to form an intimate mix and then stirred was titrated with 0.1M sodium-thiosulphate
frequently for 10-15 minutes using wooden solutions until the yellow colour almost
stirrer. Perfume and other ingredients were disappeared. Few drops of 1% starch indicator
added as additives at the last time before was added and the titration continued by adding
pouring the saponification mixture into thiosulphate drop wise until blue coloration
moulds. After pouring, the soap was allowed to disappeared after vigorous shaking. The same
harden by air-drying for 24hours to obtain the procedure was used for blank test and other
soap bars, according to the method reported by samples. The iodine value (I.V) is given by the
Warra,(2009) and the soap bars were then expression: I.V = 12.69C (V1-V2)/M, where C =
observed for colour, texture, lathering and Concentration of sodium thiosulphate used; V1
cleaning power. = Volume of sodium thiosulphate used for
Note: To reduce the harshness of soap which blank; V2 = Volume of sodium thiosulphate
may be cause by excess sodium hydroxide, used for determination, M = Mass of the
10% excess fat and oil was used in the sample.
formulations (super fatting). Acid value: 100 ml of neutral ethyl alcohol was
Analytical method: Three different fats and heated with 10g of oil or fat sample in a 250ml
oils were used for this research; shea nut oil, beaker until the mixture began to boil. The
Tallow, and Ground nut oil. The chemical heating was stopped and the solution was
analysis of the oils were carried out using the titrated with N/10 KOH solution, using two
methods adopted by Diamond, et al (1973), drops of phenolphthalein as indicator with
Bassir,(1978), Plummer,1987, Association of consistent shaking for which a permanent pink
Official Analytical Chemists(AOAC) ,(1990) colour was obtained at the end point.
Akpan et al,(2006), and Bahl, et al, (2007), The Acid value was calculated using the
with modifications. expression
Saponification value:About 2g of the oil A.V = 0.56 x No. of ml. N/10 KOH used.
sample was added to a flask with 30ml of pH Determination: The pH was determined
ethanolic KOH and was then attached to a using a pH meter (827 pH lab Model). 10g of
condenser for 30 minutes to ensure that the the soap shavings was weighed and dissolved in
sample is fully dissolved. After sample has distilled water in a 100ml volumetric flask. This
cooled 1ml of phenolphthalein was added and was made up to prepare 10% soap solution in
line with literature report (Dalen and
316
 Nigerian Journal of Basic and Applied Science (2010), 18(2): 315-321

Mamza,2009) The electrode of the pH meter Test for effectiveness in cleaning: To

was inserted into the solution. The pH reading determine the cleaning property of the prepared
was recorded. The steps were repeated using soaps, a drop of oil was placed on four separate
soaps produced from each fat or oil. strips of filter paper. The filter papers with the
Foam ability Tests: About 2.0g each of soap oil spot were immersed in a separate test tubes
(shavings) was added to a 500ml measuring containing soap solution (2g soap
cylinder containing 100ml of distilled water as shavings/100ml distilled water) each was
reported by Isah, (2006) for synthetic detergent. shaken vigorously for 1 minute The filter
The mixture was shaken vigorously so as to papers were removed and rinsed with distilled
generate foams. After shaking for about 2 water and the degree of cleanliness in each
minutes, the cylinder was allowed to stand for filter paper was observed.
about 10 minutes. The height of the foam in the
solution was measured and recorded. The steps RESULTS AND DISCUSSION
were repeated using soaps produced from each The results of the chemical analysis carried out
fat or oil. on the oils are presented in the Table 1.

Table 1: Chemical analysis of oils used

SAP value( Iodine value (I2/100g) Acid value
mgKOH/g) (mgKOH/g)
Tallow(Animal fat) 140.3 44.3 16.1
Shea-nut oil 183.9 54 .1 10.5
Ground nut oil 187.7 84.8 3.83
The values are mean of three replicates.

Chemical Analysis: The physicochemical Tallow includes; saponification

values are relatively similar to the literature value(140.3mgKOH/g) which is lower than
values. For the indigenous crude shea fat : 185.00mgKOH/g in Cyperus esculentus oil
saponification value 183.7, was obtained ,the (Hassan et al,2007) and 213mgKOH/g in neem
value is lower than that of olive oil(192.0 ) and seed oil (Akpan,1999) and 253.2mgKOH/g in
sunflower oil(188.7) but higher than that of coconut oil (Oshinowo,1987) which are also
beeswax(93.0) which are commonly used in oils used in soap making. This is higher than
soap making (Mabrouk,2005).This indicates 56.10mgKOH/g value obtained for cassia
that the oil could be used in soap making since siamea oil also recommended for soap making
its saponification value fall within the range of (Hassan et al, 2005). 44.3I2/100g was obtained
these oils. It could also substantially be used in as the iodine value of Tallow, this value is
the preparation of cosmetic products (Warra, relatively comparable to that of Avocado seed
2009). Oils with high saponificaton values such oil (42.6) which is used in soap making (Sani
as coconut oil (257.0) and palm oil (199.1) are and Hassan ,2007). Tallow is one of the
better used in soap making (Abayeh et al , principal fatty acid material used in soap
1998). Some soap manufacturers blend their making. It contains mainly the palmitic, stearic
oils with coconut oil (with high saponification and oleic acids (Pavila et al, 1982). The acid
value) to get yield of better quality soaps. value (which indicates the amount of free fatty
Iodine value, 54.1(less than 100) was obtained acids present in the Tallow) was 16.1mgKOH/g
which shows that the oil belongs to class of relatively similar to the value reported for
Non-drying oils which are useful in the Albizia lebbeck,L seed oil (Hassan et al,2005)
manufacture of soaps (Kochhar, 1998) . The recommended for soap making. This value also
Acid value (10.5) authenticates the raw material shows that the oil is advantageous for soap
and conforms relatively to 10.49 3mgKOH/g making (Owoyale,1987) For groundnut oil the
reported by Oyedele (2002), which signifies a saponification value was 187.7 comparable to
minimum purity. The values obtained for the value obtained for corn oil (187.0)
317
 Warra et al.; Cold- Process Synthesis and Properties of Soaps Prepared from Different Triacylglycerol Sources

(Zhang,et al,1986) .Even though ground nut oil the manufacture of soaps ( Kochhar 1998 )
is a known edible oil its high saponification .3.83mgKOH / g was obtained as the acid
value is an indication of its suitability for soap value which is comparable with 4mg KOH /g
making. The value is lower than that of olive recommended by a Cordex Alimenterius
oil (192.1) ( Mabrouk, 2005) but higher than commission for ground nuts ( Abayeh et al,
that of bees wax ( 93.0 )which are all used in 1998 ) The value is lower than 16.83mgKOH /
soap making. The ground nut oil has an iodine g for cassia siamea( Hassan at et al, 2005) but
value of 84.8. This value is comparable to higher than (1.84 ) reported for sesame seed oil
(81.8) the value obtained for olive oil ( Almustapha et al, 1995 ) which are used in
(Almustapha et al, 1995) and 85.00I2 / 100g soap making.
value of Cyprus esculents oil (Hassan et al, Table 2: Foam height of soaps prepared.
2007). High iodine value justifies utilization of Prepared Soaps Height of foam
the oil in soap and shampoo productions ( over water(cm)
Hassan et al, 2007 ) groundnut oil is an
Animal fat soap 2.5
example of non drying oils whose iodine
numbers are less than 100 ( Kochhar, 1998 ) Shea nut oil soap 2.7
they have the advantage of not undergoing Ground nut oil soap 2.3
The values are mean of three replicates
oxidation to form a film, hence are useful in
Table 3: Soap Types, Lathering and Cleaning properties.
Soap Fat/oil Ingredient Type of Colour Texture Lathering Cleaning Possible
Formul Soap of soap Uses
ation
1 Mixture of Perfume Designer Cream Soft Effective Washing
tallow and ---
g/oil
2 Shea nut Perfume Multi- White Very Excellent More Antiseptic
oil purpose hard effective for bathing,
washing
3 Mixture of Honey, Toilet Brown Hard Effective Antimicrobi
tallow and bees wax --- al
g/nut oil and perfume soap for
bathing
4 Tallow Sour lemon Laundry Milk Hard Very Effective Washing
(Animal and Good
fat) Perfume
5 Groundnu Perfume Laundry Milk Soft Good Most effective Washing
t oil

Physical Analysis: Table 2 shows the results of the color of the parent oil, similar to the
physical analysis carried out on the soap findings reported by Warra, et al (2009b) with
samples produced. The result indicates that exception of formulation 3 which maintained
colours of the soap formulation 1-5 were found brown colour due to the addition of brown
to be cream, white, brown and milk colour ingredients (Honey and beeswax). For
respectively. The variation in colours could be the texture of the soap, the variations could be
due to the degree of unsaturation of the fatty or depends on the nature of their fatty acids
acids. Increase in double bonds causes increase composition length of hydrocarbon chain and
in intensity of colour (Mabrouk, 2005). Another nature of double bonds in the carboxylic acid
possibility is that in all the formulations portion of the fat or oil. Soap made from shea
glycerol was retained, salting-out was not butter oil is the hardest followed by soap from
employed since it was cold-process method tallow. Iodine number is another probable
used; therefore all the soap samples maintained explanation for this variation. Oils with very
318
 Nigerian Journal of Basic and Applied Science (2010), 18(2): 315-321

low iodine number yields soaps that are hard antiseptic. The sugar concentration plus other
(Pavila et al,1982).Shea butter has the lowest factors including low pH, hydrogen peroxide
iodine number compared to groundnut oil that and the flavonoids, phenolics and terpenes
produce soft soap. As a result of their make honey an antimicrobial agent (Mizrahi,
molecular structures soaps are capable of 2008).One student asked why we included sour
dispersing oils and similar water –insoluble lemon in the ingredient for soap formulation 4?
substances (Katz, 2000). The cleansing power Sour lemon is used to get rid of the odour in
and lather produced by different soap can be animal fat. Most fats (greases used in making
explained based on the fatty acids composition soaps are smelly and they produce smelly
of oil used in soap formulation, it was reported soaps. In order to get rids of smells in soap
that, lauric acid and myristic acid, which are all animal fats are treated by adding lemon juice,
saturated fatty acids produces soap with fluffy vinegar or sour milk as described by Norman
lather and high cleansing power (phansteil et al, (2007). We measured the pH of our prepared
1998). However, the observed difference in the soaps. Soap being salt of strong base and weak
cleansing power and nature of lather formed in acids should be weakly alkaline in aqueous
the soap formulation may be due to the method solution. But soap with free alkaline (PH 11 -
use in the soap preparation in addition the 14) can cause damage to skin. Hence pH of 9-
nature of fatty acid composition of the fat or oil 11 and 3-5 are considered as high and low
used. levels respectively by NAFDAC a regulatory
Table 4. pH of prepared soaps. Agency in Nigeria (Umar, 2002). All the
Soap formulations pH students formulated soaps were below the pH of
1 8.3 9. Our prepared soaps are closer to the pH of
2 8.0 between 7 and 9 which is better.
3 7.8 Conclusion: From this experiment the
4 8.5 students have increased their knowledge of the
5 8.8 organic chemistry of soaps. Students were
The values are mean of three replicates engaged in conversations and have expressed
their feelings such as “I learn how to combine,
The students prepared soaps were all made by many fats and oils to get soaps”. The students
the same method .The majority of students also appreciated how the modern day chemistry
preferred the soap made from shea butter oil for when blended with old tradition, accuracy and
some reasons; it can serve asa multipurpose knowledge of the right ingredients and suitable
soap, it can be used for washing because of its methods yield the desired results. Another
excellent lathering and more effective when student remarked that he enjoyed the soaps;
tested for its cleaning capability. Its use for they wash more effectively than most
bathing is related to its exceptional healing commercial soaps he used to purchase from the
properties for the skin, shea butter contains market.
vitamin A and E which are important for
Fig. 1 Cold-processed soap samples
treatment of number of skin conditions
(American Shea butter Institute, 2008). Shea
butter has been used for centuries in Africa for
its unsurpassed ability to maintain and protect
the skin from environmental damage (Warra, et
al, 2009). Shea butter oil is abundantly
obtainable in most part of Kebbi state making it
easier for students to obtain and prepare their
home made soaps. The choice of honey soap
(formula 3) as antimicrobial soap (or bathing)
lies in its unique property of being
antimicrobial agent as well as powerful
319
 Warra et al.; Cold- Process Synthesis and Properties of Soaps Prepared from Different Triacylglycerol Sources

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