N AT U R A M O N T E N E G R I N A, P o d g o r i c a , 2 0 1 1 , 1 0 ( 3 ) : 3 3 5 - 3 4 6

PALM STEARIN IN THE SOAP-MAKING PROCESS

Sad M O U L A Y *, Ahmed C H A L A N E and Zahia O U A D - F E U L
Laboratoire de Chimie-Physique Molculaire et Macromolculaire, Facult des Sciences de lIngnieur,
Dpartement de Chimie Industrielle, Universit Saad Dahlab de Blida, Route de Souma, B. P. 270,
Blida 09000, Algeria.
* Corresponding author - E-mail: polymchemlab@hotmail.com

SYNOPSIS
Key words:
Palm stearin,
Soap,
Spent lye.

A laboratory scale soap-making process using the palm

stearin in a varying percentage of the fat was undertaken.
Analysis of the spent soap lye allowed the assessing of the
amounts (wt. %) of glycerol, sodium chloride, alkali, and
water. The results were within the range of the industrial
values. Soaps made with different concentrations of palm
stearin were analyzed in terms of the titre, sodium chloride,
total fatty matter, glycerol, and water. The results showed no
significant differences from the standard values.

INTRODUCTION
Soap is considered the oldest hygienic substance and has been used since the
Egyptian era (Tsujii, 1998). Because of the advent in the detergent industry, the
soap is nowadays used mostly as toiletry soap bar. However, the third world
countries still use soap abundantly for the fabric cleansing. It is important to point
out that the soap is also a component in the detergent formulation as a foam control
agent (Fujimoto, 1985). A historical survey of the soap-making reveals that the
natures of the fat and the alkaline substance employed in the saponification played
basic roles in the final performance of the soaps. Yet, the cleansing properties of
soap are more tightly bound to the nature of the used fatty matter than to the type of
the alkaline substance. To meet the criteria of the soap detergency such as firm
texture and foaming, the soap-making industries commonly manufacture their
household soaps employing a mixture of 75-85% of hard fats such as the beef tallow
or the palm oil and 15-25% of lauric fats such as the coconut oil or the palm kernel
oil. The luxury toilet soaps require a relatively higher content of lauric fat, but a skin
irritation may be caused when exceeding a certain percentage of this matter (lauric
acid).

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In a continuation of our research on the valorisation of natural products in the

soap and detergent making (Moulay et al., 2003; Moulay et al., 2005), we herein
report some results on the use of stearin as one of the fatty constituents in a
household soap. The consideration of the palm stearin as a raw material for soapmaking is of a great interest. Besides the palm olein, about 10% of solid stearin is
obtained by fractionation of palm oil after crystallization. There are many uses of this
stearin. For example, shaving soaps are prepared using a blend of 80% of stearin
and 20 % of lauric acid as fatty matter and the alkaline system NaOH/KOH in the
ratio of 1:3. Moreover, the palm stearin has been valorised as an ingredient in
shortenings, table, bakery and pastry margarine (Norlida et al., 1996). A chemical
interesterification of the palm stearin with vegetable oils and fats resulted in hard
fats that are employed in the soft margarines production (Petrauskaite et al., 1998;
deMan & deMan, 1995).

MATERIAL AND METHODS

The chemicals and the various indicators used in this work were purchased
from manufacturers Aldrich, Sigma, and Riedel deHan. The palm stearin, the beef
tallow and the coconut oil were supplied by ENCG (Entreprise Nationale des Corps
Gras, Algiers, Algeria). Deionized water was used in the soap-making process.
The different analyses of the fat and the palm stearin-based soaps were made
with the equipment included the following:
(i)
pHmeter LpH 230T;
(ii)
Refractometer, to determine the refractive index;
(iii)
Digital densimeter DM A48, to determine the density;
(v)
Tintometer Lovibond L14, to estimate the aspect of the fat;
(vi)
Electromagnetic agitator;
(vii)
Oven Memmert (30-120 C).
F AT

ANALYSES

E XPERIMENTAL

ESTIMATION OF

A CID V ALUE , AV

In a 250ml round-bottomed flask, 30-40 ml of neutralized ethyl alcohol was

added to 1g of fat. The alcoholic solution was titrated with 0.326 N ethanolic solution
of KOH, in the presence of phenolphthalein as an indicator. The acidity expressed
as the percentage of palmitic acid was estimated using Equation 1:

Acidity =

V xN
x
1000

336

M
w

x 100
[1]

Moulay et al.: P A L M S T E A R I N I N S O AP M A K I N G P R O C E S S

V is the volume of KOH consumed in ml; N is the normality of the solution of

KOH, 0.326 N; M is the molecular weight of palmitic acid, 256 g/mole; w is the
sample weight in grams, 10.1881g.
The acid value was determined as described by Norris (1965), Equation 2, or
according to DIN 53 402, Equation 3.

AV = 2 x Acidity

[2]

V x N x 56.1
w

AV =

[3]

E XPERIMENTAL ESTIMATION OF S APONIFICATION V ALUE , SV

In a 250ml round-bottomed flask equipped with a reflux condenser, 2g of fat
and 25ml of 0.5 N ethanolic solution of KOH were charged. The mixture was stirred
under reflux for 1h. The excess of KOH was back titrated with 0.5 N aqueous
solution of H 2 SO 4 in the presence of 4% solution of phenolphthalein as indicator.
The estimation of SV was provided by Equation 4:

SV =

(V 0 - V) x N x M
w

[4]

V 0 is the volume in ml of the H 2 SO 4 solution, for the blank test, 22 ml; V is the
volume in ml of the H 2 SO 4 solution, for the fat; N is the normality of the H 2 SO 4
solution, 0.5; M is the molecular weight of KOH, 56.1 g/mole; w is the sample
weight in grams, 2.0624g.
E XPERIMENTAL ESTIMATION OF I ODINE V ALUE , IV
Initially, the Wijs reagent was prepared by dissolving 12g of iodine
monobromide (IBr) in 1L of glacial acetic acid in an amber flask.
A 0.6g of fat was accurately weighed and charged into a 250ml flame-dried
amber flask. After addition of 10ml of chloroform, the system was cooled by
immersing it in an ice-bath in order to add 25ml of the Wijs reagent. The system was
allowed to stand for 3h at room temperature. A 25ml of a 100 g/L aqueous solution
of potassium iodide was then introduced and the mixture was stirred for 2h. Finally,
70ml of distilled water was added to the mixture. The titration of this mixture with 0.1
N solution of sodium thiosulfate, Na 2 S 2 O 3, in the presence of starch was performed
to estimate the excess of iodine. Equation 5 allowed the estimation of IV:

IV =

(V0 - V) x N x M
w

[5]

V 0 is the volume in ml of the Na 2 S 2 O 3 solution, for the blank test, 22ml; V is

the volume in ml of the Na 2 S 2 O 3 solution, for the fat; N is the normality of the
Na 2 S 2 O 3 solution, 0.1; M is the molecular weight of palmitic acid, 256 g/mole; w is
the sample weight in grams, 0.7365g.

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E XPERIMENTAL ESTIMATION OF U NSAPONIFIABLE M ATTER , UM

In a 250ml round-bottomed flask fitted with a reflux condenser, a mixture of 5g
of fat and 50ml of 1 N ethanolic solution of KOH was refluxed for 1h. After cooling
the mixture to room temperature, 50ml of distilled water were added. The whole
mixture was then poured into a separatory funnel and the flask was rinsed with 50ml
of petroleum ether. After vigorously shaking the funnel, the mixture was allowed to
stand for a phase separation.
The petroleum ether layer containing the unsaponifiable matter was withdrawn.
The soapy layer was rinsed twice with 50ml of petroleum ether. The extracts were
gathered, washed twice with 50ml of ethanol, and dried over anhydrous Na 2 SO 4 for
24h. Finally, the petroleum ether was evaporated to dryness and the residue was
weighed. The UM was estimated using the Equation 6:
[6]

UM =

w x 100
w0

w 0 is the sample weight, 5.4015g; w is the residue weight in grams.

E XPERIMENTAL ESTIMATION OF THE T ITRE
An amount of 70g of fat was mixed with 70 ml of ethanol and 40 ml of NaOH
(39 B) and the mixture was heated until saponification. The soap obtained was
dissolved in hot water and 50 ml of 20% aqueous solution H 2 SO 4 was added to give
the corresponding fatty acids. The mixture was then heated until an oily layer
formed. The system was afterwards transferred into a separatory funnel in order to
extract the organic layer which was washed with warm distilled water. The system
was allowed to decant for 2h, then the organic layer was filtered off.
The filtrate was introduced into a test tube fitted with an adequate thermometer
and the temperature was gradually lowered down; the temperature at which the first
crystal appeared corresponds to the titre of the fat.
P REPARATION

OF SOAP

Eleven soap formulations (F i ) were prepared as presented in Table 1. A

general procedure for their preparation is outlined below and consists of four steps:
saponification, boiling, washing, and fitting.
1. S APONIFICATION
In an appropriate beaker, 200g of fat consisting of 10% of coconut oil and 90%
of palm stearin/beef tallow are mixed with an amount of aqueous solution of NaOH
(35% concentration). The necessary weight of NaOH, W NaOH (g/Kg of fat), was
calculated from the saponification value of the mixture, SV mix , by computing
Equations 7 and 8.

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SVmix = (SVco x Wco + SVPS x WPS + SVBT x WBT ) (1 + 0.3 %)

[7]

WNaOH = SVmix x 40 / 56.1

[8]

Where the subscripts SV CO , SV PS , and SV BT are the saponification values of

coconut oil, palm stearin, and beef tallow, respectively; W CO, W PS , and W BT , their
corresponding weight percentages, and 0.3% is the excess of NaOH used.
The mixture was stirred under nitrogen atmosphere while heated at 65C until
a homogeneous phase was observed. The saponification was controlled by the use
of phenolphthalein as indicator. The reaction was over when red colour appeared
and lasted for 10 min.
Afterwards, the salting-out process was carried out by adding an appropriate
quantity of 40% NaCl solution to the mixture. While the spent lye was drained off
and recuperated, the top soapy layer was worked up in the following steps.
Table 1: Physico-chemical characteristics of the used fats.

Parameters

Palm stearin

Coconut oil

Beef tallow

SV (mg/g)

200

259

185

M*

280.50

216.60

307.25

AV (mg/g)

0.24

8.30

6.72

EV (mg/g)

199.76

250.70

178.28

IV (mg/100g)

24

38

H 2 O (%)**

0.04

0.05

0.97

UM (%)

0.36

0.28

0.50

0.9087 (30 C)

0.919 (24 C)

0.892 (51 C)

1.447

1.448

1.471

T (C)

52

22

40

Aspect***

0.8R/3Y

2.5R/10Y

1.4R /10Y/0.6B

40

* M is the mean molecular weight calculated as (56.1/SV)1000.

** Moisture was estimated as a weight loss of a fat sample at 1052 C.
** The letters R, Y, and B stand for the red, yellow, and blue colour, respectively

2. B OILING
A small amount of 35% NaOH solution was added to the soapy paste obtained
in the saponification step, and the system was vigorously agitated under nitrogen
atmosphere and heated at 65 C for an additional time of 4h.
3. W ASHING
Sequential washings of the boiling product with water allowed adjusting both
the percentages of NaOH and NaCl to their ranges.

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4. F ITTING
A volume of water was carefully added to the soapy paste in sequential
portions to induce dissolution. A foaming was observed, and a small amount of ethyl
alcohol was added to suppress it. The system was allowed to stand for four days at
room temperature, the period within which the soap was formed at the top layer.
A NALYSES

OF THE SPENT LYE

F REE CAUSTIC ALKALI

To an aliquot of 10 ml of the spent lye, 50 ml of distilled water and few drops
of phenolphthalein solution were added. The neutralization was performed with 0.1 N
H 2 SO 4 . The free caustic alkali (% NaOH) was estimated by Equation 9.
Alkali (%) = (0.4 V) / w

[9]

V is the volume of 0.1 N H 2 SO 4 solution, in ml, necessary for the

neutralization, and w is the sample weight in grams.
F REE SODIUM CHLORIDE
Mother liquor was prepared by diluting 2 ml of spent lye with 250ml of
deionized water in a flask. To an aliquot of 10 ml were added 50ml and few drops of
10% potassium chromate solution as indicator, and the solution obtained was
titrated with 0.1 N silver nitrate solution to the endpoint. The percentage of NaCl
present in the spent lye is calculated using Equation 10.
NaCl (%) = V 5.85

[10]

V is the volume of the 0.1 N silver nitrate solution at the endpoint.

G LYCEROL CONTENT
A volume of 2ml of spent lye was diluted with 50ml of distilled water in the
presence of few drops of bromocresol blue. The solution was then neutralized with
0.1N H 2 SO 4 followed by addition of sodium hydroxide solution until the yellowish
colour turned purple. Potassium periodate (1.4g) was then introduced into the
solution, and the whole system was heated at 40C and stirred until complete
dissolution. Propylene glycol (3ml) was injected into the solution which was
neutralized with 0.1N sodium hydroxide solution. The percentage of glycerol present
in the spent lye was computed from Equation 11.
Glycerol (%) = (0.92 V) / w

[11]

V is the volume in ml of the 0.1N NaOH solution necessary for the

neutralization; w is the sample weight in grams.

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A NALYSES

OF THE SOAP FORMULATIONS ,

FI

T OTAL FATTY MATTER

The total fatty matter (TFM) was estimated using Equation 12
(100- X)
1.08

% TFM =

[12]

Where 100 is the percentage by weight of the soap and X is the percentage of
water. X was estimated as follows: An evaporating dish containing 10g of soap was
placed in the oven at the temperature of 105C until a constant weight. The
percentage of water present in the soap was calculated using Equation 13.
Water (%) =

W1 - W2

x 100

W1 - W0

[13]
W 0 is the weight of the evaporating dish; W 1 is the weight of the soap
sample/dish before drying; W 2 is the weight of the soap sample/dish after drying.
F REE CAUSTIC ALKALI
In a 250 ml round-bottomed flask equipped with a reflux condenser, 10g of
soap and 100 ml of neutralized ethanol (80% v:v) were charged. The system was
heated in a sand bath until a homogeneous phase was observed. The mixture was
cooled to room temperature and titrated with 0.1 N ethanolic solution of H 2 SO 4 in the
presence of phenolphthalein. The alkali was estimated as % of Na 2 O using Equation
14.
[14]
0.04 x V x N x 100 x 31
Na2O (%) =
w
40
40 and 0.040 are the molecular weight of NaOH in g and mg, respectively; V is
the volume of the solution of 0.1 N H 2 SO 4 in ml; w is the weight of sample in grams;
31 is the equivalent mass of Na 2 O.
F REE SODIUM CHLORIDE
An amount of 10 g of soap was dissolved in 50 ml of hot water. A few millilitres
of 20% H 2 SO 4 and few drops of the methyl orange solution were added to the soap
solution which was heated until the colour turned rose. After cooling to room
temperature, the solution was filtered off and transferred into a 250 ml flask; water
was then added to make 250 ml solution. An aliquot of 100 ml was withdrawn and
poured into a 250 ml Erlenmeyer flask, and the H 2 SO 4 excess was neutralized with
concentrated sodium hydroxide solution. The neutralized solution was titrated with
0.1 N silver nitrate solution in the presence of few drops of 10% potassium chromate
solution as indicator; at the endpoint, the colour changed to red brick. The
percentage of sodium chloride present in the soap was estimated by Equation 15.
NaCl (%) =

V x 5.85
w

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V is the volume of 0.1 N silver nitrate solution in ml at the endpoint; w is the

soap sample in grams.
T ITRE
The same procedure for the determination of the titres of fats was used for the
titre of the palm stearin-based soap. The titre was estimated using Equation 16.
TS = x1TPS + x2TBT + x3TCO

[16]

Where x 1 , x 2 , and x 3 are the weight fractions of the palm stearin, the beef
tallow, and the coconut oil, respectively; T PS , T BT , and T CO are their respective titres.
I ODINE VALUE
The iodine values, IV, were computed form the additive Equation 17.
IVS = x1IVPS + x2IVBT + x3IVCO

[17]

IV PS , IV BT , and IV CO are the iodine values of the palm stearin, the beef tallow,
and the coconut oil, respectively.
P ARTITION COEFFICIENT , K G
K G was computed via Equation 18 using the data of Tables 2 and 3.

( [glycerol]

+ [water]) soap

( [glycerol]

+ [water])

KG =

[18]
lye

Where ([glycerol] + [water]) soap and ([glycerol] + [water]) lye are the sum of
glycerol and water contents (%) in soap and spent lye, respectively.
W IGNER S CONSTANT , K S
The constant K s was determined according to the empirical Wigners equation
(Equation 19).
[NaCl] soap

= 1 - KS

[NaCl] lye

TFM

[19]

100

Where [NaCl] soap and [NaCl] lye are the percentages of salt (as NaCl) in the
soap and the spent lye, respectively, and are drawn from Tables 2 and 3. TFM is the
total fatty matter (%) of the soap taken from Table 3.

RESULTS AND DISCUSSION

The physico-chemical properties of the fats used including moisture content,
acid value (AV) and acidity, unsaponifiable matter (UM), saponification value (SV),

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ester value (EV), iodine value (IV), total fatty matter (TFM), free caustic alkali
content, density, colour, and titre (T) were experimentally determined. The results of
the different analyses are summarized in Table 1. The fact that the palm stearin is
composed of mainly palmitic acid (50-74%), therefore considered as hard oil, makes
it a suitable substitute to the beef tallow. Thus, the saponification reaction was
carried out using 10% of coconut oil and 90% of palm stearin/beef tallow; the
amount of sodium hydroxide required for the saponification was estimated as
reported (Moulay et al., 2005) using the SVs of the fats and their weight
percentages. The results are actually in the range of the known values (Woollatt,
1985; Davidsohn and Milwidsky, 1987). After the saponification process, the spent
soap lyes were analyzed and the results are gathered in Table 2. The contents in
NaCl, alkali (NaOH), glycerol, and water were found to vary with stearin
concentration but in a non systematic fashion. Yet, the estimated values are within
the range of the standard ones (Woollatt, 1985; Davidsohn and Milwidsky, 1987).
Table 2: Composition of the spent soap lyes.

Run

Stearin (%)*

NaCl (%)

Alkali (%)
(%Na 2 O)***

Glycerol (%)

Water (%)**

F1

10

0.32 (0.248)

10.02

79.66

F2

10

11.5

0.28 (0.217)

7.36

80.86

F3

20

11

0.23 (0.178)

11.38

77.39

F4

30

13

0.33 (0.255)

9.20

77.47

F5

35

08

0.40 (0.310)

11.80

79.80

F6

40

9.5

0.50 (0.387)

12.88

77.12

F7

50

10.20

0.11 (0.085)

10.58

89.11

F8

60

12.50

0.24 (0.186)

10.01

77.25

F9

70

10.50

0.35 (0.271)

9.84

79.31

F 10

80

09

0.31 (0.240)

8.46

82.23

F 11

90

12

0.36 (0.279)

12.50

75.14

* % Palm stearin + % beef tallow = 100

** Estimated as 100-(% NaCl + % alkali + % glycerol)
*** % Na 2 O = % Alkali 0.775

Table 3 compiles the analyses results of the soap produced at different palm
stearin extents. It can be noticed that the titre of the soap, T S , increases with an
increasing palm stearin concentration. The best soap formulations with respect to
the recommended titre (38-42 C) are the runs 2-4 corresponding to 10-35% of palm
stearin. The experimentally estimated titres presented in Table 3 are closer to the

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theoretical ones. As shown in Table 3, the iodine values IV of the soap would be
lowered as the palm stearin content increased in the fat blend.
The salt content was found to be lower than unity and this finding is in a fair
agreement with the recommended salt concentration (<1%). Moreover, the total fatty
matter, TFM, was found to be in the range of 64-70% which is an acceptable value.
The lower salt concentrations coupled with the TFM values would indicate that the
actual saponification product is a neat soap and that the liquidation process, a
critical saponification step, was successful. The free caustic alkali of the soap was
about 0.05-0.11% suggesting an efficient washing process during the manufacture,
and this caustic amount would not cause a hand irritation.
Another parameter of the soap-making process is the partition coefficient, K G ,
which is the glycerol repartition between the final soap (neat soap) and the spent
lye. For a successful process, this factor was reported to be 0.4 (Woollatt, 1985). As
can be seen in Table 4, the value for K G is within 0.326 and 0.385 which is closer to
the commonly found one.
Table 3: Physico-chemical characteristics of the soap.

Run

IV
T (C) NaCl (%)
(mg/100g) S

Alkali (%)
(% Na2O)

TFM (%) Water (%)

Glycerol*
(%)

F1

34.9

38.2

0.30

0.11 (0.085)

69.55

23.88

6.16

F2

33.5

39.4

0.33

0.09 (0.070)

67.49

27.11

4.98

F3

32.1

40.6

0.39

0.04 (0.030)

68.12

26.44

5.01

F4

30.7

41.8

0.48

0.09 (0.070)

67.03

27.60

4.80

F5

30.0

42.4

0.54

0.12 (0.093)

66.70

27.96

4.68

F6

29.3

43.0

0.45

0.06 (0.046)

64.71

30.11

4.58

F7

27.9

44.2

0.40

0.08 (0.062)

66.93

27.11

4.88

F8

26.5

45.4

0.47

0.10 (0.077)

68.06

26.49

4.88

F9

25.1

46.6

0.35

0.05 (0.038)

70.41

22.90

6.29

F10

23.7

47.8

0.59

0.07 (0.054)

69.37

25.08

4.89

F11

22.3

49.0

0.44

0.07 (0.054)

67.21

27.41

4.87

*% Glycerol = 100 (% NaCl + % alkali + % water + % TFM)

It is worth mentioning that the present experimental results were in line with
the Wigners rule, also called the 66% rule. Indeed, the constant K S in the
empirical equation of Wigner, Equation 19, was found in the range of 1.374-1.471 as
given in Table 4. These values are not far from the common one, 1.50-1.53.

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Table 4: KS and KG from different soap-making runs.

Run

F1

KS

1.395

KG

0.335

F2
1.439
0.364

F3
1.416

F4
1.437

0.354

0.374

F5

F6

1.398

1.472

0.356

F7
1.436

0.385

0.326

F8

F9

1.414

1.373

0.360

0.327

F10

F11

1.347

1.434

0.330

0.368

The palm stearin-based soap was a white material with a pleasant smell;
usually, the neat soap is devoid of smell and the use of a fragrant is always
necessary for the toilet soap-making. Soap, made wholly of beef tallow as the hard
fat component, frequently tends to give off rancidity in the long run. Thus, a
substitution extent of the tallow by the palm stearin may screen this drawback.
The cleaning performance tests were assessed on a tomato paste-dirtied white
fabric according to a described process (Moulay et al., 2003; Moulay et al., 2005).
The results were acceptable as the degree of whiteness of the washed fabric
specimen was high. Besides, the water solutions of the different soap samples gave
copious foaming, indicating a high washing performance.

CONCLUSION
In conclusion, the palm stearin is, in addition to its cost effectiveness, a good
tallow substitute in the soap-making as revealed by the properties of the soap. Also,
the soap-making process using the palm stearin as a part of hard fat showed that
the different parameters of the process were within the norms.
ACKNOWLEDGEMENTS
The authors are indebted to the ENCG firm (Entreprise Nationale des Corps Gras, Algiers)
for their supply of fats. We greatly thank the ENCG technicians for their helpful discussion.

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Received: 8 February 2011.

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