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Formulating Neem Oil Emulsion as Potent


Agrochemicals Using a Binary Emulsifier System
a a
Shrinivas C. Kothekar & Shamim A. Momin
a
Department of Oils , Oleochemicals and Surfactants, Institute of Chemical Technology ,
Matunga, Mumbai, India
Published online: 31 May 2008.

To cite this article: Shrinivas C. Kothekar & Shamim A. Momin (2008) Formulating Neem Oil Emulsion as Potent
Agrochemicals Using a Binary Emulsifier System, Journal of Dispersion Science and Technology, 29:6, 919-929, DOI:
10.1080/01932690701783630

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Journal of Dispersion Science and Technology, 29:919–929, 2008
Copyright # Taylor & Francis Group, LLC
ISSN: 0193-2691 print/1532-2351 online
DOI: 10.1080/01932690701783630

Formulating Neem Oil Emulsion as Potent


Agrochemicals Using a Binary Emulsifier System
Shrinivas C. Kothekar and Shamim A. Momin
Department of Oils, Oleochemicals and Surfactants, Institute of Chemical Technology,
Matunga, Mumbai, India

Neem oil is a natural pesticide and has excellent insecticidal properties. Hence, in this study the
efforts have been made to formulate the Neem oil emulsions which would be used as agrochem-
icals. In order to formulate stable Neem oil emulsions, a binary emulsifier system of Hydol-6
(Polyoxyethylene Alkyl Ether-6 moles of ethylene oxids) and Hydol-10 (Polyoxyethylene Alkyl
Ether-10 moles of ethylene oxids) were employed. Stability of Neem oil emulsions as a function of
concentration of Neem oil, Hydol-6, Hydol-10, the amount of water, homogenization speed, and
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homogenization time was studied in depth. Apart from this, it was observed that the nature of
water also affects the stability of the emulsions. The concentration of Neem oil in the stable
emulsions was also found to exhibit the varying effects on the properties like dispersibility,
spreading power, and droplet size of the emulsions. Larvasidal effects of stable Neem oil
emulsions were examined.
Keywords Dispersibility, droplet size, hydol-6, hydol-10, larvacidal activity, neem oil
emulsions, spreading power

INTRODUCTION Neem oil, has been rated as the most potent naturally
Most of the neurotoxic insecticides which are being used occurring insect feeding deterrent[5,6] and has generated
globally are damaging to the environment and=or pose a wide academic and industrial interests.[7,8] Azadirachtin
threat to public health via food residues, groundwater con- (AZA) functions as a natural insect control agent because
tamination, or accidental exposure. Although the risks of its antifeedant as well as insect growth regulatory
associated with the proper use of these pest control materi- properties.[9]
als should be minimal, the exaggerated perception of these AZA is dually advantageous as a natural insect control
risks among the public is increasing demand for alternative agent because it possesses both antifeedant and insect
and safe environmentally sound pest controlling materials. growth regulatory properties against insects. Over 200 spe-
One such source available for natural insecticides is the cies of pest insects are known to be susceptible to the bioac-
Neem oil. Neem oil is obtained from the seeds of Neem tivity of AZA.[2] The lack of acute toxicity in lab animals
tree.[1–2] Azadirachta indica, A. Juss. (Neem) of the family and lack of evidence for chronic effects in animals, com-
Meliaceae, is native to the Indian subcontinent. Neem, bined with a long historical use of Neem oil preparations
today, is grown in many Asian countries and in tropical in traditional medicines in India should make a Neem
regions of the western hemisphere.[3] Native of Indian sub- oil-based insecticide a highly acceptable alternative to
continent, this fast-growing shade tree is widely cultivated synthetic neurotoxin- type insecticides.[4]
in Africa, Australia, the Carribean region, and Central Advantages of Neem oil preparations over pure AZA
and South America.[4] Azadirachtin (C35H44O16), a tetra- include the presence of other potentially active constitu-
nortriterpenoid and major anti-insect active present in ents.[10,11] One derivative of Neem that may serve as a start-
ing point for the development of an insecticide is the oil
obtained from crushing of the dried seeds. Neem seed,
Received 14 May 2007; accepted 28 May 2007.
This work was supported by Unitop Industries Ltd. Mumbai, which contains approximately 40% oil, has the highest
India Ltd. by providing the gift samples of emulsifiers for concentrations of AZA. India currently produces over
research work. 80,000 metric tons of Neem oil annually. Aqueous emul-
Address correspondence to Shrinivas C. Kothekar and sions of Neem oil are efficacious against insects in field
Shamim A. Momin, Senior Research Fellow, Department of Oils, trials, which suggest that the crude Neem oil may be a use-
Oleochemicals and Surfactants, Institute of Chemical Tech- ful starting material for the development of Neem oil-based
nology, Matunga, Mumbai 400 019, India. E-mail: s_kothekar@
insecticides.[12–13]
yahoo.com, skothekar2007@rediffmail.com

919
920 S. C. KOTHEKAR AND S. A. MOMIN

Neem, like all other botanical preparations, will vary


considerably with respect to its active ingredients depend-
ing on thee genome of thee trees from which seed is col-
lected, the geographic area of origin and the variations in
environmental conditions.
The objective of the present study was to devise the
stable emulsions containing the high concentrations of
Neem oil and relatively low concentrations of emulsifiers
in deionized water as well as hard water. The stability stu-
dies were carried out at room temperature and extended
temperature as well. The stable emulsions were further
FIG. 2. Curve showing the variation of emulsifying power with
assessed for their insecticidal properties. change in concentration of Hydol-6.

MATERIALS AND METHODS


Neem oil (unrefined) was procured from local market
and the free samples of emulsifiers Hydol-6 and Hydol-10
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were supplied by the Unitop Industries (Mumbai, India).


Hard water of 340 ppm was prepared by adding a mixture
of hydrous calcium chloride and magnesium carbonate.

Analysis of Emulsifiers Hydol-6 and Hydol-10


Foaming Power and Foamability
Determination of foaming power and foamability was
performed by using the Bartsch (shaking test) method. FIG. 3. Curve showing the variation of emulsifying power with
Emulsifier solutions of different concentrations, that is, change in concentration of Hydol-6.
0.01%, 0.1%, 0.25%, 0.5%, and 1% were vigorously sha-
ken in a 100 mL graduated cylinder (20 mm inner diameter)
by hand, 30 times in 30 seconds, as uniformly as possible, respects, as described for the foaming power and foamabil-
and the foam volume was noted immediately. This reading ity except, to each 20 mL volume of the emulsifier solution
for foam volume was considered as the 0th minute (initial) 20 mL volume of the paraffin oil was added.
foam volume. The similar foam volumes were noted after
5, 10, 15, 20, 25, and 30 minutes. All the experiments were Surface Tension and Interfacial Tension Measurements
performed at ambient temperature, that is, 30C. Surface tension measurements for different emulsifier
solutions of different concentrations were carried out by
Emulsifying Power using a SL. NO- 163 tensiometer with Du-Nouy ring
The experimental procedure to determine the emulsify- method at controlled room temperature, that is, 30C.
ing power of emulsifiers of different concentrations, that Triplet tests were performed for each measurement and
is, 0.01%, 0.1%, 0.25%, 0.50%, and 1% was same in all the average of three readings was considered as the final

FIG. 1. Curve showing the variation of foamability with change in FIG. 4. Curve showing the variation of surface tension with change
concentration of Hydol-6 and Hydol-10. in concentration of Hydol-6 and Hydol-10.
NEEM OIL EMULSION AS POTENT AGROCHEMICALS 921

reading. Before the measurement, the platinum ring was


cleaned with a chromic acid mixture and washed thor-
oughly with twice-distilled water, then burned red using
the oxidizing portion of the flame of an alcohol burner.
Surface tensions of different emulsifier solutions were
measured for their various concentrations, that is, 0.01%,
0.1%, 0.25%, 0.50%, and 1%. The ring was hung from
the load cell and lowered about 5 mm below the surface
of the emulsifier solution placed in a glass-tub (30 mL vol-
ume), and held still for another 30 minutes. The ring was
pulled from the surface and the apparent surface tension
was recorded.
FIG. 5. Curve showing the variation of interfacial tension with The experimental procedure for determination of the
change in concentration of Hydol-6 and Hydol-10. interfacial tension of different emulsifier solutions and of
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TABLE 1
Formulation of Neem oil emulsions using Hydol-6 and Hydol-10 surfactants in deionized water
Neem oil Hydol-6 Hydol-10 Deionized Homogenizer Homogenization
Sr. no. (%) (%) (%) water (%) speed time Results
1 10 1 4 85 3000 rpm 60 minutes S
2 10 1 2 87 3000 rpm 60 minutes S
3 10 1 1 88 3000 rpm 60 minutes 0.5 ml CL
4 10 1 0.5 88.5 3000 rpm 60 minutes 1 ml CL
5 10 0.5 0.5 89 3000 rpm 60 minutes 1 ml CL
6 15 1 2 82 3000 rpm 60 minutes S
7 15 1 1 83 3000 rpm 60 minutes S
8 15 0.5 1 83.5 3000 rpm 60 minutes 0.5 ml CL
9 15 0.5 0.5 84 3000 rpm 60 minutes 2 ml CL
10 15 0.5 0.25 84.25 3000 rpm 60 minutes 2 ml CL
11 20 1 2 77 3000 rpm 60 minutes 1 ml CL
12 20 1 4 75 3000 rpm 60 minutes 1 ml CL
13 20 1 3.5 75.5 3000 rpm 60 minutes 1 ml CL
14 20 1 3 76 3000 rpm 60 minutes 1 ml CL
15 20 1 2.5 76.5 3000 rpm 60 minutes S
16 20 1 2.2 76.8 3000 rpm 60 minutes 1 ml OL
17 20 0.5 2.5 77 3000 rpm 60 minutes S
18 20 0.75 2.5 76.75 3000 rpm 60 minutes 0.5 ml CL
19 20 0.25 2.5 77.25 3000 rpm 60 minutes 0.5 ml CL
20 25 1 2 72 3000 rpm 60 minutes S
21 25 1 3 71 3000 rpm 60 minutes 7 ml CL
22 25 1 1.5 72.5 3000 rpm 60 minutes 0.5 ml OL
23 25 1 1 73 3000 rpm 60 minutes 2 ml CL
24 25 1 0.5 73.5 3000 rpm 60 minutes 2 ml CL
25 25 1 0.25 73.75 3000 rpm 60 minutes S
26 25 0.5 0.25 74.25 3000 rpm 60 minutes 3.5 ml CL
27 25 0.75 0.25 74 3000 rpm 60 minutes 6 ml CL
28 30 1 2 67 3000 rpm 60 minutes S
29 30 1 1 68 3000 rpm 60 minutes 4.5 ml CL
30 30 1 0.5 68.5 3000 rpm 60 minutes 7.5 ml CL
31 30 0.5 1 68.5 3000 rpm 60 minutes 7.5 ml CL
S.E.: stable emulsion; S: stable; CL: creamy layer.
922 S. C. KOTHEKAR AND S. A. MOMIN

different concentrations, that is, 0.01%, 0.1%, 0.25%, While optimization of different process parameters, homo-
0.50%, and 1% was same in all respects, as described for genization time, and speed of homogenization were taken
the surface tension measurements, except in the interfa- into consideration in order to make the process as econ-
cial tension measurement, equal quantities of emulsifier omical as possible.
solution and the paraffin oil were taken in a glass tub.
Also, the position of the platinum ring was adjusted at Analysis of Stable Emulsions
the interface of emulsifier solution and the paraffin oil. In the present research work, ‘‘creaming’’ was con-
sidered as the measure of unstability of an emulsion. When
Formulation of Emulsions there was no occurrence of creaming, the emulsion was
Neem oil emulsions were formulated by means of high considered as a stable emulsion.
speed homogenizer using 10–30% concentrations of Neem The droplet size of stable Neem oil emulsions was ana-
oil, 0.25–1% of Hydol-6, and 0.25–2.5% of Hydol-10. The lyzed by means of Coulter LS-230 particle size analyzer.
emulsions were prepared in deionized water as well as hard The dispersion power of the stable emulsion was analyzed
water of 340 ppm hardness. Initially, the homogenization by adding a minute drop of an emulsion into the water
time of above mentioned ingredients was fixed to 1 hour. (100 ml) contained in a measuring cylinder. The time
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TABLE 2
Formulation of Neem oil emulsions using Hydol-6 and Hydol-10 surfactants in hard water (340 ppm)
Neem oil Hydol-6 Hydol-10 Hard water Homogenizer Homogenization
Sr. no. (%) (%) (%) (%) speed time Results
1 10 1 2 87 3000 rpm 60 minutes S
2 10 1 1 88 3000 rpm 60 minutes S
3 10 1 0.5 88.5 3000 rpm 60 minutes S
4 10 1 0.25 88.75 3000 rpm 60 minutes 0.5 ml CL
5 10 0.5 0.5 89 3000 rpm 60 minutes 0.5 ml CL
6 10 0.25 0.5 89.25 3000 rpm 60 minutes 1 ml CL
7 15 1 2 82 3000 rpm 60 minutes 2 ml CL
8 15 1 1 83 3000 rpm 60 minutes S
9 15 1 0.5 83.5 3000 rpm 60 minutes S
10 15 1 0.25 83.75 3000 rpm 60 minutes S
11 15 0.5 0.25 84.25 3000 rpm 60 minutes 1.5 ml CL
12 15 0.25 0.25 84.5 3000 rpm 60 minutes S
13 20 1 2 77 3000 rpm 60 minutes 11 ml CL
14 20 1 0.5 78.5 3000 rpm 60 minutes 3 ml CL
15 20 1 0.25 78.75 3000 rpm 60 minutes 3 ml CL
16 20 0.5 0.25 80.25 3000 rpm 60 minutes S
17 20 0.25 0.25 80.5 3000 rpm 60 minutes 4 ml CL
18 25 1 2 72 3000 rpm 60 minutes 14 ml CL
19 25 1 1 73 3000 rpm 60 minutes 15 ml CL
20 25 1 0.5 73.5 3000 rpm 60 minutes 8.5 ml CL
21 25 1 0.25 73.75 3000 rpm 60 minutes 4 ml CL
22 25 0.5 0.25 74.25 3000 rpm 60 minutes S
23 25 0.25 0.25 74.5 3000 rpm 60 minutes 4.5 ml CL
24 30 1 2 67 3000 rpm 60 minutes 21 ml CL
25 30 1 1 68 3000 rpm 60 minutes 24 ml CL
26 30 1 0.5 68.5 3000 rpm 60 minutes S
27 30 1 0.25 68.75 3000 rpm 60 minutes 22.5 ml CL
28 30 0.5 0.25 69.25 3000 rpm 60 minutes 22 ml CL
29 30 0.25 0.25 69.5 3000 rpm 60 minutes 21 ml CL
30 30 0.25 3 66.75 3000 rpm 60 minutes 19.5 ml CL
31 30 0.25 2.5 67.25 3000 rpm 60 minutes 22.5 ml CL
S.E.: stable emulsion; S: stable; CL: creamy layer.
NEEM OIL EMULSION AS POTENT AGROCHEMICALS 923

TABLE 3
Optimization of homogenization speed and homogenizer time for Neem oil emulsions using Hydol-6 and
Hydol-10 surfactants in deionized water
Neem oil Hydol-6 Hydol-10 Deionized Homogenizer Homogenization
Sr. no. (%) (%) (%) water (%) speed time Results
S.E 1 10 1 2 87 3000 rpm 60 minutes S
1 10 1 2 87 3000 rpm 40 minutes S
2 10 1 2 87 3000 rpm 20 minutes 0.5 ml CL
3 10 1 2 87 2500 rpm 60 minutes S
4 10 1 2 87 2500 rpm 40 minutes 1 ml CL
5 10 1 2 87 2500 rpm 20 minutes 2 ml CL
6 10 1 2 87 2000 rpm 60 minutes 1 ml CL
7 10 1 2 87 2000 rpm 40 minutes S
8 10 1 2 87 2000 rpm 20 minutes 2.5 ml CL
S.E 2 15 1 1 83 3000 rpm 60 minutes S
1 15 1 1 83 3000 rpm 40 minutes 2 ml CL
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2 15 1 1 83 3000 rpm 20 minutes 4 ml CL


3 15 1 1 83 2500 rpm 60 minutes 3.5 ml CL
4 15 1 1 83 2500 rpm 40 minutes 3 ml CL
5 15 1 1 83 2500 rpm 20 minutes 3 ml CL
6 15 1 1 83 2000 rpm 60 minutes 2.5 ml CL
7 15 1 1 83 2000 rpm 40 minutes 2.5 ml CL
8 15 1 1 83 2000 rpm 20 minutes 3 ml CL
S.E 3 20 0.5 2.5 77 3000 rpm 60 minutes S
1 20 0.5 2.5 77 3000 rpm 40 minutes 2 ml CL
2 20 0.5 2.5 77 3000 rpm 20 minutes 2 ml CL
3 20 0.5 2.5 77 2500 rpm 60 minutes S
4 20 0.5 2.5 77 2500 rpm 40 minutes S
5 20 0.5 2.5 77 2500 rpm 20 minutes 2 ml CL
6 20 0.5 2.5 77 2000 rpm 60 minutes 1 ml CL
7 20 0.5 2.5 77 2000 rpm 40 minutes 1 ml CL
8 20 0.5 2.5 77 2000 rpm 20 minutes 2 ml CL
S.E 4 25 1 0.25 73.75 3000 rpm 60 minutes S
1 25 1 0.25 73.75 3000 rpm 40 minutes 2 ml CL
2 25 1 0.25 73.75 3000 rpm 20 minutes 4.5 ml CL
3 25 1 0.25 73.75 2500 rpm 60 minutes 5 ml CL
4 25 1 0.25 73.75 2500 rpm 40 minutes 5 ml CL
5 25 1 0.25 73.75 2500 rpm 20 minutes 5 ml CL
6 25 1 0.25 73.75 2000 rpm 60 minutes 4 ml CL
7 25 1 0.25 73.75 2000 rpm 40 minutes 5 ml CL
8 25 1 0.25 73.75 2000 rpm 20 minutes 4.5 ml CL
S.E 5 30 1 2 67 3000 rpm 60 minutes S
1 30 1 2 67 3000 rpm 40 minutes 4.5 ml CL
2 30 1 2 67 3000 rpm 20 minutes 5 ml CL
3 30 1 2 67 2500 rpm 60 minutes 5.5 ml CL
4 30 1 2 67 2500 rpm 40 minutes 5.5 ml CL
5 30 1 2 67 2500 rpm 20 minutes 6 ml CL
6 30 1 2 67 2000 rpm 60 minutes 2 ml CL
7 30 1 2 67 2000 rpm 40 minutes S
8 30 1 2 67 2000 rpm 20 minutes 2 ml CL
S.E.: stable emulsion; S: stable; CL: creamy layer.
924 S. C. KOTHEKAR AND S. A. MOMIN

TABLE 4
Optimization of homogenization speed and homogenizer time for Neem oil emulsions using Hydol-6 and
Hydol-10 surfactants in hard water (340 ppm)
Neem oil Hydol-6 Hydol-10 Hard water Homogenizer Homogenization
Sr. no. (%) (%) (%) (%) speed time Results
S.E 1 10 1 0.5 88.5 3000 rpm 60 minutes S
1 10 1 0.5 88.5 3000 rpm 40 minutes 3 ml CL
2 10 1 0.5 88.5 3000 rpm 20 minutes 4 ml CL
3 10 1 0.5 88.5 2500 rpm 60 minutes 2.5 ml CL
4 10 1 0.5 88.5 2500 rpm 40 minutes 3 ml CL
5 10 1 0.5 88.5 2500 rpm 20 minutes 4.5 ml CL
6 10 1 0.5 88.5 2000 rpm 60 minutes 2.5 ml CL
7 10 1 0.5 88.5 2000 rpm 40 minutes 2.5 ml CL
8 10 1 0.5 88.5 2000 rpm 20 minutes 3 ml CL
S.E 2 15 0.25 0.25 84.5 3000 rpm 60 minutes S
1 15 0.25 0.25 84.5 3000 rpm 40 minutes 3 ml CL
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2 15 0.25 0.25 84.5 3000 rpm 20 minutes 3.5 ml CL


3 15 0.25 0.25 84.5 2500 rpm 60 minutes 4 ml CL
4 15 0.25 0.25 84.5 2500 rpm 40 minutes 5 ml CL
5 15 0.25 0.25 84.5 2500 rpm 20 minutes 4.5 ml CL
6 15 0.25 0.25 84.5 2000 rpm 60 minutes 5 ml CL
7 15 0.25 0.25 84.5 2000 rpm 40 minutes 5 ml CL
8 15 0.25 0.25 84.5 2000 rpm 20 minutes 5.5 ml CL
S.E 3 20 0.5 0.25 80.25 3000 rpm 60 minutes S
1 20 0.5 0.25 80.25 3000 rpm 40 minutes 6 ml CL
2 20 0.5 0.25 80.25 3000 rpm 20 minutes 6 ml CL
3 20 0.5 0.25 80.25 2500 rpm 60 minutes 6.5 ml CL
4 20 0.5 0.25 80.25 2500 rpm 40 minutes 7 ml CL
5 20 0.5 0.25 80.25 2500 rpm 20 minutes 7.5 ml CL
6 20 0.5 0.25 80.25 2000 rpm 60 minutes 11.5 ml CL
7 20 0.5 0.25 80.25 2000 rpm 40 minutes 12 ml CL
8 20 0.5 0.25 80.25 2000 rpm 20 minutes 16 ml CL
S.E 4 25 0.5 0.25 74.25 3000 rpm 60 minutes S
1 25 0.5 0.25 74.25 3000 rpm 40 minutes 16 ml CL
2 25 0.5 0.25 74.25 3000 rpm 20 minutes 18 ml CL
3 25 0.5 0.25 74.25 2500 rpm 60 minutes 19 ml CL
4 25 0.5 0.25 74.25 2500 rpm 40 minutes 18 ml CL
5 25 0.5 0.25 74.25 2500 rpm 20 minutes 18.5 ml CL
6 25 0.5 0.25 74.25 2000 rpm 60 minutes 20 ml CL
7 25 0.5 0.25 74.25 2000 rpm 40 minutes 15 ml CL
8 25 0.5 0.25 74.25 2000 rpm 20 minutes 15 ml CL
S.E 5 30 1 0.5 68.5 3000 rpm 60 minutes S
1 30 1 0.5 68.5 3000 rpm 40 minutes 15 ml CL
2 30 1 0.5 68.5 3000 rpm 20 minutes 25 ml CL
3 30 1 0.5 68.5 2500 rpm 60 minutes 25 ml CL
4 30 1 0.5 68.5 2500 rpm 40 minutes 22 ml CL
5 30 1 0.5 68.5 2500 rpm 20 minutes 25.5 ml CL
6 30 1 0.5 68.5 2000 rpm 60 minutes 24 ml CL
7 30 1 0.5 68.5 2000 rpm 40 minutes 26 ml CL
8 30 1 0.5 68.5 2000 rpm 20 minutes 26.5 ml CL
S.E.: stable emulsion; S: stable; CL: creamy layer.
NEEM OIL EMULSION AS POTENT AGROCHEMICALS 925

TABLE 5
Analysis of dispersibility of stable Neem oil emulsions formulated in deionized water
Neem oil Hydol-6 Hydol-10 Deionized Homogenize-r Homogenizatio-n
Sr.No. (%) (%) (%) water (%) speed time Dispersibility
1 10 1 4 85 3000 rpm 60 minutes 56 seconds
2 10 1 2 87 3000 rpm 60 minutes 57 seconds
3 10 1 2 87 3000 rpm 40 minutes 56 seconds
4 10 1 2 87 2500 rpm 60 minutes 51 seconds
5 10 1 2 87 2000 rpm 20 minutes 63 seconds
6 15 1 2 82 3000 rpm 60 minutes 107 seconds
7 15 1 1 83 3000 rpm 60 minutes 143 seconds
8 20 1 2.5 76.5 3000 rpm 60 minutes 155 seconds
9 20 0.5 2.5 77 3000 rpm 60 minutes 160 seconds
10 20 0.5 2.5 77 2500 rpm 60 minutes 101 seconds
11 20 0.5 2.5 77 2500 rpm 40 minutes 92 seconds
12 25 1 2 72 3000 rpm 60 minutes 121 seconds
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13 25 1 0.25 73.75 3000 rpm 60 minutes 147 seconds


14 30 1 2 67 3000 rpm 60 minutes 52 seconds
15 30 1 2 67 2000 rpm 40 minutes 56 seconds

consumed by an emulsion drop to get uniformly dispersed replications for each concentration of emulsion. After 24
into the water was the measure of the dispersion power of hours the mortality of each group was counted in terms
that emulsion. In case of the spreading power of an emul- of ‘‘percentage of mortality.’’
sion sample, a fine droplet of it was carefully placed at the
center of the circle made on the leaf of a coconut tree and
time required by the droplet to spread across the diameter RESULTS AND DISCUSSION
of the circle was taken as a measure of the spreading power Foamability
of that Neem oil emulsion formulation. Figure 1 indicates the variation of foamability of Hydol-
6 and Hydol-10 with the increasing concentration range
Larvacidal Activity 0.01%, 0.1%, 0.25%, 0.5%, and 1%. As can be seen from
This test was carried out at room temperature, that is, the results, out of these two surfactants Hydol-6 showed
30C in 500 ml capacity glass beakers each containing the best foamability, that is in the range of 61.33% to
250 ml of distilled water. Twenty larvae (third stage=early 88.89% at all concentrations as compared to Hydol-10,
forth stage) of culex and anopheles were added in to the which on the contrary showed relatively poor foamability
beaker containing 0.5%, 1%, 1.5%, and 2% of the single in the range of 19.23% to 58.82% at the same concentra-
emulsion at a time. Each bioassay was performed in three tions. As can be seen from Figure 1, for the foamability

TABLE 6
Analysis of dispersibility of stable Neem oil emulsions formulated in hard water (340 ppm)
Neem oil Hydol-6 Hydol-10 Homogenizer Homogenization
Sr.no. (%) (%) (%) Hard water speed time Dispersibility
1 10 1 1 88 3000 rpm 60 minutes 52 seconds
2 10 1 0.5 88.5 3000 rpm 60 minutes 56 seconds
3 15 1 1 83 3000 rpm 60 minutes 87 seconds
4 15 1 0.5 83.5 3000 rpm 60 minutes 90 seconds
5 15 1 0.25 83.75 3000 rpm 60 minutes 95 seconds
6 15 0.25 0.25 84.5 3000 rpm 60 minutes 95 seconds
7 20 0.5 0.25 80.25 3000 rpm 60 minutes 126 seconds
8 25 0.5 0.25 74.25 3000 rpm 60 minutes 118 seconds
9 30 1 0.5 68.5 3000 rpm 60 minutes 142 seconds
926 S. C. KOTHEKAR AND S. A. MOMIN

of Hydol-6 and hydol-10, the best values were obtained the higher absorption ability of Hydol-6 and Hydol-10 at
with Hydol-6 as compared to the Hydol-10. This would the interface of oil and water which reduced the interfacial
be due to the reason that Hydol-10 was not able to generate energy to higher extent and hence, produced a negative
the sufficient surface area required by minimizing the sur- interfacial tension. In other words, these two emulsifiers
face tension of the solution. The other probable reason produced a condition which was favorable for an increase
behind this would be, due to the higher surface tensions in the interfacial area.
of Hydol-10; it failed to increase the surface area to ease
the foam generation, and hence showed poor foaming Surface Tension and Interfacial Tension
power and foamability. On the other hand, Hydol-6 Figures 4 and 5 indicate the variation of surface tension
yielded the best foamability results due to its ability to and interfacial tension with the increasing concentration
create the necessary surface area needed and also because range 0.01%, 0.1%, 0.25%, 0.5%, and 1% of Hydol-6
of its lower surface tensions, it could be able to increase and Hydol-10, respectively. As shown in the results,
the surface area to ease the foam generation. Hydol-6 was found to be more efficient as compared to
Hydol-10 in reducing the surface tension and interfacial
Emulsifying Power tension of water. In case of different concentrations of
The emulsifiers show their emulsifying power by adsorb- Hydol-6 analyzed, the surface tension and interfacial
ing at the interface of the water and oil and reducing the tension values were obtained in the range of 29.5 to 30.1
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interfacial energy. It is the existence of this interfacial dynes=cm and 0.9 to 1.9 dynes=cm, respectively. On the
energy that is essentially responsible for the instability of other hand, in case of Hydol-10, the surface tension and
an emulsion, since the large increase in interfacial area interfacial tension values were in the range of 33 to 33.9
upon the formation of emulsion droplets will cause an dynes=cm and 2.6 to 4.5 dynes=cm respectively. The better
increase in the free energy of the system. The lower surface tension and interfacial tension reducing ability of
stabilization of emulsion can also be explained by micelli- Hydol-6 would be because of its slow micellization in
zation of emulsifiers in water. Figures 2 and 3 indicate water. On the other hand, the fast micellization of
the variation of emulsifying power with the increasing con- Hydol-10 would be the reason for its higher surface tension
centration range 0.01%, 0.1%, 0.25%, 0.5%, and 1% of and interfacial tension values.
Hydol-6 and Hydol-10, respectively. The analysis of these
emulsifiers showed that the emulsifying power of these Stability Studies of Emulsions
two surfactants was almost same, that is in the range of The stability studies of emulsions forms an essential part
30 to 1735 seconds. In other words, the emulsifying power of the present research work. An emulsion which is very
of these two emulsifiers was almost comparable as can be much capable of re-tenting the internal phase in its finely
seen from Figures 2 and 3, respectively. This is because, dispersed state possesses the best stability in terms of

TABLE 7
Analysis of spreading power of stable Neem oil emulsions formulated in deionized water
Neem oil Hydol-6 Hydol-10 Deionized Homogenizer Homogenization
Sr. no. (%) (%) (%) water (%) speed time Spreading power
1 10 1 4 85 3000 rpm 60 minutes 7 seconds
2 10 1 2 87 3000 rpm 60 minutes 9 seconds
3 10 1 2 87 3000 rpm 40 minutes 8 seconds
4 10 1 2 87 2500 rpm 60 minutes 8 seconds
5 10 1 2 87 2000 rpm 20 minutes 9 seconds
6 15 1 2 82 3000 rpm 60 minutes 16 seconds
7 15 1 1 83 3000 rpm 60 minutes 18 seconds
8 20 1 2.5 76.5 3000 rpm 60 minutes 22 seconds
9 20 0.5 2.5 77 3000 rpm 60 minutes 23 seconds
10 20 0.5 2.5 77 2500 rpm 60 minutes 22 seconds
11 20 0.5 2.5 77 2500 rpm 40 minutes 21 seconds
12 25 1 2 72 3000 rpm 60 minutes 29 seconds
13 25 1 0.25 73.75 3000 rpm 60 minutes 31 seconds
14 30 1 2 67 3000 rpm 60 minutes 37 seconds
15 30 1 2 67 2000 rpm 40 minutes 36 seconds
NEEM OIL EMULSION AS POTENT AGROCHEMICALS 927

TABLE 8
Analysis of spreading power of stable Neem oil emulsions formulated in hard water (340 ppm)
Neem oil Hydol-6 Hydol-10 Hard water Homogenizer Homogenization
Sr.no. (%) (%) (%) (%) speed time Dispersibility
1 10 1 1 88 3000 rpm 60 minutes 10 seconds
2 10 1 0.5 88.5 3000 rpm 60 minutes 12 seconds
3 15 1 1 83 3000 rpm 60 minutes 14 seconds
4 15 1 0.5 83.5 3000 rpm 60 minutes 14 seconds
5 15 1 0.25 83.75 3000 rpm 60 minutes 13 seconds
6 15 0.25 0.25 84.5 3000 rpm 60 minutes 13 seconds
7 20 0.5 0.25 80.25 3000 rpm 60 minutes 15 seconds
8 25 0.5 0.25 74.25 3000 rpm 60 minutes 19 seconds
9 30 1 0.5 68.5 3000 rpm 60 minutes 21 seconds

shelf-life. Therefore, an emulsion can be considered stable hard water was added such that the total formulation will
as long as there is no separation of internal phase. Appear- be 100% by weight. Initially, the homogenization speed
Downloaded by [Umeå University Library] at 00:50 10 October 2014

ance of creaming as a ‘‘layer’’ generally is considered as a and homogenization time were kept as 3000 rpm and 60
measure of instability of an emulsion. Hence, in the pre- minutes, respectively (Tables 1 and 2). Once, the stable
sent research studies the emulsions which did not show emulsions were obtained using 10%, 15%, 20%, 25%,
any creaming were considered as the ‘‘stable’’ emulsions. and 30% oil phase of Neem oil, efforts were taken to
Formulation of Neem oil emulsions using Hydol-6 and reduce the other parameters like homogenization speed
Hydol-10 using deionized water as well as hard water of and homogenaization time to reduce the overall process
340 ppm hardness are shown in Tables 1 and 2, respect- cost (Tables 3 and 4).
ively. The emulsions were prepared by varying the concen-
trations of Neem oil, deionized=hard water, Hydol-6, and Analysis of Dispersibility, Spreading Power, and
Hydol-10. Apart from this, the formulation studies were Droplet Size of Stable Neem Oil Emulsions
also carried out by considering homogenizer speed and After formulating the stable emulsions of Neem oil in
homogenization time parameters. The Neem oil emulsions deionized=hard water (Tables 1 and 2) and optimizing
were formulated by varying the oil phase from 10% to the process parameters like homogenization speed and
30%. Other ingredients like Hydol-6 and Hydol-10 were homogenization time (Tables 3 and 4), only those emul-
added on trial and error basis. The quantity of deionized= sions which were overall cost-effective were selected for

TABLE 9
Analysis of droplet size of stable Neem oil emulsions formulated in deionized water
Neem oil Hydol-6 Hydol-10 Deionized Homogenizer Homogenization
Sr. no. (%) (%) (%) water (%) speed time Droplet size
1 10 1 4 85 3000 rpm 60 minutes 0.910 mm
2 10 1 2 87 3000 rpm 60 minutes 0.668 mm
3 10 1 2 87 3000 rpm 40 minutes 1.060 mm
4 10 1 2 87 2500 rpm 60 minutes 0.933 mm
5 10 1 2 87 2000 rpm 20 minutes 1.089 mm
6 15 1 2 82 3000 rpm 60 minutes 0.906 mm
7 15 1 1 83 3000 rpm 60 minutes 1.197 mm
8 20 1 2.5 76.5 3000 rpm 60 minutes 0.986 mm
9 20 0.5 2.5 77 3000 rpm 60 minutes 1.199 mm
10 20 0.5 2.5 77 2500 rpm 60 minutes 1.141 mm
11 20 0.5 2.5 77 2500 rpm 40 minutes 1.398 mm
12 25 1 2 72 3000 rpm 60 minutes 1.327 mm
13 25 1 0.25 73.75 3000 rpm 60 minutes 2.156 mm
14 30 1 2 67 3000 rpm 60 minutes 1.233 mm
15 30 1 2 67 2000 rpm 40 minutes 1.660 mm
928 S. C. KOTHEKAR AND S. A. MOMIN

TABLE 10
Analysis of droplet size of stable Neem oil emulsions formulated in hard water (340 ppm)
Neem oil Hydol-6 Hydol-10 Hard water Homogenizer Homogenization
Sr. no. (%) (%) (%) (%) speed (rpm) time Droplet size (mm)
1 10 1 1 88 3000 rpm 60 minutes 0.876 mm
2 10 1 0.5 88.5 3000 rpm 60 minutes 0.932 mm
3 15 1 1 83 3000 rpm 60 minutes 0.986 mm
4 15 1 0.5 83.5 3000 rpm 60 minutes 1.004 mm
5 15 1 0.25 83.7 3000 rpm 60 minutes 1.710 mm
6 15 0.25 0.25 84.5 3000 rpm 60 minutes 0.985 mm
7 20 0.5 0.25 80.2 3000 rpm 60 minutes 1.934 mm
8 25 0.5 0.25 74.2 3000 rpm 60 minutes 2.072 mm
9 30 1 0.5 68.5 3000 rpm 60 minutes 1.859 mm

the further analysis like dispersibility, spreading power, 1.398 mm (Table 9) and 0.932 mm to 2.072 mm (Table 10),
Downloaded by [Umeå University Library] at 00:50 10 October 2014

and droplet size measurements (Tables 5, through 10). respectively. It was noticed that the dispersibility and the
The dispersibility of stable Neem oil emulsions formulated spreading power was increased with increase in the Neem
with deionized water and hard water was found to be in the oil concentration in case of the Neem oil emulsions formu-
range of 51 seconds to 160 seconds (Table 5) and 52 sec- lated with deionized water as well as hard water. But, this
onds to 142 seconds (Table 6), respectively. The spreading pattern of linearity was not observed in case of the droplet
power of stable Neem oil emulsions formulated with deio- size of the Neem oil emulsions formulated with deionized
nized water and hard water was found to be in the range of water as well as hard water.
7 seconds to 36 seconds (Table 7) and 10 seconds to 21 sec-
onds (Table 8), respectively. Similarly, the droplet size of Larvacidal Activity
stable Neem oil emulsions formulated with deionized water
The larvacidal activity (as percentage of mortality of lar-
and hard water was found to be in the range of 0.668 mm to
vae) of various Neem oil emulsions formulated in deionized
water as well as hard water is reported in Tables 11 and 12,
respectively. The percentage of mortality of different
TABLE 11 emulsions varied widely irrespective of the concentration
Percentage of mortality of larvae using various stable of Neem oil that was used in a particular emulsion. It
emulsions formulated in deionized water was observed that the percentage of mortality of larvae
% Mortality of larvae was less when 0.5% of the Neem oil emulsion was
Sample no.
Emulsion concentration 0.5% 1% 1.5% 2%
1 58 72 88 96 TABLE 12
2 57 72 88 96 Percentage of mortality of larvae using various stable
3 57 72 87 96 emulsions formulated in hard water (340 ppm)
4 57 72 87 96 % Mortality of larvae
Sample no.
5 58 72 87 96
Emulsion concentration 0.5% 1% 1.5% 2%
6 64 77 90 97
7 64 77 90 97 1 55 69 85 91
8 68 81 92 99 2 55 69 85 91
9 68 81 91 99 3 61 73 88 95
10 68 81 92 99 4 61 73 88 94
11 68 81 92 100 5 66 79 91 97
12 74 85 97 100 6 67 79 91 97
13 74 85 97 100 7 67 81 94 100
14 81 89 100 100 8 72 84 96 100
15 81 89 100 100 9 77 87 10 100
Note: Please refer Table 9 for the composition of various emul- Note: Please refer Table 10 for the composition of various
sions enlisted in Table 11. emulsions enlisted in Table 12.
NEEM OIL EMULSION AS POTENT AGROCHEMICALS 929

employed. On the contrary, when the concentration of an [2] Arnason, J.T., Philogene, B.J.R., and Morand, P. (1989) In
emulsion was increased the percentage of mortality of Insecticides of plant origin; ACS Symposium Series 387;
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centage of mortality of larvae was almost 100% when [3] Sidhu, O.P., Kumar, V., and Behl, H.M. (2003) J. Agri. Food
Chem., 51: 910–915.
2% concentration of Neem oil emulsion was tested against
[4] Koul, O., Amanai, K., and Ohtaki, T. (1990) J. Insect
the larvae. From the results shown in Tables 11 and 12, it
Physiol., 33: 103–108.
firmly can be said that as the concentration of Neem oil in [5] Ruscoe, C.N.E. (1972) Nat. New Biol., 236: 159–160.
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activity also increases. Tetrahedron Lett., 25: 4729–4732.
[7] Balandrin, M.F., Klocke, J.A., Wurtele, S., and Bollinger,
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Washington, DC; pp. 206–219.
but other parameters like the emulsifier system, the nature
[9] Yamasaki, R.B. and Klocke, J.A. (1987) J. Agri. Food Chem.,
of water, speed of homogenization and the time of
35: 467–471.
homogenization are equally important. Without imple- [10] Kraus, W., Baumann, S., Bolel, M., Keller, U., Klenk, A.,
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menting the proper emulsifier system it is very difficult to Pohnl, H., and Schwinger, M. In Natural Pesticides from
obtain the stable Neem oil emulsions. The concentration the Neem Tree (Azadirachta indica A. Juss) and Other Trop-
of Neem oil employed in the emulsion formulations ical Plants, Proceedings of the Third International Neem
strongly affects the properties like dispersibility, spreading Conference, Nairobi, Kenya, edited by H. Schmutterer and
power, droplet size, and the larvacidal activity of final K.R.S. Ascher; German Agency for Technical Cooperation,
emulsions. It also can be concluded that larvacidal activity Eschborn, Germany; pp. 111–122.
increases as the concentration of Neem oil in emulsion [11] Balandrin, M.F., Lee, S.M., and Klocke, J.A. (1988) J. Agri.
formulation increases. Food Chem., 36: 1048–1054.
[12] Olaifa, J. I. and Adenuga, A.O. Insect Sci. Its Appl., 9:
267–270.
[13] Chiu, S.F. (1989) In Insecticides of Plant Origin; edited by
REFERENCES J.T. Arnason, B.J.R. Philogene, and P. Morand, ACS Sym-
[1] Isman, B.M., Koul, O., Luczynski, A., and Kaminski, J. posium Series 387; American Chemical Society, Washington,
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