HAWASSA UNIVERSITY INSTITUTE OF TECHNOLOGY

CHEMICAL ENGINEERING DEPARTMENT

Research Methods and Project Proposal

Research title: Formulation of shampoo from black cumin seed (Nigella Sativa) oil
extract

By
1. Abdulkudus Abdushukur Tech/0369/09
2. Nuredin Mustefa Tech/0352/09
3. Nathan Sisay Tech/1824/09

Submission date: 29/05/2021

Submitted to: Mr. Muluken Z.
 Table of Contents
List of table................................................................................................................................................ii
List of Abbreviations and Acronyms......................................................................................................iii
Executive Summary.................................................................................................................................iv
1 Introduction.......................................................................................................................................1
1.1 Background................................................................................................................................1
1.2 Statement of problem................................................................................................................2
1.3 Research Questions....................................................................................................................3
1.4 Objectives...................................................................................................................................3
1.4.1 General objective...............................................................................................................3
1.4.2 Specific objectives..............................................................................................................4
1.2. Significance of the Research......................................................................................................4
2 Literature Review..............................................................................................................................5
2.1 Introduction...............................................................................................................................5
2.2 Physicochemical properties of black cumin seed oil................................................................6
2.3 General Formulation of shampoo.............................................................................................7
3 Methodology.......................................................................................................................................8
3.1 Materials Chemicals and Equipment.......................................................................................8
3.2 Methods......................................................................................................................................9
3.2.1 Extraction of oil:................................................................................................................9
3.2.2 Physical characteristics of seed oil..................................................................................10
3.2.3 Shampoo preparation......................................................................................................11
4 Timeline of the proposed Research................................................................................................12
5 Budget...............................................................................................................................................13
References................................................................................................................................................14

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 List of table
Table 1 physical properties of black cumin seed oil........................................................................6
Table 2 Chemical properties of black cumin seed oil......................................................................7
Table 3 list of equipment used.........................................................................................................8
Table 4 Lists of chemicals and reagents..........................................................................................9
Table 5 Timeline of the study........................................................................................................12
Table 6 Budget of the study...........................................................................................................13

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 List of Abbreviations and Acronyms
CEH: center for environmental health
cp: heat capacity
g: gram
ID: identification
Kg: kilo gram
KOH: potatium hydro oxide
mg: mili gram
PEG: Polyethylene Glycols
UV: ultra violate
W1: weigt of oil
W2: weight ot water

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 Executive Summary
Hair loss is a major problem in the world society which can affect just your scalp or your entire
body and it can be the result of heredity, hormonal changes, medical conditions or normal part of
aging. Herbal shampoo from different plant extracts have been used to treat hair. black cumin
seed is one of remedial seed that have been used for hair treatment by extracting its oil. So, the
aim of this research is to prepare and formulate herbal shampoo from black cumin seed extract
and asses its physiochemical functions. To extract the oil from the seed, Solvent extraction by
using Soxhlet extraction method. Laboratory mixer and other equipment’s are used to prepare the
shampoo and the formulation will be made by trial-and-error experiment. Lastly, the
physiochemical properties like viscosity and detergency of the shampoo as well as the extracted
oil like density, viscosity, acid value and saponification number will be measured and analyzed.
This research will be significant in many ways. For instance, it will make the farmers produce
more black cumin seed, give information to other researchers, play an important role in fighting
baldness and increasing people’s quality of live and boost their confidence.

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1 Introduction
1.1 Background
Shampoos are most probably used as cosmetics. It is a hair care product that is used for cleaning
scalp and hair in our daily life. Shampoos are most likely utilized as beautifying agents and are a
viscous solution of detergents containing suitable additives preservatives and active ingredients.
It is usually applied on wet hair, massaging into the hair, and cleansed by rinsing with water. The
purpose of using shampoo is to remove dirt that is build up on the hair without stripping out
much of the sebum. Many synthetic shampoos are present in the current market both medicated
and nonmedicated; however, herbal shampoo popularized due to natural origin which is safer,
increases consumer demand and free from side effects[CITATION San \l 1033 ].

In synthetic shampoos, surfactants (synthetic) are added mainly for their cleansing and foaming
property, but the continuous use of these surfactants leads to serious effects such as eye irritation,
scalp irritation, loss of hair, and dryness of hairs [CITATION mai \l 1033 ]. Alternative to synthetic
shampoo we can use shampoos containing natural herbals. However, formulating cosmetic
products containing only natural substances are very difficult [ CITATION mai \l 1033 ]. There are a
number of medicinal plants with potential effects on hair used traditionally over years around the
world and are incorporated in shampoo formulation [ CITATION San \l 1033 ][ CITATION mai \l
1033 ]. These medicinal plants may be used in extracts form, their powdered form, crude form, or
their derivatives [ CITATION Agh07 \l 1033 ]. To develop a shampoo containing an only one natural
substance which would be safer with milder effect, then the synthetic shampoo is difficult and
also it should possess good foaming, detergency, and solid content as such synthetic shampoo.
Hence, we considered in detailing an unadulterated natural cleanser utilizing conventional
technique using regularly utilized plant material for hair washing.

In the present study, herbal shampoo was formulated containing suitable ingredient such as
Hibiscus rosa-sinensis and Emblica officinalis, Acacia concinna, Sapindus indica, Eclipta
prostrata, Aloe barbadensis, and Cassia auriculata in different proportions to formulate and
evaluate its physicochemical properties. The pericarp of S. indica Poir. (Soapnut), products of
Phyllanthus emblica (Amla), and units of dried A. concinna (Shikakai) have been utilized

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customarily as old stories framework for purging hair [ CITATION Agh07 \l 1033 ]. Cleanser nut and
shikakai when shaken with water create rich foam due to their high saponin content [ CITATION
Agh07 \l 1033 ] it indicates frothing impact. Amla fruit and C. auriculata flowers are used to
promote hair growth, anti-dandruff agent, strengthen hairs, and prevent hair fall [ CITATION
Kar19 \l 1033 ]. E. prostrate leaves (Bhringraj) commonly known as false daisy in English and
Bhringraj in India, to promote hair growth and prevent graying of hair [ CITATION San \l 1033 ]. H.
rosa-sinensis flower and A. barbadensis used as a conditioning agent.

Black cumin (Nigella sativa) seed is also one of the most remedial seed that have a lot of health
benefits. Nigella sativa has been broadly studied in the last few decades and studies have
reported that it possesses a number of medicinal properties and pharmacological actions.

1.2 Statement of problem

Hair loss is a problem that affects virtually all adults worldwide. Hair loss(alopecia) can affect
just your scalp or your entire body, and it can be temporary or permanent. It can be the result of
heredity, hormonal changes, medical conditions, poor diet, or a normal part of aging. Anyone
can lose hair on their head, but it is common in men.

Baldness typically refers to excessive hair loss from your scalp. Hereditary hair loss with age is
the most common cause of baldness. But the role other causes of hair loss play in baldness is
undeniably huge[ CITATION Kar19 \l 1033 ]. Some people prefer to let their hair loss run its course
untreated and unhidden. Others may cover it up with hairstyles, makeup, hats or scarves. And
still others choose one of the treatments available, like herbal shampoos and oils, to prevent
further hair loss or restore growth.

Most hair products are loaded with toxic chemicals that give your hair instant gratification.
They help give us clean, shiny, bouncy and smooth locks, which often makes us settle for
them. However, these short-term benefits come along with long-term ill effects - ranging
from cancer to hormone imbalance. Presently the entire world is endeavoring to return towards
the natural herbal materials through it has a no some other side effects towards ailments.
Formaldehyde is a well-known carcinogen, yet it can be found in so many shampoos and
conditioners. This dangerous preservative can be absorbed through your scalp as well as seep
from the packaging and into the air over time. This additive can cause toxicity, affect or Hair loss
is a problem that affects virtually all adults worldwide. Hair loss(alopecia) can affect just your
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scalp or your entire body, and it can be temporary or permanent. It can be the result of heredity,
hormonal changes, medical conditions, poor diet, or a normal part of aging. Anyone can lose hair
on their head, but it is more common in men. cause asthma, and has been linked to cancer. As the
center for environmental health (CEH) revealed independent testing on finding a cancer-causing
chemical in 98 shampoo, soaps and other personal care products sold by major national retailers
the chemical cocamidedieethanolamine chemically modified form of coconut oil used as
thickener or foaming agent in many products was listed by California as known carcinogen. This
carcinogen was listed in 2012 prop 65 law in California which requires warning label on
products with carcinogen. To solve this problem, they have taken some measures according to
this study. This measure to check shampoo labels and stay away from products with this
ingredients such as carcinogen, triclosan, polysorbates, polyethyleneglycol, potassium sorbat etc.

So, in this research black cumin seed is used as a raw material for shampoo production. Nigella
sativa has been broadly studied in the last few decades and studies have reported that it possesses
a number of medicinal properties and pharmacological actions. Some of them are Anticancer
Activity, Antifungal Activity and so on

1.3 Research Questions

 Which solvent, Hexane or methanol, will give more oil yield and can easily separated?
 What effect does viscosity of extracted oil have on the viscosity of shampoo?
 What impact have acid value of the oil extract have on the cleaning property of the
shampoo?
 Which are compatible ingredients that can be used with black cumin oil extract in the
formulation?
 What is the most effective procedure of herbal shampoo production?

1.4 Objectives
1.4.1 General objective
The general objective of this research is formulation of herbal shampoo from black cumin seed
oil extract.

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1.4.2 Specific objectives
The specific objective of this research is

1. To compare the oil yield by using hexane and methanol as a solvent in Soxhlet extraction
method
2. To study the physical and chemical properties of black cumin seed oil. Specifically,
physical properties like Density and viscosity, and chemical characteristics like, Acid
value of oil and Saponification number of the oil extract.
3. To analyze the physical and chemical properties of produced shampoo

1.2. Significance of the Research

This research is aimed to replace the synthetic shampoo ingredient with natural one, to be
specific black cumin seed. As a result, black cumin production will increase as industries that
will be engaged in production of this product will demand more black seed and farmers will be
beneficiary. This research can be a base for other researches on this type or other herbal products
other than herbal shampoo, for example conditioner, hair gel, hair wax and hair spray by
providing experimental data

It prevents the harmful effect of the synthetic ingredient since they are replaced with natural one
in the formulation. There are many advantages to the end users of the formulated herbal product
and one the function is reduction in hair fall and increasing the growth of the hair. herbal
shampoo is one of the best shampoo which not only remove the dirt from the hair and make if
shine more but also strengthen the root which in turn helps in increasing the growth of the hair.

Alopica (baldness) not only affects our health, but also have psychological effects. Some people
even could not go outside or go to work without covering their head [CITATION NHu05 \l 1033 ] . In
some cases, the alopica was the catalyst to end a relationship. so, by helping the hair regrow and
increase its shines, this shampoo will improve the quality of life of the people with this problem.

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2 Literature Review
2.1 Introduction
Shampoos are liquid detergents designed to clean a particular substrate, that is, hair and scalp.
They bear some resemblance to hand dishwashing liquids in that they are essentially unbuilt
surfactant solutions.
Esthetic properties, such as appearance (clear or pearlescent), viscosity, and fragrance, are
perhaps more important in this product group than in any other product category discussed in this
book. Development and maintenance of an adequate foam level is at once a performance
property and also an esthetic property in that it is noticed and evaluated by the user.
Shampoos almost always contain additives with activity in areas other than cleaning and
foaming, designed to provide specific performance attributes that confer such properties as
luster, manageability to hair, and elimination of dandruff[ CITATION Kar19 \l 1033 ].
The concentration in use of shampoos is estimated as near 8%. This is an order of magnitude
greater than the use concentrations of laundry and dishwashing liquids. Mildness to skin and low
irritation to eyes are therefore important requirements for shampoos. Salts, generally sodium but
also triethanolamine, of long-chain alcohol sulfates and alcohol ether sulfates are the most
widely used surfactants in shampoo formulations. Alkanolamines act as viscosity regulators as
well as foam stabilizers[ CITATION CLA97 \l 1033 ].
This hair products are loaded with toxic chemicals that give your hair instant gratification.
They help give us clean, shiny, bouncy and smooth locks, which often makes us settle for
them. However, these short-term benefits come along with long-term ill effects - ranging
from cancer to hormone imbalance.

Here is a list of ingredients in your shampoos and conditions that can turn out to be harmful
in the long run

 Sulfates  Triclosan
 Parabens  Dimethicone
 Polyethylene Glycols (PEG)  Fragrances
 Phthalates  Colors
 Formaldehyde

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Therefore, researches have been made over the past decades to minimize the harmful effect
of these chemicals. One of them are including herbal ingredient to the formulation produce
herbal shampoo that can protect hair from any sort of damage, specifically, from breakage,
thinning, and balding. These herbal ingredients are Emblica officinalis, Hibiscus rosa-
sinensis, Acacia concinna, Sapindus indica Aloe Vera. Using these ingredient, harmful
synthetic ingredient can be substituted with safe natural ingredients[CITATION DrK20 \l 1033 ].

Black cumin (Nigella sativa) seed is also one of the most remedial seed that have a lot of
health benefits. Nigella sativa has been broadly studied in the last few decades and studies
have reported that it possesses a number of medicinal properties and pharmacological actions.
Some of them are

 Antioxidant Activity  Antibacterial Activity

 Antidiabetic Activity  Antiparasitic Activity
 Neuroprotective Effect  Antifungal Activity
 Anti-inflammatory Effect  Anticancer Activity
 Antimicrobial Activity  Effects on male Infertility

Nigella sativa is rich in antioxidants that help to fight free radicals, which can cause
accelerated aging, reading to hair fall, balding and brittle hair. For women, it normalizes
hormonal levels, which help to prevent alopecia(balding)[ CITATION DrK20 \l 1033 ].

2.2 Physicochemical properties of black cumin seed oil

These data obtained from research made in Sudan University of Science and Technology,
College of Agricultural Studies[ CITATION Ena17 \l 1033 ].

Table 1 physical properties of black cumin seed oil

Mean Std. Deviation

Viscosity{40ºC} (cp) 40.12 0.6729
Density 0.906 0.0058
Refractive index{40ºC} 1.463 0.00041
Color (degree of color mixture) * R 1.0333 0.23094
B 0 0
Y 10.343 0.0577

Table 2 Chemical properties of black cumin seed oil

Mean Std. Deviation

Peroxide value (mEq/Kg) 1.7033 0.2977
Saponification (mgKOH/g) 186.55 1.0443

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 Iodine value (mg I2/g) 97.733 0.5907
Acid value(mgKOH/g) 0.396 0.0115
Un saponification matter(mg/g) 1.51 0.1473

2.3 General Formulation of shampoo

Shampoos consist of several types of ingredients that usually include many of the following
types of components:

 Primary surfactant for cleaning and foaming

 Secondary surfactant for foam and/or viscosity enhancement
 Viscosity builders: gums, salt, amide
 Solvents to clarify or lower the cloud point
 Conditioning agents
 Opacifier for visual effects
 Acid or alkali for pH adjustment
 Colors (D&C or FD&C colors) for visual effects
 Fragrance
 Preservative
 UV (ultraviolet) absorber, usually for products in a clear package Specialty active
ingredients, such as antidandruff agents and conditioning agents

 Hair conditioners, on the other hand, are very different compositionally from
shampoos. These are usually composed of many of the following types of ingredients:

 Oily and/or waxy substances, including mineral oil, long-chain alcohols, and/or
triglycerides or other esters, including true oils and waxes, silicones, and/or fatty acids

 Cationic substances: monofunctional quaternary ammonium compounds or amines or

polymeric quaternary ammonium compounds or amin
 Viscosity builders,

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3 Methodology
Since the process is formulation of shampoo from black cumin seed and because of some
constraints, laboratory apparatuses will be used for the experiment, which involves extraction
of oil from black cumin seed and use the extracted oil for the shampoo formulation by mixing
it with other ingredients in laboratory mixer.

3.1 Materials Chemicals and Equipment

The main raw materials, chemicals and equipment that are required to our study listed in the
table below.

Table 3 list of equipment used

Materials/Equipment Functions

Heating mantle Heat source

Round bottom flask to contain chemical reactions

Soxhlet extraction chamber To extract the oil from the black seed oil

Condenser Changing the state of the solvent from vapor to

liquid
Water pipe Cooling Water circulate stream to condenser

Funnel used to channel liquids into labware with a

narrow neck or opening
Filter paper separate fine solid particles from liquids

Glass rod

Distillation To separate the solvent and the oil

Beaker

Laboratory Mixer For shampoo preparation

Pycno-meter Used to measure density

Viscometer Used to measure viscosity

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Table 4 Lists of chemicals and reagents

Lists of chemicals and reagents

Oil extraction shampoo

Chemicals Function Chemicals Function
Black cumin seed Black cumin seed Used in
oil transesterfication
reaction
Petroleum ether Solvent Water Neutralize the base
catalyzed
transesterfication
reaction
Water Solution Surfactant Active ingredient
preparation
Phenolphthalein Color Foam boosters Increase
indicator
Ethyl alcohol Thickeners Increase viscosity

Alcoholic KOH Special additives

solution

3.2 Methods
3.2.1 Extraction of oil:
The seed will be bought from nearby shop and dried and the impurities will be removed by
handpicking. The seed will be crushed by using laboratory mixer grinder. Normally the
grinded seed containing some of the desired compound will be placed inside a thimble made
from thick filter paper, which is loaded into the main chamber of the Soxhlet extractor. The
Soxhlet extractor will be placed onto a flask containing the extraction solvent. The Soxhlet is
then will be equipped with a condenser. Then, the solvent will be heated to reflux. The
solvent vapor will travel up a distillation arm, and will floods into the chamber housing the
thimble of solid. The condenser will ensure that any solvent vapor cools, and drips back
down into the chamber housing the solid material. The chamber containing the solid material

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slowly will fills with warm solvent. Some of the desired compound will then dissolve in the
warm solvent. When the Soxhlet chamber is almost full, the chamber is automatically will
emptied by a siphon side arm, with the solvent running back down to the distillation flask.
This cycle may be allowed to repeat many times, over hours or days. During each cycle, a
portion of the non-volatile compound will dissolve in the solvent. After many cycles the
desired compound will be concentrated in the distillation flask.
After extraction, the solvent will be removed, typically by means of a rotary evaporator,
yielding the extracted compound. The non-soluble portion of the extracted solid will remains
in the thimble, and is usually discarded.

3.2.2 Physical characteristics of seed oil

Density of oil
The oil density will be determined according to AOAC (2008) methods, using pycno-meter.
An empty stoppered psycho-meter will be weighed, filled with water and kept at constant
temperature of 25ºC in a water bath for 30 min. the weight of water at 25ºC will be
determined by subtracting weight of empty pycno-meter from its weight when filled with
water. The end of time coppered pycno-meter will be adjusted to proper level, dried with a
cloth and weighted. In the same manner, the weight of the oil at 25ºC will be determined. The
density will be calculated as follows: The density at 25ºC

W1/W2 Where, W1 = Weight of oil at 25ºC, W2 = Weight of water at 25ºC

Viscosity
The instrumental will be exactly filled to the mark at the top of the lower reservoir with the
oil by means of pipette inserted in the side arm, so that the tube wall above the mark will not
be wetted. The instrument will be then left to stand for few minutes before reading in order to
equilibrate the sample temperature with that of the instrument(35ºC). By means of pressure
on the respective aim of the tube, the oil will be moved into the other the arm so that the
meniscus is (1 cm) above the mark at the top of upper reservoir. The liquid will then be
allowed to flow freely through the tube and the time required for the meniscus to pass from
the mark above the upper reservoir to that at the bottom of the upper reserve was recorded.
W1 = weight of water at 40ºC.

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3.2.3 Shampoo preparation

The manufacturing process can be broken down into two steps. First a large batch of
shampoo is made and then the batch is filled into the packaging.

Compounding: The process of any large-scale cosmetic production is called compounding.

All the ingredients will be mixed together in stainless steel tanks (laboratory mixer). The raw
materials will be poured into the batch mixer and will thoroughly be mixed. The order and
temperatures are determined by the formulating chemist. Some ingredients like water or the
primary detergents which make up the bulk of the product will be pumped and metered
directly into the batch tank. A computer interface is often used to control mixing speed and
temperature.

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4 Timeline of the proposed Research

Table 5 Timeline of the study

2013
Months
I Task
Start Finish Duration
d name Jun July Aug
W W W W W W W W W W W W
1 2 3 4 1 2 3 4 1 2 3 4
1 Studding the 01/10/13 15/10/13 2 weeks
problem in
detail
2 Literature 15/10/13 30/10/13 2 weeks
review
3 Proposal 01/11/13 07/11/13 1 week
approval
4 Collection of 07/11/13 21/11/13 2 weeks
raw materials
5 Conducting 01/10/13 15/10/13 2 weeks
experiment
and data
generation
6 Analysis of 01/10/13 15/10/13 2 weeks
data,
7 Compilation 01/10/13 15/10/13 2 weeks
of the
proposal
8 Final report 01/10/13 15/10/13 2 weeks

9 Thesis
submission

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5 Budget
Funding will be applied for the research through the group members Endowment Fund.
The budget for this study Is detailed in table
Table 6 Budget of the study

Item Explanation Quantity Unit cost Cost ETB

ETB
Black cumin seed Main ingredient 0.5 kg 300/kg 150
Petroleum ether Solvent 0.25 liter 428/liter 107
Water Used for solution 0
preparation
And as a raw
material for
shampoo
production
Phenolphthalein Color indicator From lab
Surfactant Active ingredient 0.5 liter 110/liter 55
Foam boosters Increase 0.2 liter From lab
Thickeners Increase viscosity 0.2 liter From lab
Equipment’s Used for both oil 12 From lab
extraction and
shampoo
preparation
Total 312

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 References
Enas Abdulhadi, M. E. (oct,2017). Physico chemical properties of Black Cumin seed oil.
Sudan.

Guha, D. K. (April 21,2020). 15 Harmful Ingredients In Shampoos And Conditioners That

You Should Avoid, Starting Today. Sowmya T, 12.

Karim, E. M. (12 may 2019). A promising matural Remedy for wide range of illnesses.
Hindawi, 16.

ROBBINS, C. R. (1997). Shampoo and Conditioner. In K.-Y. Lai, liquid detergent (p.
671). New York: Marcel Dekker.

Aghel N, M. B. (2007). Formulation of Herbal Shampoo using total saponins of

Acanthophyllum Sguarrosm. Iran J pharm Res, 72-73.

Enas Abdulhadi, M. E. (oct,2017). Physico chemical properties of Black Cumin seed oil.
Sudan.

Guha, D. K. (April 21,2020). 15 Harmful Ingredients In Shampoos And Conditioners That

You Should Avoid, Starting Today. Sowmya T, 12.

Karim, E. M. (12 may 2019). A promising matural Remedy for wide range of illnesses.
Hindawi, 16.

mainkar AR, J. C. (oct,2001). Formulation and Evaluation of Herbal Shampoo. Int J

cosmet Sci, 59-62.

ROBBINS, C. R. (1997). Shampoo and Conditioner. In K.-Y. Lai, liquid detergent (p.
671). New York: Marcel Dekker.

Sanfeetha S, R. N. (10 oct 2018). Formulation and Evaluation of Herbal Shampoo. Nnovare
Academic Sciences, 3.
McHale, N. H. (2005). The Pyscological impact of Alopecia. researchgate, 3-7.

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