1

ADAMSON UNIVERSITY
College of Engineering
Chemical Engineering Department
M a ni l a

Ch.E. Industrial Chemistry

Laboratory Manual

Prepared by:

Committee for Laboratory Manual of the Chemical Engineering Department

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Table of Contents:

Course Description (i)

Laborator y Rules and Guidelines (ii)

Preparation of Laborat ory Reports (iii)

Experiment Title

No.

1 Preparation of Soap

2 Fabric Conditioner (Cold Processes)

3 Facial Cleanser

4 Powdered Detergent

5 Preparation of Nata De Coco

6 Cologne/Cologne Gel

7 Cream Perfume / Cold Cream

8 Decorative Candle Making

9 Fruit Wine Making

10 Tomato Catsup Making

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CH.E. INDUSTRIAL CHEMISTRY

(Laboratory)

Course Description:

This is a laboratory course that involves actual preparation of industrial products

commonly encountered in the chemical process industries such as manufacture of vegetable oil,
refined vegetable oil, soap, wine, refined sugar, paper etc.

No. of hours : 54 hours

Course Credit Units : 1 unit

General Objectives:

After completing this course, the student must be able to:

1. Do the research on the laboratory procedures in the preparation of industrial

products.

2. Conduct experiments dealing with common chemical processes with

important consideration on safety, economy and product quality.

3. Exhibit confidence and ease in the laboratory preparation of the selected

industrial products in preparation for industrial exposure.

4. Be familiarized with other chemical processes especially those conducted in

the Philippines.
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POLICIES AND GUIDELINES ON THE

USE OF CHEMICAL ENGINEERING/CHEMISTRY LABORATORIES

1. Chemical Engineering laboratories are open for equipment review and other preparatory work
from 8 am to 5 pm Monday through Friday. Equipment may only be operated and chemicals
will be dispensed during scheduled laboratory hours. Written approval of the faculty adviser,
laboratory coordinator, and ChE chairperson are required for anyone (e.g. research students) to
use the laboratory during Saturdays or to operate equipment on non-scheduled laboratory days.

2. For the use of equipment, computers, and chemicals, students and faculty members must sign in
the log books for proper monitoring of the equipment.

3. No equipment is to be operated until the approval of the instructor and laboratory coordinator
has been obtained at the check-in meeting. Only the equipment pertaining to the assigned
experiment is to be operated. All members of a group are to be properly informed on the safety
aspects of their assigned experiment and to be familiar with the safety aspects of surrounding
experiments. Before any apparatus can be operated in the laboratory, the group must have a
second on-site safety check-in.

4. Students are required to prepare handling and storage procedures of chemicals and materials to
be used and waste disposal/treatment procedures approved by the faculty adviser and laboratory
coordinator prior to any experiment.

5. Transfer or movement of equipment or devices from the laboratories will not be allowed without
approval of advance notice (at least 2 days before the request schedule) from the laboratory
coordinator.

6. In borrowing glassware and accessories of the equipment, equipment and in using laboratory
facility, students must accomplish Form A (Request for the Use of Laboratory Facilities and
Equipment) with the signature of the professor.

7. In case of breakages, damages, or losses:

(A) A student accomplishes three copies of the Breakage Forms/Charge Slip Form (Form B)
duty signed by all members of the group.
(B) The student requests the signature of the instructor and returns the form to the laboratory
personnel.
(C) The laboratory personnel indicate the price of the damaged or lost item.
(D) The students are given one week to replace the items with the same brand or specifications.
If the students fail to replace the said item, the item is then forwarded to the Cashiers Office
for payment.
(E) After payment, the students return the forms to the laboratory personnel with the photocopy
of the official receipt.
(F) They must be advised to keep the original receipt for future reference.

8. Students should always wear their laboratory gowns or aprons when working in the laboratory.
Safety goggles and safety gloves must also be worn whenever applicable. Students must also
observe proper attire specifically closed footwear to protect them from spilled chemicals or hot
fluids. Neckties, dangling clothing or jewelry and other unsafe items are prohibited.
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9. Sleeping is prohibited in the laboratory. Violation of this rule will result in dismissal from the
laboratory for that day.

10. Horseplay of any sort is absolutely prohibited in the laboratory.

11. As a general rule, eating, drinking, chewing gum, and smoking are not allowed inside
laboratories.

12. All safety precautions must be followed at all times.

13. No operating equipment will be left unattended. At least two members of the group must be
present while the equipment is operating.

14. The laboratory floor must be kept dry, clean, and uncluttered at all times. Any spills should be
cleaned up immediately.

15. All injuries, accident, hazardous situation, losses, leaks, malfunctions or breakages must be
reported to the laboratory personnel or professor immediately.

16. All chemicals must be transported in a safety carrier. All mercury and alcohol thermometers and
more than one item of glassware must be transported in a bucket or other suitable container.

17. The students are expected to be familiar with the safety aspects of all chemicals used in the
laboratory.

18. Listening to radios, walkman, MP3s, MP4s, etc. is strictly prohibited in the laboratory.

19. Playing computer games; using and recharging of cellular phones; or viewing DVDs is
prohibited in the laboratory.

20. Applying cosmetics are prohibited in the laboratory.

21. Precautions should be taken to prevent long hair from being entangled in moving parts of the
equipment.

22. A violation notice will be issued by the Laboratory Coordinator or Laboratory Student Assistant
or by the assigned Laboratory Professor to any student found violating any of these rules and
regulations.

23. Any SERIOUS VIOLATION of any of these safety rules or laboratory policies may lead to
immediate dismissal from the laboratory. A person who repeatedly disregards the safety rules
or laboratory policies for at least 3 times will be called in for disciplinary action with the ChE
chairperson. A penalty that suits the violation may be imposed and, at the discretion of his/her
laboratory professor, the students grade may be severely affected.

Other policies may be given as situation arises and in consideration of our best interest. It is expected
that these sets of policies serve as a guide for us to work safely and efficiently.
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EXPERIMENT NO. 1

PREPARATION OF SOAP

In chemistry, soap is a salt of a fatty acid. Soap is mainly used for washing, bathing, and
cleaning, but soaps are also used in textile spinning and are important components of lubricants.
Soaps for cleansing are obtained by treating vegetable or animal oils and fats with a strongly
alkaline solution. Fats and oils are composed of triglycerides: three molecules of fatty acids
attached to a single molecule of glycerol. The alkaline solution, often called lye, brings about a
chemical reaction known as saponification. In Saponification, the fats are first hydrolyzed into
free fatty acids, which then combine with the alkali to form crude soap. Glycerol, often called
glycerin, is liberated and is either left in or washed out and recovered as a useful by-product
according to the process employed. Soaps are key components of most lubricating greases, which
are usually emulsions of calcium or lithium soaps and mineral oil. Calcium and Lithium-based
greases are widely used in engineering applications. Other metallic soaps are also useful,
including those of aluminum, sodium, and mixtures of them. Such soaps are also used as
thickeners to increase the viscosity of oils. In ancient times, lubricating greases were made by the
addition of lime to olive oil.

Saponification is a process that produces soap, usually from fats and lye. In technical
terms, saponification involves base (usually NaOH) hydrolysis of triglycerides, which are esters of
fatty acids, to form the sodium salt of a carboxylates. In addition to soap, such traditional
saponification processes produces glycerol. "Saponifiable substances" are those that can be
converted into soap.
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EXPERIMENT NO. 1

PREPARATION OF SOAP

OBJECTIVES:
1. To prepare a simple soap using the available raw materials indicated in the experiment.
2. To teach the students how to make soaps using simple raw materials which they can
find in their homes.

APPARATUSES:
1. 1000 mL Beaker
2. Stirring rod
3. Bunsen burner
4. Evaporating dish
5. Cloth filter
6. Molder

RAW MATERIALS:
1. 100 mL of Cooking Oil
2. 60 mL of 50% NaOH
3. 210 mL of 35% NaCl
4. 80 mL distilled water

PROCEDURES:
1. Place the cooking in a beaker and apply heat. When the oil is already hot, add the NaOH
solution little by little, stirring it during the addition (Caution: Spattering may occur).
2. Continue applying heat until the mixture is homogeneous and fairly thick.
3. Stop applying heat. Immediately add NaCl solution and stir well. Soap, being insoluble in
salt solution will separate put. The liquid which contains the glycerol and the excess
NaOH is called nigre.
4. Filter the precipitated soap through a cloth filter and rinse it well with cold water.
5. Transfer the soap into an evaporating dish and dissolve it by boiling with distilled water.
6. Evaporate the solution to a jelly like consistency and transfer it in a mold. Allow it to
solidify.
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EXPERIMENT NO. 2

FABRIC SOFTENER
(Cold process)

A fabric softener is a liquid composition added to washing machines during the rinse cycle
to make clothes feel better to the touch. These products work by depositing lubricating chemicals
on the fabric that make it feel softer, reduce static cling, and impart a fresh fragrance. The first
fabric softeners were developed by the textile industry during the early twentieth century. At
that time the process that was used to dye cotton fibers left them feeling harsh. In the early
1900s, preparations known as cotton softeners were developed to improve the feel of these
fibers after dyeing. A typical cotton softener consisted of seven parts water, three parts soap,
and one part olive, corn, or tallow oil. With advances in organic chemistry, new compounds were
created that could soften fabric more effectively. These improved formulations soon found their
way into the commercial market.

By the 1960s several major marketers, including Procter and Gamble, had begun selling
liquid fabric softener compositions for home use. The popularity of these products dramatically
increased over the next decade as manufacturers developed new formulations that provided
improved softness and more appealing fragrances.
In the late 1970s manufacturers found a way to deliver fabric softening benefits in a dryer sheet
format. These sheets provide some of the benefits of fabric softeners but give the added
convenience of being able to be added in the dryer instead of the washer rinse cycle. However,
while dryer sheets are very popular today, liquid softeners are still widely used because they are
more effective.

In the 1990s, environmentally minded manufacturers began test marketing ultra-

concentrated formulations. These "ultra" formulations are designed such that only about one-
quarter as much product has to be used and therefore they can be packaged in smaller
containers. However the perceived value to the consumer is lower because there are fewer
products and the price is higher. It remains to be seen if these ultra concentrates will succeed in
today's marketplace.
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EXPERIMENT NO. 2

FABRIC SOFTENER
(Cold process)

OBJECTIVES:
1. To be familiar with the use of the ingredients in the experiments.
2. To determine the effectiveness of the experiment.

APPARATUSES:
1. Strainer
2. Spoon
3. 1000 mL Beaker
4. 12-13 L Pail
5. Containers or bottles

REAGENTS:
1. 1 Kg softener flakes
2. 12-13 L water
3. Colorant
4. 12 mL Preservative / antibac
5. 30 mL Anti-foam
6. 100 mL Downy scent

PROCEDURES:
1. Dissolve 1kg softener flakes in 12-13 liters of water.
2. Add colorant (as desired), preservative / antibac (12 mL), anti-foam (30 mL) and Downy
scent (100 mL).
3. Mix all ingredients completely.
4. Repack in containers or bottles.
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EXPERIMENT NO. 3

FACIAL CLEANSER

Cosmetics are substances used to enhance the appearance or odor of the human body.
Cosmetics include skin-care creams, lotions, powders, perfumes, lipsticks, fingernail and toe nail
polish, eye and facial makeup, towelettes, permanent waves, colored contact lenses, hair colors,
hair sprays and gels, deodorants, hand sanitizer, baby products, bath oils, bubble baths, bath
salts, butters and many other types of products. A subset of cosmetics is called "make-up," which
refers primarily to colored products intended to alter the users appearance. Many
manufacturers distinguish between decorative cosmetics and care cosmetics.

A lotion is a low- to medium-viscosity, topical preparation intended for application to

unbroken skin. By contrast, creams and gels have higher viscosity.

Lotions are usually applied to external skin with bare hands, a clean cloth, cotton wool or
gauze. Many lotions, especially hand creams and face cream are formulated not as a medicine
delivery system, but simply to smooth, re-hydrate, and soften the skin. These are particularly
popular with the aging and aged demographic groups, and in the case of face usage, can also be
classified as a cosmetic in many cases, and may contain fragrances.

Most lotions are oil-in-water emulsions using a substance such as cetearyl alcohol to keep
the emulsion together, but water-in-oil lotions are also formulated. The key components of a skin
care lotion, cream or gel emulsion (that is mixtures of oil and water) are the aqueous and oily
phases, an emulgent to prevent separation of these two phases, and, if used, the drug substance
or substances. A wide variety of other ingredients such as fragrances, glycerol, petroleum jelly,
dyes, preservatives, proteins and stabilizing agents are commonly added to lotions.

In this experiment, anti-bacterial face lotion is made. Face lotion will be composed mainly
of ethyl alcohol. Color and oiliness of the solution will be enhanced by adding Ferric Chloride and
glycerol, respectively.
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EXPERIMENT NO. 3

FACIAL CLEANSER

OBJECTIVES:
1. To be familiar with the ingredients in the experiment.
2. To know how oiliness of the product be increased.
3. To prepare a simple face lotion made up of only few ingredients.

APPARATUSES:
1. Analytical Balance
2. 10 and 50 mL Graduated Cylinder
3. Medicine Dropper
4. Stirring Rod
5. Beaker

RAW MATERIALS:
1. 1.65 mL of 95% ethyl alcohol
2. 10mL of water
3. 5mL of glycerol
4. 0.5g of menthol
5. 0.1g of salicylic acid
6. one drop of 1% FeCl3 solution

PROCEDURES:
1. To 65 mL of 95% ethyl alcohol, add 10mL of water, 5mL of glycerol, 0.5g of
menthol, 0.1g of salicylic acid and one drop of 1% FeCl3 solution.
2. The intensity of the color may be increased by the addition of more ferric chloride
solution. This lotion dries quickly and has a pleasant after-glow. Its oiliness may be
increased by increasing the glycerol content, with a corresponding decrease in the
alcohol content.
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EXPERIMENT NO. 4

POWDER DETERGENT

The chemistry of soap manufacturing remain primarily the same until the year 1916,
when the first synthetic detergent was developed in Germany in response to the shortage of fats
for making soaps during the World War I. Commonly known as detergents today, synthetic
detergents are non-soap washing and cleaning products, which are put together chemically or
synthesized to produce a variety of raw materials. The invention of detergents was also driven
by the need for a cleaning agent, which, unlike soap, would not combine with the mineral salts
in water to form an insoluble substance (soap curd) on the fabric.

A detergent is a surfactant (Surfactants are compounds that lower the surface tension of
a liquid, the interfacial tension between two liquids, or that between a liquid and a solid.
Surfactants may act as detergents, wetting agents, emulsifiers, foaming agents, and dispersants.)
Or a mixture of surfactants having "cleaning properties in dilute solutions." In common usage,
"detergent" refers to alkylbenzenesulfonates, a family of compounds that are similar to soap but
are less affected by hard water. In most household contexts, the term detergent by itself refers
specifically to laundry detergent or dish detergent, as opposed to hand soap or other types of
cleaning agents. Detergents are commonly available as powders or concentrated solutions.

One of the largest applications of detergents is for cleaning clothing. The formulations are
complex, reflecting the diverse demands of the application and the highly competitive consumer
market. In general, laundry detergents contain water softeners, surfactants, bleach, enzymes,
brighteners, fragrances, and many other agents. The formulation is strongly affected by the
temperature of the cleaning water and varies from country to country.
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EXPERIMENT NO. 4

POWDER DETERGENT

OBJECTIVES:
1. To know how mixtures of different bases increase the effectiveness of the detergent.
2. To know the proportions of the components of a detergent.
3. To be able to prepare a powder detergent.

APPARATUSES:
1. Basin
2. 50 mL Graduated cylinder

RAW MATERIALS:
1. 1 kg linear alkyl benzene sulfonate (LABS) powder (grease remover)
2. 1 kg coconut fatty alcohol sulfate (CFAS) powder (soap-base)
3. 2 kg soda ash
4. 6.5 kg sodium sulfate
5. 100 g speckles
6. 30 mL scent oil

PROCEDURES:
1. In a basin, mix 1 kg LABS powder and 2 kg of SODA Ash.
2. Add 1 kg of CFAS powder and 6.5 kg sodium sulfate. Mix.
3. Add 100g speckles and 30 mL scent oil. Press and mix well.
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EXPERIMENT NO. 5

PREPARATION OF NATA DE COCO

Nata de coco is a chewy, translucent, traditional Philippine dessert which is "coconut gel-
product from coconut water by bacterial fermentation-prepared". It is produced through
fermentation of coconut water, which gels through the production of microbial cellulose by
Acetobacter xylinus. It is very sensitive to environmental conditions, finding the right place and
temperature in which the mother nata would set the coconut juice required a lot of
experimentation. Nata de coco is most commonly sweetened as a candy or dessert, and can
accompany many things including pickles, drinks, ice cream, puddings and fruit mixes. The
product originates from the Philippines.

Nata de coco comes from Spanish "cream of coconut". Cream in this sense means the fat
from the coconut milk. The Spanish name is a result of Spain's colonization of the Philippines.

Nata de coco is highly regarded for its high dietary fibre, and its low fat and cholesterol
content. Strips of nata de coco are used in mass-produced bubble tea drinks as a healthier
alternative to tapioca.

The primarily coconut water dessert is produced through a series of steps from:
1. Extraction of coconut water
2. Fermentation of the coconut water with bacterial cultures
3. Separating and cutting the produced mat of nata de coco
4. Cleaning and washing the acetic acid out of the nata de coco
5. Cutting to packaging

Commercial nata de coco is made by small farms in the Philippines and Indonesia.
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EXPERIMENT NO. 5

PREPARATION OF NATA DE COCO

OBJECTIVES:
1. To have an idea on how to make nata de coco.
2. To compare the taste and quality of nata de coco produced in the laboratory and in the
industry.

RAW MATERIALS:
1. 12 cups of coconut water
2. 1 cup sugar
3. 2 tbsp. ammonium sulfate
4. 2 tbsp. glacial acetic acid
5. cup nata starter

PROCEDURES:
1. Strain the coconut water through a chess cloth.
2. Add the sugar and the acetic acid.
3. Boil for ten minutes and let cool.
4. Add the nata starter and distribute the mixture equally in gallon glass jars to about 2 to 3
inches deep (add a pinch of ammonium sulfate to each jar for a more rapid growth of
nata).
5. Cover the jars with papers and set aside undisturbed for about two weeks.
6. Harvest the nata when there are about an inch thick.
7. Wash thoroughly and cut into cubes.
8. Immerse in water for 2 days, changing often to remove the sour odor.
9. Boil in plenty of water for 2 or more times until the sour taste and odor are removed.
10. Drain and then weigh.
11. Add an equal weight of sugar and stir thoroughly.
12. Allow to soak overnight.
13. Boil for 10 min and add desired flavoring (pineapple or nangka).
14. Pack in 12 oz. preserving jar and sterilize in boiling water for 25 minutes and seal tightly.
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EXPERIMENT NO. 6

SHIITAKE MUSHROOMS CULTIVATION

The Shiitake (Lentinula edodes) is an edible mushroom native to East Asia, which is
cultivated and consumed in many Asian countries, as well as being dried and exported to many
countries around the world. It is a feature of many Asian cuisines including Vietnamese, Chinese,
Japanese, Korean and Thai. In the East, the shiitake mushroom has long been considered a
delicacy as well as a medicinal mushroom.

The common name for this mushroom, "shiitake," comes from the Japanese language.
"Shii" in Japanese refers to wood belonging to the Pasania species of tree on which shiitake
mushrooms naturally grow. "Take" simply translates as "mushroom." You may sometimes also
hear shiitake mushroom being referred to as the "Black Forest mushroom," and they do indeed
grow naturally in that German mountain range.

Shiitake mushrooms are popular for their rich and smoky flavor and are used in many
recipes. The easiest and most productive method of growing shiitake mushrooms is with plug
spawn. Wooden "plugs" are inoculated with mushroom spawn and pushed into tree logs. Not
only is this method effective but the logs can also beautify gardens. Each time it fruits, the
quantity of mushrooms will increase. It will continue to fruit for a few years until the wood cells
have been used up.

Freshly harvested mushrooms are highly perishable because of high moisture content,
metabolism and susceptibility to enzymatic browning. Its quality starts declining soon after
harvesting, rendering the produce unsalable. Hence, the development of appropriate storage
and processing technology in order to extend their marketability and availability to the
consumers in fresh or processed form is of great significance. Drying, canning and freezing are
initially accepted methods of mushroom preservation.

Drying being cheaper can be employed on commercial scale.

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EXPERIMENT NO. 6

SHIITAKE MUSHROOMS CULTIVATION

OBJECTIVES:
1. To produce processed mushrooms that extends its availability for further consumption.
2. To practice shiitake mushroom cultivation to increase production.

APPARATUSES:
1. 25 Wooden plugs inoculated with shiitake mushroom mycelium
2. Freshly-cut tree log
3. 5/16-inch drill bit
4. paintbrush
5. a mallet preferably with a rubber head
6. Beeswax
7. Water

PROCEDURES:
1. Buy 25 shiitake mushroom plugs (per log). These are wooden dowels that are colonized
by shiitake mushroom mycelium. They are usually about -inch wide and 1-inch long.
2. Find a good, freshly-cut tree log between 4 to 10 inches wide and cut to no more than 2
feet long.
3. Preparing the Log: a freshly cut log is best, as this means other fungus havent yet had a
chance to colonize it (and less competition means more shiitake mushrooms for you).
Fresh means cut in the last 72 hours or so. Apparently 100-150mm diameter is ideal,
length preferably no less than 2 ft. long.
4. Drill holes in the log with a 5/16-inch drill bit. The holes need to be about 2 inches deep
and 4 inches apart. A spiral pattern will result in a beautiful appearance once the
mushrooms begin to grow.
5. Push the shiitake mushroom plugs into the holes on the log and tap on each with a rubber
mallet until they fit snugly. Be careful not to damage the log bark.
6. Melt bees wax to about 145 degrees F. Seal each plug with melted bees wax using a brush
or turkey baster. This will protect against other fungi and insects.
7. Stand the log up in a shaded area. The log can be set against a fence, wall or planted by
burying one end of it in the ground. It will look great in a garden among flowers and other
plants, especially once the mushrooms begin to sprout. Water the log regularly to
maintain an internal moisture level of about 35 to 60 percent. Every 2 weeks will do. Be
sure to only use chlorine-free water, such as filtered water, well water or rain water.
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8. Wait for 6 months to 1 year for mushrooms to appear. A well colonized log will last about
3 to 4 years, until most of the wood cells have been replaced by shiitake mushroom
mycelium cells.

THE FINAL PRODUCT, TIPS AND WARNINGS:

1. The optimum temperature is 62 to 78 degrees F. The mushrooms will grow in other
temperatures, but not as well. The log will go dormant below 40 degrees F and above 80
degrees F. Freezing for a short while won't hurt and provide a strong shock to force the
mushrooms to fruit. It also needs air, normal or high humidity, and a natural day and night
cycle, alternating between shade and indirect sunlight or artificial lighting.
2. To harvest the mushrooms, use a knife and cut at the bottom of the stem or twist the
stem out.
3. Be sure to only use chlorine-free water to water the log.
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EXPERIMENT NO. 7

COLOGNE

Cologne is a toiletry, a perfume in a style that originated from Cologne, Germany. It is

nowadays a generic term for scented formulations in typical concentration of 2-5% essential oils.
However as of today cologne is a blend of extracts, alcohol, and water. Colognes may be used by
men or women but are generally marketed to men as an alternative to perfume.

In a base of dilute ethanol (70-90%), Eau de Cologne contains a mixture of citrus oils
including oils of lemon, orange, tangerine, bergamot, lime,grapefruit and neroli. It can also
contain oils of lavender, rosemary, thyme, petit grain (orange leaf), and jasmine.

The original Eau de Cologne is a spirit-citrus perfume launched in Cologne in 1709

by Giovanni Maria Farina (16851766), an Italian perfume maker from Santa Maria
Maggiore Valle Vigezzo, Italy. In 1708, Farina wrote to his brother Jean Baptiste: "I have found a
fragrance that reminds me of an Italian spring morning, of mountain daffodils and orange
blossoms after the rain". He named his fragrance Eau de Cologne, in honor of his new hometown.

The Original Eau de Cologne composed by Farina was used only as a perfume and
delivered to "nearly all royal houses in Europe". His ability to produce a constantly homogenous
fragrance consisting of dozens of monoessences was seen as a sensation at the time. At the time,
a single vial of this aqua mirabilis (Latin: miracle water) cost half the annual salary of a civil
servant. When free trade was established in Cologne by the French in 1797, the success of Eau
de Cologne prompted countless other businessmen to sell their own fragrances under the name
of Eau de Cologne.

Giovanni Maria Farina's formula has been produced in Cologne since 1709 by Farina
opposite the Jlichplatz and to this day remains a secret. His shop at Obenmarspforten opened
in 1709 and is today the world's oldest fragrance factory. Other Colognes were launched over
100 years after Farina's one, such as the famous Cologne 4711, named after its location at
"Glockengasse No. 4711". In 1806, Jean Marie Joseph Farina, a grand-grand-nephew of Giovanni
Maria Farina (16851766), opened a perfumery business in Paris that was later sold to Roger &
Gallet. That company now owns the rights to Eau de Cologne extra vieille in contrast to
the Original Eau de Cologne from Cologne.

Eau de Cologne, or just "cologne", has now become a generic term.

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The term "cologne" can be applied to perfume for men or women, but modern
convention dictates, in the English language, that it should be assumed the term is most likely
when talking about men's fragrance.

EXPERIMENT NO. 7

COLOGNE

OBJECTIVES:
1. To give students the idea of making cologne.
2. To compare the output cologne of the experiment from the standard commercial
cologne.

APPARATUSES:
1. Pyrex glass
2. Stirring rod or mixer

REAGENTS:
1. Fragrance Oil 8%
2. Propylene Glycol 2%
3. Deionized water 10%
4. Ethyl Alcohol 80%
(Excipients)
5. EDTA-Chelating Agent
6. Anti-Oxidants
7. Colorants

PROCEDURES:
1. Mix the fragrance oil and alcohol together with propylene glycol by a stirring rod or
mixer in a pyrex glass.
2. Add water, colorant, EDTA, anti-oxidant, and mix.
3. Stand for 2-3 weeks.
4. Chill at 40C overnight.
5. Filter while cold then pack using bottles.
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EXPERIMENT NO. 8

COLOGNE GEL

A cologne gel is a solid, jelly-like material and a mixture of fragrant essential

oils and/or aroma compounds, fixatives, and solvents that is gelatin like used to give the human
body, animals, objects, and living spaces a pleasant scent that can have properties ranging from
soft and weak to hard and tough.

The odoriferous compounds that make up a cologne gel can be manufactured

synthetically or extracted from plant or animal sources.

Cologne gels have been known to exist in some of the earliest human civilizations either
through ancient texts or from archaeological digs. Cologne gels are defined as a substantially
dilute cross-linked system, which exhibits no flow when in the steady-state and possess the
pleasant odor of perfume. By weight, cologne gels are mostly liquid, yet they behave like solids
due to a three-dimensional cross-linked network within the liquid. It is the crosslinks within the
fluid that give a cologne gel its structure (hardness) and contribute to stickiness (tack). In this way
cologne gels are a dispersion of molecules of a liquid within a solid in which the solid is the
continuous phase and the liquid is the discontinuous phase.
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EXPERIMENT NO. 8

COLOGNE GEL

OBJECTIVES:
1. To distinguish the quality of cologne gel made in the laboratory from the standard one.
2. To give the students an idea on how to make cologne gel
3. To compare cologne gel and liquid cologne

APPARATUSES:
1. Beaker (1000 mL)
2. Stirring rod

REAGENTS:
1. 51.7 g Distilled water
2. 0.7 g Carboner 940 (Polycarboxylic acid)
3. 0.5 g D-Panthenol 50P
4. 0.2 g Methyl Paraben
5. 0.9 g Tea(Triethanol Amine)
6. 3.0g Emulsogen EL
7. 3.0g Fragrance
8. 40.0 g Ethyl Alcohol
9. 0.05 g Irgasan AP 300

PROCEDURES:
1. Mix Methyl Paraben into the distilled water.
2. Add carboner 940, then tea and mix.
3. After adding, the gel has thickened. If the gel becomes watery, add additional tea.
4. Mix panthenol 50P, Fragrance and Irgasan AR300 into the alcohol. Add this to the gel
solution and mix.

Note:
If there will be additional ingredients/materials, reduce correspondingly the amount of distilled
water.
Emulsogen EL is a solubilizer that creates clear gel.
 23

EXPERIMENT NO. 9

CREAM PERFUME

Solid perfumes or cream perfumes are perfumes in solid form. It is usually uncommon
compared to liquid type of perfumes. Historically, ointment-like unguents have been used as a
type of solid perfume since Egyptian times. Normally the substance that gives the cream its base
comes from a type of wax that is initially melted. Once melted, a scent/or several scents may be
added and then furthered developed until the cream base reaches the desired consistency. Solid
perfumes have seen resurgence in recent years.
Solid perfume is used either by rubbing your finger against it and then onto skin, or
dipping a cotton swab into it and then onto your skin. Sometimes solid perfume can take more
time for the deeper notes to come out that an Eau de Toilette spray perfume.
 24

EXPERIMENT NO. 9

CREAM PERFUME

OBJECTIVES:
1. To produce a cream perfume that has a quality that will be marketable.
2. To know the difference of making solid perfume from liquid perfume.

APPARATUSES:
1. Tripod
2. Burner
3. Stirring rod
4. Beaker
5. Thermometer
6. Watch glass

RAW MATERIALS:

GROUP A:
2.0 g glycerol monostearate
14.0 g stearic acid
3.0 g lanoline
0.1 g propyl paraben

GROUP B:
4.0 g deionized water
0.5 g glycerine
5-10% perfume
0.25 g methyl paraben

PROCEDURES:
1. Add materials in A. Heat to 85-90 C.
2. Add materials in B except perfume. Heat to 75 80 C.
3. When both A and B are melted combine and stir continuously until cool.
4. When temperature reaches 35 C add perfume.
5. Age for 7-14 days. Put inside the freezer to stabilize their pack.
 25

EXPERIMENT NO. 10

COLD CREAM

Cold cream is an emulsion of water and certain fats which includes beeswax and various
scented chemicals. Cold cream is designed to make the skin smooth and it also helps in removing
makeup marks. The name is derived from the cool feeling that the cream leaves on the skin.
Variations of the product have been used for nearly two-thousand years.

OBJECTIVES:
1. To produce a good quality cold cream.
2. To be able to determine key ingredients that was used for the cold cream.

APPARATUSES:
1. Beaker
2. Medicine dropper
3. Jar
4. Stirring Rod
5. Evaporating Dish
6. Test Tube

RAW MATERIALS:
1. 10 g White Beeswax
2. 5.0g Paraffin
3. 20 mL Borax Solution Na2B4O7
4. 5 drops lemon oil

PROCEDURES:
1. Fill the beaker half-full of water, and set it to boil. This will serve as a water bath for
controlled heating of the evaporating dish to be placed on top of the beaker.
2. Cut 10 grams of portion of white beeswax into smaller pieces and place it in an
evaporating dish.
3. While the beeswax is melting, place 5 grams of shredded paraffin in a test tube. Add 20
mL of mineral oil to the beeswax and heat the mixture with constant stirring until it is
completely melted 70 degrees Celsius.
4. Now, add 25 mL of borax solution, a little at a time with constant stirring.
5. Finally, stir in a few drops of rose oil.
6. Carefully pour the cream into a jar and observe the contents.
 26

EXPERIMENT NO. 11

WAX

There are lots of kinds of wax depending on its source. They

may be from animal, vegetable, mineral and synthetic. Vegetable
waxes that are used as coatings derived from stems, leaves, flowers
and seeds. Animal waxes that are used as protective coatings are
secreted by most insects. Mineral waxes are paraffin waxes
obtained from petroleum, and such waxes are yielded by coal, peat
and lignite, though mineral waxes are not true wax (esters), still,
they are classified for having the physical properties of a wax.

Paraffin wax (or simply "paraffin") is mostly found as a

white, odorless, tasteless, waxy solid, with a typical melting point between about 46 and 68 C
(115 and 154 F), and having a density of around 0.9 g/cm3. It is insoluble in water, but soluble in
ether, benzene, and certain esters. Paraffin is unaffected by most common chemical reagents,
but burns readily.

The simplest paraffin molecule is that of methane, CH4, a gas at room temperature.
Heavier members of the series, such as octane, C8H18, and mineral oil appear as liquids at room
temperature. The solid forms of paraffin, called paraffin wax, are from the heaviest molecules
from C20H42 to C40H82. Paraffin wax was identified by Carl Reichenbach in 1830.

Paraffin waxes are used as fuels in gaseous states. In liquid state, it is used as fuels, paints,
pigments, dyes and inks, in culinary, cosmetics and toiletries, fire breathing and fire juggling, in
leather industry, used as pull up finish, in medicine (laxatives), in biomedical science, like
evaporation during PCR. In solid state, it is used as candle, waxed paper or cloth, crayons and the
like.

In chemistry, paraffin is a term that can be used synonymously with "alkane",

indicating hydrocarbons with the general formula CnH2n+2. Paraffin wax refers to a mixture of
alkanes that falls within the 20 n 40 range; they are found in the solid state at room
temperature and begin to enter the liquid phase past approximately 37C.
 27

EXPERIMENT NO. 11

WAX

OBJECTIVES:
1. To introduce to the students the production of wax.
2. To be knowledgeable about the functions and process involved and its other products.
3. To impart the concepts and increase the laboratory skills of the students as if working in
real industry.
4. To use its products as well as the its waste efficiently.

RAW MATERIALS AND PROCEDURE:

WAXES paraffin wax in blocks or pellets
- soft wax
- container candle

ADDITIVES:
Hard wax
1. Synthetics shiny, retention of scent by color
a. polyethylene
b. crystals
c. vybar
2. Organic combination of plants and animals waxes
a. camauba wax lifetime candle
b. palm wax off white
c. stearic acid dull

Suggested Wax Mixture

1. Ordinary Candle
90% paraffin
10%polyethylene
2. Cemetery Candle
95% paraffin
5%polyethylene
3. Vigil Candle
100% paraffin
4. Decorative Candle
90% paraffin
5%polyethylene
5%crystal
5. Organic Mixture
80% -90% paraffin
10% - 20% camauba wax
 28

6. 80% paraffin wax 70%

20% palm wax 30%
If 50% of palm wax become brittle
7. 10% stearic acid 20%
90% paraffin wax 80%

*MELTING IS HEATED ALL AT THE SAME TIME

WICK nylon wick

- container candle
- decorative
Code # 18,24,36,44
- ordinary cotton wick
- ordinary candle
By ply size depends on the candle diameter
Under sized wick forms a concave
Over sized wick fast melting with candle
Proper size dripless
#18 2.5 diameter of candle
#24 3.5 diameter of candle
#36 4.5 diameter of candle
#44 5 diameter of candle

6-9 ply 0.5 diameter

12-15 ply 1 diameter
17 -25 ply 2 diameter
27 -35 ply 3 diameter
37 45 ply 4 diameter

Gel wax for container candles

Micio wax glue wax
Beeswax
white
yellow
sheet form
Dye-oil soluble
Neon green, lavender, pink, orange; 70oC melting point
Ordinary - primary colors: red, yellow, blue
- secondary colors: green, orange, violet; 85oC melting point
Scent organic or essential oil by drops
Synthetic scent 15 30 mL / kg of wax
 29

Methods of melting
1. Direct melting time is 20 minutes
2. Indirect 1 to 2 hours melting time; using a double boiler

Methods of forming
1. Dipping using hanger type or caroussel
2. Pouring container like glass, paper, can, ceramics / nylon with wick sustainer
3. Hand forming
4. Molding

Pouring Temperature Separating Agent

75oC plaster mold water 20 min. soak
85oC silicon rubber mold none
85oC metal mold none
75oC paper petroleum
85oC glass none
75oC PVC with petroleum gel (blue and orange)
75oC wood petroleum gel
Gel wax ordinary dye only

Materials for Mold Making

1. Plaster of Paris 4. Knife
2. Modeling clay 5. Card board
3. Model 6. Rubber band

Plaster Mixture
For every cup of water add 1.5 cup of plaster of Paris

Water Plaster of Paris

1 1.5 cups
2 3 cups
3 4.5 cups
4 6 cups
5 7.5 cups
6 9 cups
7 10.5 cups
8 12 cups
9 13.5 cups
10 15 cups
 30

SYNTHETIC SCENT BLENDING

1. After Glow candle
Equal parts: Orange and Pineapple

2. Baby Powder candle

Equal parts: Rose and Vanilla

3. Candy Apple candle

Equal parts: cherry and Apple

4. Candy Cane candle

Equal parts: Strawberry and Peppermint

5. Cucumber Citrus candle

Equal parts: Cucumber and Lemon

6. Love candle
6 parts Rose
2 parts Jasmine
1 part Patchouli
7. Midnight Rose candle
Equal parts: Rose and Jasmine

8. Summer Breeze candle

Equal parts: Jasmine and Orange

ESSENTIAL OIL BLENDING

1. Migraine: 3 drops lavender and 1 drop eucalyptus.
2. Memory: 1 drop peppermint, 1 drop rosemary, drop lavender and 3 drops basil.
3. Study aid: 8 drops grapefruit and 4 drops jumper.
4. Impotence: 1 drop patchouli and 1 drop sandal wood.
5. Mental Fatigue: 8 drops ylang-ylang, 4 drops basil, 8 drops rosemary.
6. Romance candle: 7 drops ylang-ylang, 7 drops palmarosa, 6 drops bergamot.
7. Honeymoon: 10 drops ylang-ylang, 10 drops patchouli.
8. Children candle: 4 drops sweet orange, 2 drops bergamot.
9. Citronella: insect repellant.
 31

EXPERIMENT NO. 12

FRUIT WINE MAKING

Wine making is gardening of a sort. Selected yeasts are the seed. They need nutrients in
the form of sugar and all the elements associated with life. As in gardening, the selection of good
seed ensures a good wine. Wild yeasts are found on almost all fruit, but these generally produce
a wine which is inferior in flavor and of lower alcohol content than wines produced by select
strains of yeast. Good wine yeasts costing no more than a package of flower seed will provide a
variety of controlled flavors and 16-20% alcohol. Baker's yeast will give a "beery" taste and low
alcohol content, but could be used in a first attempt at raisin jack or apple cider.

There are microorganisms that feed on alcohol and cause a poor flavor. Vinegar bacilli will
change sugar to vinegar. Molds give a stale flavor. To prevent these unwelcome intruders,
cleanliness is the only answer. An effective agent is sal soda (sodium carbonate). This is
inexpensive and does not contribute a taste of its own. Baking soda is fairly effective if given time
to work. Either of these agents will remove odors and flavors from the containers. If soap or
detergents are used, the containers must be carefully rinsed. Even the slightest trace will be
apparent in the taste of a light wine.

A second means of ensuring that the wine yeast dominates the brew is to start a culture
into vigorous growth a few days ahead of the fermentation of the must (the fruit pulp and syrup).
By this means the selected yeast will have such a head start that it will consume the sugar and
render the wine antiseptic before any unwanted organism can gain a foothold.
 32

EXPERIMENT NO. 12

FRUIT WINE MAKING

OBJECTIVES:
1. To produce quality wine from fresh fruits.
2. To be able to perform fermentation and to be familiar with wine industry process.

A. PINEAPPLE WINE MAKING

APPARATUSES:
1. 1\4 glass tubing
2. Cotton plug
3. 1 strainer
4. 1 spoon
5. 2 bottles sterilized
6. 2 corks for the bottles

RAW MATERIALS:
1. 1 part ripe pineapple
2. 1 part water
3. 1\4 part sugar
4. 1 table spoon Red star yeast

PROCEDURES:
1. Peel the pineapple and chop.
2. Measure and add water (1 part water to 1 part pineapple).
3. Boil until the fruits are soft, cool and strain. Add sugar to the extract (1 part to every 4
parts extract). Stir and boil.
4. Cool and place in a glass container (with cotton plug).
5. Inoculate with yeast (1 tablespoon yeast to every 40 liters of the juice). Ferment for a
month. Decant into wine barrels and age for two years. Clarify with the use of egg white
(8 egg whites for every 30 liters of wine) by heating the aged wine in a steam or a double
boiler to a temperature of 55 degree Celsius to 60 degree Celsius and adding the well
beaten egg white. Stir to maintain the temperatures, for 15-20 minutes and cool.
6. Filter the wine and bottle by siphoning in to clear and sterilized bottles.
 33

EXPERIMENT NO. 12

FRUIT WINE MAKING

B. MANGO WINE MAKING

APPARATUSES:
1. 1\4 glass tubing
2. Cotton plug
3. 1 strainer
4. 1 spoon
5. 2 bottles sterilized
6. 2 corks for the bottles

RAW MATERIALS:
1. 1.2kilos of fresh ripe mangoes
2. Sugar
3. 1 teaspoon yeast
4. Water

PROCEDURES:

Juice Preparation
Wash fully ripe fruits, cut and scoop out the flesh. Weigh and blend in waring blender.
Add 3 liters of water for every kg of juice. Add sugar to adjust to 20 degree brix (grams/millilitre
of water) for dry wine and 25 degree brix for sweet wine. Cover the jar and stand for 16-18 hours
at room temperature.

Starter Preparation
Gather 10% of the total volume of juice and pasteurize for 30 minutes. Cool to 40 to 45
degree centigrade or until it can be touch comfortably by hand. Inoculate with pure culture of
yeast. Ferment for 18-24 hours and inoculate into prepared juice.

Fermentation
Cover the container with cotton plug and ferment for two days. Replace the cover with
fermentation lock and continue fermentation for 3 to 4 weeks.

Aging and Clarification

Freshly harvested wine is ready for consumption but storing for at least one year improves
its clarity and flavor. After aging, siphon the clear wine, taking care to avoid the settled solids at
the bottom of container. Pack into tightly sealed wine bottle.
 34

EXPERIMENT NO. 13

ESSENTIAL OILS FROM FLOWERS

An essential oil is a concentrated hydrophobic liquid containing volatile aroma

compounds from plants. Essential oils are also known as volatile oils, ethereal oils or aetherolea,
or simply as the "oil of" the plant from which they were extracted, such as oil of clove. An oil is
"essential" in the sense that it carries a distinctive scent, or essence, of the plant. Essential oils
do not form a distinctive category for any medical, pharmacological, or culinary purpose.
Essential oils are generally extracted by distillation. Other processes include expression,
or solvent extraction. They are used in perfumes, cosmetics, soaps and other products,
for flavoring food and drink, and for adding scents to incense and household cleaning products.
Various essential oils have been used medicinally at different periods in history. Medical
application proposed by those who sell medicinal oils range from skin treatments to remedies
for cancer, and often are based on nothing better than historical accounts of use of essential oils
for these purposes. Claims for the efficacy of medical treatments and treatment of cancers in
particular, are now subject to regulation in most countries.

EXPERIMENT NO. 13
 35

ESSENTIAL OILS FROM FLOWERS

OBJECTIVES:
1. To be able to extract essential oil(s) from flowers.

RAW MATERIALS:
1. Wide-necked jar with tight fitting lid
2. Base oil (olive oil, sesame oil, canola oil, vegetable oil, or safflower oil)
3. Dark glass bottle / jar with tight fitting lid
4. Fresh flowers (Many)
5. Cheesecloth
6. Rolling pin / small wooden mallet
7. Plastic storage bag
8. Paper Towel

PROCEDURES:
1. Rinse the flowers with clear water and pat it dry with a paper towel. Place one cup of cup
of flowers in a plastic storage bag and bruise them with a rolling pin or small wooden
mallet. Bruise the petals just enough to cause them to release oils.
2. Prepare a jar with at least 1 cup of good base oil. The oil could be olive oil, which many
prefers to use but vegetable oil can also be used. Other kinds of oil stated in the material
section can also be used.
3. Add the bruised flowers to the oil and seal the container. Allow them to steep in a warm
area for 24-48 hours. Use caution and do not expose them to direct afternoon sunlight,
as this will quickly heat the oil and cook the matter. Open the container and strain the
flowers with a piece of cheesecloth. Return the oil to the jar and discard the flowers.
4. Repeat procedures 1-3 at least three times or until the oil reaches the desired degree of
fragrance. Store essential oils in dark bottles to block out light or store them in a dark
area.

EXPERIMENT NO. 14
 36

ESSENTIAL OILS FROM HERBS

An essential oil is a concentrated hydrophobic liquid containing volatile aroma

compounds from plants. Essential oils are also known as volatile oils, ethereal oils or aetherolea,
or simply as the "oil of" the plant from which they were extracted, such as oil of clove. An oil is
"essential" in the sense that it carries a distinctive scent, or essence, of the plant. Essential oils
do not form a distinctive category for any medical, pharmacological, or culinary purpose.
Essential oils are generally extracted by distillation. Other processes include expression,
or solvent extraction. They are used in perfumes, cosmetics, soaps and other products,
for flavoring food and drink, and for adding scents to incense and household cleaning products.
Various essential oils have been used medicinally at different periods in history. Medical
application proposed by those who sell medicinal oils range from skin treatments to remedies
for cancer, and often are based on nothing better than historical accounts of use of essential oils
for these purposes. Claims for the efficacy of medical treatments and treatment of cancers in
particular, are now subject to regulation in most countries.

EXPERIMENT NO. 14
 37

ESSENTIAL OILS FROM HERBS

OBJECTIVES:
1. To be able to extract essential oil(s) from Herbs.

RAW MATERIALS:
1. Wide-necked jar with tight fitting lid
2. Base oil (olive oil, sesame oil, canola oil, vegetable oil, or safflower oil)
3. Dark glass bottle / jar with tight fitting lid
4. Fresh flowers (Many)
5. Cheesecloth
6. Rolling pin / small wooden mallet
7. Plastic storage bag
8. Paper Towel

PROCEDURES:
1. Rinse the herbs with clear water and pat it dry with a paper towel. Place one cup of cup
of herbs in a plastic storage bag and bruise them with a rolling pin or small wooden mallet.
Bruise the leaves just enough to cause them to release oils.
2. Prepare a jar with at least 1 cup of good base oil. The oil could be olive oil, which many
prefers to use but vegetable oil can also be used. Other kinds of oil stated in the material
section can also be used.
3. Add the bruised herbs to the oil and seal the container. Allow them to steep in a warm
area for 24-48 hours. Use caution and do not expose them to direct afternoon sunlight,
as this will quickly heat the oil and cook the vegetable matter. Open the container and
strain the herbs with a piece of cheesecloth. Return the oil to the jar and discard the
vegetable matters.
4. Repeat procedures 1-3 at least three times or until the oil reaches the desired degree of
fragrance. Store essential oils in dark bottles to block out light or store them in a dark
area.